TW533225B - Novel elastomer composites, method and apparatus - Google Patents

Abstract

Elastomer composites are produced by novel continuous flow methods and apparatus in which fluid streams of particulate filler and elastomer latex are fed to the mixing zone of a coagulum reactor to form a mixture in semi-confined flow continuously from the mixing zone through a coagulum zone to a discharge end of the reactor. The particulate filler fluid is fed under high pressure to the mixing zone, such as to form a jet stream to entrain elastomer latex fluid sufficiently energetically to substantially completely coagulate the elastomer with the particulate filler prior to the discharge end. Highly efficient and effective elastomer coagulation is achieved without the need for a coagulation step involving exposure to acid or salt solution or the like. Novel elastomer composites are produced. Such novel elastomer composites may be cured or uncured, and combine material properties, such as choice of filler, elastomer, level of filler loading, and macro-dispersion, not previously achieved.

Description

533225 Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs A7 ___— B7____ V. Description of Invention (1) Field of Invention The present invention relates to a novel manufacturing method and device for manufacturing elastic composites, and a novel manufacturing method using this manufacturing method and device Elastic compound. More specifically, the present invention relates to a continuous flow manufacturing method and apparatus to produce a granular filler elastomer master batch finely dispersed in the elastomer, for example, a carbon black granular filler finely dispersed in natural rubber, such as non-aging A master batch composition, a cured base composition, and rubber materials and products formed from the master batch composition. Background Many products of commercial importance are formed from elastic composites in which granular fillers are dispersed in any of a variety of synthetic elastomers, natural rubbers, or elastomer blends. For example, 'Inhibition Black' is widely used as a strengthening agent for natural rubber and other elastomers. Master batches, i.e., premixes of fillers, elastomers, and various optional additives such as extender oils are usually manufactured. Carbon black master batches are prepared with different grades of commercially available carbon black, and their surface area per unit weight and f, structure, are different. The product of commercial importance of Xu Xi is formed from an elastic composition of carbon black granular filler finely dispersed in natural rubber. This product includes, for example, vehicle tires, in which different elastic compositions can be used for the tread portion, the sidewall, the wire layer, and the skeleton. Other products include, for example, engine bushings, conveyor belts, wipers, and the like. Although a wide range of performance characteristics can be obtained using currently available materials and manufacturing technologies, the industry still has a long-standing need to develop elastic compositions with improved properties and reduce the cost and complexity of current manufacturing technologies. In particular, for example, the degree of macrodispersion is known, that is, the uniformity of dispersion of carbon black or other fillers in the elastomer, which greatly affects the performance characteristics. By thoroughly mixing carbon black or other fillers with natural rubber or its f Is · (Please read the precautions on the back of this page vim first)

-4- 533225 A7 B7 printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs V. Description of the invention (2) Other flexible preparations (such as in Banbury mixer, etc.), and any increase in the dispersion of the prepared elastic composition needs to be more than Longer or more thorough mixing results in the disadvantage of increased energy costs, manufacturing time, and similar concerns. For carbon black fillers with specific surface area and structural characteristics, it is not possible or non-commercially feasible to use a known mixing device and technique to disperse beyond a certain degree. In addition, this extended or more thorough mixing degrades natural rubber by reducing its molecular weight, making the finished elastomeric compound unsuitable for specific applications. It is known to use carbon blacks with higher or lower structure and surface area to manipulate the performance characteristics of elastic compositions. The higher surface area of carbon black and the lower and lower structure are known to improve resistance to cleavage growth and chip resistance, generally and abrasion resistance, and other performance qualities. Commercially available blending technologies have not been able to achieve the excellent dispersion uniformity of carbon black across all elastomers; however, there is no unacceptable degradation of natural rubber. In fact, for typical carbon black filling levels in natural rubber, such as 45 phr to 75 phr, and 0 phr to 10 phr, oil filling, low structural carbon blacks, such as DBPA carbon blacks below 110 cc / 100 grams, especially have With a surface area (CTAB) of about 45 m² / g to 65 m² / g (CTAB), compounds with less than about 1% undispersed carbon black (as measured by the macrodispersion described below) have not been obtained, regardless of the period and degree. In addition, as shown above, in the currently widely used high-energy-concentration, concentrated-drying mixing process, the natural rubber elastomer polymer chains produced by the kneading of the elastomer required to disperse the carbon black have an unacceptable degree of fragmentation. Formation: The reduction in molecular weight of natural rubber is not suitable for many industrial applications. For example, for use on a wheel surface, a reduced molecular weight has caused an undesired increase in the so-called tire rolling resistance. In addition, although theoretical analysis has shown that the use of higher surface area and lower structure -5- This paper size applies to China National Standard (CNS) A4 size (210X 297 mm) (Please read the precautions on the back before this page) Order

. ^ 1. 533225 A7 printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economics. Description of the specific performance characteristics of the elastic composition of carbon black (3) | Method to obtain the molecular weight of the cut gel and obtain a satisfactory carbon black macrodispersion procedure: elastic = product, it is not possible. For example, it is generally found that the elasticity of carbon black 髀 2 properties decreases as the carbon black particle size decreases. Increasing. However, the use of rather fine zeros is known to encounter irregularities, of which nature has not been expected. I: It is understood that at least in part due to the conventional elastomeric compounding method, local dispersion in natural rubber is not possible. And the undue elastic polymer is broken = this, as a result, in this case of carbon black, the full advantages of the natural affinity of carbon black and natural rubber cannot be obtained. Because carbon black is sometimes considered to be one of the natural rubber compounds Good dispersion is one of the most important goals to obtain good quality and consistent product performance. Big = Efforts have been devoted to the development of steps to evaluate the dispersion quality in rubber. Development method package For example, the Cabot distribution table and various image analysis steps. Dispersion quality can be defined as the resulting mixed state. The ideal carbon black dispersion is where carbon = dimer flakes are broken into uniform separation from each other (completed by distributed mixing). In the state of coagulation (completely mixed by knife), the surface of all carbon black agglomerates is completely wetted by the rubber matrix (commonly called bonding). The common problems often associated with poor dispersion in the rubber industry can be classified into four main foot categories: product performance, surface defects, surface appearance, and dispersion efficiency. The functional properties and durability of carbon black rubber formulations, such as tensile strength, fatigue, life and water resistance, are substantially affected by the quality of the macrodispersion. Undispersed carbon black also produces surface defects on the product, including visible defects. Exclude the existence of surface defects due to functional reasons in thin plastic parts and original appearance and function. 6- This paper size is applicable to China Ceramics Standards (CNs).

533225 A7 V. Description of the invention (4) Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs Because it is of great importance in extruding the shape. 3, commercial 3V image knife, analyzer, as known from 〇〇〇〇〇〇11〇Electronics Co., Ltd. RIBAS '] "5V image analyzer' can be used to measure the macroscopic dispersion of carbon black or other fillers. -In general, in the qualitative macrodispersion test in the rubber industry, the critical break size is 10 microns. Defects larger than about 10 microns-generally include undispersed carbon black or other fillers, and are allowed to be exposed to #,, ^ ^ sighs or other pollutants, which affect visual and functional performance. Therefore, when measuring Wu Gyaye and Zhi M, Liju dispersion involves using an image analyzer to measure the total area of the defects that are inspected on the surface and are larger than 10 microns per unit area. The macrodispersion D (%) is calculated as follows:% undispersed area (%) = 丄 Ν Π · where Am = the total sample surface area of the test has a large + number of defects with a diameter of a circle with the same surface area as the defect t (equivalent circle) Shape diameter) m = number of images Macrodispersion of carbon black or other fillers in uncured natural rubber or other appropriate elastomers can be evaluated using image analysis of cut samples. Generally speaking, five to ten arbitrarily selected optical images are taken from the slice for analysis. Knife marks and the like are preferably removed using digital filtering techniques. The cross-sectional image analysis thus provides information on the carbon black dispersion quality of natural rubber compounds. In particular, the percentage D (0/0) of the undispersed area represents the carbon black macrodispersion quality. When the macrodispersion quality is degraded, the percentage of the 'undispersed area increases. Therefore, the dispersion quality can be improved by reducing the percentage of undispersed area. As shown above, the mixed operation pair

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533225 A7

Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs and the huge dispersion have a direct impact = sex = for example, natural rubber master batches, borrowed from a longer mix: and borrowed = bottom = mouth. However, unfortunately, it takes longer and more thorough mixing ^ „Destroy ..., the elastic body scattered in the knife. It is particularly problematic in natural: gum 4 shape, it is very easy to mechanical / thermal degradation. People have used: mixing Technology and devices, such as Banbury mixers, are longer and more thorough to reduce the molecular weight of the natural rubber master batch composition. Therefore, the improved macrodispersion of carbon black in natural rubber is known to use a corresponding, generally unsuitable rubber molecular weight It is reduced. In addition to the dry mixing technique, it is known that the latex and the material are continuously fed to the coagulation tank. This wet technology is usually used with synthetic elastomers such as SBR. The coagulation tank contains agglomerates such as salt or water or Acid solution, generally has a p 约 of about 2.5 to 4. The latex carbon black slurry is mixed and coagulated into small particles (usually several millimeters in diameter) in the coagulation tank, which is called wet crumbs. The crumbs are separated from the acid effluent Generally, it is filtered by shaking and shaking, etc. The chips are then poured into a second stirring tank, where they are washed to obtain a neutral or near-neutral pH. Then the chips are subjected to additional vibration filtration and drying steps. Body Poly suggests a change in this manufacturing method. In U.S. Patent No. 4,0029,633 to Hagopian et al., Which is transferred to Cabot Corporation as described in the present invention, describes a continuous process for the preparation of elastomeric master batches. Natural or synthetic elastomer latex mixing. This mixture undergoes a so-called thickening operation, optionally using any of a variety of known thickeners. After the carbon black / latex mixture is thickened, it undergoes a coagulation step. In particular, the thickening The carbon black / latex mixture is introduced into the core of the agglomerated solution flow as a single coherent flow. The solid flow of the thick carbon black / latex mixture is said to have been read first.

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-8- This paper size is in accordance with Chinese National Standard (CNS) A4 (210X 297 mm) 533225 A7 B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economy Change and vaporize, and then send to the appropriate reaction zone for complete condensation. After this agglomeration step, the rest of the method is essentially ‘conventional,’ which involves the separation of crumbs from the waste product “milk” and the cleaning and drying of crumbs. A slightly similar approach is described in U.S. Patent No. 3,048,559 to Heller et al. The aqueous slurry of carbon black is continuously blended with the flow of natural or synthetic elastomers or latex. The two streams are mixed under conditions described as involving severe water pressure disturbances and shocks. As in the case of the aforementioned Hagopian et al. Patent, the combined flow of carbon black slurry and elastomer latex is then agglomerated by the addition of an acid or salt agglomerate solution. There has been a long-standing need in various industries for improved macrodisperse elastomer compounds dispersed in particulate fillers of suitable elastomers, for example, carbon black in particular dispersed in natural rubber. As mentioned above, the improved macrodispersion can provide corresponding improved aesthetic and functional characteristics. It is particularly desirable to be a novel elastic compound of carbon black in natural rubber, in which improved macrodispersion and higher molecular weight of natural rubber are obtained. The purpose of this invention is to meet some or all of these long-term needs. SUMMARY OF THE INVENTION According to a first state, a method for preparing an elastomeric master batch involves simultaneously feeding a granular filler fluid and an elastomeric latex to a mixing zone of a coagulation reactor. The agglomeration zone extends from the mixing zone, and it is preferable to gradually increase the cross-sectional area in the downstream direction from the inlet end to the discharge end. Elastomer latexes can be natural or synthetic, and the particulate fillers include carbon black or other particulate fillers that effectively agglomerate the latex. The granular filler fluid is preferably fed continuously, at high speed, as an injection fluid into the mixing zone, while the latex fluid is fed at a low speed. The speed, flow rate and particle concentration of the granular filler fluid are sufficient to cause the mixture to have a high shear force for the latex fluid and the mixture -9-(Please read the precautions on the back before this page)

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This paper size applies to China: Standard (CNS) A4 (210X297 mm) 533225 Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs A7 B7 V. Invention Description (7) Flow of the compound in the upper part of the condensation area Perturbed to substantially fully agglomerate the elastomeric latex with the particulate filler before the discharge end. According to the preferred embodiment, substantially complete aggregation can be obtained without the need to use an acid or salt coagulant. According to another state, the continuous flow manufacturing method for manufacturing the elastomeric master batch includes continuous and simultaneous feeding of latex fluid and granular filler fluid to the mixing zone of the agglomeration reactor, and establishing the elastomer latex and granular filler in the agglomeration zone. Continuous, semi-restricted flow of the mixture. Elastomer master batch scraps in the form of "worms" or balls are discharged from the discharge end of the agglomeration reactor as a substantially fixed flow, while continuing to feed the latex and granular filler fluid to the mixing and mixing area of the agglomeration reactor. Obviously, the insert-type flow and atmospheric or near-atmospheric pressure conditions at the discharge end of the coalescing reactor are very advantageous for the control and collection of the elastomeric master batch product, such as for immediate or later further processing steps. According to the state of the device, a device for feeding the elastomer latex fluid to the mixing zone of the above-mentioned coagulation reactor is provided, preferably under low pressure, substantially laminar flow conditions, and provided with a jet sufficient to produce sufficient speed or thermodynamic energy to A device for conveying the elastomeric latex as described above, and simultaneously feeding the granular filler fluid under pressure to obtain agglomeration before the mixture flowing downstream reaches the discharge end of the agglomeration reactor from the mixing zone. According to a specific preferred embodiment detailed below, the device for feeding the elastomer latex fluid and the device for feeding the granular filler fluid may each include a mixing head that integrates the feeding of a substantially tubular member that defines a coacervation zone. aisle. The mixing zone can provide the junction of this feed channel in the mixing head. According to a specific preferred embodiment, the mixing zone is only a coaxial extension of the condensation zone. In a specific preferred embodiment, the gradual increase in the cross-sectional area of the agglomeration reactor is continuous, and in its -10- paper size, the Chinese National Standard (CNS) A4 · (210X297 mm) is applied (please read it first) (Notes on the back page)

• ^ 1. 533225 A7 B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (8) His preferred embodiment is a step by step. In addition, the coalescing reactor may have optional features like a diffuser at its discharge end, as described further below. Additional conditions and preferred features of the continuous flow manufacturing apparatus for the elastomeric master batch disclosed herein are discussed in the detailed description below. According to another state, the elastic compound is provided as a product of the method or device described above. According to a preferred embodiment, the choice of granular dispersion with previously unobtained granular fillers, the molecular weight of the elastomer, the degree of particle filling, and the choice of granular fillers (including, for example, unexpectedly high surface area and low structure) is provided. Carbon black filler), and / or novel elastic complexes of other characteristics. In this regard, the disclosed manufacturing method and device can obtain excellent macrodispersion, even for specific fillers, such as carbon black with a structure-to-surface area ratio DBP ·· CTAB of less than 1.2 or even 1, in elastomers such as natural rubber Medium, with little or no degradation of the molecular weight of the elastomer. According to other aspects of the present invention, intermediate products and final products are provided, which are formed from elastic composites made by the processes and devices disclosed herein. According to another aspect, a novel elastic composite is provided, which comprises granular filler dispersed in natural rubber, and the degree of macro-dispersion of the filler in the elastic composite is less than about 0.2% undispersed area, preferably less than about 0.1% undispersed area. . Consistent with the discussion 1 above, the macrodispersion here means the macrodispersion D (%) of carbon black measured for defects larger than 10 micrometers if the area percentage is not dispersed. In the natural rubber master batch and other elastic compounds disclosed herein, the molecular weight of the natural rubber, that is, the MWSQl (average weight) of the sol portion, is preferably at least about 300,000, more preferably at least about 400,000, and is particularly preferred The specific embodiment is between 400,000 and 900,000. The elastic compound contains incremental oil as appropriate, such as about 0 to 20 -11-This paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) Please read the notes and notes before reading

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533225 A7 B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. 5. Description of the invention (9) phr, more preferably about 0 to 10 phr of incremental oil, and / or other ingredients, if known, compound natural as appropriate. Rubber and carbon black fillers. As discussed further below regarding specific preferred and illustrated specific embodiments, the novel elastic composites disclosed herein can provide much needed physical properties and performance characteristics. Therefore, the present invention proposes important technical advances. According to another state, a novel elastic compound is provided, which has a novel combination of properties that have not been obtained so far, including the specific macrodispersion degree of carbon black filler, the molecular weight of natural rubber, the degree of carbon black filling, and the characteristics of carbon black (including surface area and structure, For example, unexpectedly high surface area and low structure carbon black fillers), and / or other features. According to various states of the present invention, a master batch composition and an intermediate product, and a final product formed therefrom are provided. These and other states and advantages of the specific embodiments of the present invention will be further understood with reference to the following detailed description of specific preferred embodiments. Brief description of the drawings The discussion of the following specific preferred embodiments is described with reference to the accompanying drawings, in which FIG. 1 is a schematic flowchart of an apparatus and method for preparing an elastomer master batch according to the specific preferred embodiments; FIG. 2 is Fig. 3 is a schematic front view of a part of the preferred embodiment consistent with the outline flow chart of Fig. 1; Fig. 3 is a schematic diagram of an alternative part of the preferred embodiment consistent with the outline flow diagram of Fig. 1 View; FIG. 4 is a partial cutaway front view of the mixing head / condensation reactor assembly of the specific embodiment of FIG. 3; FIG. 5 is a partial cutaway front view, which corresponds to the drawing of FIG. This paper size applies to China National Standard (CNS) A4 (210X297 mm)

533225 A7 Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs

、 Explanation of the invention (U Hereby, the 7FI manufacturing method and device can be used in the continuous flow method involving a mixture of elastomer latex and granular fluid, which is sufficient to obtain the degree of disturbance of aggregation and flow control even without the use of traditional coagulants. Conditions, manufacturing elastomer master batches. In fact, it is immediately understood that elastomers and fillers do not need to be thoroughly dried and kneaded, or the liquid latex / granular composition i is exposed to the flow or tank of the coagulant, and the elastomer is known The master batch crumb, that is, the coagulation of the milk, has two great commercial benefits. Therefore, in a fixed commercial implementation, the cost and recovery of the acid coagulation solution can be avoided. Prior technology involving premixed latex and particles As in the aforementioned Heller et al. Patent and Hagopian. Et al. Patent, it is not even known about the possibility of agglomeration without exposing the latex / particle mixture to a general coagulation solution, its associated costs, and the disadvantages of waste disposal. Latex fluids and granules Rate of granular filler fluid to the mixing zone of the agglomeration reactor: accurately metered to obtain a high production rate and have extremely high levels of product debris at the discharge end of the agglomeration reactor Free latex and very few undispersed fillers. Without wishing to be bound by theory, it is now understood that a quasi-single-phase system is established in the mixing zone, except that agglomerated solids are formed here and / or downstream of the agglomeration zone. Particulate filler fluid to agglomerate reaction The relatively high feed speed in the mixing zone of the reactor and the speed difference relative to the feed of the latex fluid, it is believed that a significant disturbance is obtained by the impact of the spray of the granular filler fluid, that is, the latex shear force with sufficient energy to completely mix the particles It is important to disperse into latex fluid and agglomerate. High mixing energy = Second product master batch crumbs with excellent dispersion and controlled product transport. Produce agglomerate and then form the required extrudate. Manufacture the novel elasticity disclosed here Specific preferred embodiments of the method for manufacturing the composite and the device are discussed below. Although various preferred embodiments of the present invention are ^ Example -14-This paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X297: v%) 533225 A7 B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. 5. Description of the Invention (12) Many different fillers and elastomers can be used. For convenience, this Certain parts of the following detailed description of the method of manufacturing and the state of the invention describe in some cases its use primarily in the manufacture of mother batches containing natural rubber and carbon black. In order to impart the benefit of this disclosure, use is made in accordance with the principles of operation discussed below. The disclosed method and apparatus for making a master batch containing many alternative or additional elastomers is within the ability of those skilled in the art. In short, this method of preparing a master batch of elastomers involves simultaneously The slurry of other fillers and natural rubber latex fluid or other appropriate elastomeric fluid are fed to the mixing zone of the coalescing reactor. The coalescing zone extends from the mixing zone, preferably in a direction that increases gradually from the inlet end to the discharge end downstream. Sectional area. The slurry is preferably fed to the mixing zone in a continuous, high-speed jet, such as a jet fluid, while the natural rubber latex fluid is fed at a relatively low speed. The high velocity, flow rate, and particle concentration of the filler slurry are sufficient to cause high shear forces of the mixture and the latex fluid, flow disturbance of the mixture in at least the upstream portion of the agglomeration zone, and substantially completely agglomerate the elastomer latex just before the discharge end. According to the preferred embodiment, substantially complete aggregation can be obtained without the need to use an acid or salt coagulant. A preferred continuous flow method for making an elastic composite includes continuous and simultaneous feeding of latex fluid and filler slurry to the mixing zone of the agglomeration reactor, and establishing a continuous, semi-restricted flow of the mixture of latex and filler slurry in the agglomeration zone . Elastic compound crumbs in the form of "worms" or balls are discharged from the discharge end of the agglomeration reactor as a substantially fixed flow, while the latex and carbon black slurry are continuously fed to the mixing zone of the agglomeration reactor. Obviously, the insert-type flow and atmospheric or near-atmospheric pressure conditions at the discharge end of the coalescing reactor are very advantageous in favor of the control and collection of the elastic composite product, such as for immediate or later further processing steps. Day -15- (Please read the note on the back first)

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This paper size applies to Chinese National Standard (CNS) A4 specification (210X297 mm) 533225 A7 ________B7 V. Description of the invention (13)

The Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs of the People's Republic of China. The feed rate of the rubber latex fluid and carbon black paddle to the mixing zone of the condensation reactor can be accurately measured to obtain high production rates at the discharge end of the condensation reactor. There is very little free latex and very little undispersed filler in the crumb. Without wishing to be bound by theory, it should be understood that a quasi-phase system is established in the mixing zone, except that agglomerated solids are formed here and / or downstream of the condensation zone. The relatively high feed rate of the carbon black slurry to the mixing zone of the agglomeration reactor and the difference in feed rate relative to the feed of the natural rubber latex fluid are believed to be significantly disturbed by the impact of the particulate filler fluid jet, that is, the energy is sufficient Latex shearing force is important to disperse particles into the latex mud and agglomerate. The high mixing energy produces a product master batch with excellent dispersion and controlled product delivery. The coagulation is then made to form the desired extrudate. The above-mentioned preferred devices and techniques for manufacturing the elastic composites disclosed herein are discussed with reference to the accompanying drawings, in which the continuous flow manufacturing method for manufacturing the elastomeric master batch is used in a coalescing reactor to mix a filler slurry such as a carbon black water-based material. The continuous and semi-restricted flow of the elastomer latex of natural rubber latex (field latex or concentrate) forms an elongation and aggregation zone, which extends from the inlet end to the discharge end, preferably with a gradually increasing cross-sectional area. The term "semi-restricted" flow refers to very advantageous characteristics. The use of this term here is intended to indicate the flow path followed by the latex fluid and filler slurry mixed in the coagulation reactor, which is closed or substantially closed upstream of the mixing zone, and at the opposite end, the downstream end of the coagulation reactor is open. That is, at the discharge end of the coalescing reactor. The turbulent conditions in the upstream part of the agglomeration zone continue to maintain at least a quasi-steady state mode, while at the same time, the open discharge end of the agglomeration reactor is essentially a flow-type condition. The discharge end is "open" at least to allow the discharge of condensate, usually at or near the atmosphere. -16- This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) (Please read the precautions on the back first

1 <?-533225 A7 _________ B7 V. Description of the invention (17 ^ — printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs, and generally falls by simple gravity (in the package or filtered flow path as appropriate) appropriately collected Device, such as the feed and feed funnel 脱水 of the dehydration extruder. Therefore, the semi-restricted flow is generated in the condensing reactor at least-part of the axial or longitudinal extension of the perturbation gradient. Do not want to be bound by theory, should be decondensed It is important to allow for highly turbulent mixing and coagulation in the upstream part of the coagulation reactor, and the substantial plug-in discharge flow of the solid product at the discharge end. Injection of carbon black or other filler slurry, such as continuous injection into the mixer, is important. Occurs in a record-keeping manner, and at the same time is easy to collect in the substantially plug-in flow conditions and at the discharge end of the condensing reactor, the elastic slag batches are usually discharged under ambient pressure. Similarly, the slurry passes through the slurry nozzle to the mixing zone The neutral and generally axial speeds at the upstream end of the condensation zone are substantially higher than at the discharge end. The axial speed of the slurry is generally hundreds of feet per second when entering the mixing zone. It is preferably from the small-hole, axially-oriented feed tube according to the preferred embodiment of the following discussion. In typical applications, the axial velocity of the flow at the inlet end of the condensation reactor with an expanded cross-sectional area can be, For example, 5 to 20 feet per second, and more often 7 to 15 feet per second. In contrast, in typical applications, the axial velocity of the mother batch product discharged at the discharge end is about 1 to 2 10 feet, and more often 2 to 5 feet per second. Therefore, the above-mentioned semi-restricted disturbed flow obtains a very important advantage. Natural rubber or other elastomer latex is mixed with carbon black or other fillers, even without Handle in the flow or tank of acid, salt or other coagulant solution, use control, preferably quasi-plastic product from coagulation reactor is transported for coagulation at later processing. In this regard, it should be understood that reference is made to the discharge The open end of the condensation reactor does not mean that the 7F discharge end needs to be exposed for viewing or easy to touch by hand. And -17- This paper size is applicable to the Chinese National Standard (CNS) Α4 specification (210x797 Public E 533225 Α7 Β7 V. Description of the invention (15) It is permanently or releasably connected to the collection device or later processing devices, such as launchers (discussed further below), dryers, etc. The discharge end of the coalescing reactor is open for coalescing reactions. Turbulent flow in the coalescing region of the vessel, which is under high pressure and sealed to prevent any significant backward (i.e., upstream) passage in the mixing region, which can establish the above-mentioned pressure and / or velocity gradient as it exits towards and towards the discharge end Important feeling. Central Standards Bureau of the Ministry of Economic Affairs! Printed by the Industrial and Consumer Cooperatives. At this point, it should also be understood that the disturbance of flow is reduced along the condensation reactor toward the discharge end. A large number of solid products are inserted into the flow before the discharge end, which is used as capacity. The percentage, the choice of material, etc .. In this reference, the flow of the flow is essentially inserted at or before the discharge end of the condensation reactor. It should be understood that the flow at the discharge end is mainly or completely composed of the parent batch. , That is, the ball of agglomerated elastomer mother batch or, "worm". The crumbs are generally quasi-molded into the inner shape of the condensed area along the place where the condensate = flow becomes substantially inserted into the flow. The "worm" or ball that has been advancing the mass passes through it usually or mainly axially toward the discharge end, and the given cross section of the condensation area near the discharge end has a fairly uniform velocity at any time, making it easy to collect And the feeling of controlling one-step processing is advantageous to have an insert flow. Therefore, the mixed state of the mobile phase disclosed herein can be advantageously performed under steady state or quasi-stable state conditions, resulting in a high degree of product uniformity. The production method disclosed here Preferred embodiments of the device are briefly described in 1. Those skilled in the art should understand that each of the system configuration, component selection, etc., the θ state depends on the specific characteristics of the intended application. Therefore, for example Factors such as the maximum system output capacity and material selection flexibility affect system groups such as size and design. Generally, in order to give the benefits of this disclosure, emphasis may be placed on

533225 A7 B7 V. Description of Invention (16) It is within the ability of the artist. It can be seen that the system described in Figure i includes a device for continuously feeding natural rubber latex or other elastomer latex fluids to the mixing zone of the coagulation reactor at low pressure and low speed. More specifically, the latex pressure tank 10 is shown to suspend the feed supply of latex under pressure. Alternatively, a latex storage tank equipped with a peristaltic pump or series of pumps, or other suitable feeding device suitable for suspending the feeding of the elastomeric latex lacquer body via the feed line 12 to the mixing reactor M t mixing zone, may be used. The latex fluid in the tank 10 can be kept under air or nitrogen pressure, etc., so that the latex fluid is fed at a line pressure of preferably less than 10 psig, more preferably about 2-8 psig, and generally about 5 psig. To the mixed zone. The latex feed pressure and flow lines, connections, etc. of the latex fluid device should be configured so that the shear force in the flowing latex fluid is reasonably as low as possible. For example, it is better that all mobile lines are smooth, if there is only a large radius turn, and smooth or clear lines are connected to the line. The pressure is selected to produce the required flow velocity into the mixing zone; an example of a usable flow velocity is not more than about 12 suction per second. Employees of the Central Standards Bureau, Ministry of Economic Affairs, Consumer Cooperatives, Benzene. Suitable elastomer latex fluids include natural and synthetic elastomer latex and latex blends. Of course, the latex must be suitable for agglomeration by the particulate filler selected, and must be suitable for the intended purpose or application of the final rubber product. To give the benefit of this disclosure, it is within the skill of those skilled in the art to select the appropriate elastomeric latex or appropriate blend of elastomeric latexes for the processes and devices disclosed herein. Exemplary elastomers include, but are not limited to, polymers of rubber, butadiene ethylene, isoprene, isobutylene, 2,3-dimethyl-i, 3-butadiene, acrylonitrile, ethylene, and propylene, etc. (For example, homopolymers, copolymers, and / or trimers). Elastomers can have a measuring range by differential scanning calorimeter (DSC) 19- This paper size is applicable to China National Standard (CNS) A4 (210X297 mm) 533225 Printed by A7 B7 of the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs The invention description (17) is about -120X: to a glass transition temperature (Tg) of about 0 ° C. Examples include, but are not limited to, epi-butylene-butadiene rubber (SBR), natural rubber and its derivatives such as gasified rubber, polybutadiene, polyisoprene, poly (styrene-co-butadiene ) And any of its oil-blended derivatives. Any of the above blends can be used. Latex can be used in aqueous carrier liquids. Alternatively, the liquid carrier may be a hydrocarbon solvent. In any case, the elastomeric latex fluid must be suitable for continuous feeding into the mixing zone at an appropriate speed, pressure, and concentration. Particularly suitable synthetic rubbers include: a copolymer of about 10 to about 70% by weight of styrene and about 90 to about 30% by weight of butadiene, such as 19 parts of styrene and 81 parts of butadiene Copolymer of 30 parts of styrene and 70 parts of butadiene, copolymer of 43 parts of styrene and 57 parts of butadiene, and copolymer of 50 parts of styrene and 50 parts of butadiene; II #, polymers and copolymers of conjugated difluorene such as polyisoprene, polychloroprene, etc., and copolymers of this conjugated diene and vinyl-containing monomer, this monomer can be used with benzene Ethylene, methylphenethylfluorene, chlorostyrene, acrylonitrile, 2-ethylfluorenyl-specific bite, 5-fluorenyl 2-vinylpyridine, 5-ethyl 2-vinylpyridine, 2-fluorenyl 5- Acetyl π specific bite, substitution of propionate by fluorenyl, acetophenone, fluorenyl isopropyl ketone, methyl vinyl ether, methylene carboxylic acid, and its esters and fluorenamines, such as propionate Copolymerized with fluorenyl monoacrylate. It is also suitable for use here as copolymers of acetamidine and other high-carbon alpha olefins, such as propylene, butadiene and pentamidine-1. As further shown below, in addition to the elastomer and the filler, the rubber composition of the present invention may contain a curing agent, a coupling agent, and various processing aids, extenders, and anti-degradants as appropriate. In this regard, it should be understood that the elastomeric compositions disclosed herein include vulcanized compositions (VR) thermoplastic vulcanizates (TP V) 'thermoplastic elastomers (τρε) and thermoplastics _____ · 2〇_ I paper size applies to China National Standard (CNS) Α4 Specification (210 × 297 mm) ^-(Please read the precautions on the back page first)

Order printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 533225 A7 B7 V. Description of the invention (18) Polyolefin (TPO). TPV, TPE, and TPO substances are further classified based on their ability to be extruded and molded several times without loss of performance characteristics. Therefore, in the manufacture of elastic composites, for example, sulfur, sulfur precursors, activators, accelerators, peroxides, and other systems for curing the elastic composites can be used. Where elastomeric latex contains natural rubber latex, it is possible that rubber latex can include field latex or latex concentrate (for example, made by evaporation, centrifugation, or condensation). Of course, natural rubber latex must be suitable for coalescence by carbon black. Latex is typically provided in an aqueous carrier liquid. Alternatively, the liquid carrier may be a hydrocarbon solvent. In many cases, natural rubber latex fluids must be suitable for continuous feeding at the appropriate speed, pressure, and concentration to a controlled mixing zone. The known instability of natural rubber latex is advantageously adjusted because it accepts fairly low pressure and low shear forces in all systems until it encounters the ultra-high speed and thermodynamic energy of the carbon black slurry in the mixing zone and is transported to the aforementioned semi-limit Disturb the flow so far. In certain preferred embodiments, for example, natural rubber is fed to the mixing at a pressure of about 5 psig, at a feed rate of about 3-12 feet per second, and more preferably at a range of about 4-6 feet per second. Area. In order to impart the benefit of this disclosure, the choice of a suitable latex or latex blend is within the abilities of those skilled in the art, and knowledge of the selection criteria is generally recognized in the industry. A particulate filler fluid, such as a carbon black slurry, is fed to the mixing zone via the feed line 16 at the inlet end of the coalescing reactor 14. The slurry may contain any suitable filler in a suitable carrier fluid. The choice of carrier fluid depends mainly on the choice of granular filler and system parameters. Both aqueous and non-aqueous liquids can be used. Regarding the cost, availability and applicability of the carbon black and certain other filler pastes. -21-This paper size applies to China National Standard (CNS) Α4 size (210X 297 mm ) (Please read the notes on the back before ^? ^ This page) Order printed by the Consumers Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 533225 A7 ------ B7 -------------- -V. Description of the invention (19) Synthetic properties' In many embodiments, water is preferred. When carbon black filler is used, the choice of carbon black mainly depends on the intended use of the elastomeric master batch product. Optionally, the carbon black filler may also include any substance that can be slurried and fed into the mixing zone in accordance with the principles disclosed herein. Suitable additional particulate fillers include, for example, conductive fillers, reinforcing fillers, fillers containing short fibers (typically having an L / β aspect ratio of less than 40), flakes, etc. ^ This can be used in accordance with the manufacturing methods disclosed herein Exemplary granular fillers used in the manufacture of elastomeric master batches are carbon black, aerosol-like gravel, sunkenite, coated carbon black, chemically functionalized carbon black, such as those with attached organic groups, and silicon Deal with black, alone or in combination with each other. Suitable chemically functionalized carbon blacks include those disclosed in International Application PCT / US95 / 16194 (W09618688), the disclosure of which is incorporated herein by reference. In silicon-treated carbon black, silicon containing species such as silicon oxides or carbides is distributed in at least a portion of the carbon black aggregate, as part of f of carbon black. It is known that carbon black exists in the form of aggregates, and each aggregate includes a single phase, which is carbon. This phase can exist as crystalline and / or amorphous graphite, and is usually a mixture of the two forms. As discussed elsewhere, carbon black aggregates can be modified by depositing silicon-containing species on at least a portion of the surface of the carbon black aggregates, such as silica. The results can be described as silicon-coated carbon black. The materials described here as silicon-treated carbon black are not coated or modified carbon black aggregates, but actually provide different types of aggregates. The silicon-treated carbon black 'M collective contains two phases. One phase is carbon, which still exists as graphite crystalline and / or amorphous carbon, and the second phase is silica (and possibly its second species). Therefore, the species of the carbon black-cutting species is the intrinsic component of the aggregate I; all of it is distributed in at least a part of the aggregate. Yes ______ -22- This paper size applies to China National Standard (CNS) Α4 specification (210 × 297 mm)

533225 Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 V. Description of the Invention (20) The polyphasic aggregate is quite different from the silicon-treated carbon black described above, which includes 2 silicon-containing species deposited on its surface Pre-formed, single-phase carbon black aggregates. This carbon black can be surface treated to place a silicon functional carbon black based aggregate surface. In this method, existing aggregates are treated to deposit or coat silica (and possibly other silicon-containing species) on at least a portion of the aggregate surface. For example, an aqueous solution of sodium silicate can be used to deposit amorphous silica on the surface of a post-black agglomerate in an aqueous slurry with a thickness of 11 to 11 mm, such as 6 or more. ) Discussed in Announcement 63-63755. More particularly, carbon black can be dispersed in water to obtain an aqueous slurry including, for example, about 5 wt% carbon black and 95 wt% water. The slurry is heated to higher than about 70 × :, such as to 85-95 ° C, and JLpH 値 test solution is adjusted to higher than 6, such as to the range of CD- ^. Separate preparation of a sodium silicate solution containing the required amount of silica deposited on carbon black, and an acid solution that brought the sodium silicate solution to a neutral pH. Sodium silicate and acid solution are added dropwise to the slurry, which is maintained at its starting point with a suitable acid or alkaline solution. The temperature of the solution was also maintained. The recommended addition rate for the sodium silicate solution is a calibrated dropwise addition to add about 3% by weight of silicic acid per hour to the total amount of carbon black. The slurry should be stirred for a few minutes (such as 30) to several hours (that is, 2-3) during the addition and after its completion. In contrast, silicon-treated carbon black can be obtained by making carbon black in the presence of a volatile silicon-containing compound. This carbon black is preferably manufactured in a module or segmented " furnace carbon black reactor, which has a combustion zone followed by a contracted diameter zone, a raw material injection zone with a restricted ' diameter, and a reaction zone. The quench zone is located downstream of the reaction zone. Generally, a quench fluid, usually water, is sprayed onto a stream of newly formed carbon black particles from the reaction zone. When manufacturing silicon-treated carbon black, the above-mentioned volatile silicon-containing compounds introduce carbon at the upstream of the quench zone. -23- This paper size applies to the Chinese National Standard (CNS) M specification (210X297 mm) (please read the back first) (Notes on this page)

Order 533225 A7 B7 V. Description of the invention (21 black reactor. Available compounds are compounds that are volatile at the temperature of the carbon black reactor. Examples include, but are not limited to, such as tetraethoxy orthosilicate (TEDS) and dimethyloxy Silicates based on orthosilicates, silanes such as tetrachlorosilane and trichloromethylsilane, and volatile polysiloxane polymers such as octamethylcyclotetrasiloxane (〇MTS). Volatile compounds The flow rate determines the weight percentage of silicon in the treated carbon black. The weight percentage of silicon in the treated carbon black generally ranges from about to 25%, preferably from about 5% to about 10%, and more preferably about To about 6%. Volatile compounds can be premixed with carbon black to form a raw material and introduced into the reaction zone. Alternatively, volatile compounds can be introduced into the reaction zone from upstream to downstream of the raw material injection point. As shown above, additives can be used, and about In this regard, it is possible to couple silica or carbon black (the coupling agent is expected to be used with silicon-treated carbon black. Carbon black and many other suitable particulate fillers are commercially available and are known to those skilled in the art .. granular filler or granular filler The selection of the mixture depends mainly on the intended use of the elastomeric master batch product. The granular fillers used herein may include any material that is slurried and fed to the mixing zone in accordance with the principles disclosed herein. Suitable granular fillers, For example, conductive fillers, reinforced fillers, including: printed by employees' cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (usually having an L / D aspect ratio of less than 40), tablets, etc. Except for the black and crushed stone types mentioned above Fillers, fillers can be formed from dots, 7 kinds of clay, broken glass, such as aromatic sleepers .. In order to give the benefits of this disclosure, the appropriate granular fillers for this process and device are selected. Within the capacity, and any fillers that are expected to be suitable for elastomeric compositions can be used without the addition of elastic composites. Of course, the various granularity disclosed herein can also be used. ) A4 specification director) 533225 A7 B7 Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs 5. Description of the invention (22) Blends of fillers. The preferred embodiment of the present invention consistent with FIG. 1 is special Preparation of granular filler fluids containing carbon black aqueous slurry. According to known principles, it should be understood that carbon black with a lower surface area per unit weight must be used at a higher concentration in the particle slurry to obtain, for example, a low concentration The same agglomeration effect of carbon black with a high surface area per unit weight. The stirring mixing tank 18 receives water and carbon black, for example, granulated carbon black, as appropriate, to prepare a starting mixture fluid. This mixture fluid passes through the discharge port 20 to The fluid line 22 equipped with a pumping device 24 such as a membrane pump. The line 2 8 sends the mixture through the suction port 30 to the colloid mill 32, or a pipe mill, etc. The carbon black is dispersed in water. The carrier liquid forms a dispersion fluid, which passes through the outlet 31 and the fluid line 33 to the homogenizer 34. The pumping device 36 is provided on the line 33, and preferably includes a forward cavity pump and the like. The homogenizer 34 finely disperses the carbon black in the carrier liquid to form a carbon black slurry, which is fed to the mixing zone of the coagulation reactor 14. It has an inlet 37 for the fluid connection 33 by a colloidal mill 32. The homogenizer 34 preferably includes, for example, a Microfluidizer® system commercially available from Microfluidic International Corporation (Newton, Mass., USA). Also suitable are MSI 8, MS45 and MC120 series homogenizers such as those available from the APV homogenizer division of APV Gaulin, Wilmington, Mass., USA. Other suitable homogenizers are commercially available and will be apparent to those skilled in the art in order to impart the benefits of this disclosure. In general, carbon black prepared according to the above system has at least about 90% of a polymer with a size of less than about 30 microns in water, and preferably at least about 90% of a polymer with a size of less than about 20 microns. Preferably, the carbon black is broken to an average size of 5-15 microns, for example, about 9 microns. The outlet 38 passes the carbon black slurry through the homogenizer through -25- (Please read the precautions on the back first

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This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) 533225 V. Description of the invention (23 A7 B7 Printed feeding line 16 printed by the staff consumer cooperative of the Central Standards Bureau of the Ministry of Economic Affairs and sent to the mixing area. Carbide to-and leave the horse at about ~ or higher, using carbon black content to reduce the removal of excess or other carriers-generally carbon black with f 'about 1G to 30 weight percent is preferred. This person should understand that in order to give the benefit of this disclosure, the carbon black content of the material; the percentage of the material and the flow rate of the material to the mixing zone should be matched with the natural rubber latex to In order to obtain the required carbon, Li Bendanshuai selects the carbon black content according to known principles to obtain a sound map suitable for the production of J: heart material characteristics and performance properties. In general, for example, ctab_ or more Carbon black is used in an amount sufficient to obtain at least about 30 coffee in the master batch. 'U The slurry is preferably used in the manufacture of the master batch immediately after the preparation. Situations troughs, etc., should be established or maintained with substantial retention ^ Black Condition 1 of the dispersion in the slurry should prevent or reduce the large amount of re-aggregation or sedimentation of the granular filler in the paddle material to a reasonable level. Preferably, for example, all the flow lines are smooth and have Smooth line-to-line transfer. As appropriate, use an accumulator between the homogenizer and the mixing zone to reduce the pressure or speed of the slurry on the top of the nozzle in the dead zone. The above is appropriate for Na Under the processing parameters, the natural rubber latex fluid or other elastomeric latex fluid is mixed through the feed line i 2 and the carbon black slurry fed to the mixing area through the feed line 16 to produce a novel elastic compound. , Especially the elastomer mother batch scrap. It can also provide a device for adding various additives to the elastomer mother batch. Additives containing one or more additives can be incorporated into the carbon body (please read the note on the back first) matter

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26- The paper size is suitable for financial affairs (cWs) A4 & (Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 533225 A7 B7 V. Description of the invention (24 bodies can be fed to the mixing, or Multi-additives and carbon ... One t ... can be pre-mixed-water, or more often with elastomeric additives can also be mixed into the master batch later, for example, borrowed. Materials are known to those skilled in the art, and include: for example; odorants, plasticizers, processing aids (eg, liquid polymers, Yousi), resins, flame retardants, heavy oils, lubricants Agent, and any crystals thereof. The general purpose and choice of this additive are known to those skilled in the art: its use in the system disclosed here is from the benefit of this disclosure: and easy to understand, In place of the specific embodiment, the curing agent can also be added in a similar manner to produce a curable elastic compound, which is called a compound. ^ The mixing zone / coagulation zone assembly is discussed in more detail below. Elastomer master batch scrap From the discharge end of the coalescing reactor 14 to appropriate drying In the preferred embodiment of the figure, the master batch is dried in multiple stages. It is first sent to the dewatering extruder 40 and then dried by a conveyor or simple gravity drop or other suitable device 41 to dry the extruder 42. The consistent and preferred embodiment of fixing the natural rubber master batch and carbon black filler as described in FIG. I. The dehydration / drying operation generally reduces the water content to about 0 to 5 weight percent, more preferably 0 to 5 weight percent. Suitable dryers are known and commercially available, including, for example, extruder dryers 'fluid bed dryers, hot air or other oven dryers, etc.' as obtained from French Petroleum Machinery Company (piqua, Ohio, USA). French Mills 0 Dry master batch scraps obtained from the drying extruder 42 are carried by the cooling conveyor 44 to the baler 46. The baler is a conditional and advantageous feature of the device of FIG. China National Standard (CNS) A4 specification (210 > < 297 public directors)

Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 533225 A7 -------- ^ B7__ V. Description of the invention (25) The s chamber of the company's batch of crumbs is shrunk to form stable compression blocks, etc. — In general, elastomer master batches of 25 to 75 pounds are compressed into blocks or bales for transport, further processing, and the like. Or, for example, the product is provided by a tablet. The size and specific design characteristics of the condensing reactor 14 suitable for the specific embodiment shown in FIG. 1 include the mixing zone / condensing zone components, depending in part on design factors such as the required output capacity, the choice of material to be treated, and the like. A preferred embodiment is illustrated in Fig. 2 in which the coalescing reactor 48 has a mixing head 50 connected to the coalescing zone 52 and a fluid-tight seal at the joint 54. —Figure 2 schematically illustrates the first system 56 for feeding the elastomer latex into the mixing zone, the secondary system 57 for feeding carbon black slurry or other particulate filler fluids into the mixing zone, and as appropriate Additive fluid, pressurized air, etc. are fed to the secondary system 58 of the mixing zone. It can be seen that the mixing head 50 has three feed channels 60, 61, 62. A feed channel 60 is provided for the natural rubber 4 latex fluid and a feed channel 62 is provided for direct feeding of the gas and / or additive fluid. With regard to preferred embodiments of direct injection using additives, significant advantages are obtained with regard to hydrocarbon additives or more often non-water-miscible additives. Although the use of emulsified intermediates is known to make additive emulsions suitable for blending with elastomeric latexes, the preferred specific embodiments of direct injection using additives not only eliminate the need for emulsified intermediates, but also exclude previously used Requirements for emulsion-forming devices, such as tanks, dispersion devices, etc. Therefore, a reduction in manufacturing cost and complexity is available. As discussed further below, the feed channel 6 through which the slurry is fed to the mixing zone is preferably coaxial with the mixing zone and the coagulation zone of the coagulation reactor. Although only a single feed channel is shown to receive the elastomeric latex fluid, any appropriate number of feed channels -28- This paper size applies to China National Standard (CNS) A4 specifications (210X297 mm) f Please read the precautions on the back first This page}

-Order 533225 A7 ___— _B7 V. Description of the invention (26) The channel can be arranged around the central feeding channel, and the slurry is fed to the mixing zone through it. Therefore, for example, in the specific embodiment of FIG. 2, a fourth feeding channel may be provided through which ambient air or high-pressure air or other gases are fed to the mixing zone. Pressurized air can be injected similarly to the slurry through the central shaft feed channel 61. When not in use, the auxiliary feed channel can be temporarily or permanently sealed. It can be seen that the coagulation zone 52 of the coagulation reactor 48 has a first portion 64 which has a shaft length selected for the design purpose of the particular application intended. Optionally, the agglomeration region may have a fixed cross-sectional area at all or substantially all of its axial length. Thus, for example, a coalescing reactor can define a simple, straight tube flow path from mixing to discharge. However, preferably, for the reasons discussed above and the preferred embodiment described in the drawings, it is seen that the cross-sectional area of the condensing zone 52 gradually increases from the inlet end 66 to the discharge end 68. More specifically, the cross-sectional area increases in the longitudinal direction from the inlet end to the discharge end. In the specific embodiment of Fig. 2, the agglomeration area gradually increases the cross-sectional area with the feeling that it continuously increases after fixing the cross-sectional portion 64. Unless otherwise indicated, the diameters and cross-sectional areas of the coalescing reactor (or more appropriately the 'coalescing zone defined within the coalescing reactor') and other components are intended to indicate the cross-sectional area of the open flow path and within this flow path. path. Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. It can be seen that the elastic compound, especially the condensed elastomer latex in the form of master batch 7 2, is discharged from the condensing reactor 48 via the diffuser 70. The diffuser 70 is an adjustable duct connected to the condensation and reactor at the discharge end 68. It can be adjusted to selectively deliver the elastomeric master batch 7 2 to any of a variety of different receiving locations. This feature is beneficial for the removal of mother batch scraps from the product stream when the unsettled product is temporarily generated at the beginning of temporary production. For example, for inspection or manufacture -29- This paper applies Chinese National Standard (CNS) A4 Specifications (210X 297 mm) 533225 A7 B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs V. Invention Description (27) At the beginning of the trip. In addition, the diffuser provides design flexibility for self-condensing reactors or different post-processing routing guidance products. According to the preferred embodiment according to Fig. 1, it is seen that the mother batch scraps 72 discharged from the condensing reactor 48 via the diffuser 70 are received by the dryer 40. It can be seen that the cross-sectional dimension of the coalescing reactor 48 is "increased at a total angle between the inlet end 66 and the discharge end 68. The angle" is greater than 0. And in the preferred embodiment it is less than 45. , More preferably less than 15. , The best is 0.5. To 5. . It can be seen that the angle α is a half-angle because it is measured from the central longitudinal axis of the agglomeration zone to the point A at the end of the agglomeration reactor at the periphery of the agglomeration zone. In this regard, you should know the cross-sectional area of the upper part of the agglomeration reactor, that is, the part close to the inlet end 6 6 is preferably slow enough to increase it in order to obtain the standard of agglomeration according to the principles discussed above Plastic mold. Too large agglomeration zone expansion angle to produce the elastomeric master batch was not made in the form of pellets or worms, and was sprayed only through the agglomeration reactor. In a specific embodiment, the pores of the coagulation reactor are increased too slowly to accumulate or block the feed and reaction products in the mixing head. Downstream of the agglomeration zone, where the latex has been substantially agglomerated and the flow has become essentially inserted into the flow ' the agglomeration zone can be extended with or without an increase in cross-sectional area. Therefore, referring to the condensed region of the preferred embodiment with gradually increasing cross-sectional area, it should be understood that the part of the condensed region in which the flow is not substantially inserted into the flow is understood. The cross-sectional area of the Ning area (i.e., at least its upstream portion, as immediately adjacent to the above) can be increased in a stepwise manner instead of the continuous manner described in the specific embodiment of FIG. In the specific embodiment described in FIG. 3, it can be seen that the continuous flow system for the manufacture of elastomeric master batches according to the TJT t manufacturing method and device disclosed herein. -30- (Please read the precautions on the back before this page) .Teach-• 11— I---, in 1- i!-Dry--I r {VO ζ mm 533225 A7 B7 Head / condensation zone assembly, where the cross-sectional area of the condensation zone increases in a stepwise manner. Preferably, the individual parts of the coacervation zone in this step-by-step embodiment have a good connection to adjacent motifs. That is, the combination forms a smooth and substantially continuous surface of the condensed zone, for example, as opposed to a sharp or instant increase in diameter from one part to the next. The coacervation zone of Figure 3 is increased in three steps, resulting in four different sections or sub-zones 74-77. Consistent with the design principles discussed immediately above, the cross-sectional area of the condensing zone 53 increases from the inlet end 66 to the point A of the discharge end 68 to increase the total angle required to obtain the desired flow control in the upstream portion of the condensing reactor. The first portion 74 may be comprised of a fixed diameter portion of the w-joint 50 immediately downstream of the &) mixing area, and (b) the same or adjacent diameter portion connected by the joint 54 at the inlet end 66. This first part has a fixed cross-section, a direct control Di and an axial dimension or length Li. In this first part 74, the length Li should be greater than three times the diameter D1, more preferably greater than five times D1, and most preferably about 12 to 18 times O1. In general, this part has a length of about fifteen times that of 仏. Each subsequent part preferably has a fixed cross-sectional size and a cross-sectional area of about twice the front (i.e., 'upstream') part. Therefore, for example, the portion 7 5 has a sufficient cross-section size and the portion 74 has a cross-sectional area twice as large. Similarly, the cross-sectional area of the ground injury 76 is twice that of the portion 75, and the cross-sectional area of the portion 77 is twice that of the portion 76. In each section 75-77, the length is preferably more than three times its straight, more preferably about three to seven times its diameter, and usually about five times its diameter. Therefore, for example, the longitudinal dimension L3 in the portion 76 is preferably about five times its diameter D3. Tongshi Lutong ’s, θ θ I /, embodiment of the mixing head and the condensation zone assembly are partially cut away. The mixing head 50 is integrated with the condensation zone extender 5 3 through the joint 5 4 as shown in FIG. 4. (Please read the caution page on the back first)

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-—__ ____-31-533225 A7 B7 Printed by the Consumers' Cooperative of the Central Bureau of Standards, Ministry of Economic Affairs. 5. Description of the Invention (29) Defines a mixed zone in which multiple feed channels 60, 61, 62 and essentially extender 53 The inner condensing area is partially coaxially elongated, and the substantially cylindrical channel 80 forms a contact. It should be understood that it is not important for the process and apparatus operating forces disclosed herein to precisely define the boundaries of the mixing zone and / or the cohesive zone. Many variations in the design of the flow channel junction area are possible, and will be apparent to those skilled in the art in order to impart the benefit of this disclosure. In this regard, as a generally preferred guideline, for example, in a specific embodiment of the type described in FIG. 4 'the slurry tip 67 is usually upstream of the beginning of the cylindrical portion', approximately longitudinally at the feed channel junction in. In this specific embodiment, it is preferred that the minimum cross-sectional area defined by the imaginary core of the circumference at the beginning of the slurry from the top 67 to the cylindrical portion 80 is advantageously greater than or at least equal to the cross-sectional area of the latex feed channel 60 . Preferably, the channel 80 and at least the upstream portion of the agglomeration region where there is a flow disturbance before the elastomer latex is substantially completely agglomerated, both have circular cross-sections. It can be seen that the device for feeding the carbon black slurry or other granular filler fluid includes a feed tube 82 which is substantially the same as the opening from the mixing chamber to the condensation zone or the top 67 of the slurry. This is a very advantageous advantage of the preferred embodiment discussed here. As shown above, the carbon black slurry is fed into the mixing zone at a very high feed rate relative to the latex feed rate, and the axial arrangement of the narrow-hole feed pipe 82 produces excellent flow disturbances. The diameter of the channel 80 (as shown above, preferably substantially equal to the diameter A of the immediately adjacent portion 74 below the condensation zone) is preferably at least twice the inner diameter of the slurry feed tube 82, and more preferably The diameter of the "feed tube" is about four to eight times, generally this diameter is about seven to eight times. It can be seen that the feed tube M and the inlet 83 at the upstream end of the feed channel 61 of the mixing head 50 form an impervious fluid tightness (please first (Read the notes on the back again ^ this page)

Order

32- 533225 Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs A7 ____ ______ B7 V. Description of Invention (30). The straightness of the axial feed pipe 82 is mainly determined by the required volume flow rate and axial velocity when the slurry channel tip 67 of the slurry nozzle reaches the mixing chamber. In order to give the benefit of this disclosure, the correct or required volume and speed can be easily determined by those skilled in the art, and part is the function of the concentration and selection of the substance. A specific embodiment, as described and disclosed herein, wherein the carbon black slurry is a removable feed tube ' provides the required flexibility when manufacturing different master batch compositions at different times. The feed tube for one manufacturing stroke can be removed and replaced with a larger or fortunately smaller perforated tube suitable for subsequent fabrication. The pressure and speed at which the slurry exits the feed tube may be referred to as mouthwatering or spraying into the mixing zone. It should be understood that, at least in particular embodiments, it means high-speed injection of slurry into an area that has been substantially filled with fluid. Therefore, it is a spray of a feeling of immediate distribution as it passes through the tip of the slurry nozzle, and it does not need to be a feeling of freely flying material droplets in a simple trajectory. It can be seen that the other feeding channels 60 and 62 each form a contact 84, 85, and the feeding channel 60 and the downstream channel 80 have an angle of 0. In many embodiments, the angle Lu may have a value greater than 0 to less than 180. . In general, cold can be, for example, 30-90. It is desirable to avoid negative pressure, i.e., cavitation of the latex fluid when the slurry tip 67 is transported at a high speed slurry, as this disadvantageously causes inconsistent mixing and inconsistent mother batch products. Air or other gases can be injected or fed into the mixing zone to help break up any such emptying. Further, it is desirable that the natural rubber latex guided to the inlet 86 of the feed passage 60 is provided with an expanded feed line as a latex fluid reservoir. In the preferred embodiment of FIG. 4, the latex feed channel 60 is a mixing zone adjacent to the top end of the slurry nozzle 66 of the parent fork. However, alternatively, the latex feed channel may cross the mixing channel upstream or downstream of the slurry nozzle tip 67. (Please read the notes on the back before this page)

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-I -33- This paper size applies Chinese National Standard (CNS) M specifications (210X; 297 mm) 533225 A7 B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (31 Carbon black paste or other particles The filler-like fluid is generally supplied to the feed tube 82 at a pressure higher than about 300 psig, such as about 500 to 5000 psig, for example, about 1000 psig. It is preferred that the liquid slurry be higher than 1 second At a speed of OO feet through the top 67 of the slurry nozzle into the mixing zone, preferably from about 5,000 to about 8,000 feet per second, more preferably from about 2,000 to about 5,000 feet per second, For example, about 350 feet per second. The arrow 51 in FIG. 4 indicates the general flow direction of the elastomer latex and the auxiliary feed material through the feed channels 60 and 62 to the channel 80 under the slurry nozzle top 67. Therefore, According to the above-mentioned number, the slurry and latex fluid are fed into the mixing zone at very different feed flow speeds. Although it is not intended to be bound by theory, it should be understood at present that the differential feed in the mixing zone has caused a huge Dispersion and coagulation of latex shearing conditions. Alternative preferred embodiment description 5 and 6, where the single-axis feed tube 82 of the embodiment of FIG. 4 is replaced by a multi-axis extended feed tube 90-92. A large number of feed tubes can be used, for example, up to about 6-8 An axially extending feed tube. By using different feed tubes with different diameters, it is advantageous to obtain manufacturing bombs for different formulas. Multiple feeds can also be used at the same time to condense in the mixing zone and the coalescence reactor. Good flow disturbances were obtained in the zone. = A combination of t and t is shown in Fig. 7. The mixing head 150 defines the mixing zone 179. The axial feed channel 161 receives a carbon black slurry or other suitable for high speed The granular filler fluid is fed to the feed pipe in the mixing chamber. 79. 82. It can be seen that the feed pipe 182 lacks a central hole and terminates at the top end of the slurry nozzle 167. The fixed diameter nozzle 168 is immediately upstream of the nozzle top 167. , Resulting in a large hole area of 169. Preferably, the pumping dimension of the 168 is about 2 to 6 times its diameter, for example, about 5 times. The second feed channel 16 and the mixing zone opening 9 are at an angle ( (Please read the notes on the back first)

1T 1 -34-

533225 Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 ———_ __ B7 V. Description of the invention (32) The contact 184 is formed to feed the elastomer latex fluid to the mixing zone. The cross-sectional diameter of the latex fluid feed channel 160 is substantially larger than the cross-sectional diameters of the top ends 167 and 168 of the slurry nozzle. Without wishing to be bound by theory, the axial elongation of 168 at the nozzle, combined with the expanded diameter hole portion upstream of the nozzle, is believed to provide favorable stability in the flow of slurry through the feed tube 182 to the mixing zone 179. The hole in the feed tube 182 was found to be 20. The chamfering works well, i.e., the conical region 169 that expands at an angle of about 20 degrees in the upstream direction. Downstream of the mixing zone 179 is an extension and long condensation zone. Consistent with the principles discussed above, this agglomeration zone need only be marginally elongated. That is, the axial dimension only needs to be longer than the diameter and length at the edges. However, it is preferable to use a gradually enlarged condensation region. As discussed above, the coagulation of the elastomeric master batch is substantially completed at or before the end of the coagulation reactor. That is, the coagulation occurs in the reaction zone of the coagulation reactor, and a stream such as a coagulation solution needs to be added. It does not exclude the possibility that some initial agglomerations will occur in the mixed zone. Therefore, the mixing zone can be regarded as an extension of the condensation zone. Also referring to the fact that the elastomeric master batch is fully condensed substantially before leaving the coagulation reactor, for any of the various purposes suitable for the intended use of the final product, it does not mean that the possibility of subsequent processing and further processing steps is excluded. In this regard, the substantially complete agglomeration in the preferred embodiment of the novel manufacturing method using natural rubber latex disclosed herein indicates that at least about 95 weight percent of the latex's rubber hydrocarbon agglomerates, and more preferably at least about 97 weight Percent, and most preferably at least about 9 9 weight percent agglomeration. The manufacturing method and apparatus disclosed herein produce an elastic composite having excellent physical properties and performance characteristics. The novel elastic compound of the present invention includes a master batch composition manufactured by the manufacturing method and device disclosed above, and the master batch composition _______ 35_ This paper size is applicable to Chinese National Standard (CNS) A4 specification (210X297) Li) -i: i · * C, please read the notes on the back '-item deposit ^^ 本 K) sub-A. • ii-I j J. 533225

V. Description of the invention (33) Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs < Intermediate compounds and final products. Obviously, natural rubber latex (latex concentrated or field latex) and various grades of carbon black can be used to make the elastomer batch 2. It has excellent physical properties and performance characteristics. Carbon blacks that have been successfully used, which are widely used commercially for applications such as wheel treads, and carbon blacks that have hitherto been considered unsuitable for commercial use in manufactured devices and processes. Because of its low surface area and low structure, which makes it possible to obtain an acceptable degree of large dispersion in the fixed commercial filling level of carbon black and / or to retain the molecular weight of the elastomer is impractical and unsuitable, for the novel elastomer master batch disclosed herein The composition is not preferred. It was found that this elastic compound has excellent dispersion of carbon black in natural rubber and good molecular weight retention of natural rubber. Furthermore, these advantageous results are obtained without the need for a coacervation step involving a treatment tank or the flow of an acid solution or other agglomerating agent. Therefore, not only can the cost and complexity of this agglomeration process be avoided, but also the effluent stream from this operation can be treated. Previously known dry kneading techniques were not able to obtain an equal dispersion of this filler without significant molecular weight degradation, and therefore, it was not possible to make a novel natural rubber master batch composition in accordance with certain more specific embodiments of the present invention. In this regard, the unveilable novel elastic compound has excellent carbon black and natural rubber great dispersion, even if the carbon black has a structure to surface area ratio of less than 1.2 and even less than io DBPA: CTAB, and high molecular weight natural rubber . The known mixing technology in the past could not obtain this excellent carbon black macrodispersion without significant natural rubber molecular weight degradation 'and therefore, the novel master batch composition and other elastic composites of the present invention could not be manufactured. According to this disclosure, a better novel elastomeric master batch composition having a degree of black macrodispersion that has not been obtained so far can be used to replace previously known master batches with poor macrodispersion. Therefore, it is revealed here that -36- This paper size applies to the Chinese National Standard (CNS) A4 specification (210X 297 mm) ------ (Please read the precautions on the back before this page)

533225 A7 B7 V. The master batch of the invention description (34) can be added to the curing compound according to known techniques. This novel mature compound was found to have generally comparable physical properties and performance properties in the preferred embodiments, and in some cases, far better than comparable mature compounds that contained poorer macrodisperse master batches. The master batch can be made in accordance with the present invention, however, it has reduced mixing time, reduced energy input, and / or other cost savings. Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs. In particular, specific preferred embodiments can produce natural rubber latex and carbon black filler master batches with excellent physical and performance properties. Get excellent carbon black macrodispersion, that is, use unexpected carbon black with high surface reading and low structure without the degradation degree of natural rubber, because it is enough time and sufficient strength to obtain the same carbon black dispersion. Caused by dry kneading. In this regard, it is particularly advantageous to use a carbon black having a structure-to-surface area ratio of less than 1.2 and even less than 1.0, such as DBPA: CTAB, to obtain a novel natural rubber master batch composition in which a high degree of dispersion is obtained. The carbon black structure used herein can be measured as dibutyl phthalate adsorption (DBPA) 値, which is expressed as DBPA cubic centimeters per 100 grams of carbon black, following the procedure described in ASTM D2414. The carbon black surface area can be measured as CTAB, which is expressed in square centimeters per gram of carbon black, following the procedure described in ASTM D3765-85. Therefore, a novel natural rubber master batch is obtained which has physical characteristics that have not been obtained so far, such as molecular weight distribution and degree of filler dispersion, and / or adding fillers that have not been suitable so far, such as a combination of ultra-high surface area and low structure. The dispersion quality of natural rubber master batches made in accordance with the methods and apparatus disclosed herein can be demonstrated with reference to known MWSQ1 (weight average) and macrodispersion characteristics. In particular, the degree of dispersion of the master batch produced in accordance with the preferred embodiment is far greater than that in use. -37- This paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) 533225 A7 B7 Economy Printed by the Consumer Standards Cooperative of the Ministry of Standards of the People's Republic of China. 5. Description of the Invention (35 Dry batches of approximately equal mwsq1 master batches are preferred. Most notably, the dispersion quality of these preferred embodiments does not significantly depend on carbon black. The morphology of the filler depends on other factors that affect the degree of dispersion available using the manufacturing methods and devices disclosed herein, including the concentration of carbon black in the slurry, the total energy input in the slurry, and the fluid flow. Energy input during mixing, etc. The great dispersion quality of the natural rubber master batch disclosed by carbon black here is much better than previously known master batches of approximately equal MWSQl (weight average). In some preferred embodiments, the MWSQl of natural rubber in the latex state (for example, about 1,000,000), a condition that cannot be obtained before washing, obtains an excellent carbon black distribution. Dispersion Advantages are in the preferred embodiments described above using carbon black with low structure and high surface area, for example, DBPA less than 110cc / 100 grams, CTAB greater than 45 to 65 square meters / gram, and less than 1.2 and preferably low DBPA: CTAB at 1.0 is particularly important. Example Test Procedures The following test procedures are used in the examples and comparisons presented below. 1. Combined rubber: Weigh a sample weighing 0.25 grams and weigh 0.25 grams and place it in a sealed flask. 100 ml of toluene, and stored at ambient temperature for about 24 hours. The toluene was then replaced with 100 ml of fresh toluene, and the flask was stored for 4 days. The sample was then removed from the solvent and air-dried at ambient temperature under a fume hood for 24 hours. The sample was then It was further dried in an air oven at ambient temperature for 24 hours. The sample was then weighed and the combined rubber was calculated from the weight loss data. 2. MWSQl: The MWSQl used in this disclosure and patent application refers to natural rubber -38- This paper is applicable to China Standard (CNS) A4 (210X297 mm) Please read the notice on the back first

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It 533225 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 V. Description of the invention (36) The weight average molecular weight of the colloidal sol. The following standard GPC techniques were used for molecular weight measurement: 2.1 Two 10 / im 106a columns, one 10 # m50OA column and 10em mixed bed column obtained from the British Polymer Laboratory. 2.2 UV detection at 215nm. 2.3 Solvents · Tetrahydrofuran (THF). 2.4 Concentration, nominally 2 mg / ml in THF. 2.5 The samples were allowed to stand in THF for 3 days to dissolve and stabilized with BHT. 2.6 Centrifuge the solution to ram away any gel and inject the supernatant into the column. 2.7 Sample preparation Sample preparation is designed to prepare a sol concentration in the range of 0.5 to 0.05 weight percent to provide a good detection response to the correct measurement of the molecular weight distribution. Depending on the filler filling, adjust the sample weight according to the following formula: Sample weight = (100+ filler filling (phr): T20 / 100 mg +/- 2 mg. The sample is placed in a UV protective glass vial and dissolved in 4 ml containing 0.02% D The stable tetrahydrofuran (THF) of the butylated hydroxytoluene (BHT) was obtained for a day. The supernatant from the dissolution step, which contained most of the sol fraction, was transferred to a Teflon centrifuge tube, and was placed in an Avanti 3 0 (Beckman The centrifuge was centrifuged at 26,000 revolutions per minute (corresponding to a maximum field strength of 57,500 grams) for 60 minutes. At this field strength, most of the gel phase was deposited to obtain a gel-free supernatant. This gel-free solution was stable. THF was diluted 1: 5. At this time, the sample was transferred to a GPC glass vial and placed in a Waters 717 autosampler-39- This paper size applies to China National Standard (CNS) A4 (210X297 mm) (please read the back first) Note again ^^ this page) clothes · [reorder

533225 Α7 Β7 V. Invention Description (37) (Waters, Miiford, Mass., USA) to prepare for GPC test. To 1 sub-quantity ^, then the weight average molecular weight MWsol of the sol portion was measured. Using Millenium software (available from Waters, Milford, Mass., U.S.A.), a valley-to-valley pattern was used to define baselines in time increments of 15 to 35 minutes. This time increment is suitable for the column described in paragraph 2. Jade, with the mobile phase flow rate set at 0.75 strokes / min. Once a reasonable baseline is established, the distribution can be determined. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs / Granulation time is converted into molecular weight. A polystyrene solution made from commercially available standards (EasiCal: British Polymer Laboratory) was prepared, which contained a range of molecular weights with a very narrow distribution. The conversion of polystyrene knife weight to polyisoprene molecular weight equivalent is based on a universal calibration method based on Benoit and colleagues. The hydrodynamic radius is proportional to the product of multiplied by the intrinsic viscosity. After converting polystyrene ^ to polyisoprene equivalents, the calibration curve relates to absolute molecular weight versus dissolution time. The standard is run under the same conditions as the sample, and the standard is integrated to specify the appropriate molecular weight for the eluate time given based on the data taken from the standard. Once the time-based distribution is properly converted to molecular weight, the appropriate molecular 値 is calculated by Waters' Millenium software. 3. Menner viscosity: according to] ^^ (1 + 4) @ 1〇〇. (: Standard procedure. 4. Ageing conditions for test specimens .... Ageing of test specimens to i5 (rc time: 41 tension sheet. 20 minutes. 4.2 Elasticity: 23 minutes. L-__ ____-40-This paper size Applicable to the country of China} (21 {3χ ^^ 533225 A7 B7 printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs V. Description of the invention (38) 4 · 3 Hardness: 23 minutes. 4 · 4 Heat accumulation: 25 minutes. 5. Dispersion : Target evaluation using Cabot distribution table method and 50 × optical micrograph (ASTM D2663 method) 6. Stress and strain: test BS903: Α2 and ISO 37. 7. Hardness test ISO 48 (1994), temperature 23 ° C. 8 · Elasticity: Test BS903 ·· A8 (1990), method A, temperature 23 ° C (8 mm mold plate test piece). 9 .Heat accumulation: test ASTM D623, method A. ~ 9.1 starting temperature : 23 ° C. 9.2 Static load: 23 lbs. 9.3 Stroke: 0,225 inches. 9.4 Frequency: 30 Hz. 9.5 Run for 30 minutes. 10 · Tan 6: Measured on Rheometrics® RDS Type II. Reported 値 is the strain bending The maximum strain is strained between 0 °, 30 °, and 60 °, 1Ηζ, and 0.1% to 60% strain. 11. Cracking Long Resistance: measured in accordance with ASTM D3629-94.

Example A An elastomeric master batch was made in accordance with the present invention. In particular, an elastomeric master batch containing a standard natural rubber field latex from Malaysia was made with 5255 phr of filler including commercial grade N234 carbon black from Cabot Corporation. The properties of natural rubber field latex are provided in Table 1 below. -41-This paper size is in accordance with Chinese National Standard (CNS) A4 (210X297mm) (Please read the precautions on the back before this page) * ψ -I 1-1—--1--1--- = · 1 533225 A7 B7 V. Description of the invention (39) Table 1 Natural rubber latex additives% Dry rubber% Total solids% Gray nitrogen ppm Volatile fatty acid ML (l + 4) @ 100 C 0.15% HNSa 0.3% NH3 ZnO , TMTDb 28.4 34.2 0.38 0.366 0.052 68 Employees' cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs a. HNS: Hydroxylamine neutral sulfate, Menner viscosity stabilizer. b. ZnOnMTD ·· For bio-preservation, generally a 1: 1 mixture of 0.025%. All compound formulations are described in Table 2 below, and are representative of commercial truck wheel treads known to have excellent reversion resistance upon aging. Table 2 Master batch formula "Ingredient rubber carbon black ZnO stearic acid 6PPD (antioxidant) Sunscreen improver (wax) Ennerflex 74 (aromatic oil) 3.0 Total = 165.5 An elastomer master batch manufacturing device and the above reference drawing The devices described in Figures 1 and 7 are essentially the same. The tip of the slurry nozzle (see reference number 167 in Figure 7) is .039 inches in diameter and has an axial length of 0.2 inches (see reference number in Figure 7) 168). The agglomeration zone is 0.188 inches in diameter and has an axial length of .985 inches. It has a fixed diameter between the mixing zone and its discharge end. The preparation of the master batch is further detailed immediately below. 1 Carbon black slurry preparation The carbon black bag was mixed with deionized water in a carbon black slurry tank equipped with a stirrer. The stirrer broke the pieces into pieces and formed a coarse slurry with carbon black of 12.5% by weight. During operation, the slurry is 100 52.0 4.0 2.0 2.0 2.0 by weight of the air film (please read the precautions on the back page first) Order-42- This paper size applies to China National Standard (CNS) A4 specification (210X297) %) 533225 A7 B7 V. Description of the invention (4 ) 2. Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs, continuously pumped to the colloid mill to disperse initially. The slurry is then fed to the homogenizer by advancing the cavity, especially the M3 type homogenizer from APV Gaulin. A homogenizer. This homogenizer produces finely ground slurry. The slurry flow rate from the homogenizer to the mixing zone is set by the homogenizer speed. The homogenizer acts as a high-pressure positive displacement pump. The slurry flow rate is measured using a Micromotion® mass flow meter. The black slurry is fed to the homogenizer at a pressure ranging from 50 to 100 psig, and the homogenization pressure is set to 4000 psig, so that the slurry is flowed at a flow rate of 4.1 to 4.4 hours per minute and about 13 The speed of 0 feet per second is introduced into the mixing zone by spraying. The latex is loaded in a 100 gallon pressurized feed tank. The antioxidant emulsion is loaded such as adding latex. The addition includes 0.3 phr ginsyl nonylphenylarsinic acid. Salt (TNPP) and 0.4 phr Santoflex® 134 (mixture of alkylaryl p-phenylene diamine). Each antioxidant uses 3 parts of potassium oleate per 100 parts of antioxidant, and Potassium hydroxide adjusts the emulsion to a pH of about 0, such as 5 wt% 3 phr of extender oil is also added. Use air pressure (51 psig) to move the latex from the feed tank to the mixing zone of the coagulation reactor. The latex flow rate is 32 to 34 pounds per minute and per second. It is about 3.8 feet, and # Micr〇m〇ti〇n⑧ mass flow meter and rubber tube spring valve are automatically measured and controlled. By maintaining the appropriate ratio of latex feed rate to carbon black water feed rate, 52 5 Carbon black filling required for pllr. The m Lm carbon black slurry latex is mixed by transporting the latex into the carbon black slurry. When transported, the carbon black was tightly mixed into the Rusheng, and the mixture agglomerated. Leaving the coalescence reactor is a soft, wet sponge of the condensate "(Please read the precautions on the back before this page) n m-(reorder

, 1 -1-1 II -43 533225 A7 B7 V. Description of the invention (41) 4. The wet debris discharged from Mi self-coagulation reactor is about 79% water. Wet chips are dewatered with a dewatering extruder (French Petroleum Mills; 31/2 inch diameter) to about 5 to 10% moisture. In the extruder, wet chips are compressed and water is squeezed out of the chip and passed through a slotted bucket of the extruder. 5. [The curled-up but dehydrated chips fall into the second extruder, where they are compressed and heated again. Water dries as the chips are expelled through the die plate of the extruder. The product exit temperature was about 300T, and the moisture content was about 0.05 to 1% by weight. The hot drying debris is rapidly cooled (about 20 seconds) to about 100F by a powerful air-drying vibration conveyor. The resulting dry crumbs had rubber solids of about 66 wt.% ❶ / ❶ and about 33% by weight of carbon black.

Example B A control master batch was prepared by dry kneading. The control used the same formulation as in Example 8 (see Table 2 above) 'except that the natural rubber was SMR 10 instead of latex. It was prepared by kneading rubber in an OOC Banbury mixer (approximately 3 kg) at 50 rpm using i 〇 carbon black. Reduce kneading is carried out for about 3 minutes to a total of _ hall cubic meters. Comparison of Examples A and B ^ The mother batch of Example A and the control mother batch of Example B are printed at the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economics and Trade of the Ministry of Economic Affairs and Economics (please read the precautions on the back and then this page) (Approximately 3 kg) in a two-stage mixing operation. The following table] summarizes the mixed stroke of the first stage. It can be seen that the master batch of Example A follows a modified mixing schedule. 44- 533225 A7 B7 V. Description of the invention (42) Table 3 Mixing stroke time of stage 1 (min) Example A Example B Dry mixing control 0.0 All ingredients are pre-kneaded rubber 0.5 Carbon black and oil 1.0 Cleaning 1.5 Other ingredients 2.0 2.5 Sweep 3.0 X Pour at about 700 MJ / m 'and pour at about 1,000 MJ / mj. In the second stage, the curing agent listed in Table 4 below is added at a further mixing cycle of 500 MJ / m3. Table 4 The weight of the maturation and addition components in the final stage _ [Set the compound of phase 1165 · 5 Goodyear Winstay 100 (antioxidant) TBBS (sulfur accelerator) Ϊ · 8 ^ ____ 1.0 Total — 169.3 (Please read the notes on the back first (See page again) m ml m —ϋ nn mm

---1 sis--T Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. Therefore, the Banbury mixing energy used for the compounding of the master batch of Example A is required for the pre-kneading and compounding of the master batch of Example B. About 53% of Banbury's mixed energy. Regardless of the reduced energy input, the substance of Example A was found to have a very good macrodispersion, and the molecular weight MWS () 1 (weight average) of its sol fraction was substantially higher than that of the control. These data are summarized in Table 5 below. Table 5 Compound and maturation data Sample mixing energy (MJ / m3) ML (l + 4, 100C) MW Pre-kneaded phase 1 Final total phase 1 Final weight average Example A 0 694 500 1,194 102 72 444,900 Example B 800 965 500 2,265 92 67 327,000 _ _____ -45- This paper size is suitable for Guancai County (CNS) M specifications (2lGx297 public directors) 瓤. 533225 A7 B7 V. Description of the invention (43 Ageing (non-aging) of case A and the reference substance t In addition, the test results are described in Table 6 below. Sample hardness 6 Additional test data 100% modulus (MPa) 300% modulus (MPa) Tension (MP ^ ~ 16.1 28.7 Example A 71 2.82

Example C C Please read the precautions on the back and then on this page} Manufacture the elastomeric master batch according to the present invention. In particular, an elastomeric master batch containing a standard natural rubber field latex from Malaysia I was manufactured with a phr of filler including commercial grade Regal (g) 66 ° carbon black from Cabot Corporation. The compound formulations (except for small amounts of general latex additives) are described in Table 7 below. Table 7 Master batch formula Ingredients Rubber Carbon black Santoflex I34 (antioxidant) TNPP (antioxidant) I Total multiple parts

Order ^ Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs / Elastomer master batch manufacturing equipment is substantially the same as the equipment described in the above referenced drawings, 3 and 7. The tip of the slurry nozzle (see reference number 167 in FIG. 7) has a diameter of .25 inches, which has an axial length of 0.2 inches (see reference number 168 in the figure). Condensation zone (see reference number 53 in Figure 3) includes part __ 188 inches in diameter and approximately .985 shots in axial length (partially in the mixing head -46- This paper size applies to Chinese National Standards (CNS) A4 specification (210 × 297 mm) 533225 A7 V. Description of the invention (44) and part sealed in the extender); Article diameter and i 6-inch axial long-term production < brother one-piece; · 376 inches The third part of the diameter and the axial length of 2 256 inches; .532 inches of diameter and the fourth part of the 3.19 () inch length, there is a good exchange of axial shortness between the above parts. The master batch is described in further detail immediately below. 1. Blanket-ink slurry preparation of carbon black bag. Deionized water was mixed in a carbon black slurry tank equipped with a stirrer. The agitator breaks the sheet into pieces, and forms a coarse slurry with 14 9% by weight (carbon black. The coarse slurry is recirculated using a line grinder. In operation, this slurry is continuously pumped to the air film pump to The colloidal grinder is initially dispersed. The slurry is then fed to a homogenizer by a forward cavity pump to pressurize and shear, especially the Model M210 microfluidizer from Micromotion International, to produce a finely ground slurry. From The flow rate of slurry from the microfluidizer to the mixing zone is set by the speed of the microfluidizer. The microfluidizer is used as a positive pressure displacement pump. The aggregate mud speed is monitored by a Micromotimo mass flow meter. The carbon black slurry is A pressure of 30 psig was fed to the microfluidizer, and the output pressure was set to 3000 psig, and the output pressure of the accumulator was set to 4500 psig, so that the slurry was at a flow rate of about 39 lbs / min and about 300 sigma. The speed per second is introduced into the mixing zone by spraying. 2 · _ milk .. Acoustic free latex is installed in the tank, especially 55 gallon feed barrels. Antioxidant emulsion is added to the latex before loading. Adding 0.3 phr parameters Nonylphenyl Phosphite I (TNfP) and 0.4 phr Sant oplex® 134 (an aryl p-phenylene diamine mixture) antioxidant. Each antioxidant uses 4 parts of oleic acid per 100 parts of antioxidant, and the emulsion is adjusted to a pH of about 10 with hydroxide.値, prepared as a 40% by weight emulsion. Use a peristaltic pump to move the latex from the feed tank to the mixing zone of the coagulation reactor. Latex flow -47- This paper size applies to China National Standard (CNS) A4 specifications (2l0X297) (Mm) (Please read the note on the back first, then this page) Order printed by the Consumer Standards Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 533225 A7 ___ B7 V. Description of the invention (45) The speed is from 3.2 to 3. J / min and About 39 feet per second, and measured by Endress + Hauser (Greenwood, Indiana, USA) mass flow meter. By maintaining a proper ratio of latex feed rate to carbon black slurry feed rate ', 5 5 phr is obtained. After the black filling is required. 3. Carbon black is mixed with H. The black slurry and latex are mixed by transporting the latex to the carbon black slurry. During transportation, the carbon black is tightly mixed into the latex, and the mixture is coagulated. Coagulation reactor is soft, Sponge "worm". 4. The wet debris discharged from the coalescing reactor is about 78% water. The wet debris is dehydrated to about 12 to 13 by a dewatering extruder (French Petroleum Milling Machinery Company; 31/2 inch diameter). % Moisture. In the extruder, the wet chips are compressed and the water is squeezed out of the chip and passed through the grooved barrel of the extruder. 5. The dehydrated chips fall into the second extruder, where Compressed and heated again. The water is dried as the chips are expelled through the die plate of the extruder. The product outlet temperature is about 280 ° F to 370T, and the moisture content is about 0. 3 to 4 weight / 0. The hot drying chips are cooled by a powerful air-drying vibration conveyor (about 20 seconds) to about ιοοΤ 〇

Example D and E Printed by the Consumer Cooperatives of the Central Bureau of Standards, Ministry of Economic Affairs. Two mixed control batches were prepared by dry kneading. The control uses the same formula as in Example ct (see the table above, except that in Example D the rubber is RSS1 NR instead of gift rubber. In Example E, the rubber is SMR 10 NR. Each is prepared by pre-kneading the rubber in a BR Banbury mixer. Preparation. Example rubber was kneaded for 10 minutes at 8 rpm. The rubber of Example E was kneaded for 4 minutes. Example C, D to E ratio 与

The master batch of Example C and the two master batches of Example 〇 and E are in BR _____ -48- This paper size applies to the Chinese National Standard (CNS) (21〇 > < 297 mm) 533225 A7 B7 V. Description of the invention (46)

Compound in Banbury mixer. The following table 8 describes the compounding schedule. Table 8 The compounding schedule master batch pre-kneading stage I mixing stage II (final) mixing example C without BR Banbury 77 rpm, 4.5 min. Example D BR Banbury mixer 118 rpm, 10 min BR Banbury mixer 77 rpm, 3 min BR Banbury 77 rpm, 4.5 min. Example E BR Banbury mixer 77 rpm, 4 min BR Banbury mixer 77 rpm, 8 min BR Banbury 77 rpm, 4.5 min. The compound formula is shown in the following table 9. Please read the precautions on the back page first) Table 9 Stage II curing additives Ingredients by weight Example 4 Master batch or Example 5 or 6 Stage 1 Dry mixture 155 Azo 66 (zinc oxide) 4.0 Hystrene 5016 (Hard moon purpose acid ) 2.0 Santoflex 13 (Antioxidant) 2.0 Sunscreen Improver (Wax) 2.0 Wingstay 100 (Antioxidant) 1.0 Santocure NS (Sulfur Accelerator) 1.8 Sulfur 1.0 Total: ~ __ = ___ 168 · 8— Order. 廛 · Central Ministry of Economic Affairs The Consumer Bureau of Standards Bureau has printed all three compounds to show good maturation with minimal reversal. Regardless of lowering the energy input, the substance of Example C was found to have a much better dispersion than the dry mixed control, and its molecular weight MWSC) 1 (weight average) of the sol fraction was actually higher than that of the control. These data are summarized in Table 10 below. -49- This paper size applies to China National Standard (CNS) A4 (210X297 mm)

• 14 »I IJ 533225 A7 B7 V. Description of the invention (47) Table 1 0 Master batch and comparison properties

(Please read the precautionary page on the back first) (The examples and comparisons printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs are based on the manufacturing methods and devices disclosed above. In particular, a master batch composition formed from natural rubber latex and carbon black filler, which has a far greater degree of dispersion and / or natural rubber than far hitherto found in known compositions from the same or similar starting materials ^ Figure 8 shows the surface area and structure of the various carbon black fillers used in these preferred master batch compositions, in particular, the CTAB surface area as expressed in square meters per gram of carbon black in accordance with ASTM D3765_85, and Dibutyl terephthalate adsorption (DBPA) as shown in DBP cubic meters per hundred grams of carbon black according to ASTM D 2414. It can be seen that Figure 8 is divided into three different regions. The region I has a lower black. Structure and higher surface area carbon black, which is the most difficult to disperse in natural rubber and other elastomers using traditional dry mixing techniques. Therefore, the carbon black of region I cannot be widely used commercially as other carbon blacks. Carbon black region 1 using conventional drying techniques for producing a mixed master batch and aging of the elastomeric compositions

Order i— I- I It ·· 533225 A7 A --------- B7_ V. Description of the invention (48) It has relatively poor macro dispersion and generally lower MWSQl. The carbon black of the region II has a structure higher than that of the region I. Generally speaking, if the extended dry mixing of MWsoi which is naturally degraded is accepted, it will reasonably obtain good dispersion in natural rubber for vehicle tire products and the like. The carbon black of the area hi in Fig. 8 has a lower surface area relative to its structure. Therefore, it has been dry-mixed in natural rubber for acceptable dispersion and use, but again has undesired "... to degrade. Carbon black dispersion, especially macro-dispersion, in all three regions of Figure 8 is disclosed here. The elastic compound is greatly improved, and according to the preferred embodiment, MWSC with # 常 高 的 NR is obtained. Comparative Example 1 -443 For the purpose of comparison of the elastic compound of the present invention, follow the following In the step, the master batch control sample is prepared by dry mixing. 1. Kneading of natural rubber In order to produce a dry master batch with a wide range of molecular weights, commercial natural rubber (RSS1, SMR CV, and SMR 10) are wrapped in BR banbury and mixed. The following conditions are used for pre-kneading in the device (filling factor: 0.75): Table 11 Samples of natural rubber kneading conditions ρα code Kneading rotor speed (rpm) Cooling water kneading time (min) Ml No M2 Yes 77 On 4 M3 is 118 On 6 M4 is 118 On 10 2 · Mixed carbon black and pre-kneaded natural rubber For natural rubber dry master batches, the following mixing steps are used in the BR Banbury mixer. The filler factor is 0.70. The masterbatch ratio ingredients and mixing steps are described in Table 12. -51-This paper size applies to Chinese national standards ( CNS) 8 4 square (21〇 × 297 mm) 533225 A7 B7 V. Description of the invention (49) Table 1 2 Natural rubber dry master batch formula ingredient phr (rubber percentage weight ratio) Natural rubber 100 carbon black See the table below. Santofex (Antioxidant) 0.4 TNPP (Antioxidant) 0.3 Mixing steps: 0 minutes: adding pre-kneaded natural rubber (77 rpm, 45 C) 1 minute: adding carbon black, oil and antioxidants by dry mixing M1 to M4 pre-kneaded natural rubber samples with different mixing times, as shown in Table 13 below, produce different degrees of dispersion and degree. For example, the sample code M2D1 in Table 13 indicates the pre-kneaded natural rubber M2 (see above) Table 1 1) A control sample mixed for 10 minutes according to the formula in Table 12. (Please read the precautions on the back before this page) · -Reprinted by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs Table 1 3 Mixing time Dry NR master batch sample code Pre-kneaded NR mixing time M1D4 Ml 4 M1D3 Ml 6 M1D2 Ml 8 MIDI Ml 10 M2D4 M2 4 M2D3 M2 6 M2D2 M2 8 M2D1 M2 10 M3D4 M3 4 M3D3 M3 6 M3D2 M3 8 M3D1 M3 10 M4D4 M4 4 M4D3 M4 6 M4D2 M4 8 M4D1 M4 10 • f! —I t I-Bend · -52- This paper size applies to China National Standard (CNS) A4 size (210X297 mm) 533225 A7 B7 V. Description of the invention (50) 3. Final mixing of natural rubber master batch control sample In order to evaluate the composite performance, the other ingredients are added to the dry kneaded natural rubber master batch of Table 13 according to the formula shown in Table 14 Control sample. '' Table 1 4 Amount of additional ingredients for final blend (phr) Azo 66 (zinc oxide) 4.0 Hystere 5016 (stearic acid) 2.0 Santoflex 13 (antioxidant) 2.0 Sun protection improvement (wax) 2.0 Wingstay 100 (antioxidant) 1.0 Santocure NS (Sulfur Accelerator) 1.8 Sulfur 1.0 ** Compounds are cured at 150 ° C according to standard curing techniques until at least substantially complete curing, typically 10 to 30 minutes. In this regard, the same or substantially the same final mixing steps, including the formulations given in Table 14 above, for all control samples, and all samples of the elastic composite of the present invention prepared by the following method (see "preferred" Specific Example Examples "), its curing and testing composite properties and performance characteristics. The following Table 15-23 describes the sol molecular weight MWSQl and macrodispersion D (%) of the control samples 1 to 443. The samples are selected in the table according to the choice of carbon black Grouping. In the table given, the selection of sample-like natural rubber and grouping by carbon black filling and oil filling. The header shows information according to standard nomenclature. Therefore, for example, the header of Table 15 •• N330 / 55phr / 0n means 55phr N330 carbon black without oil. The sub-head shows the choice of natural rubber. In particular, it can be seen that control samples 1 to 450 are made of standard grade natural rubber RSS1, SMRCV and SMR10. The technical description of these natural rubbers can be widely Fan obtained, such as the Blue Book of Rubber World Magazine * published by Lippincott and Peto Company (Akron, Ohio, USA). Natural rubber before any pre-kneading (Ml) and various pre-kneading After refining (M2-M4), the molecular weight MWSQl is also shown in the following Table 15-23. -53- This paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X 297 mm) Please hj read back Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 533225 A7 B7 V. Description of Invention (51) Table 15 N330 / SSphr / 0 RSS1

SMRCV code sample code (K) 〇r ^) sample number ⑻ 〇ΓΛ)

iEEEEyWE 2345δ789γογί 2ί3 Pay Y5f6 12456523712 409126883308 5 3 ο 3 3 2 7 7. 7 5. 5. «. 6.6.93 · 5 9.36 4 ο 2 4.3.4.4.3.2.3.3.1.2.2.3.3.3.5.5. 7890ί234567δ90ί2 ilw / 2222222222333 Μ5β267β5083828181549) 77'9 & 26 «389394570124 ^ 6 97544 ^^ 53344 ^ 33433 ^ 3 5968410195516117 .3.88.7.4-.7.38.7.35.0. &Amp; .39.6 4.3.44.2.3.4.5.3.45.5.3.5.5.5 (Please read the precautions on the back before ^^ this page) Clothing · 9 Order too Table 1 6 Table 1 7

Black Pearl 800 / 5Sphr / 0 RSS1

SMRCV code sample number (K)

Sample Mw ^ No. (K) 〇 (%) Code N3S1 / 33phr / 20phr RSS1 'WE ~ D (%) Number (K) Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs M1 1041 869 M2 786 662 M3 663 491 M4 527 420 M1D1 113 507 12.20 129 418 5.15 M1D2 114 551 15.10 130 482 4.94 M1D3. 115 700 10.20 131 515 6.93 M1D4 • 116 786 5.72 132 583 8.74 M2D1 117 420 5.65 133 403 2.60 M2D2 118 441 6.50 134 438 2.119 M2DD 7.70 135 '434 2.83 M2D4 120 606 5.88 136 530 3.88 M3D1 121 387 3.26 137 366 2.38 M3D2 122 409 2.98 138 378 2.83 M3D3 123 456 3.61 139 399 3.04 M3D4 124 483 4.61 140 431 2.39 M4D1 125 339 2.13 141 311 311 2.311 367 2.23 142 332 2.27 M4D3 127 360 2.60 143 344 2.27 M4D4 128 403 1.96 144 390 2.73 M3D1 M3D2 M3D3 M3D4 12 3 4 DDDD 1111 MMMM 12 3 4 DDD ^ M2M2M2 M2M2 M1 Μ2Μ3 1300 3 803 8901 601 4.91 4 854 4 601 4854 1 2 7 5 8 4 6 7 2 3 3 3 5 & 6 6 7 5 5 5 5 5 6 8 0 0 7 5 6 119 7 114 0 1.2.2.4.1.2.2.4. M. This paper size applies to China Standard (CNS) A4 specification (210X297 mm) -54- 533225 A7 B7 V. Description of the invention (52

Regal 2S0 / S5phr / 0 code sample number RSS1 (K) 〇r ^) sample code

SMRCV (K) M1 M2 M3 M4 M1D1 33 M1D2 34 M1D3 * 35 M1D4 36 M2D1 37 M2D2 38 M2D3 39 M2D4 40 M3D1 41 M3D2 42 M3D3 .43 M3D4 * • 44 M4D1 45 M4D2 .46 M4D3 47 32 585 D4 6.95 659 8.03 759 10.5 896 14.1 580 2.71 602 2.61 631 3.61 667 5.43 457 1.53 476 2.09 493 2.32 495 3.54 372 1.53 382 2.09 381 2.32 403 3.54 49505Y5253545556575859606i6263s 23l8n > 4l9w129975694f033ci5 < ci> < < 4 > < < 4 > < 4 > > < " > > 5444 ^ 3919425589399293 .9.2.2.0.177281588437 1.3.2.4.2.2.46.2.3.45.2.3.4.4. (Please read the precautions on the back before this page)

Table 1 8B

Regal 250 / 65Λ) RSS1 Code—Sample M ~ ⑼ Number (K)

Regal 250/75/0 number RSS1 MWe D (%) (K)

Regal 250/65/10 RSS1 Sample No. 〇r / 〇) (K) Printed by the Consumer Consumer Cooperative of the Central Standards Bureau of the Ministry of Economy

Ml M2 M3 M4 M1D1 M1D2 M1D3 M1D4 M2D1 M2D2 M2D3 M2D4 M3D1 M3D2 M3D3 M3D4 M4D1 M4D2 M4D3 M4D4 6566676869707.4.6687.48.48.58.48.58.48.58.38.1.998.1.998.1 3333 1138 1138 901 901 660 660 483 483 81 539 2.87 97 661 1.89 82 624 4.50 98 .702 2.69 83 685 4.17 99 741 3.14 84 763 14.35 100 822 5.24 85 484 4.32 101 593 0.91 86 512 2.96 102 572 3.48 87 557 4.71 103 642 4.23 88 605 4.85 104 664 5.35 89 429 2.27 105 507 2.65 90 446 2.68 106 544 2.96 91 466 3,46 107 535 3,69 92 491 6.22 108 524 3.27 93 368 2.11 109 416 1.85 94 372 3.13 110 413 3.18 95 375 2.92 111 418 6.96 96 388 2.92 112 441 6.46 This paper size applies to Chinese National Standard (CNS) A4 (210X297 mm) -55- 533225 A7 B7 V. Description of the invention (53 Table 1 9 Table 21 (A) N326 / 55phr / 0 S6740 / 55phr / 0 RSS1

SMRCV RSS1

I Item code ## 123 ^ -123412341234 I3WDDD1 > DDDI > DDD [> DDD [> 111122223333WWWW MMMMMMMMMMMMiM ^ ii 5678901234567890 44444555 & & 5555S6 9499611783414733 4587141379187421 ... 03030450604723691485769 rK2cD32353521719i820-314a6 ^ -121c765667556645554444 OI5C4744172011610387556 ^ 13 € st4-4-693924755678902 f l1c97 & cia6756 & 655a54455 ···· ** 567 · 682 * 567890ί23456 666 Λ-666667777lt; 521062122686 # 1112112211221223 Code generation 1234123412341234 1112 £ 2wdddi > dddi &d; ddd1 > ddd1 > MWMiM1M1M1M1M1M2M2M2M2M3M3M3M3M4M4M4M4M4 Product code_sample number

D 234567890ί234567 4444444444444444 B07425I632315258791726 qe323t-5 < 33359401467889 < ^ 8755567444 & 44 ^ -43333 4213603550531206 234489512577243 & * ··· I · ♦ * ··· 1 · · · · 1111001200B Table 20 Table 21 (21 Printed by Daima N110 / 55phr / 0 Code S6740 / S5phr / 0 RSS1 SMRCV SMRCV Sample number (K) 〇 (y ^) Sample number (K) 〇 (yj Sample number Mw ^ (K) 〇 (%) M1 937 730 M1 876 M2 764 653 M2 754 M3 569 541 M3 574 M4 449 463 M4 444 M1D1 369 360 1.24 385 334 1.28 M1D1 428 433 0.25 M1D2 370 426 2.50 3B6 339 1.60 M1D2 429 441 0,4 490 2.69 3B7 372 1.42 M1D3 430 467 0.34 M1D4 372 618 4.68 388 413 2.80 M1D4 431 540 0.64 M2D1 373 340 0.69 3B9 309 0 · 72 M2D1 432 399 0.35 M2D2 374 356 0.85 390 314 1.17 M2D2 352 2433 2433 2433 1.27 M2D3 434 422 0.62 M2D4 376 433 1.17. 392 380 2.94 M2D4 435 469 0.44 M3D1 377 295 0.81 393 271 0.94 M3D1 436 340 0.44 M3D2 37 8 313 1.27 394 292 0.93 M3D2 437 363 0.81 M3D3 379 333 1.20 395 314 1.43 M3D3 438 377 0.89 M3D4 380 353 1.35 396 351 1.77 M3D4 439 403 0.86 M4D1 381 255 1.12 397 260 0.74 M4D1 440 1.64 363 363 0.93 M4D2 441 328 1.05 M4D3 383 287 1.30 399 284 1.49 M4D3 442 342 1.52 M4D4 384 316 1.67 400 297 1.83 M4D4 443 360 1.99 _-56 _ This paper size applies to China National Standard (CNS) A4 specification (210X297 mm)

533225 A7 B7 V. Description of the invention (54) Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy

Table 22 A) RSS1 code generation γ) 2) 3 > 4123μ112341234 A1fl213MDDDI > DDDI > DDD [> DDDl > mmmi ^ m1m1m1m1m2m2m2m2m3m3m3m3m3m4m4m4m4 Sample Z7f% 7 8.786 786 8.79 786 878,0086, 878,0079, 878,008,00,00,0079 7.46 181 598 8.56 182 602 3.89 183 697 6.40 1B4 659 5.71 185 473 2.03 186 506 1.66 187 562 1.94 188 559 4.33 189 :: 401 2.18 '190… 426 1.72 191 466 1.48 192 449 3.57 Table 22 (B)

Regal 660 / 45Λ) RSS1 code sample IW number (κ) ~ 1245 1 876 625 482 225 646 3.45 226 697 3.04 227 762 7.70 228 .830 6.75 229 574 4.79 230 • 589 3.02 231 636 6.41 232 675 '6.55 233 471 2.66 234 481 5.17 235 510 7.78 236 518 7.89 237 388 3.20 238 392 5.65 239 397 5.14 240 403 7.54 M2 i M3 'M4 M1D1 M1D2 M1D3 M1D4 M2D1 M2D2 M2D3 M2D4 M3D1 M3D2 M3D3 M3D4 M4D

Regal 660 / S5phr / 0

SMRCV sample secret D (% J number (K) _ 193 836 709 584 513 564 1.87 194 611 2.50 195 708 3.08 196 671 2.31 197 520 5.28 198 558 4.85 199 603 2.88 200 541 4.25 201 486 2.79 202 482 2.76 203 504 3.54 204 526 2.41 205 415 3.16 206 418 2.92 207 446 2.80 208 465 3.13

Rega 丨 660/65/0 RSSl Sample Coffee Know DT / ·) Number (K) i234567890i23456 2222222222222222 1245 876 625 482 563 638 691 790 469 507 558 543 420 426 468 471 335 344 344 361 -57- SMR10 Sample No. 90ί234567890ί234 2222222222222222 ^^ 26121 ^ 335053395534 r4c291078 & 686'599443467 76445565449533 ^ 4 ^ 33-33 4878272838909185 & 631859619494773 9.6.7.7.2.4.3.5.2.12.11112.

Regal 660/65/10 RSS1 Sample MiVjo / D (%) Number (K) _ 257 1245 876 625 482 639 1.63 258 699 3.55 259 814 5.44 260 764 11.25 261 572 2.77 262 580 4.39 263 610 5,51 264 638 7.29 265 474 4.10 266 485 5.72 267 502 6.24 268 495 7.13 269 390 5.02 270 365 5.88 271 410 7.45 272 388 7.59 533225 A7 V. Description of the invention (55 Table 23 (A)

Sample code RSS1 (K) 〇 (%) M1 M2 1060 811 M3 595 M4 466 M1D1 273 350 1.88 M1D2 274 476 3.40 M1D3 275 459 2.70 M1D4 276 665 2.70 M2D1 271 323 0.40 M2D2 278 371 0.73 M2D3 2D3 1.42 M3D1 281 278 0.47 M3D2 282 304 0.83 M3D3 283 323 0.82 M3D4 284 360 1.06 M4D1 285 251 0.61 M4D2 286 266 0.51 M4D3 287 273 0.64 M4D4 288 282 0.53 Table 23 (B)

N234 / 4S / 0 RSS1

N234 ^ Sphr / 0 SMRCV SMR10 for Dpi) Number (K) _ 289 845 712 577 477 312 0.61 290 317 0.64 291 361 1.03 292 419 1.56 293 304 0.76 294 306 0.72 295 318 0.74 296 357 1.30 297 260 0.53 298 272 0.65 299 295 0.58 300 302 1.14 301 244 0.53 302 253 0.81 303 266 0.62 304 296 0.88 Sample number (K) Dm 743 621 445 388 305 325 0.78 306 363 1.66 307 400 1.89 308 459 1.73 309 294 0.54 310 321 1.24 311 354 1.28 312 363 1.39 313 260 0.69 314 268 0.48 315 289 1.38 315 303 0.78 317 236 1.00 318 239 0.77 319 257 0.72 320 268 1.30 (Please read the note on the back first) Customs code N234 / 6SAJ RSS1 ^ MWmo, D (Vo) Code (K) N234 / 6S / 10 RSS1 Sample code Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (K) M1 1185 M2 828 M3 623 M4 462 M1D1 321 • 507 7.33 M1D2 322 598 8.15 M1D3 323 731 8.97 M1D4 324 772 12.02 M2D1 325 486 3.48 M2D2 326 479, 5.44 M2D3 327 527 5.51 M2D4 328 566 7.70 M3D1. 329 419 0.88 M3D2 330 423 1.24 M3D3 331 431 2.55 M3D4 332 458 4.03 M4D1 333 341 0.62 M4D2 334 338 1.13 M4D3 335 319 1.37 M4D4 336 354 2.06 7890ί23-456789ΰί2 3 3 3 4 ^ 4 ^^ 4445-t4a55 3333 ^ 3 ^ 3-33333-3-333 35832689658537201464344 1G70-22235702G2263 4970245508828173 Λο 1 9.Z.3-6 · 4 · 5.78.9.1.89.8 35.89.3.3.4.5.1.1.2.3.1.1.2.3. K832585752492630 5 3 1 7 182269753959-4981 ^ 6790 1186434562334-2233-2223 34 · 567890ί23 ^ · 5678 5,5 ^ 55555δ < 06 & 6-δ6δδ 3333333333333333 1869835764913991 5643523381158934 5.7.98.0.11.2.0.1.2.2.0.0.1.2.-This paper size applies the Chinese National Standard (CNS) Α4 size (210 × 297 mm)- 58- 533225 A7 B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. 5. Description of the Invention (56) Lightweight Specific Example Examples Prepare another sample of the elastic composite according to the present invention. In particular, the apparatus and steps substantially following Example A above were used to make a series of natural rubber elastic composites according to the present invention. This elastic compound contains a natural rubber field latex from Malaysia, which has the properties shown in Table 24 below. Each of the elastic composites further contains carbon black having the morphological properties (structure and surface area) of the region 1, 11 or 111 of FIG. 8. In particular, the following carbon blacks are used: Regal ® 660, N234, N236, N110, Regai (R) 250, N330, Black Pearl ® 800, Sterling ® 6740 and N351. The carbon black is filled in the range of 30 to 75 phr 'and the extender oil is filled in the amount of 0 to 20 phy. The manufacturing details of the rubber-elastic composite samples 1 to 3 are shown in Tables 2 to 5 below. As shown above, the apparatus and procedures used to prepare the elastic compound No. 1-32 are roughly in accordance with Example A, including the master batch formulation additives shown in Table 2. A more detailed description of the apparatus and procedures used for the elastic compound No. 1-32 is described below. 1. Apparatus Samples No. 1-32 of the present invention were prepared using a mother batch manufacturing apparatus substantially according to the apparatus of the present invention with reference to Figs. 1, 4, and 7. The slurry nozzles (see item 167 in Fig. 7) and the lengths of the slurry nozzles of samples No. 1-32 (see item 168 in Fig. 7) are given in Table 25. The condensing zone of the device has four zones of increasing diameter from the mixing zone to the discharge end. The diameters and axial lengths of the four zones (the first zone is partially in the mixing head and partially sealed in the extender) are described in Table 25. There is a good axial shortness between the zones. 2. Preparation of carbon black slurry The carbon black bag is mixed with deionized water in a carbon black slurry tank equipped with a stirrer. Stirring -59- This paper size applies the Chinese National Standard (CNS) Α4 specification (2 丨 〇 > < 297 mm) (Please read the precautions on the back before ^^ this page). _ Π Re-order

Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 533225 A7 B7 V. Description of the invention (57) The device breaks the sheet into pieces to form a coarse carbon black slurry. The concentration (e.g., weight percent) of carbon black in the carbon black slurry of each sample is given in Table 25. In operation, the slurry is continuously pumped to the mill by an air film pump to initially disperse. The slurry is then fed to a colloid mill via an air film pump, which is fed to a homogenizer via a forward cavity pump, especially the M210 microfluidizer from Micromotion International. A microfluidizer produces a finely ground slurry. The slurry flow rate from the microfluidizer to the mixing zone is set by the microfluidizer pressure. The microfluidizer is a high-pressure positive displacement system. Polymer flow rate is monitored with a Micromotion® mass flow meter. The pressure of the carbon black slurry fed to the homogenizer and the homogenizer output pressure (all pressures are psig) are given in Table 25. The carbon black slurry is fed from the homogenizer to the accumulator to reduce any change in slurry pressure at the tip of the slurry nozzle in the mixing zone. The pressure and flow rate of the slurry tip of each sample fed to the slurry nozzle at the mixing zone are given in Table 25. 3. Latex Conveying · Latex is packed in 5 5 gallon feed buckets. The antioxidant emulsion is then added to the latex before loading. Add antioxidants including Sanonflexyl Phosphite (TNPP) and Santoflex® 134 (alkylaryl p-phenylene diamine mixture) in the amounts shown in Table 25. Each antioxidant is prepared by using 4 parts of potassium oleate per 100 parts of antioxidant, and adjusting the emulsion to a pH of about 10 with potassium hydroxide, such as a 40% by weight emulsion. If present, extender oil is added in the amount shown in Table 25. A fill pump was used to move the 'latex from the feed tank to the mixing zone of the coagulation reactor. Latex flow rates and velocities are shown in Table 25. The latex flow rate is automatically measured using the Endress + Hauser mass flow meter. By maintaining an appropriate ratio of latex feed rate to carbon black slurry feed rate, the desired carbon black fill is obtained. -60- This paper size is in accordance with Chinese National Standard (CNS) Α4 size (210 × 297 mm) (Please read the notes on the back before ^^ this page) A7 B7 V. Description of the invention (58) 4. Carbon black and latex mixed Carbon black slurry and latex are mixed by transporting the latex to the carbon black slurry. During transportation, carbon black is tightly mixed into the latex, and the mixture is agglomerated. The soft, wet sponge leaving the condensate reactor is the condensate. 5. The water content of the wet debris discharged from the dehydration self-condensation reactor is shown in Table 2. 31/2 inch diameter) dewatering. In the extruder, the wet chips are compressed and water is squeezed out of the chip and passed through a slotted barrel of the extruder. The final chip moisture of each sample of the present invention is shown in Table 25. 6. The dried and cooled dehydrated chips fall into the second extruder, where they are compressed and heated again. The water is dried when the chips are expelled through the template of the extruder. The product outlet temperature and moisture content are shown in Table 25. Hot dry crumbs are rapidly cooled (about 20 seconds) to about 100 ° F by a powerful air-drying vibration conveyor. Table 24 Natural rubber latex properties Latex type source Additives% Dry rubber% Total solids% Ash nitrogen ppm Volatility Fatty acid concentrate TITI latex 0.35% NH3 ZnO, TMTD 0.1% HHS 60 62.0 0.15 0.29 0.022 field latex RRIM3, 9/94 0.15% HNSC 0.3% NH3, ZnO, TMIDb 28.4 34.2 0.38 0.366 0.052 a. RRIM is the Malaysian Rubber Research Institute b . ZnO / TMTD: used for biological preservation, Normally 0.025% of 1 ·· 1 mixture c. HNS ·· Hydroxylamine neutral sulfate, Menner viscosity stabilizer-61-This paper size is applicable to China National Standard (CNS) A4 (210X297 mm) (Please Read the notes on the back before ^^ this page)

533225 A7 _____B7 V. Description of the invention · (59) m

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co ^^ f ^ eoin0. τ-βΟΟί * '-. f ^ OCDCOCOOD ^ riOf ^ OCDrOeOCDCVICO ^ r-eO ^^-OC〇 ^ 2J2 < »a > C〇g bl * nmgcDCDCDN bl NOOCDCONOOCO bl NCDCDfOCOCOCO —Ibri {υ cdcdcDcdiricdVVcoi ^ WVVtoiriiOcdWV ^ voiricDiriuS ^ Vcicsicsirvi (Please read the precautions on the back before f. 〇 〇 〇〇〇〇〇 oooooooooooooop 〇〇〇〇〇〇〇〇〇1 c〇c〇c〇c〇c〇cr) c〇c〇c〇 «〇c〇c〇c〇c〇c 〇f〇c〇c〇c〇c〇c〇c〇r〇f〇c〇r0c〇c〇r〇 potential "» »_ ··· _ ·· # · · _« ····· ♦ ·· »«. ♦ 参 >> «Appealing from 100,000,000,000,000,000,000,000,000,000,000,000,000, and 100,000-this page is still on this page ) Order to (N 4 CD 卜卜 呀 OOOOCOfOCO ^ -OOCOOOO ^ -COCO ^ fCOT-xixixi inchxi cocococo «^ 文 寸 ^ • 卜卜卜 COOONtncOCOCViCsiOjCOCOCOONCO inch × ΤτΤτΤ inch COCDCDCD COCMCMCOCOCOCOCOCOCOcoco ^ coff Yeah

Real I CD CVI 04 CO CJ 04 04 04 od co ^ & n in in ui C \ | O ^ r- CO tfi 0 ^ < ^ 卜卜 Ι ^ Γ ^ Γ ^ < 〇 € 0τ-Γ > 4 ^ -Production by factory ^ uS & n uS to in id ui in to uS in in ^ to uj & ri to id i〇 Employees' Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs print 03s OSS ΟΘΓΟZ OSS 09¾ 0 s OSCNI OS 0109 ^ QSST-§ Inzs scol · 0091 ^ 00? OOH 00H § 4nzi2 002 009 000 00® se ssoos ^ oos ^ r · St s § i Is ~ s mildew $ s% xf4 This paper size applies Chinese National Standard (CNS) A4 specifications (210 X 297 mm) -64- 533225 A7 B7 V. Description of the invention (62 ro 60 zo 90 yo zo CNIO εο CNIO zo εο CNIO s εο s 0.0 ro 90 two ro oo ro εο 090 coo cslo so s 5 < ηε ose 0 $ os々__0 UJ ~ 1 Sentence #w 载 璲 ss rococo OJ CO CO MEDIA STREET MEDIA cococorocsicoroco,…… )

P ®z SCO 咚 4 咚 欢 咚 _B, ί) ~ ς < ΝΙ <-CB CO m 〇 On qqo.co Inch 1 h: ^ CO d © 1 o * 1 · «) Central Bureau of Standards, Ministry of Economic Affairs Printed by employee consumer cooperatives: Swallow- ^ CD 卜卜 0 > {^ 曦 < 0 卜 OCO 卜卜 T-〇504CN4Cs40〇l〇4〇 ▼-Corpse < € 0 ▼ -xibu CVICOCO ^-X Coe, CDCD10, COBCD, COOCD, 0 > 0 > 0 > 0 > 0 > 〇0 > 〇! 〇00, COCOCD ^ T-CMCO,.卜卜卜卜卜 卜卜卜卜卜 卜卜卜卜卜 卜卜卜 00 卜 COCO 卜卜卜卜卜 卜卜卜卜卜. This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm)- 65- 533225 A7 B7 V. Description of the invention (63) It should be noted that samples 2 and 3 were manufactured at the outlet of the microfluidizer, etc., with approximately no outlet pressure, to determine the large dispersion under adverse processing conditions. The excellent carbon black dispersion in the production of the master batch is verified by its macrodispersion quality and the molecular weight (MWSC) of the sol fraction. Table 26 below shows MWsol and macrodispersion of samples No. 1-32 of the present invention, and carbon black and oil (if any) for each sample. Carbon black filling and oil filling are shown in Table 2 as phr 値. (Please read the precautions on the back first, and then this page) Order the musk, printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs -66-This paper size applies to China National Standard (CNS) A4 (210X297 mm) 533225. A7, B7 V. Description of the invention (64) Table 2 6 The sol molecular weight and undispersed area of the sample of the present invention Sample number of the present invention i car filling / oil · m ^ (K) F (% j Printed by the staff consumer cooperative of the Central Bureau of Standards, Ministry of Economic Affairs 1 2 3 4 5 6 7 8 9 / 55Λ) Ν330 / 55Λ) Ν330 / 55Λ) R250 / 55/0 R250 / 65/0 R250 / 75/0 R250 / 65/10 BP800 / 55/0 N326 / 55/0 R660 / 55/0 R660 / 45 / 0 R660 / 65/0 R660 / 65/10 N234 / 55/0 • N234 / 55/0 N234 / 55/0 N234 / 55/0 N234 / 45/0 N234 / 65/0 N234 / 65/10 N1'10 / 55/0 Ν351 / 33/20 S6740 / 55/0 Ν234 / 48/5 Ν234 / 53/5 Ν234 / 58/5 Ν234 / 63/5 Ν234 / 68/5 Ν234 / 49/5 Ν234 / 54/5 Ν234 / 63/5 Ν234 / 65/5 .26.54.40.081603021420120504021510.151017 ^ 011171010051212131612161720 ooooo.odo.do.dooo.o.oo.oo.oo ^ ooooooodo.do.0.0.2-§sggHH88§l g: 0§§97 ^: 5 (Please read the precautions on the back and then this page) Order M-67-, this paper size applies the Chinese National Standard (CNS) Α4 size (210X297 mm) Central Ministry of Economic Standards Printed by the Bureau's Consumer Cooperative 533225 A7 B7 V. Description of the invention (65) The results of all samples of the invention with 55 phr carbon black filling are shown in the semi-logarithmic slope of Figure 9 and the corresponding series of the above-mentioned natural products manufactured by dry mixing technology Macrodispersion of rubber control samples and MWSQl 値. At least one data point of the present invention sample containing 55 phi * of each carbon black fill is shown in Figure 9 and all control samples with 55 phr carbon black fill. (Control samples 401 to 412 using 20 parts of 33 phr N531 carbon black extender oil, also shown in Fig. 9) It can be seen in Tables 26 and 9 that the samples of the present invention have excellent macrodispersion. In particular, the samples of the present invention have a D (%) 値 generally lower than 0.2%, even higher than · 85 × 106 at MWSQlQ, while the control sample never obtained this excellent macrodispersion at any MWS () 1. Therefore, the data shown in Fig. 9 clearly shows that the novel macromolecular compound has a wide dispersion quality of MWSQl 値, which is far superior to those obtained by using comparable ingredients in known dry mixing methods. The symbols used for each data point shown in Figure 9 and Figures 10-25 for later discussion are explained in the legend below. Schematic illustration Figure 9 Dispersion quality and MW sol of NR master batch ※ Control samples 177 to 224 ▲ Control samples 273 to 320 Extension control samples 145 to 176 △ Control samples 369 to 400 〇 Control samples 33 to 64 X Control samples 1 to 32 ❿Control samples 113 to 144 ', ◊Control samples 412 to 443 ♦ Control samples 401 to 412 Samples of the present invention Figure 10 Dispersion quality and MW sol of NR master batch -68- This paper size applies Chinese National Standard (CNS) A4 Specifications (210X297 mm) (Please read the precautions on the back page first) Order

533225 A7 B7 Printed by the Consumer Cooperatives of the Central Bureau of Standards, Ministry of Economic Affairs V. Invention Description (66) (Region I) ※ Control Samples 177 to 224 * Inventive Sample 10 Class Control Samples 145 to 176 · ... Inventive Sample 9 〇Control samples 33 to 64 □ Inventive sample 4 XControl samples 1 to 32 ggInventive sample 1 • Control samples 113 to 144 Inventive sample 8 Figure 11 Dispersion quality of NR master batch and MW sol (region II) ▲ Control Samples 273 to 320 Samples of the present invention 14 △ Control samples 369 to 400 □ Samples of the present invention 21 Figure 12 Dispersion quality and MW sol of the NR master batch. (Region III) ♦ Control samples 401 to 412 Samples 22 of the present invention ◊ Control sample 412 To 443 □ Sample 23 of the invention Figure 13 Dispersion quality and MW sol (N330 carbon black, 55 phr) of NR master batch • Control samples 1 to 32 Samples 1 to 3 of the invention Figure 14 Dispersion quality and MW of NR master batch sol (REGAL 250 carbon black) -69- This paper size is applicable to China National Standard (CNS) A4 specification (210X297 mm) (Please read the precautions on the back before this page) Order

533225 A7 B7 V. Explanation of the invention (67) • Control samples 33 to 64 Samples of the invention 4 〇 Control samples 65 to 80 □ Samples of the invention 5 ◊ Control samples 81 to 96 △ Samples of the invention 6 ♦ Reference samples 97 to 112 ▲ 本Invention Sample 7 Figure 15 Dispersion quality of NR master batch and MW sol (BLACK PEARL 800 carbon black, 55 phr) • Control samples 113, to 144 Samples of the present invention 8 Figure 16 Dispersion quality of NR master batch and MW sol (N326 Carbon black, 55 phr) Call for reference samples 145 to 176 Sample 9 of the present invention Figure 17 Dispersion quality of NR master batch and MW sol (REGAL 660 carbon black) Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (Notes on this page)

• Control samples 177 to 224 Inventive samples 10 〇 Control samples 225 to 240 □ Inventive samples 11 ◊ Control samples 241 to 256 △ Inventive samples 12 ♦ Control samples 257 to 272 ▲ Inventive samples 13 Figure 18 NR master batch Dispersion quality and MW sol (N234 carbon black) -70- This paper size is applicable to Chinese National Standard (CNS) A4 (210X 297mm) 533225 A7 B7 V. Description of the invention (68 瘳 Control samples 273 to 320 Samples of the invention 14 to 17 〇 Control samples 337 to 352 □ Inventive samples 19 ◊ Inventive samples 321 to 336 △ Inventive samples 18 ♦ Inventive samples 353 to 368 ▲ Inventive samples 20 Figure 19 NR master batch dispersion quality and MW sol (N110 Carbon black, 55 phr) • Control samples 369 to 400 Sample 21 of the present invention (please read the precautions on the back first, then this page) Etatu 20 Dispersion quality of NR master batch and MW sol (N351 carbon black, 33 phr) _Control samples 401 to 412 Samples of the present invention 22 Figure 21 Dispersion quality of NR master batch and MW sol (STERLING 6740 carbon black, 55 phr) Order • Control samples 412 to 443 Samples of the present invention 23 Figure 22 MW sol against cracking growth rate Effect (with 55 phr filled N234 carbon The NR compounds)

Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs for reference samples 273 to 288 Sample 16 of the present invention Figure 23 Effect of MW sol on cracking growth rate (containing 55 phr filled N326 carbon black NR compound) > Control samples 145 to 160 〇 Sample No. 71 of this invention-This paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) 533225 A7 B7 V. Description of the invention (69) Printed by the Consumers Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 24 MW sol on cracking The effect of growth rate (including 55 phr filled REGAL 660 black NR compounds) This pair ΐ 7777 to 192 □ this hair gjxen product 10__ Figure 25 NR compounds containing N234 carbon black in the different filling ^ (Strain bending at 60 ° C) Fenben # 7 rain samples 24 to 28 〇 samples 29 to 32 of the present invention □ control samples 444 to 450_ Figure 3 0 NR master batch containing biphasic (carbon black / silica) aggregate The dispersive quality of the sol fraction and the MW 1¾7 according to samples 451 to 458 _ samples 33 of the present invention 〇 samples 459 to 466 □ samples 34_ of the present invention Figure 31 NR master batch containing a mixture of carbon black and stone Dispersive quality of the sol portion of the raw material and MW stone control sample 491 to 498 _ sample of the present invention 38 〇 control sample 483 to 490 □ sample of the present invention 37 Θ control sample 475 to 482 sample of the present invention 36 • control sample 467 to 474 'sample of the present invention 35_ Figure 9 of the elastic composite of the present invention The macrodispersion is explained by the following equation: 〇 (%) < 0.2% (1) When MWSC) 1 is less than 0.45 X 106; and (Please read the precautions on the back before ^ pages). Order

-72- This paper size is applicable to China ^^ (CNS) A4 specification (210X297 mm) 533225 Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 _________ B7 V. Description of the invention (70) —-— l〇g (D) < 10 g (0.2) +2.0 X [MWso1. (0.45 x 1〇6)] x 10-6 when 0.45xi0 < MWs () 1 < 1.1x. From the above discussion, it can be understood that in the above description, the 10,000% macrodispersion D (%) is the percentage of undispersed area of defects larger than 10 microns. It can be seen from Fig. 9 that D (%) equal to 0.2% is the critical macrodispersion quality for the area of natural rubber dry master batch ΐ π and all carbon blacks. That is, the dry kneaded master batch did not obtain a huge dispersion quality of G.2% at any bribe, even after being thoroughly mixed to reduce the MWsol to below 0.45 X 106, as described in Equation ⑴ above. When the MWs of the dried master batch control sample shown in FIG. 9 is between MWs × 45 × miixi, the dispersion quality is even worse, and relatively, the dispersion quality of the sample having the MWsol in this range is maintained excellent. As shown in FIG. 9, the preferred embodiments having MWsq1 with a range of 045 × 6 to ι · ι × 106 do not exceed the limit of better macro-dispersion of 0.2%. In this regard, it should be understood that the preferred embodiment seen in FIG. 9 (and in the other figures discussed below) on the χ axis (ie, at% 疋 D (%) 値) can have a data point of 0.1%. Or even better (ie, lower) d (%) 値 of great dispersion quality. The carbon black sample of the region I includes a sample of the present invention of carbon black having the morphological properties (ie, structure and surface area) of the region I of FIG. 8 and the above-mentioned corresponding control sample made from the carbon black of the region I. Compare in drawing. In particular, Fig. 10 shows the macrodispersion and MWS of the sample of the present invention and the corresponding control · sample.値, which is filled with carbon black Regai® 660, N326, Regal® 250, N330, and carbon black pearl® 800 in the range of 30 phr to 75 phr, and an incremental oil in the range of 0phl ^ 20 phr . For all samples of the invention, see excellent in Figure 10. -73- This paper size is applicable to China National Standard (CNS) A4 (210X297 mm) (Please read the precautions on the back before ^^ this page) . (Re-order

533225 A7 B7 V. Description of the Invention (Carbon Black Dispersion printed by the Consumers 'Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs' means a preferred embodiment of the elastic compound according to the present disclosure. All samples of the invention are advantageously located in FIG. Below line 101, and all control samples have poorer dispersion, which is higher than line 01. In fact, even the most difficult-to-disperse carbon blacks from region I are included, as shown in Figure 1 The examples are all lower than 3% < B (%) 値. The best specific examples all have no more than .2% to D (%) 値, even at a MWSC which advantageously exceeds 7 x 106 (1). The data of π in Figure 10 clearly shows that in a wide range of MWw 値, the area here does not include the area. The great dispersion quality of the novel elastic compound of carbon black is far superior to the use of comparable ingredients by the dry master batch mixing method. Winner. The macrodispersion of the elastic composite of the present invention shown in FIG. 〇 is illustrated by the following equation: D (%) < 1.00 / 0 ⑺ When MWsol is lower than 0.7 × 10; and 10 g (D) < 10 g (i.〇) +2.5 X [MWs〇r (0.7x 1〇6)] x ι〇- ^ (4) When 0.7x 1〇6 < MWsc > 1 < 1.1 χ ι〇6 Time. It should be understood that D (%) is the percentage of undispersed area where defects larger than 10 microns are measured, and 1% is the critical macrodispersion quality for all carbon blacks in Region I of the natural rubber master batch according to the present invention. That is, the dry kneaded master batch did not obtain a macrodispersion quality of 1.0% or better at any MW, and after fully drying to reduce _Ws〇1 to less than 7x106, when as described in equation 方程 above, Figure 1 shows the dry master batch control samples 1 ^ 1 to 3. When 1 is between 〇7 < 106 and 1 ^ 106, the fractional quality is even worse. In contrast, the dispersion quality of the samples of the present invention having the MWsol in this range is maintained excellent. The preferred embodiment of Fig. 10 between J You · 7X106 and ux106 is below the limit of better macrodispersion. It can be seen that the present sol containing carbon black derived from the zone

X-Wrapping (Please read the precautions on the back first)-(Next page)

-74-This paper size is in accordance with Chinese National Standard (CNS) A4 (210X297 mm 533225 Printed by A7 of the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. V. Description of the invention (72) The elastic compound provides so far disperse quality and The balance between MWsols. The region II carbon black sample includes a carbon black sample of the present invention having the morphological properties (ie, structure and surface area) of the region II of FIG. 8 and the above-mentioned corresponding control sample made from the region π carbon black. Comparison in a semi-logarithmic plot of 11. In particular, Figure 11 shows the macrodispersion and MWs of the sample of the present invention and the corresponding control sample. 値, which is filled with carbon black ranging from 40 phr to 70 phr containing carbon black like "and It is filled with incremental oil in the range of 0 phr to 10 phi *. In Figure n, excellent carbon black dispersion is seen for all samples of the present invention, indicating a preferred embodiment of the elastic composite according to the present disclosure. The present invention The sample is advantageously located below the line lu in the figure, while all the I control samples have a poorer dispersion, which is higher than the line ln. In fact, the inclusions derived from the region shown in FIG. Examples fall below .3% meaning D (%) 値. The best embodiment is in any MWs. 値 値 has D (0 / 〇) 値 which does not exceed 2%. The data shown in Figure U clearly show In the wide range of MWSC) 1 値, it is revealed here that the macrodispersion quality of the novel elastic compound I containing region 11 carbon black is far superior to that obtained by using comparable ingredients in the prior dry mixing method. The present invention shown in FIG. 11 The macrodispersion of the elastic compound is described by the equation: D (%) < 0.3% 1 < (5) When 1 ^ > ^. 1 is less than 0.35 \ 106; and log (D) &log; log ( 0.3) +2.8 X [MWs〇r (.35 X 1〇6)] χ 1〇-6 When 0.35 x 106 < MWS〇1 < 1.1 χ 106.) It should be understood that .30% of D (%) Is the zone of the natural rubber master batch according to the present invention -75- This paper size applies the Chinese National Elephant Standard (cns) (please read the precautions on the back # 1 ^ 5 ^ this page), π. Zhen. 533225 A7 Β7 Consumption cooperation between employees of the Central Bureau of Standards, Ministry of Economic Affairs, Du printed 5. Invention Description (73) All of the critical black macrodispersion quality, and 0.35X106 is the critical mwsq1 値. That is, the dry master batch is in any mw ^ did not get 0 %% or better Bulk quality, even after being thoroughly dry-mixed to degrade to less than .35 × 106, as described in equation (5) above. When the MWsq ^ 〇35χ106 of the dry master batch control sample shown in Figure 11 is Between 1 and xi〇6, the dispersion of tadpoles is even worse. On the contrary, the dispersion quality of the sample 6 of the present invention having a MW in this range remains excellent. The figure " shows 35 x 106 to ΐ x 10 < MWsq1 (the preferred embodiment falls below the 2% better macrodispersion limit = below. It can be seen that the bomb of the present invention contains a carbon black derived from region II. The sex complex provides a balance between the macrodispersion quality and MWSC) that have not been achieved so far. The region III carbon black sample includes a carbon black sample of the present invention having the morphological properties (ie, structure and surface area) of the region III of FIG. 8 and the above-mentioned corresponding control sample w produced by the region claw carbon black. Comparison in log plot. In particular, Fig. 2 shows the huge difference between the samples of the present invention and the corresponding samples. It is filled with carbon black in the range of 30 phr to 70 phr with carbon black 6740 and incremental oil in the range A 0 phi * to 20 phi *. In Figure 2, excellent carbon black dispersion is seen for all samples of the present invention, indicating a preferred embodiment of the elastic composite according to the present disclosure. All the samples of the present invention are advantageously located below 皋 121 in Figure 2 and all the control samples have a poorer dispersion, which is higher than that of Table 121. As a matter of fact, the preferred embodiment comprising the region claws which is not in FIG. 12 falls at or below D (%) 値 of 1%, even when it advantageously exceeds 3 > < 100 and even 7 × 106 MW ”. Shown in the picture! The data of 2 clearly show that, in a wide range, the new elastic compound containing the area m carbon black is revealed here -76- (Tin V Α Μ-, (Please read the precautions on the back before reading this page)

t ^ n · if ·-533225 A7 B7 V. Description of the invention (? 4) The quality of printed matter printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs is much better than that obtained by using comparable ingredients in the advanced dry mixing method . The macrodispersion of the elastic composite of the present invention shown in FIG. 2 illustrates the following equation: Knife 0 (%) < 0.!% When MWsol is less than 0.35 X 106; and log (D) < 10 g ( 〇.i) + 2.0 × [MWsor (0.30 X 1006)] χ 1〇-6-j ⑻ 0.30xi〇6 < MWsol < 1.150. It should be understood that .1% of D (%) is for all carbon blacks (critical macrodispersion quality, and 0 × χ 106) of region III1 of the natural rubber master batch according to the present invention are critical chambers. 値. That is, dry The master batch did not obtain a macrodispersity of 1% at any MWsc > i, even after being thoroughly dry-mixed to degrade MWw to less than 35 × ιδ, as described in equation (7) above. When FIG. 12 The dry master batch control sample] ^ 1 \ ^. When 1 is between 0.30 < 106 and 1.1 > < 106, the dispersion quality is even worse. On the contrary, it has a value in this range. The dispersion quality of the sample of the present invention of MWsq1 is maintained excellent. The preferred embodiment shown in FIG. 12 having a MWw of between 30xm6 and L1 xl06 falls below the 2% best macrodispersion limit, and In fact, it is at or below 0.1% D (%) 値. It can be seen that the elastic composite of the present invention containing the carbon black obtained from the region m provides a balance between the macrodispersion quality and MWsol that have not been obtained so far. From the above discussion, .8 to 12, the huge dispersion of the sample of the present invention, such as its MWsol 値 t function, is shown in Figures 丨 3 to 21 semi-log plot In particular, in Figs. 13 to 21, all the above-mentioned samples of the present invention containing a specific carbon black (in this case, limited to those specified in the carbon black charge) are plotted on a single half logarithm with the corresponding pair sol (read first Note on the back --- --- on this page)

-77- + Paper size applies Chinese National Standard (CNS) M specification (210X297mm) Printed by Central Standards Bureau of the Ministry of Economics & Beigong Cooperative Cooperative 533225 A7 ------- B7 V. Description of Invention (75) Shown together with the sample. (See the legends given above, which give the reference numbers of the samples of the present invention and control samples included in the drawings.) Therefore, Figure 13 shows the dispersion quality and MWsol of the present invention and control samples containing 55 phr N330 carbon black as described above. . The data shown in Figures 1 and 3 clearly show that, over a wide range of ..., the macrodispersion of the novel elastic complex of the present invention containing N3 3 0 carbon black has a much better inhibitory effect than the control sample. The macrodispersion of the elastic composite of the present invention including N33o carbon black shown in FIG. 13 is illustrated by the following equation: D (%) < 1% (9) When MWS () 1 is less than 0.6 X 1 〇6 Time; and ~ 10 g (D) < log⑴ + 2 · 5 X [MWs〇r (0.6 X 1〇6)] X 1〇 · 6 (ι〇) when 0.6X 1〇6 < MWso1 < 1.1 X 106 hours. The dry kneaded master batch did not obtain a macrodispersion quality of 10% at any time, even after thoroughly dry-mixing to degrade Mw ^ to less than 0.6 χ 〖00 (see above t10,000) Equation (9)). In a control sample containing 55 phr N33〇, MWsol was maintained between 1 × 106, d (% m straight or even higher, such as more than 4% undispersed area. Figure 14 shows that the above contains REGAL⑧25. Dispersion quality and MWsol of the present invention and control samples of carbon black. The selected present invention and control samples are shown in Fig. 14, which contains oil as described above. The data shown in Fig. 14 clearly show that in the wide range of tMWSQl 値The macro-dispersion and bulk quality of the novel elastic compound of the present invention containing REGAL⑧250 carbon black are much better than those of the control sample. The "dispersion of the macro-dispersion of the elastic compound of the present invention containing REGAL® 250 carbon black" is shown in the figure. Note: ^ D (%) < 1% (9) -78-This paper size is applicable to Chinese National Standard (CNS) Α4 size (210 X 297 mm) (Please read the precautions on the back before ^^ this page ), 1T 533225 A7 B7 V. Description of the invention (76) When MWsol is lower than 0.6X106; and log (D) < log (l) +2.5 X [MWs〇r (0.6 x 106)] X ΙΟ'6 (10) When 0.6 parent 106 < 乂 \ ^. 1 < 1.1 / 106. The control sample is not in any MWSC ^ 々 A macrodispersion quality of 1.0% or better is obtained, even after sufficient dry mixing to degrade MWsq1 to below 0.6X 106. In contrast, Regal® 250 carbon black is included and has a MWSC above 0.6X 106) 1 The elastic composite of the invention has excellent macrodispersion, such as D (%) below 0.2%. The properties and performance characteristics of the compounds of the present invention and control samples containing REGAL® 250 carbon black shown in Figure 14 are described in Table 27 below. It can be seen that the sample No. 4 of the present invention has exceptionally good resistance to lytic growth, as shown by its very low lytic growth rate of only 0.92 cm / million cycles. In fact, the samples of the invention are far superior to the corresponding control samples. It is believed to be mainly due to the better MWSC of carbon black in the samples of the present invention1 and the great dispersion quality, as discussed above. 0 Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. Standard (CNS) A4 specification (210X mm) 533225 Μ B7 V. Description of invention (77) Table 2 7 Compound properties of NR compound containing REGAL 250 carbon black filled with 55 phr £ 100 (psl) E300 (psi) tension ( ps〇EB ΓΛ)

Sample number Mennerium 3 3 60.63 55.35 18126 999.82 4090.24 675.0 Control 34 73.58 57.80 235.14 1293.88 3978.24 595.0 Control 35 81.49 58.65 243.66 126526 4103.41 613.0 Control 36 84.04 59.95 244.23 1215.87 3960.32 6035.05. 107.5 Control 757.5 216.75 1206.60 4023.65 620.0 Control 39 68.28 57.25 225.44 1256 * 23 4134.06 621.0 Control 40 77.40 59.10 255.15 1330,87 4059.01 597.0 Control 41 44.40 56.25 216.00 1214.78 4038.68 618.0 Control 42 47.96 56.50 214.53 492.5 290.5 * * , 07 4018 ^ 4 611.0 Control 44 50.10 56.60 210.50 1140.90 4058.33 638.0 Control 45 36.82 52.90 177.47. 982.86 3790.56 533.0 Control 46 • 38.23 54.50 198.63 Γ, 1111.04 3860.56 629.0 Control 47:; 35.35 54.60 199.03'.0.00 : 40:58 55.50 204.52 1139.94 3961.06 632.0 The present invention 4 • 57.00 218.18 1230.30 4036.30. 611.0 Sample number rebound (cm / million cycles) Tan δ @ 60 # C Wear < g)

Tan δ & o * c (please read the notes on the back before ^^ this page) Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs-System Control 33 64.50 2.00 * .- · 0.191 Control 34 64.55 1.83 0.182 Control 35 63.75 2.38 .0.192 Control 36 63.30 1.42 • 0.180 Control 37 • 64.65 3.00 Ό.168 Control 38 63.45 2.99 0.163 Control 39 .63.90 2.17 0.186 Control 40 62.30 1.69 0.182 Control 41 64.20 2.84 0.190 Control 42 64.20 3.24: 0.182 Control 43 64.50 3.52 0.177 Control 44 63.90 3.50 0.179 Control 45 63.80, 3.86 0.199 Control 46 64.30, 3.94 '0.191 Control 47; :: 64V35 3.81; 0.192 Control 48 ::: 63.65 •: U3.46r / :. · 0.180 Uninvented 4 :: 64: 70 • 0 · 92-: 0.190 75026405983574 65567 & 7786B89 & 0.182 0.148 0.091 0.083 0.091 0.0910.100 0.099 0.092 0.0930.102 0.1030.101 0.104 0.104 0.107 0.1060.110 0.096 This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 (Mm) -80- 533225 A7 B7 V. Description of the invention (78) Figure 15 shows the above invention containing BLACK PEARL® 800 carbon black with 55 phr filling. And control sample dispersion quality and MWS. !! . The data shown in Figure 15 clearly shows that the macrodispersion quality of the novel elastic composite of the present invention containing Black Pearl® 800 carbon black is much better than the control sample. The macrodispersion of the elastic composite of the present invention containing Black Pearl® 800 carbon black shown in Figure 15 is explained by the following formula. D (%) < 1.5% (11) When 1 ^ \ ^. When 1 is less than 0.65 / 106; and log (D) < log (1.5) +2.5 X [MWs〇r (0.65 X 106)] X ΙΟ'6 (12) When 0.65 x 106 < MWS〇1 < 1.1 X 106 hours. Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. The control samples did not achieve a macrodispersion quality of 1.0% or better at any MWSC) 1, even after being thoroughly dry-mixed to degrade MWSC) 1 to below 0.65 XI06. In contrast, the elastic composite of the present invention, which contains Black Pearl® 800 carbon black and has a MWsol higher than 0.65 X 106, has excellent macrodispersion, such as a D (%) lower than 0.2%. The properties and performance characteristics of the compounds of the present invention and control samples containing Black Pearl® 800 carbon black shown in Figure 15 are described in Table 28 below. It can be seen that Sample No. 8 of the present invention has exceptionally good resistance to lytic growth, as shown by its very low lytic growth rate of only 0.27 cm / million cycles. In fact, the samples of the invention are far superior to the corresponding control samples. It is believed to be mainly due to the better MWSC) 1 and macrodispersion quality of the carbon black in the samples of the present invention, as discussed above. ', -81-This paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) 533225 A7 B7 V. Description of the invention (79) Table 2 8 Fill 55 phr of NR compounds containing BLACK PEARL 800 carbon black with 55 phr Compound Properties Sample Number

Menner ML (1 ^ 4) Q100C E100 (P · 0 Tension eb (%) Control 113 Control 114 Control 115 Control 116 Control 117 Control 11 8 Control 119 Control 120 Control 121 Control 122 Control 123 Control 124 Control 125 Control 126 Control 127 Control 128 The present invention 8 110.5 66.4 345.0 1333.0 3878.0 598 109.0. 67.3 367.0 1427.0 4033.0 606 106.4 67.2 363.0 1311.0 3896.0 610 105.7 69.0 322.0 1202.0 3856.0 626 110.6 67.1 316.0 1400.0 4180.0 616 118.9 67.1 310.0 1395,0 3967.0 607 111.9 67.7 309.0 132 110.6 67.6 373.0 1188.0 .. 4199.0 653 114.7 66.3 287.0. 1262.0 4329.0 667 110.6 65.8 288.0 1223.0 4217.0 659 115.0 67.5 280.0 1282.0 4071.0 624 116.5 66.5 309.0 1388.0 4166.0 623 113.4 65.4 281.0 1274.0 3978.0 631 101.4 '66.8 280.0; 122420 1150. 105: 5 .: 66.4 262.0 4167.0 670 110.7 66.8 292.0 • 1301.0 4209.0 643 131: 3 · 62.5 227.0 1291.0 3418.0 532 Sample number, '; bounce, ···· / · solution growth rate (cm / million cycles) wear ( g) Tan δ @ 0.C Tan δ-@ 60 # C Control 113 · 44.7 3.14 0.14 8 0.281 0.184 # Photo 114 45.0 2.72 0.125 0274 0.185 4 Photo 115 47.0 2.54 0.163 0.233 0.171 Control 116 46.6 2.41 0.194 0.244 0.163 Control 117.4 40.9 4.56 0.0B6 0.327 0.214 Control 11 8 418 2.80 0.112 0.335 0.225 Control 119 41.7 4.33 0.091 0.321 0.216 Control 120 42.1 3.89 0.095 0.301 0.207 Control 121 39.2 3.38 0.075 0.312 0.256 Control 122 38.7 4.58 0.108 0.344 0.236 Control 123 40.2 4.79 0.103 0.329 0.232 Control 124 41.7 3.78 0.102 0.321 0.209 Control 125 38.9 3.40 0.076 0.352 0.248 Control 126 38.1 5.57 0.070 0.355 0.241 Control 127 38.2 4.79 0.073 0.346 0.254. Contrast 128 • η 39: 4 ·; ^ 3.40 0.113 0.357 0.23 4 · taste; Ό.27 0.130 0.297 0.199

-82- This paper is suitable for financial standards _ home standard (CNS) (21GX 297 male tT (Please read the precautions on the back before this page), tr

533225 A7 B7 V. Description of the invention (80) Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs Figure 16 shows the dispersion quality and MWsol of the present invention and the control sample filled with N326 carbon black at 55 phr. The data shown in Fig. 16 clearly shows that the macrodispersion quality of the novel elastic composite of the present invention containing N326 carbon black is much better than that of the control sample. The macrodispersion of the elastic compound of the present invention containing N326 carbon black shown in FIG. 16 is explained by the following equation: D (%) < 1% (13) When the percentage of 3.1 is less than 0.7 \ 106; And 10 g (D) < log (l) +2.5 X [MWsor (0.7 X 1006)] χ (Η) when 0.7 × 106 < MWSC) 1 < 1.1 X 100. .. Control samples at any MW. All of them obtained a macrodispersion quality of 丨 · 〇% or better, even after being thoroughly dry-mixed to degrade MWsq1 to less than 0.7 × 1〇ό. In contrast, the elastic composite of the present invention, which contains N326 carbon black and has a value higher than 0.7x106 tMW ^, has excellent macrodispersion, such as less than%). The properties and performance characteristics of the compounds of the present invention and control samples containing N326 carbon black shown in Fig. 16 are described in Table 29 below. It can be seen that Sample No. 9 of the present invention has exceptionally good resistance to lytic growth, as shown by its very low lytic growth rate of only 077 cm / million cycles. In fact, the samples of the invention are far superior to the corresponding control samples. It is believed to be mainly due to the better MWsol and macrodispersion qualities of post-black in the samples of the present invention, as discussed above.

Please read the back 5 and order I * 533225 A7 B7 V. Description of the invention (81) Table 2 9 Filling the compound properties of the NR compound containing N326 carbon black with 55 phr Sample number Menner, hardness E10 ° E3 00 tension EB ML ( 1 «^ 4) @ 100 # C (f» i) (psi) (psi) (%)

Control 145 64,6 60.5 Control 146 88 * 2 62.4 Control 147 91.7 63.3 Control 148 96.8 64.3 Control 14 $ 62.4 61.5 Control 150 67.7 62.6 Control 151 76.5 60.6 Control 152 79.4 63.6 Control 153 57.2 60.1 Control 154 57 «2 62.8 Control 155 57.3 62.2 Control 156 60.1 61.9 Control 157 45.1 61 * 2 Control 158 50.1: 60.6 Control 159 53.2 61.3T Control 160 50.5 62.6 Uninvented 9: 77.8 60.9 I 9Ό160679243085617 85921a8l2 (a & 2121O (3'7 23-3333.2a2333333la6772647 3718743647393780474685718718r916 111 87ΙΘ 7 7e7; 1111111 3921 548 4094 553 3991 528 4045 572 4029 552 4055 551 4015 575 3980 559 3968 579 3879 525 3975 556 3918 564 3768 533 3817 546 3886 563 3884 549 4167 593 (Please read the precautions on the back first (This page)

Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs

Tan δ @ 0.C Tan δ @ 60.C Control 145 57.8 2.84 1: 0.0952 0.225 0.129 Control 146 5B.1 2.52 0.0887 0.217 0.126 Control 147 57.6 2.03 0.0946 0.205 0.123 Control 148 56.3 1.63 0.0927 0.221 0.129 Control 149 57-2 3.39 0.0827 0 ^ 34 0.142 Control 150 56.8 2.77 0.0866 0.234 0.150 Control 15 1 55.6 2.61 0.0933 0.241 0.149 Control 152 54.5 2.79 0.0857 0,249 0.155 Control 153 55.4 3.12 0.0911 0.258 0.170 Control 154 56.0 3.35 0.0858 0.241 0.147 Control 155 55.4 3.63 0.0811 0.254 0.152 Control 156 54.9. 3.55 0.0906 0.261 0.153 Control 157.555.5 3.02 0.0931 0.254 0.149 Control 158 55.4 3.81 0,0914 0.249 0.150 Control 159 54.9 3.23 0.0933 0 · 240 0.158 Control 160 55 ^ 3.19 0.0942 0.246 0.163 Uninvented 9 58: 4 0.77 0.0939 0.225 0.136

This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) -84- 533225 A7 B7 V. Description of the invention (82) Figure 17 shows the above invention and control samples containing REGAL (trademark) 660 carbon black The dispersion quality and MWSQl. Selected invention and control samples are shown in Figure 17, which contains oil as described above. The data shown in Figure 17 clearly shows that in a wide range of MWS. Range, the macrodispersion quality of the novel elastic complex of the present invention containing REGAL® 660 carbon black is much better than the control sample. The macrodispersion of the elastic composite of the present invention containing REGAL® 660 carbon black shown in Figure 17 is illustrated by the following equation: D (%) < 1% (15) when MWsol is below 0.6 X 106; and-log (D) < log (l) +2.5 X [MWS〇1- (0.6 X 106)] X 10'6 (16) When 0.6 \ 106 < ^ \\ ^. 1 < 1.1 \ 106 hours. The control sample did not achieve a macrodispersion quality of 1.0% or better at any MWSQl, even after being thoroughly dry-mixed to degrade MWSQl below 0.6 X 106. In contrast, the elastic composite of the present invention, which contains Regal® 660 carbon black and has MWsq1 higher than 0.6X 106, has excellent macrodispersion, such as D (%) below 0.2%. The properties and performance characteristics of the compound 10 and various control samples of the present invention including Regal® 660 carbon black shown in FIG. 17 are described in Table 30 below. It can be seen that sample No. 10 of the present invention has exceptionally good resistance to lytic growth, as shown by its very low lytic growth rate of only 0.69 cm / million cycles. In fact, the samples of the invention are far superior to the corresponding control samples. It is believed to be mainly due to the better MWSQl and macrodispersion qualities of carbon black in the samples of the present invention, as discussed above. -85- This paper size applies to Chinese National Standard (CNS) A4 (210X 297mm) (Please read the precautions on the back first

Printed by the Consumers 'Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 533225 A7 B7 V. Description of the invention (83 Table 3 0 Compound properties of NR compounds containing REGAL 660 carbon black with 55 phr Sample number Control 177' Control 178 Control 179 Control 180 Control 181 Control 182 Control 183 Control 184 Control 185 Control 186 Control 186 Control 187 Control 188 Control 189 Control 190 Control 191 Control 192 The present invention 10 c • ο ο @ 1 4) II! 6 16140418713 τ · 1 1 7.7.50.39.30.9.6.2.4.5 : 1.8. 8 8Β89887677 & 5 6 8 02900004035021049 ····· * ·········· 13441912003211502 66 & & 6566666a6666a 32516253866123 1 9 1387t > 9127aa9CN9 9 4 2222212Z1111Z1 1 2 I l42s34H § 114202 'Tension eb (ps〇 (%) 4002 702 694 4016 644 4058 618 4098 661 3924 733 4134 696-4236 694 3768 717 4051 666 4157 720 4182 704 4240 674 4125 692 4189 710 4292 634

Sample number rebound cracking growth rate wear Tan δ Tan δ '__ (cm / million cycles) (g) @tTC @ 6CTC Printed by the Consumer Consumption Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 177 .. 54.6 0.131 Control 178 55.6 2.34 0.1649 0.194 0.129 Control 179 53.7 2.78 0.1620 0.200 0.140 Control 180 52.9 2.98 0.1385 0.220 0.153 Control 181 51.0 3.41 0.1189 0.257 0.185 Control 182 49.9 3.11 0.1076 0.270 0.194 Control 183 50.1 3.15 0.1086 0,254 0.192 Control 184 48.0 3.11 0.1085 0.264 0.208 Control 185 47.5 4.59 0.0937 '0.306 0.209 Control 186 48.5 4.06 0.1008 0.295 0.211 Control 187 47.7 3.53 0.1041 0.297 0.198 Control 188 47.8 3.79 0.0985 0.285 0.207 Control 189 47.5 3.71 0.0957 0.306 0.203 Control 190 46.8 4.14 0.0962 0.300 0.200 Control 191 47.4 0.226 Control 192 46.5 4.78 0.0897 0.301 0.226 The present invention 10; 48.2 0.69 0.0942 0.271 0.178 -86-

This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) 533225 A7 B7 V. Description of the invention (84) Figure 18 shows the dispersion quality and MWSC of the present invention and the control sample containing N234 carbon black mentioned above1 . Selected inventive and control samples are shown in Figure 18, which contains oil as described above. The data shown in Fig. 18 clearly show that, over a wide MWsol range, the huge elasticity of the novel elastic compound of the present invention containing N234 carbon black is superior to that of the control sample. The macrodispersion of the elastic composite of the present invention containing N234 carbon black shown in FIG. 8 is illustrated by the following equation: D (%) < 0.3% (17) When the MWsol is below 0.35 X 106; and log ( D) < log (0.3) + 2.8 X [MWsor (0.35 X 1006)] X 10-6 〇8) When 0.35 X 106 < MWSC) 1 < 1.1X106. The control sample did not obtain a macrodispersion quality of 0.3% or better at any MWSQ1, even after being thoroughly dry-mixed to degrade it to less than 0.35 × 0.6. In contrast, the elastic composite of the present invention containing N234 carbon black and having a ratio higher than 0.35 < 1/10 " 3 of 3.1 has excellent macrodispersion, such as not exceeding 0.3% /% or even 0.2%. D (%). The sample of the present invention containing N234 carbon black shown in FIG. 18 丨 The compound properties and performance characteristics of the bucket number and various control samples are described in Table 31 below. It can be seen that the sample of the present invention No. 4 has a particularly good The lysis growth resistance is as high as 2.08 cm / million cycles. Very low lysis growth rate 値 = (Please read the precautions on the back first, then this page).

Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs-87- 533225 A7 B7 V. Description of the invention (85) ) @ 100 # C Ε100 < _ Ε300 (f) i Tension (psf) EB (⑹ Control 273 94.5 68.0 386 2077 3718 511 Control 274 121.6 69.6 464 2299 3925 501 Control 275 121.4 72.5 564 2545 3994 472 Control 276 132.2 71.9 511 2259 3964 520 Control 277 79.6 68.5 468 2453 3857 469 Control 278 96.3 70.0 531 2499 3874 469 Control 279 108.6 69.0 406 2131 3863 532 Control 280 120.3 71 · 5 476 2273 3852 502 Control 281 76.4 69.7 556 2723 • 4027 451 Control 282 89.8 69.8 553 2574 3896 465 Control 283 93.6 69.6 506 2416 3867 475 Control 284 106.7 71.8 526 2384 3788 484 Control 285 73.3 69.3 529 2586 3831 444 Control 286: '· 79 · 2 · 69.5 531 2574 3856 456 Control 287 77: 8 丨 70.7 544: 2486 3834 461 Control 288 82.8 71.2 485 2295 3799 499 Uninvented 14 82.6: * 715 '500 2440 3883 531

Sample No. 1 rebound cracking growth rate wear T * ηδ TanS -l ·, (cm / million cycles). ⑹ @ 0 # c @ 6CTC (Please read the precautions on the back before this page) (re-order the central standard of the Ministry of Economic Affairs) Bureau Cooperative Consumer Cooperative printed Control 273 Control 274: Control 275 Control 276 Control 277 Control 278 Control 279 Control 280 Control 281 Control 281 Control 282 Control 283 Control 284; Control 285 Control 286 Control 287 Control 288 The present invention 14.9.2: 1: 9.18. 4.2.3.5.4.2.0.6.4.01 · 5.7.6: 6: 7.5.5.4.6.6.64.7.5.5.i4 · .5. 4444 (444 buckets 4 & 444-44444 2.14 1.84 1.70 1.21 2.22 2.40 2.00 1.81 3.10 2.33 2.41 1.99 2.99 2.85 .2.93 2.39 2.08 0.0563 0.05B3 0.0538 0.0620 0.0628 0.0534 0.0680 0.0646 0.0598 0.0537 0.0594 0.0579 0.0554 0.0551 0.0569 0,0647 .0.0698 0.285 0.274 0.284 0.270 0.370 0.299 0.306 0.298 0.293 0.307 0.309 0.304 0.272 0.273 0.205 0.316 0.310 0.183 0.173 0.172 0.173 0.173 0.173 0.196 0.198 0.198 0.174 0.182 0.186 0.190 0.178 0.172 0.187. 0.198 0.198 This paper size applies to China National Standard (CNS) Α4 size (210 × 297 mm) -88- Central Ministry of Economic Affairs Printed by the Consumer Bureau of the Associate Bureau 533225 A7 B7 V. Description of the invention (86) Figure 19 shows the dispersion quality and MWSC of the present invention and the control sample containing N110 carbon black filled with 55 phi * above. 1) Shown in Figure 19 The data clearly show that in the broad MWSQ1 range, the macrodispersion quality of the novel elastic composite of the present invention containing N110 carbon black is much better than that of the control sample. The elastic composite of the present invention containing Nilo carbon black is shown in Figure 19 Macrodispersion is described by the following equation: D (%) < 0.5% (19) when Mwsol < 0.35 X 106; and log (D) < log (0.5) +2.5 X [MWs〇r (0.6 X ΙΟ6) )] X 10 · 6 (20) When 0.35 X 106 < MWSC) 1 < 1.1 X 106. • Control samples did not achieve 0.5% or macrodispersion quality at any MWSC) 1, even after being thoroughly dry-mixed to degrade MWSC) 1 to less than 0.35 X 106. In contrast, the elastic composite of the present invention containing N110 carbon black and having MWS () 1 higher than 0.35 × 106 has excellent macrodispersion, such as D (%) lower than 0.2%. FIG. 20 shows the dispersion quality and MWSC of the sample No. 22 of the present invention containing N351 carbon black and a control sample filled with 33 phr as described above. The data shown in Figure 20 clearly shows that, over a wide range of MWSC) 1, the macrodispersion quality of the novel elastic composite of the present invention containing N351 carbon black is much better than the control sample. The macrodispersion of the elastic composite of the present invention containing N351 carbon black shown in FIG. 20 is illustrated by the following equation: D (%) < 0.3% (21) when Mwsol < 0.55 X 10δ; and log (D) < log (0.3) +2.0 X [MWsor (0.55 x 106)] x 10-6 (22) When 0.55 x 106 < MWSC) 1 < 1.1 X 1006. The control sample did not obtain a huge dispersion quality of 1.0% in any MWSQl, even at -89- This paper size applies the Chinese National Standard (CNS) Α4 specification (210X297 mm) (read the precautions on the back before reading this page) 1T

533225 A7 B7 5. Description of the invention (87) Dry and mix thoroughly to degrade MWscl to below 0.35 X 10th. In contrast, the elastic composite of the present invention, which contains N351 carbon black and has a MWSC higher than 0.35 × 106) 1, has excellent macrodispersion, such as an EK% lower than 0.2%). Figure 2 1 shows the dispersion quality and MWSC of the sample No. 2 and No. 3 of the present invention containing STERLING® 6740 carbon black at 55 phr as described above. The data shown in Figure 21 clearly show that, over a wide range of MWSC) 1, the macrodispersion quality of the novel elastic composite of the present invention containing STERLING® 6740 carbon black is far superior to the control sample. The macrodispersion of the elastic composite of the present invention containing STERLING® 6740 carbon black shown in Figure 21 is illustrated by the following equation:-D (%) < 0.1% (23) When MwSC) 1 < 0.3 X 106 ; And log (D) < log (0.1) +2.0 X [MWsOR (0.3 X 1006)] X 10.6 (24) when 0.3 / 106 < 1 ^ > ^. 1 < 1.1 \ 106 hours. Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. The control sample did not obtain a macrodispersion of 0.1% or even 0.2% at any MWSC ^, even after being thoroughly dry-mixed to degrade MWS. ! To below 0.3 X106. In contrast, the elastic composite of the present invention containing STERLING® 6740 carbon black and having MWSQl higher than 0.3 X 106 has excellent macrodispersion, such as D (%) of less than 0.2% and even less than 0.1%. The properties and performance characteristics of the compound No. 2 and No. 3 of the present invention containing STERLING® 6740 carbon black and various control samples shown in Fig. 21 are described in Table 32 below. It can be seen that Sample No. 23 of the present invention has exceptionally good resistance to lytic growth, as shown by its very low lytic growth rate of only 0.91 cm / million cycles. In fact, the samples of the invention are far superior to the corresponding control samples. It is believed to be mainly due to the better MWSC) 1 and macrodispersion quality of carbon black in the samples of the present invention, as discussed above. • 90 · CNS) (210X297 / ^) '533225 A7 B7 V. Description of the invention (88) Table 3 2 Compound properties of NR compound containing STERLING 6740 carbon black at 55 phr Sample number

Menner ML (1-t4) @ 10 (rC Hardness E100 (p «0 E300 (f» 0 'Tension (ps〇E5 (%) Control 412 Control 413 Control 414 Control 4 15 Control 4 16 Control 4 17 Control 418 Control 4 19 Control 420 Control 421 Control 422 Control 423 Control 424 Control 424 Control 424 Control 426 Control 427, Inventive 23 Sample No. 66.9 65.8 67.1 66.0 67.8 66.0 67.8 65.8 66.5 66.5 65.5 66.9 68.1 64.8 467.0 469.0 462.0 492.0 521.0 502.0 534.0 540.0 515.0 488.0 548.6 487.0 541.0 524.0 546.0 554.0 453: 6 2308.0 2314.0 2243.0 2260.0 2460.0 2468.0 2372.0 2418.0 2330.0 2382.0 2310.0 2440.0 2440.0 2440.0 2440.0 2241.0 3519 3655 3613 3572 35S4 3445 3604 3620 3468 3375 3549 3452 3397 3474 3428 3322 3324 451 479 472 477 445 436 453 475 444 440 442 466 425 445 446 435 443

Rebound

If

Tan δ @ 0 # C

Tan δ @ 60.C Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 412 Control 4 13 Control 414 Control 415 Control 416 Control 417 Control 418 Control 419 Control 4201 Control 421 Control 422: Control 423; Control 424: Control 425; ' Control 426 Control 427 The present invention 23: 59.8 .60.0 • 59.3 58.8 60.3 60.0 59.3 57.5 60.0 58.8 59.8 56.8 58.3 '! 58.8 58.0 56.9 57.3 5.04 3.63 3.96 4.56 5.67 4.67 4.23 3.22 4.23 3.84 3.98 3.85 4.54 3.65 3.07 3.25 0.91 .0.127 0 : 128 0.126 0.12 0.117 0.112 0.125 • 0.122 0.131 0.127 0.126 '0.12 0.131 0.129, 0.134 0.126 • 0.1642 0.202 0.203 0.208 0.217 0.188 0.202 0.204 0.218 0.204 0.206 0.206 0.210 0.213 0, 200 0.207 0.211 0.217 0.204 0.207 0.107 0.108 0.114 0.118 0.194 0.094 0.104 0.105 0.117 0.099 0.105 0.105 0.105 0.117 0.104 0.100 0.110 0.115 0.124 This paper size applies to the Chinese National Standard (CNS) A4 specification (210X297 mm) 91-Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 533225 A7 B7 V. Description of the invention (89) Additional examples ·· Matured samples matured and tested many of the aforementioned master batch samples, including Selecting the sample of the present invention and the corresponding control sample. Specifically, the samples were mixed using the formulation of Table 9 in accordance with Phase II of Table 8 above to make the final compound. The final compound in each case is then cured in a mold at about 150 ° C using standard techniques until it is substantially completely cured. The performance characteristics of the cured samples were measured by the above-mentioned measurement techniques, i.e., using a rotary bending machine in accordance with ASTM D3629-94, to determine their respective cracking growth rates. Rotary bending machines for measuring lysing growth are commercially available. For example, it was discussed in the Proceedings of the International Rubber Conference 1995 (Kobe, Japan), Paper 27A-6 (pp. 472_475). This compound was tested at 100 ° C and at a 45 ° bending angle. Those skilled in the art generally accept that the cleavage growth rate in this compound is affected by the amount of dispersed mass molecules of natural rubber and carbon black, that is, the MWSQ1 and D (° / 〇) 値 of the compound. Higher MWSC) 1 is associated with lower D (%) reduced crack growth rate. The cleavage growth rates and other information of samples 9, 10, and 16 of the present invention are described in Table 13 below. Corresponding test results of corresponding control samples are described in Tables 3 and 4 below, grouped by the choice of carbon black. Tan β max @ 60 ° C of samples No. 24-32 of the present invention and corresponding control samples were also measured. The Tand max @ 60 ° C of the sample of the present invention is described in Table 35 below. The corresponding test results of the control samples are described in Table 36 below. Using RSS1 natural rubber, the pairs shown in Table 3 and 6 were manufactured according to the above-mentioned control sample code M2D1, according to samples No. 444-450. They are all used in the filling level (phr) shown in Table 36 and 5 phr incremental oil using Junhei N234. -92- This paper size is in accordance with Chinese National Standard (CNS) A4 (210X297mm) (Please read the precautions on the back before reading this page)--Too much 533225 A7 B7 V. Description of the invention (9) Table 33: Fragmentation growth rate of samples of the present invention Sample number of the present invention: CS / 塡 charge / oil Mw ^ fK) CGR (cm / million cycles) 9 Ν326 / 55Λ) 666 0.77 10 R660 / 55/0 678 0.69 16 Ν234 / 55 / 0 500 0.88 Table 34 The lysing growth rate of the control sample N234 / S5phrm N326 / 55phr / 0 (Please read the precautions on the back before code code RSS1 HwZi CGR (K) (cm / million cycles) Code Green Product Code_ _RSS1 CGR (K) (cm / million cycles)

Page I 1234123412341234 DDDdDDDr5DDD [> DDD [> 1111222233334444 MMMMM, MMMMMMMiMMi 73747576777879808i8283848586s788; 996021776352213 865 & 803657997880 5678566 & 4444333-

Regal 660 / 55phr / 0 RSST 2.14 M1D1 145 550 2.84 1.84 M1D2 146 636 2.52 1.70 M1D3 147 650 2.03 1.21 M1D4 148 724 1.63 2.22 M2D1 149 517 3.39 2.40 M2D2 150 572 2.77 2.00 M2D3 151 2 613 2.61 1.61 1.81 M1 489 3.12 2.33 M3D2 154 521 3.35 2.41 M3D3 155 504 3.63 1.99 M3D4 156 538 3.55 2.99 M4D1 157 415 3.02 2.85 M4D2 158 447 3.81 2.93 M4D3 159 466 3.23 2.39 M4D4 160 469 3.19

Regal 660 / 55phr / 0 RSST Subsidiary Central Labor Standards Consumer Cooperatives Printing Code

CGR (K) (cm / million cycles) M1D1 ιπ 674 M1D2 178 792 M1D3 179 891 M1D4 180 676 M2D1 1B1 598 M2D2 182 602 M2D3 183 697 M2D4 1B4 659 ^ • 88115 ^ .S.7.9.4.1.11 2.2.2.3 .3.3.3. Code 1234123Θ DDD0DDD0 3333WW4W ΜΜΜΜ ^^ Μ ^ This paper size is applicable to China National Standard (CNS) A4 specification (210X29 * 7 mm) Sample CGR (K) (cm / million cycles) i ^ JC «^ 88888999 36291669 70 (650264 4555444 ^. 9 6 3 9 14 8 5.0I.5J7.17 44.3.33.4. -93- 533225 A7 B7 V. Description of the invention (91) Table 3 5 Samples of the present invention & 11 (^ At 60 ^:

The sample number of the present invention is from 塡 charge / oil (P⑽ Mw ^ (K) maximum TenJ @ 6 £ TC) 9r6M979184 .16.17.19.21.22.15.17.2222 οοοοοο.ο.ο. Hsgs / 5/5/5 5 «JP55 18 /) 3 / '8 /' 3 / -8 / j9 / 43 / j5 / 455664 '& 66j 456789012 222222333 (Please read the precautions on the back before re-dressing-π then this page) Table 3 6 Control sample of & 11 (^ at 60 ° 〇 sample number M state 〇 (K) (¾) _ filling / oil (Phr) Max Tan £) (@ 6〇C) Order 3 5 6 7 8 9 0 444444444445 8 9 9 16 0 6 2 0 7 6 6 9 »4 4 3 3 3 2 2 0.154 0.170 0.179 0.195 0.212 0.215 0.245

Printed by the Employees' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs-94- This paper size applies to the Chinese National Standard (CNS) A4 specification (210 × 297 mm) 533225 A7 V. Description of the invention (92: = Comparison with 34 can be seen, Comparing the control samples, the beneficially low lysing growth rate was observed. The good resistance of the sample inhibition to many applications and related; = Health = there are temples. In addition, it can be seen from the comparison of Tables 35 and 36 that the better T First, that is, lower than the quality of the control sample: 値: Because the sample has improved performance for many product applications, for example, including: low-resistance tire applications with low rolling resistance, etc., and the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs The advantageous performance characteristics of printing the elastic composite of the present invention are illustrated by graphically showing the cleavage growth rate of the corresponding sample No. 16 of the present invention containing N234 carbon black and the corresponding test results of the control Xupin 273 to ^. In particular, FIG. 22 illustrates = The relationship between the MWSQl and the lysing growth rate of the ground test control samples, and the beneficial effect of macrodispersion in the elastic composite of the present invention. It should be answered, showing: 22-24 and Tables 33-36 of MWS (jl 値 is cooked The former master batch material. The molecular weight of the matured material is related to the "mature ~" of the unripened master batch. It can be seen that the control sample has a MWs of about .25 XW to · 6 XW. The linear relationship of the range along MWSC & gt The linear relationship of 1 and 1. In contrast, due to the sample of the present invention. The car ^ Jiaju disperse D (%), the sample of the present invention at MWsol of 0.5 x 106, No. 6 has far more than any corresponding control sample Good (ie, lower) cleavage growth rate. It is further established by a similar display in FIG. 23, where it can be seen that the cleavage growth rate of Sample 9 of the present invention containing carbon ^ is much lower than that of any corresponding control 145 to 160, And 'below the relationship line. Similarly in FIG. 24, it can be seen that the excellent macrodispersion of sample No. 10 of the present invention regenerates much lower than the relationship line between the lysed growth rate and MWs〇1 established for the corresponding control samples Nos. 177 to 192. Lysis growth maggots. In Figure 25 'Sample samples 24 to 28 of the present invention and samples 29 to 95 of the present invention-This paper size applies Chinese National Standard (CNS) 4 ^ grid (210X297 mm) 533225 A7 B7 Central Standard of the Ministry of Economic Affairs Printed by the Bureau's Consumer Cooperatives Description of the Invention (93) Tan dmax @ 60 ° C of No. 32 graphically shows that it is better than control samples No. 444 to 450, ie, lower. The excellent crack growth results of the elastic composites of the present invention discussed above not only prove favorable fatigue properties It also shows favorable rupture properties, such as excellent cracking and chipping resistance. The excellent hysteresis results of the elastic composite of the present invention discussed above not only favorably verify the low rolling resistance (and correspondingly higher fuel economy) for the application of electric vehicle tires ), Also shows favorable improvements in related performance properties such as reduced heat buildup. One or more of these excellent properties, fatigue and rupture resistance, low hysteresis, low heat accumulation, etc., make the flexible composite of the present invention extremely suitable for commercial applications such as tire applications and industrial rubber products. Regarding the application of tires, various preferred embodiments of the present invention are particularly suitable for: wheel treads, especially wheel treads for radiating and biased truck tires, off-road (OTR) tires, aircraft tires, etc .; secondary wheel faces; line layers ; Sidewalls for tire overhaul (buffer rubber; and similar tire applications. The excellent performance characteristics obtained from various preferred embodiments of the present invention can provide improved tire durability, wheel surface life and packaging life, and comparison with electric vehicles Good fuel economy and other advantages. Regarding industrial rubber products, the various preferred embodiments of the present invention are particularly suitable # · Engine stands, water stands, bridge bearings and seismic isolators, grooved rails or wheel faces, mining conveyor belts and the like Product application. The excellent performance characteristics obtained by various preferred embodiments of the present invention can provide improved fatigue life, durability, and other advantages for this product application. Figures 26-29 are roughly corresponding to the carbon black form of Figure 8 Graphical representation of the structure (腑 and surface area (CTAB). The carbon black morphology region 26m in Figure 26 includes carbon black which is currently commercially used for OTR tire tread applications. Arrow The head plus indicates the area plus ^ paper size is suitable for money _ home standard (⑽) (Please read the precautions on the back before this page) Order

• 1--I- 533225 A7 B7 V. Description of the invention (94) The direction in which the invention can be advantageously extended. It should be understood that performance characteristics such as chipping resistance, resistance to I growth and cracking resistance are usually improved in the direction of the arrow%], and the direction is improved ...: In the past, because of this higher surface area and lower structure carbon black I was used The reduced molecular weight and / or poor macrodispersion of the resulting natural rubber offsets its degradation and other characteristics. Regarding its excellent macrodispersion, the foot elastic compound of the present invention can use the lower structure and higher surface area carbon black indicated by the moving arrow 262 to obtain a greatly improved TR surface material. Similarly, the carbon black morphology region 271 in FIG. 27 includes carbon black currently commercially used for truck and bus (T / B) tire tread applications. The arrow 272 indicates the direction in which the region 271 can be advantageously extended according to the invention. It should be understood that performance characteristics such as abrasion resistance are generally improved in the direction of the main body of the arrow 272. However, in the past, the reduced molecular weight and / or poor macrodispersion of rubber generated by the use of this higher surface area carbon black has offset its degradation With other characteristics. Regarding its excellent macrodispersion and MWS (> 1), the elastic compound of the present invention can use the direction arrow 272 to show that this higher surface area carbon black is greatly improved by the D / B tread material. Staff of the Central Standards Bureau of the Ministry of Economic Affairs Consumption cooperatives print similarly, the carbon black morphology areas 281 and 283 in Figure 28 each show the carbon black currently commercially used on the tread base and the tread of passenger car (PC) tires. The tread arrows 282 and 284 each indicate Regions 281 and 283 can be advantageously extended in accordance with the present invention. It should be understood that for wheel bases, performance characteristics such as heat buildup (HBU) and rolling resistance are generally improved in the direction of the main body of arrow 282. However, in the past due to The lower molecular weight and / or poor macrodispersion of the rubber produced by the use of higher surface areas and lower structure blacks to offset its degradation and other characteristics. Similarly, it should be understood that for PC treads, such as rolling resistance performance characteristics It is usually improved in the direction of the main body of the moving arrow 284. However, in the past, as the paper size of -97-, the Chinese National Standard (CNS) A4 specification (210X29 * 7 mm) was applied. 533225 A7 B7 (95 The reduced molecular weight and / or poor macrodispersion of the rubber resulting from the use of higher surface area and lower structure carbon blacks, offsetting its degradation and other characteristics. About the excellent macrodispersion of this elastic compound and the molecular weight retained as the case may be For the elastic composite of the present invention, the higher surface area and lower structure carbon black indicated by the moving arrows 282 and 284 can be used to improve the wheel base and the PC wheel surface.

Similarly, the carbon black morphology regions 291, 293, and 294 in Figure 29 each show carbon black that is currently commercially used for sidewall, vertex, and steel strip applications. The tread arrows 292 and 295 each indicate a direction in which the regions 291 and 294 may advantageously extend in accordance with the present invention. It should be understood that for sidewalls, performance characteristics such as heat build-up (HBU) and fatigue life-life are generally improved in the direction of the main body of arrow 292. However, in the past, the molecular weight of rubber produced by the use of this lower structure carbon black has been reduced. And / or poorly dispersed, offsetting its degradation and other characteristics. Similarly, it should be understood that for steel strip elastic materials, performance characteristics such as heat accumulation, processing, and wire adhesion are generally improved in the direction of the main arrow 295. However, in the past due to this higher surface area and lower structure carbon black The reduced molecular weight and / or poor macrodispersity of the resulting rubber is offset by its degradation and other characteristics. Regarding the excellent macrodispersion of this elastic compound and the molecular weight retained as the case may be, the elastic compound of the present invention can use the higher surface area and / or lower structure carbon black indicated by the direction arrows 292 and 295, respectively. Rubber substance. Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs Additional Examples: Preferred Specific Examples and Comparative Examples Including Other Fillers Prepare additional samples of the elastic composites according to the #determined preferred embodiment of the present invention, and corresponding control samples. The first group uses a heterogeneous aggregate filler of the type referred to above for silicon-treated carbon black. In particular, samples 33 to 34 of the present invention are commercially available from Cabot Corporation (Ma-98- this paper size applies Chinese National Standard (CNS) A4 specifications (210X297 mm) 533225 A7 B7 V. Description of the invention (96) Billerica) ECOBLACK® silicon-treated carbon black. This ECOBLACK® filler has morphological properties similar to carbon black N234, ie, structure and surface area. Sample 3 No. 3 uses 45 phr of ECOBLACK® packing and is free of extender oil. Sample 34 uses 68 phr of ECOBLACK® and is free of extender oil. Table 37 shows typical fillers and extender oils for various product applications for the elastic composites of the present invention containing natural rubber and a blend of carbon black and silica fillers. It should be understood that the use of silica fillers in the composition shown in Table 37 generally replaces an equivalent amount of carbon black filler. (Please read the precautions on the back before printing the table by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. 37 Typical NR formula for tire applications. Carbon black type. Carbon black filled with oil. Filled with silica filled with wheels. N110, N116, N121, N134 , N220, N299 40-60 phr 0-20 phr 0-10 phr OTR tread N110, N115, N220, N231 45-55 phr 5-10 phr 5-20 phr steel strip N326 50-75 phr 0-5 phr 0 -20 phr truck bus wheel base N330, N550 40-60 phr 0-20 phr car shell N326, N330, N550 40-60 phr 5-30 phr sidewall N330, N351, N550 30-60 phr 5-30 phr Vertex N326, N330, N351 50-90 phr 0-20 phr LRRPC wheel surface N234, N299, N339, N343, N347, N351 40-60 phr 0-30 phr order -99- This paper size applies to the Chinese National Standard (CNS) A4 specification (210X297 mm) 533225 A7 V. Description of the invention (97) The second group of samples uses a blend of stone sapphire and carbon black. In the specific embodiment of using the disc black slate filler blend, this example is usually It is preferably used in a weight ratio of at least _, that is, carbon It is preferred to include at least about 60% by weight (filler to obtain good elastomeric cohesion and to reduce or exclude the re-cohesion of Miao Shi in the master batch. In particular, in Example 35_38 shown in Table 40, …, Used together with HiSil® 233, a granular training 2 filler from PPG Industries (Pittsburgh, PA, USA), which has a surface area BET of 15 square meters per gram, a surface area of 190 tnils / 100 grams DBpA, and 7 of Qiu値 and! The main particle size of 9 nm. · _ Prepare all samples according to the invention according to the procedures and apparatus used for samples 1-32 of the present invention as described above, that is, additional examples 33-38. Each of the samples 38 of the present invention Details of the manufacturing method and device are shown in the following table 38. Depending on the situation, the latex or concentrate used in the sample port 33-38 is the same as the reference table 24 above. It should be understood that the comparison of the data in table 38 is provided above Samples No. 1-32 of the present invention in Table 25. The carbon black fillers listed in Table 3 "CRX2000" are the above-mentioned ECOBLACK® silicon-treated carbon blacks. (Please read the precautions on the back before printing this page) (Reprinted by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs __ -100- This paper size applies to the Chinese National Standard (CNS) (210X297 mm) 533225 A7 B7 \ J / 98 / \ Explanatory note ft ^ 1? 8 t ^ mo ST- i srol 6.ετ- SH g ·?

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co xr in cd Ν- co ΓΟ Γ0 CO CO CO CO -101 533225 A7 B7 V. Description of the invention (99) Prepare the control samples 451-498 according to the procedures and devices for control samples 1-450 as described above. The processing codes of master batch Nos. 451-466 (see Table 13 above), filler filling, rubber, MWSQl and macrodispersion are described in Table 39 below. The processing code, filler filler, rubber, MWSQl and macrodispersion (and filler and oil filler for convenience of reference) of sample No. 33-38 of the present invention are shown in Table 40. As can be seen from Table 39, control samples 451-466 correspond to the compositions of samples 33 and 34 of the present invention. Similarly, the control sample No. 467-498 corresponds to the sample No. 35-38 of the present invention. Table 39 (read the precautions on the back and then ^^ this page) CRX 2000/44/0 CRX 2000/58/0 RSS1 RSS1 code sample Number (K) Sample number DPi) (K) 12341234 12! 3dddi > ddde > 5ί52535455565758 © 014953259 σ9678τ-9ζ34 95414453444- 38789753 .4] 61C488.1 ^ 3.3.7.62.Z4.3 5960616263646566 90328 ^ -0809 09398 & 8957 11853352 674021.0.2 8.5.9.8.2.2.4.7. Printed by the Consumer Cooperative of the Central Bureau of Standards, Ministry of Economic Affairs, Table 4 0 The sol molecular weight and undispersed area of the sample of the present invention. ) 33 CRX 2000/44/0 380 0.18 34 CRX 2000/58/0 448 0.10 35 N220 / Hilsil 233/43/10/5 500 0.14 36 N234 / Hilsil 233/40/10/0 490 0.36 37 N234 / Hilsil 233 ^ 0/20/0 399 0.23 38 STERUNG 6740 / HilsiI 233/30/20/0 354 0.39 -102- This paper size applies to Chinese National Standard (CNS) A4 specification (210X297 mm) 533225 A7 B7 5. Description of the invention ( 100) Table 41 Code N220 / HHSII233 / 43/10/5 N234 / HHS 丨 233/40/10/0 RSS1 RSS1 Sample number Mw ^ o, (K) Product number ^^ 90 / (K) Jing M2 803 909 M3 601 590 M2D1 457 493 1.51 475 443 8.74 M2D2 468 537 2.61 476 517 10.9 M2D3 469 523 2.82 477 569 12.5 M2D4 470 615 2.95 478 592 8.25 M3D1 479 417 0.9 6.65 M3D2 472 438 1.40 480 420 13.8 M3D3 473 433 2.15 481 516 13.9 M3D4 474 485 222 482 447 7.25 N234 / HUsll 233/30/20/0 STERUNG 6740 / HilsiI 233 ^ 0/20/0 RSS1 RSS1 code Mw ^ D〇 i) Sample number (Κ) Sample code (Κ) M2 909 909 M3 590 590 M2D1 483 394 4.37 491 430 3.77 M2D2 484 507 5.66 492 488 4.39 .M2D3 485 526 4.7 493 517 5.37 M2D4 486 568 5.94 494 553 4.66 M3D1 487 8.39 495 375 3.5 M3D2 488 363 4.49 496 380 2.73 M3D3 489 376 5.07 497 419 2.72 M3D4 490 432 5.26 498 448 3.29 (Please read the precautions on the back before this page)

Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs -103- This paper size applies to the Chinese National Standard (CNS) A4 (210 X 297 mm) 533225 A7 B7 V. Description of the invention (101)

The excellent carbon black dispersion of the master batch No. 33-38 of the present invention was confirmed by the comparison of the giant dispersion quality shown in Table 39-41 and the MWSQl 値. Samples Nos. 33-34 of the present invention made of ECOBLACK® silicon-treated carbon black, and corresponding control samples were compared in the semi-logarithmic plot of Figure 30. In FIG. 30, excellent carbon black dispersion is seen for the sample of the present invention, which shows a preferred specific embodiment of the elastic composite according to the present disclosure. The sample of the invention is advantageously below the line 301 in Figure 30, while all the control samples have a poorer dispersion, which is higher than the line 301. In fact, the preferred embodiment shown in FIG. 30 falls below D (%) 値 of .2%, even if it favorably exceeds MWSQ1 値 of .4X106. The data shown in Figure 30- clearly show that the great dispersion quality of the novel elastic composites containing silicon-treated carbon black is much better than those obtained by using comparable ingredients in the prior dry mixing process. The macrodispersion of the elastic composite of the present invention shown in Fig. 30 is illustrated by the following equation: D (%) < 1.0% (25) is MWS. When it is less than 0.4 X106; and log (D) < log (1.0) +2.0 X [MWS〇1- (0.4 X ΙΟ6)] X 10.6 (26) When 0.4X106 < MWSC) 1 < 1.1X106 . The printing of the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs should understand that D (%) is the percentage of undispersed area measuring defects larger than 10 microns, and 1% is the criticality for the parent batch according to these preferred embodiments of the present invention. Great dispersion quality. That is, the dry-kneaded master batch did not obtain a giant or disperse quality of 1.0% or better in any MWSQl, even after being thoroughly dry-mixed to reduce MWSQl to less than .4X 106. The preferred embodiment shown in Figure 30 falls below the threshold. It can be seen that the elastic composite of the present invention containing silicon-treated carbon black provides a balance between the macrodispersion quality and MWSC) that have not been achieved so far. 104- This paper size is in accordance with Chinese National Standard (CNS) A4 (210X297 mm) 533225 A7 B7 V. Description of the invention (102) The sample of the present invention which contains the ocher filler mixed with stone slate, and the corresponding control sample Compare in the semi-logarithmic performance graph of Figure 31. In particular, Fig. 31 shows macrodispersion 値 and MWSC) 1 値 of samples 35-38 of the present invention and corresponding control samples 467_498. In FIG. 31, excellent carbon black dispersion is seen for the sample of the present invention. Table π shows a preferred embodiment of the π elastic composite according to the present disclosure. The sample according to the invention is advantageously located below line 311 in Fig. 31, while all pairs are identical. Has poorer dispersion, above line 311. In fact, the comparison shown in Fig. 31: the specific embodiments are all below D (%) 値 of .4%. The data shown in Figure 31 is clearly shown in a wide range of MWS. ^ Range, it is revealed here that the macrodispersion quality of a novel elastic compound containing a carbon black / silica blend is far superior to that obtained by using comparable ingredients using a dry master batch method. The elastic composite of the present invention shown in FIG. 31: The macrodispersion of the present invention is described by the following equation: " D (%) < 0.8 ° / 〇 (27) when the MWsol is less than 0.5 × 106; and 10 g ( D) < log (0.8) +2.2 X [MWsor (0.5 X 106)] x 6-6 (2 when 0.5xi06 < MWSC) 1 <: Llx106. Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back and then this page). It should be understood that D (%) is the percentage of undispersed area measuring defects larger than 10 microns, and .8% is in accordance with The critical macrodispersion quality of the master batches of these preferred embodiments of the present invention. That is, the dry-kneaded master batch has a macrodispersion quality of 0.8% or less at all, even after being thoroughly dry-mixed to reduce MWS01 to less than · 4χ, .106. The preferred embodiment shown in Fig. 31 is described in this section, and the critical macro-dispersion to 4% is achieved. It can be seen that the elastic composite of the present invention containing a carbon black spar blend filler provides a balance between the quality of megadispersity and MWsol that has not been obtained so far. $ 105- Paper size · Quiet_Fresh (CNS) A4 · (210X297) Chu < Printed by various consumer organizations of the Central Standards Bureau of the Ministry of Economic Affairs, Consumer Cooperative 533225 A7 B7 V. Description of the invention (103) About the above disclosure For those who are familiar with this skill, obviously add, modify, etc. without departing from the scope and spirit of the present invention. All such enhancements and modifications are intended to be covered by the following patent application scope. -106- This paper size is applicable to China Standard (CNS) A4 specification (21 OX297 mm)

Claims (1)

533225 Patent Application No. 086103947 Chinese Patent Application Replacement (March 1992) A8 B8 C8 φ8 Nine applications for patent scope \ Announcement A method for manufacturing an elastic compound, each comprising: feeding a continuous flow of a first fluid containing an elastic latex to a mixing zone of a coagulation reactor, which is defined to extend from the mixing zone to a discharge end The slender agglomeration zone feeds a continuous flow of the second fluid containing granular filler to the mixing zone of the agglomeration reactor under pressure to form a mixture with the elastic latex. The mixture is sent to the discharge end in a continuous flow, and the granular filler It is an effective cohesive elastic latex, in which feeding the first fluid against the second fluid in the mixing zone is sufficient energy to substantially completely condense the elastic latex and granular filler before reaching the discharge end; and the discharge end of the self-coagulation reactor, The substantially continuous flow of the discharged elastic compound. 2. The method for manufacturing an elastic composite according to item 1 of the scope of patent application, wherein the second-flow system is fed into the mixing zone through a nozzle at a speed of 100 to 800 feet per second. 3. The method for manufacturing an elastic composite according to item 2 of the scope of patent application, wherein the first-rate system is continuously fed to the mixing zone at a speed of less than 12 feet per second. 4. The method for manufacturing an elastic composite according to item 1 of the scope of patent application, wherein the elastic latex is a natural rubber latex and the granular filler is carbon black. 5. The method for manufacturing an elastic composite according to item 1 of the patent application scope, further comprising feeding an auxiliary fluid to the mixing zone, the auxiliary fluid being substantially non-reactive with the mixture. 6. Installation The method for manufacturing an elastic composite according to item 5 of the patent application, wherein the auxiliary fluid is air. This paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) 533225 AB c D 6. Application scope of patent 7. The method for manufacturing elastic composites according to item 1 of the scope of application for patent, where the cohesion zone is in From the mixing zone to the discharge end, it has a gradually increasing cross-sectional area. 8. A continuous flow method for preparing an elastic composite dispersed with granular fillers in an elastomer, comprising: A) In a coalescing reactor, it is formed to extend from an inlet end to a discharge end with a gradually increasing cross-sectional area The slender agglomeration zone establishes a continuous, semi-restricted flow of the mixed elastic latex and granular filler under pressure, which is achieved by (i) continuously feeding the elastic latex fluid to the mixing zone at the inlet end of the agglomeration reactor 'and ( ii) By feeding the granular filler fluid into the mixing zone in a continuous jet, the energy is sufficient to resist the elastic latex fluid, so that the elastic latex and the granular filler are substantially completely agglomerated, and the elastic latex fluid is transported to the granular filler fluid. ; And B) the substantially constant flow of the elastic composite sphere is discharged from the discharge end of the agglomeration reactor, while the fluid flow is fed in according to steps A (i) and A (ii). 9. The continuous flow method for manufacturing an elastic compound according to item 8 of the scope of the patent application, wherein the aggregation effect of the elastic latex is substantially completed when the elastic compound sphere is discharged from the discharge end of the condensation reactor. 10. The continuous flow method for manufacturing an elastic composite according to item 8 of the scope of patent application, further comprising dispersing the high energy of the granular filler in the liquid in a homogenizer having an outlet hole in fluid communication with the mixing zone To prepare a granular filler fluid. 11. The continuous flow method for manufacturing elastic composites according to item 8 of the scope of patent application, in which the liquid slurry is fed through a nozzle at a speed of 100 to 800 feet per second -2- This paper size applies to Chinese National Standards (CNS) A4 size (210 X 297 mm) 12. Into the mixing zone. 13. 14. 15. 16. 17. 18. 19. 20. The continuous flow of elastic composites for manufacturing elastic composites applying for item i! Of the patent scope #M +1, the speed of the middle liquid coarse slurry through the nozzle is 200 to 500 feet in seconds. The continuous flow method for manufacturing elastic composites according to item 8 of the patent is to include a step in which a small amount of additives are added to the elastic latex before feeding the elastic latex to the mixing zone. : According to the declared continuous flow method for the production of elastic composites according to Item 8 of the patent, the granular filler fluid is an aqueous carbon black dispersion. According to Shen Qiao's patent, the continuous flow method for the production of elastic composites includes The granular filler fluid includes silicon-treated carbon black, aerosol, stone, precipitated silica, and any mixtures thereof. The continuous flow of the elastic composite according to item 8 of the patent application claims that the elastic latex fluid is basically Including natural rubber latex. Continuous flow method for preparing elastic composites according to item 6 of the patent application range, wherein natural rubber latex is a natural rubber latex concentrate. Continuous flow for preparing elastic composites according to item 16 of the patent application range Method, in which the natural rubber latex is a field latex. According to the continuous flow method of manufacturing an elastic composite according to item 8 of the patent application scope, it further includes continuously feeding the additive fluid with the elastic latex fluid and the granular filler fluid simultaneously and separately. The step of mixing the materials into the mixing zone to mix the additives into the semi-restricted flow. Continuous Flow Method for Manufacturing Elastic Composites of Scope 8 'wherein the additive is selected from the group consisting of anti-ozonants, antioxidants, plasticizers, processing aids, resins, flame retardants, extender oils, lubricants and any of them Mixed-3-This paper size applies to Chinese National Standard (CNS) A4 (21〇X 297 cm) 533225 A8 B8 C8 Thing. D8 21 • The continuous flow method for manufacturing elastic composites according to item 8 of the patent application scope which further includes injecting a pressurized gas into the mixing zone. • The continuous flow method for manufacturing elastic composites according to item 21 of the scope of patent application ', wherein a pressurized gas system is separately injected into the mixing zone. • Continuous flow for manufacturing elastic composites according to item 21 of the patent application. Wanfa ’where the pressurized gas system is injected into the mixing zone together with the granular filler fluid through a nozzle. 24. A continuous flow method for producing an elastic composite according to item 8 of the scope of the patent application, wherein step A (ii) includes continuously feeding a plurality of granular filler streams through a multi-nozzle to a mixing zone. 25. The continuous flow method for producing an elastic composite according to item 8 of the scope of the patent application, which further comprises simultaneously feeding at least one auxiliary stream of the elastic latex fluid to the mixing zone in steps A⑴ and A (ii). %. The continuous flow method for manufacturing an elastic composite according to item 8 of the scope of patent application, further comprising the step of drying the elastic composite spheres received by the discharge end of the agglomeration reactor via at least one dryer. 27. The continuous flow method for making an elastic compound according to item 26 of the scope of patent application, further comprising the step of packing the elastic compound by sequentially compressing the elastic compound of 25 to 75 pounds I after the drying step. 28. A continuous flow method for making an elastic composite according to item 8 of the scope of the patent application, wherein the elastic latex flow system is fed at a pressure of less than 10 psig, and the granular filler flow system is fed at a pressure of at least 75 psig material. 29 · —The connection of making rubber master batch by aggregating natural rubber latex and carbon black -4- This paper size applies to Chinese national standard ((:) ^ 3) A4 size (210X297 mm) 533225 A8 B8 C8 D8 A patent application for continuous flow method, including: A) In a coalescing reactor, it is formed into a generally tubular coalescing area, with a gradually increasing cross-sectional area extending from the inlet end to the open discharge end to establish a mixed natural rubber Continuous, semi-restricted flow of latex and carbon black by simultaneously (i) continuously feeding the liquid stream of natural rubber latex to the mixing zone at the inlet end of the coalescing reactor, and (ii) by feeding the liquid slurry to Continuous jet feeding into the mixing zone and continuous delivery of natural rubber latex to the liquid slurry of carbon black; and B) At the same time, the rubber mother batch spheres are discharged from the discharge end of the coalescence reactor. 30. A continuous flow method for manufacturing an elastic composite, the composite comprising a particulate filler selected from carbon black, silicon-treated carbon black, fumed silica, precipitated silica, and mixtures thereof, finely dispersed in nature In rubber, the method includes: utilizing a high energy dispersion of the granular filler in an aqueous liquid in a homogenizer to prepare a granular filler fluid; and in a coagulation reactor, it forms a generally tubular coagulation zone to gradually The increased cross-sectional area extends from the inlet end to the discharge end to establish a continuous, semi-restricted flow of the mixed natural rubber latex and granular filler by simultaneously (i) passing the liquid flow of the natural rubber latex below Continuous feed at 10 feet per second to a mixing zone defined by a mixing head connected to the inlet end of the agglomeration reactor by a sealed fluid, the mixing zone extending coaxially with the agglomeration zone, and (ii) by moving toward the inlet end of the agglomeration zone The granular filler fluid is fed into the mixing zone through a feeding tube which is substantially coaxial with the coagulation zone, and the paper size is continuously adapted to the Chinese National Standard (CNS) A4 specification (210 X 29) 7 mm) decoration 6. Scope of patent application: Natural rubber latex is transported into the granular filler fluid, and the granular filler flow system leaves the feed pipe at a speed of 200 to 500 feet per second; the mother batch is discharged simultaneously and continuously from the discharge end of the coalescence reactor. Spheres, in which the coagulation of natural rubber latex by granular fillers is substantially completed; and the batches of mother batch spheres discharged from the coagulation reactor are simultaneously and continuously dried and granulated in a series of dryers. 31. —A device for manufacturing an elastic composite with granular filler dispersed in an elastomer, comprising: a coalescing reactor which defines a mixing zone and an elongated coalescing zone extending from the mixing zone to the discharge end, where The zone has a gradually increasing cross-sectional area between the mixing zone and the discharge end; a latex feeding device to continuously feed the elastic latex fluid to the mixing zone, and a filler feeding device to continuously spray the granular filler fluid It is fed into the mixing zone to form a mixture with the elastic latex fluid, and it runs from the mixing zone to the discharge end of the coagulation zone. Before reaching the discharge end, the elastic latex is substantially completely coagulated. 32. The device for manufacturing an elastic composite according to item 31 of the scope of the patent application, wherein the filler feeding device continuously feeds the granular filler fluid to the mixing zone through a nozzle at a speed of 100 to 600 feet per second. 33. The device for manufacturing an elastic compound according to item 32 of the scope of the patent application, wherein the latex feeding device continuously feeds the elastic latex fluid to the mixing zone at a speed of less than 8 feet per second. 34. The device for manufacturing elastic composites according to item 31 of the scope of the patent application, the paper size of this paper applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) D8. The feed device continuously feeds the granular filler fluid to the mixing zone at a pressure of at least 75 pounds per square inch (meter). 35. The device for manufacturing elastic composites according to item 34 of the scope of patent application, wherein the latex feeding device continuously feeds the elastic latex fluid to the mixing zone at a pressure of less than 12 pounds per square inch. 36. The device for manufacturing an elastic compound according to item 31 of the scope of the patent application, further comprising an auxiliary feeding device to simultaneously feed an additional pressurized fluid stream to the mixing zone. 37. The device for producing an elastic composite according to item 36 of the scope of the patent application, wherein the pressurized fluid is air. 38. —A device for continuous flow manufacturing of granular filler elastic composite dispersed in an elastomer, comprising: a coalescing reactor, which forms an elongated coalescing area to gradually increase the cross-sectional area from the entrance The end extends toward the discharge end; a device for continuously feeding the elastic latex fluid to the mixing zone at the inlet end of the condensation reaction zone; and a device for feeding the granular filler fluid into the mixing zone in an energy-rich manner, The semi-restricted flow of the mixed elastic latex and the granular filler is generated in the agglomeration area toward the discharge end, and the substantial aggregation of the elastic latex and the granular filler is achieved before the discharge end. 39. —A device for manufacturing a granular filler elastic compound dispersed in an elastomer, comprising: a coalescing reactor, which forms an elongated coalescing area, and gradually increases the cross-sectional area from the inlet end to the discharge end ; This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) Binding 533225 A8 B8 C8 The scope of Shenqing's patents is a device that continuously feeds the elastic latex fluid to the mixing zone at the inlet end of the coalescence reactor; and a device that continuously feeds the granular filler fluid to the mixing zone, effectively transporting the elastic latex fluid, so that It becomes a mixture with the granular filler fluid 'and substantially completely coagulates the elastic latex and the granular filler before the mixture reaches the discharge end. 40. A continuous flow manufacturing apparatus for an elastic compound according to item 39 of the scope of the patent application, wherein the mixing zone is inside the mixing head and is substantially coaxial with the elongated condensation zone. 41 · Continuous flow manufacturing of elastic compound according to item 40 of the scope of patent application • The device 'where the mixing head is sealed in the condensing zone extender, 42 · Continuous flow of the elastic compound according to item 4 of the scope of patent application The manufacturing device, wherein the device for feeding the granular filler fluid stream includes a first feeding officer, which extends substantially coaxially in the mixing zone to the front end of the slurry nozzle facing the condensing zone. The mixing head forms a first feeding channel that is substantially coaxial with the agglomeration area and extends from the inlet agglomeration area; and a first feeding tube that coaxially extends in the first feeding channel in the moon direction, and the orifice is formed with the mixing head Impervious to fluid. μ in According to the elastic compound of Item 43 of the scope of the applied patent ^ "device", where the first feeding pipe is extended by the inlet hole and the first of which is immediately upstream of the front end of the slurry nozzle -8- 533225 A8 B8 It has an axial dimension of at least three times its diameter. 45. The continuous flow manufacturing device for an elastic compound according to item 43 of the scope of the patent application, wherein the device for feeding the elastic latex fluid includes a second feed channel, and the mixing head is set to 3 to the first feed channel. . To 90. It is formed by the angle from the second entrance hole at the far end of the mixing zone to the junction with the mixing zone. 6. The continuous flow manufacturing device for an elastic compound according to item 44 of the patent application, wherein the cross-sectional area of the agglomeration zone immediately downstream of the mixing zone exceeds twice the cross-sectional diameter of the first feed pipe. 7. The continuous flow manufacturing device of elastic compound according to item 46 of the patent application. The cross-sectional area of the condensation area immediately downstream of the mixing zone is the first. • The cross-sectional area of the feed pipe is about 4 to § times. The continuous flow manufacturing device of the elastic compound according to the item 1 of the scope of the patent application, wherein the mixing head is 30 for the first feeding channel. To 90. The angle extends from the entrance hole at the far end of the mixing zone to the junction with the mixing zone to form at least one additional feeding channel. 49 · Continuous flow manufacturing of elastic composites according to item 39 of the scope of patent application The device, wherein at least the first part of the condensation area extending from the inlet end toward the discharge end has a circular cross section and a central longitudinal axis, and the size of the circular cross section is increased by a total angle of greater than zero degrees and less than 25 degrees to the central longitudinal axis. 50. A continuous flow manufacturing device for an elastic compound according to item 39 of the scope of the patent application, wherein the cross-sectional area of the condensation area is continuously increased toward the discharge end. Mobile manufacturing equipment, in which the cross-sectional area of the condensation area is calculated from the entrance end to the discharge end. 9- This paper is applicable in the standard @CN 标准 (CNS) A 视 格 (21GX297 公 爱) a -------- 533225 "Step by step" • The continuous flow manufacturing device of the elastic compound according to item 50 of the scope of the patent application, wherein the first part of the coacervation zone includes: a substantially fixed diameter of 0, extending from the inlet end to the discharge end! ^ Of Section-At least three times the LigDi, and each of the other sections has a substantially fixed cross-sectional diameter that is at least twice the cross-sectional area of the immediately preceding section and equals at least the cross-sectional diameter Three times the length. 53. The continuous flow manufacturing device of an elastic compound according to item 52 of the application for patent, wherein the length Li of the first section is about 12 to 18 times its diameter 仏. 54. The continuous flow manufacturing device for an elastic compound according to item 53 of the application, wherein the condensing zone extending from the inlet end toward the discharge end has a circular cross-section 'increasing in size toward the discharge end and has: starting at the inlet end The first section has a substantially fixed cross-sectional diameter Di, a cross-sectional area A}, and a length L! Equal to 5 to 8 times the diameter of the cross-section of the nozzle, which is 12 to 18 times Dii; A second section extending toward the discharge end, which has a substantially constant cross-sectional diameter, approximately equal to, twice the cross-sectional area a2, and approximately two to three to seven times d2 l2; The third section extending toward the discharge end has a fixed cross-sectional diameter D3 on the impurity, a cross-sectional surface approximately equal to two times eight 2 ^ 8, and three to seven times D3 L3; and The fourth section, which extends from the third section toward the discharge end, has miscellaneous 10- This paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) Hold 533225 A B c D 6. Scope of patent application The diameter d4 of the fixed cross-section is substantially fixed, the cross-sectional area a4 is approximately equal to a3, and three to seven times d4 is l4. 55. The continuous flow manufacturing device for an elastic compound according to item 39 of the patent application scope, further comprising a diffuser to receive the elastic compound from the discharge end of the condensation zone, and selectively sending the elastic compound to any multi-receiver position. 56. A continuous flow manufacturing device for an elastic compound according to claim 55, wherein the diffuser includes a flexible conduit having a first end connected to the discharge end of the agglomeration reactor, and a movable one to any multi-receiving position. Second end. 57. A continuous flow manufacturing device for an elastic compound according to claim 55, wherein the device for feeding granular filler fluid includes a pumping device to develop the pressure to greater than 75 psig, and the elastic latex fluid is fed into the device. The device includes a holding tank and a feed tube to develop an elastic latex fluid pressure below 10 psig. 58. The continuous flow manufacturing device for an elastic composite according to item 39 of the scope of the patent application, wherein the granular filler fluid is a carbon black slurry containing carbon black in a carrier liquid, which further includes feeding the granular filler fluid The device to the mixing zone is a carbon black slurry preparation device in fluid communication, which includes: a mixing tank for a mixture of carbon black and a carrier liquid, which has a discharge hole for discharging the mixture fluid; a colloid mill to disperse the carbon black In the carrier liquid to form a dispersion fluid, which has a suction hole in fluid communication with the discharge hole of the mixing tank, and an outlet hole to discharge the dispersion fluid; and a homogenizer to more finely disperse the carbon black in the carrier liquid , In the shape of -11-This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) 533225 AB c D 6. The scope of the patent application is carbon black slurry, which has an inlet hole in fluid communication with the discharge hole of the colloid mill, and sends the carbon black slurry to the granular filler fluid feed to the mixing zone. Exit hole of the device. 59. An elastic composite comprising an elastomer, wherein the granular filler has been dispersed in the following manner: A continuous flow of a first fluid containing an elastic latex is fed to a mixing zone of a coagulation reactor, which is defined by mixing The zone extends to an elongated coagulation zone at the discharge end; a continuous flow of a second fluid containing granular filler is fed to the mixing zone of the coagulation reactor under pressure to form a mixture with the elastic latex, and the mixture is sent to the The discharge end, and the granular filler is effective for agglomerating the elastic latex, wherein the first fluid is fed in the mixing zone to oppose the second fluid, and the energy is sufficient to substantially substantially aggregate the elastic latex and the granular filler before the discharge end; and A substantially continuous flow of the elastic compound is discharged from the discharge end of the agglomeration reactor. 60. An elastic composite containing granular fillers finely dispersed in an elastomer, which is formed by a continuous flow method including the following steps: A) In a coagulation reactor, it is formed to gradually increase the cross section Area and an elongated condensation reaction zone extending from the inlet end to the discharge end, under pressure to establish a continuous, semi-restricted flow of the mixed elastic latex and granular filler, which simultaneously (i) continuously feeds the elastic latex fluid to Mixing zone at the inlet end of the coalescing reactor, and -12- This paper size applies to China National Standard (CNS) A4 (210X297 mm) 533225 ABCD VI. Application for Patent Range (π) By continuously spraying granular filler fluid into the mixing zone, the energy is sufficient to resist the elastic latex fluid, so that the elastic latex and the granular filler are substantially completely agglomerated, and the elastic latex is The fluid is conveyed into the granular filler fluid; and B) the substantially constant flow of the elastic mother batch sphere is discharged from the discharge end of the coalescence reactor, while the fluid is fed in accordance with steps A⑴ and A (ii). 61. An elastic composite formed by a continuous flow method including the following steps: A) In a coalescing reactor, it is formed into a generally tubular shape that gradually increases the cross-sectional area from the inlet end to the open discharge end Condensing zone, establishing a continuous, semi-restricted flow of mixed natural rubber latex and carbon black, which is simultaneously (i) continuously feeding the natural rubber latex liquid stream to the mixing zone at the inlet end of the condensing reactor 'and (ii) ) By continuously feeding the liquid slurry into the mixing zone with sufficient energy to fight against the natural rubber latex fluid, to substantially completely condense the natural rubber latex and granular fillers, the natural rubber latex is continuously transported to the carbon black In the liquid slurry; and B) at the same time, the elastic composite sphere is discharged from the discharge end of the coalescence reactor. 62. An elastic composite formed by a continuous flow method including the steps of: preparing a granular filler fluid in a homogenizer by high-energy dispersion of the granular filler in an aqueous liquid; and in a coagulation reactor , Which forms a mixed zone and extends from the entrance end. 13- This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) 6. The scope of the patent application to the open discharge end is a generally tubular condensed area that gradually increases the cross-sectional area. A continuous, semi-restricted flow of mixed natural rubber latex and granular filler is established, which is achieved by (i) simultaneously The liquid stream is continuously fed at a rate of less than 10 feet per second to a mixing zone defined by a mixing head connected to the condensing zone extender in a sealed fluid, the mixing zone extending coaxially with the condensing unit, and (ii) by A feeding tube substantially coaxial with the agglomeration zone injects the granular filler fluid into the mixing zone to have sufficient energy to resist the natural rubber latex fluid, to substantially completely agglomerate the natural rubber latex and the granular filler, and continuously transport the natural rubber latex to In the granular filler fluid, the granular filler flow system leaves the feed pipe at a speed of 200 to 500 feet per second; the discharge end of the agglomeration reactor simultaneously and continuously discharges the spheres of the elastic compound, in which the natural rubber latex is substantially completed Coagulation by granular fillers; and simultaneous and continuous drying and granulation of balls discharged from the coacervation reactor 63.-A kind containing dispersed in The particulate filler of the composite body of an elastic, resilient granular filler in the composite huge dispersion D (%) less than 0.2% based undispersed area. 64. The elastic compound according to item 63 of the scope of the patent application, wherein the granular filler is carbon black, silicon-coated carbon black, silicon-treated carbon black, fuming silica, Shendian crushed stone, or Any mixture. 65. The elastic compound according to item 63 of the scope of the patent application, in which the elastomer is natural rubber, a chlorinated derivative of natural rubber, or butene, acetophenone, iso-14. This paper applies Chinese national standards ( CNS) A4 size (210 X 297 mm) 533225 A8 B8 Homopolymers and ugly polymers of glutarin, isobutylene, 3,3_dialkyl_u_ butadiene (wherein the alkyl group is ^ to C3 alkyl), propyltrinitrile, ethylidene, or propylidene. He, 66. The elastic compound according to Item 65 of the scope of the patent application, and the package ^ ^ 邛 Phr is a granular filler dispersed in the elastomer. This granular filler ^ is made of carbon black and coated with silicon. Carbon black, silicon-treated carbon black, fumed silica, precipitated silica, or any mixture thereof, and the elastic system is selected from the group consisting of celestial spheres or butylenes, phenethylfluorene, isoprene, isobutylene, 3, Homopolymers, copolymers or terpolymers of 3 · dialkyl_1,3_butadiene (where the fluorenyl group is CjC3 alkynyl group), propionate, acetylene or acetylene, in which the granular filler is elastic The macrodisperse D (%) in the composite is less than 0.2% undispersed area. 67. An elastic compound according to item 66 of the scope of the patent application, which further comprises at least one additive 'selected from an anti-ozone agent', an antioxidant, a plasticizer, a processing aid, a resin, a flame retardant, and an extender oil , Lubricants, and any mixtures thereof. 68. The elastic compound according to item 66 of the application, wherein the macrodispersion in%) is less than 0.1% undispersed area. 69. An elastic compound comprising natural rubber and 30 to 75 carbon blacks having a structure-to-surface area ratio DBPA: CTAB lower than h2, which has a macrodisperse D (0 / o) of not more than 0.3%. 880. The elastic compound according to item 69 of the scope of patent application, wherein carbon black has a structure-to-surface area ratio DBPA: CTAB of less than 1.0. 7L The elastic compound according to item 65 of the scope of patent application, which contains carbon black dispersed in natural rubber, and the large dispersion of carbon black in the elastic compound D (%) -15- It is less than 0.2% of undispersed area. According to the elastic compound of item 71 in the scope of the patent application, the macroscopic dispersion D (%) of carbon black in the elastic compound is measured by the percentage of undispersed area of defects larger than 10 microns, which is less than 0/10 / 〇 . 73. The elastic compound according to item 71 of the scope of the patent application, wherein the elastic compound is not vulcanized, and the MW ^ (weight average) of the elastic compound is at least · 45 × 106074. The elastic compound of the item wherein the carbon black has a surface area CTAB greater than 45. 75. The elastic composite according to item 7 of the scope of the patent application, wherein the elastic composite contains at least 30 phr of carbon black. 76. The elastic compound according to item 71 of the scope of patent application, which further comprises 0 to 20 phr of extender oil. 77 · An elastic composite containing carbon black dispersed in natural rubber, the carbon black has the structure and surface area properties of area I of FIG. 8, wherein the elastic composite has a large dispersion in the area below the line 10 d (%). 78. An elastic composite containing carbon black dispersed in natural rubber, the carbon black has the structure and surface area properties of the area Π in FIG. 8, wherein the elastic composite has Spite ... with the giant dispersion D (%). 79 · An elastic compound containing carbon black dispersed in natural rubber, this black has the structure and surface area properties of region III of Fig. 8, wherein the elastic compound has a MWsol and Macrodispersion 0 (0 / 〇). 8〇 · —an elastic compound comprising natural rubber, 30 to 75 phr of carbon black with a surface area CTAB of 45 to less than 250, and 0 to 20 phr of extender oil, this -16-this paper size applies China National Standard (CNS) A4 specification (210X 297 mm) 533225 A8 B8 C8 --- D8 VI. Patent application scope The elastic compound has a large dispersion D (%) of carbon black in natural rubber as follows: (i) D (%) < .2 ° / 〇 when MWs〇i < 45 X 106; and (ii) lOg (D) < log (0.2) +2.0 X (MWs〇r0.45 X 106) X 10 * 6 When 0 · 45 X 106 < MWsol < 1.1 X 106. 81 · —An elastic compound containing natural rubber, 30 to 75 phr of carbon black, which has a surface area CTAB of 45 to 250, and a structure of less than 1 10 when the CTAB is greater than 65 and less than 250. DBPA (cc / 100g), and when CTAB is from 45 to less than 65, DBPA is less than 80 + 1.6 (CTAB-45), and 0 to 20 phr * is an incremental oil. This elastic compound has carbon black in The disperse D (%) in natural rubber is as follows: (i) D (%) < 1.0% when MWs〇i is lower than 0.7X106; and (ii) log (D) < log 1.0 + 2.5X ( MWS〇1-0.7X 106) X 10'6 When 0.7 X 106 < MWSQl < 1.1 x 106. 82. An elastic composite comprising natural rubber, 30 to 70 phr of carbon black having a structure of u0 to less than 80 + 1.6 (CTAB-45) and a surface area CTAB of more than 65 to less than 250, and 0 to 20 phr of extender oil, this elastic compound has a large dispersion D (%) of carbon black in natural rubber as follows: (i) D (%) < 1.3% when MWsol is lower than 35 × 106; and ( ii) 10 g (D) < log X (0.3) +2.8 X (MWsr. 35 X 106) X 10 * 6 when 3 5 X 106 < MWsol < 1.1 X 106. 83 · —An elastic compound containing natural rubber, 40 to 70 phr with -17-This paper size applies to China National Standard (CNS) A4 specification (210X297 mm) 533225 8 0 + 1.6 ((: Ding 8-8-45) to 160 structure 03-80 (: / 100 grams) and 45 to less than 90 surface area CTAB carbon black, and 0 to 20 phr incremental oil The elastic compound has a large dispersion D (%) of carbon black in natural rubber as follows: ⑴ D (%) < 0.1% when MWsol is lower than 0.35 × 106; and (ii) 10g (D) & lt log (0.1) +2.0 X (MWs〇r0.30 X 106) X 10 * 6 When 0.3 X 106 < MWsol < 1.1 X 106. 84 ·-an elastic compound containing natural rubber, 30 to 70 phr of STERLING® 6740 carbon black, and 0 to 20 phr of extender oil. This elastic compound has a large dispersion of carbon black in natural rubber. D (%) is as follows: (i) D (%) & lt 0.1% when 1 ^ ~ 5 () 1 is less than 0.3 \ 106; and (ii) log (D) < log (0.1) +2.0 X (MWs〇r0.3 X 106) X 10 * 6 when 0.3 X 106 < MWsol < 1.1 X 106. 85. An elastic compound comprising natural rubber, 30 to 70 phr of N234 carbon black, and 0 to 20 phr of extender oil, this elasticity The composite has a large dispersion D (%) of carbon black in natural rubber as follows: (i) D (%) < 0.3% when 1 ^ 3.1 is less than 0.35 乂 106; and (ii) log (D ) < log X (0.3) +2.8 X (MWs〇r 0.35 X 1006) X 1 (Γ6 when 0.35 X 106 < MWsol < 1.1 X 106). 86. An elastic compound comprising Natural rubber, 30 to 70 phr of N110 carbon black, and 0 to 20 phr of extender oil. This elastic compound has a large dispersion D (%) of carbon black in natural rubber as follows: -18- This paper size Applicable to China National Standard (CNS) A4 specification (210 X 297 mm) 8 8 8 8 AB c D 533225 6. Scope of patent application (i) D (%) < 0.5% When MWS () 1 is less than 0.35 X 106 And (ii) log (D) < log (0.5) +2.5 X (MWs〇r0.35 X 106) X l〇 * 6 when 0 · 35 × 106 < MWsol < 1.1 X 106. 87 · -An elastic compound containing natural rubber, 30 to 70 phr of N326 carbon black, and 0 to 20 phr of extender oil. This elastic compound has a large dispersion D (%) of carbon black in natural rubber as follows: (i) D (%) < 1.0% when MWS () 1 (weight average) is less than 0.7X106; and (ii) log (D) < log (1.0) +2.5 X (MWs〇r0.7 X 106) X 10 * 6 when 0 · 7 × 106 < MWS () 1 < 1.1 · 106. 88. An elastic compound comprising natural rubber, 30 to 70 phi * of BLACK PEARL® 800 carbon black, and 0 to 20 phr of extender oil. This elastic compound has a large dispersion of carbon black in natural rubber. D (%) Are as follows: (i) D (%) < 1.5% when MWs〇i is lower than 0.65 X 106; and (ii) log (D) < log (1.5) +2.5 X (MWs〇r 0.65 X 106) X 10 " 6 when 0.65X 106 < MWsol < 1.1 · 10. 89. An elastic compound comprising natural rubber, 30 to 70 phr of REGAL® 660 carbon black, and 0 to 20 phr of extender oil. The elastic compound has a large dispersion of carbon black in natural rubber D ( %) Are as follows: (i) D (%) < 1.0% when MWs〇i is lower than 0.6 × 106; and (ii) log (D) < log (1.0) +2.5 X (MWs〇r0.6 X 106) X 10 * 6 -19- This paper size is applicable to China National Standard (CNS) A4 (210X297 mm) AB c D 533225 6. The scope of patent application is 0 · 6 × 106 < MWsol < 1.1 X 1 〇6 o'clock. 90 · —An elastic compound containing natural rubber, 30 to 70 phr of REGAL® 2 50 carbon black, and 0 to 20 phr of extender oil. This elastic compound has a large dispersion of carbon black in natural rubber. D (%) Are as follows: (i) D (%) < 1.0% is MWS. When it is less than 0.6 × 106; and (ii) log (D) < log (1.0) +2.5 X (MWs〇r0.6 X 106) X 1〇 * 6 when 0.6X 106 < MWsol < 1 At 1 X 106. 91 · An elastic compound containing natural rubber, 30 to 70 phr of N330 carbon black, and 0 to 20 phr of extender oil. The elastic compound has a large dispersion D (%) of carbon black in natural rubber as follows : (I) D (%) < 1.0% when MWsol is lower than 0.6 × 106; and (ii) log (D) < log (1.0) +2.5 X (MWs〇r0.6 X 106) X l 0.6 When 106X 106 < MWsol < 1.1 X 106. 92 · —An elastic compound comprising natural rubber, 30 to 70 phr of N351 carbon black, and 0 to 20 phr of extender oil. The elastic compound has a large dispersion of carbon black in natural rubber D ( %) Are as follows: (i) D (%) < 0.3% when MWsol is less than 0.55 X 106; and (ii) log (D) < log (0.3) + 2.0X (MWsol-0.55 X 106) X 10 * 6 When 0.55 X 106 < MWsol < 1.1 X 106. 93 · —An elastic compound comprising natural rubber, 30 to 70 phr of granular filler containing a blend of carbon black and silica, and 0 to 20 phr of extender oil, -20- paper Zhang scale is applicable to China National Standard (CNS) A4 specification (210X 297 mm) __ _ D8 VI. Patent Application Scope This elastic compound has a large dispersion D (%) of carbon black in natural rubber as follows: (i) D ( %) < 0.8% when MWsol is less than 0.5 X 106; and (ii) lOg (D) < log (0.8) + 2.2 X (MWs〇r0.5 X 106) X l0'6 When 0.5 X 106 < MWsol < 1.1 · 106. 94. The elastic composite according to item 93 of the application, wherein the particulate filler contains at least about 60% carbon black. 95. An elastic compound comprising natural rubber, 30 to 70 phr of silicon-treated carbon black, and 0 to 20 phr of extender oil. The elastic compound has a large dispersion of carbon black in natural rubber D (%) Are as follows: (i) D (%) < 1.0% when MWS () 1 is less than 0.4X106; and (ii) log (D) < log (1.0) + 2.0X (MWs〇r0.4X 106) X 10'6 When 0.4X 106 < MWsol < 1.1 x 106. 96. A vulcanized rubber containing carbon black dispersed in natural rubber. The macroscopic dispersion D (%) of carbon black in the elastic compound is less than 0.2%. 97. The vulcanized rubber according to item 96 of the scope of patent application, wherein the macroscopic dispersion D (%) of carbon black in the elastic compound is less than 0.1%. 98. A cured elastic compound according to any one of claims 59 to 95 of the scope of patent application. 99. A tire tread comprising a cured elastic compound according to item 98 of the scope of patent application. 100 · —A kind of tire secondary tread, which includes the maturity according to item 98 of the patent application scope. -21-This paper size is applicable to China National Standard (CNS) A4 specification (210 X 297 mm) 533225 Λ8 Β8 C8 Chemical elastic complex. 101. 102. The elasticity of the 98th item of the 98th item of the elasticity of the 98th item is a wire layer for a tire, which includes an elastic compound according to the application. A tire sidewall comprising a compound according to the patent application. Muscle-type cushioning rubber for tire repair, which comprises an elastic compound according to item 98 of the scope of patent application. A rubber component for an engine frame, which includes an elastic compound according to the scope of application of the patent No. 98. m-seed track, which contains the elastic compound 0 according to the scope of the patent application. Fox-seed mining conveyor belt, which contains the elastic compound according to the f of the application patent, μ. ιοί-rubber for the water rack Ingredients, which contain the elastic compound according to the scope of the patent application item 98. 108 ·-Kind of bridge bearing, which contains the elastic compound according to the scope of the patent application item "". 109. A seismic isolator comprising an elastic compound according to item 98 of the scope of patent application. 110. A cured elastic compound according to any one of the claims 59 to 95 in the scope of the patent application, which has a crack growth rate measured in accordance with ASTM D3629-94 of not more than 1.2 cm / Million revolutions. 111. A vulcanized rubber containing a granular filler finely dispersed in an elastomer having a crack growth rate of not more than -22 as measured in accordance with ASTM D3629-94- This paper is sized to the Chinese National Standard (CNS) A4 specification ( 210 X 297 public love) AB c D 533225 々, patent application scope 1.20 cm / million revolutions, and the macroscopic dispersion D (%) of granular fillers in vulcanized rubber does not exceed 0 · 2% undispersed area. 112. A method of manufacturing an elastic composite, comprising: feeding a flow of a first fluid containing an elastic latex to a mixing zone of a coalescing reactor, the reactor defining an elongated coalescing zone extending from the mixing zone to a discharge end; The flow of the second fluid containing the granular filler is fed to the mixing zone of the coagulation reactor under pressure to form a mixture with the elastic latex. This mixture is sent to the discharge end in a continuous flow, and the granular filler is effective to condense the elasticity. Latex, in which the first fluid is fed in the mixing zone against the second fluid with sufficient energy to substantially completely agglomerate the elastic latex and the granular filler before the discharge end; and the elastic compound is discharged from the discharge end of the agglomeration reactor. flow. -23- This paper size applies to China National Standard (CNS) A4 (21 × 297 mm)