KR100736442B1 - Low scattering latex/silica composite and its preparing method - Google Patents

Abstract

Provided is a latex-bound silica composition, which shows a low powder silica scattering degree, improves work environment during the preparation thereof, and has excellent dispersibility while maintaining other physical properties. The latex-bound silica composition is obtained by the method comprising the steps of: coating 3-15 parts by weight of a silica coating agent onto 100 parts by weight of silica; binding 80-150 parts by weight of a latex-containing binder solution onto 100 parts by weight of the coated silica; and drying the latex-bound silica at 110-150 deg.C to a water content of 5-10 wt%. The silica coating agent is obtained by mixing 60-70 wt% of a silane coupling agent, 10-20 wt% of a surfactant, 10-20 wt% of wax and 10-20 wt% of processing oil.

Description

Latex-bound low arsenic silica composition and its preparation method {Low scattering latex / silica composite and its preparing method}

       1 is a photograph showing a state of preparing a rubber compound in the kneader using powder silica.

       Figure 2 is a photograph showing the appearance of producing a rubber compound in the kneader using a latex-bound low arsenic silica composition according to the present invention.

       The present invention relates to a latex-bound low arsenic silica composition and a method for producing the same, and more particularly, to a surface of the silica using a silane coupling agent, a surfactant, a wax, a processing oil, and the like, Latex binding, characterized in that by controlling the scattering of the silica by spraying and binding the binder solution prepared by using a latex prepared in a liquid form and an emulsified liquid adhesive evenly on the surface of the silica and then drying it It relates to a low arsenic silica composition and a method for producing the same.

       In general, silica is used as a reinforcing filler in the rubber industry, such as carbon black, and various types of silica have been developed with the development of the rubber industry. In particular, the masterbatch, which is pre-dispersed in rubber for the poor working environment improvement and quality control and improvement of the rubber industry, has been widely spread, and the working environment of the rubber industry has been dramatically improved. However, silica has not been commercialized due to silica's bulk structure and surface chemistry, so rubber compound manufacturers that use silica have been concerned with environmental issues and product quality due to dust generation. It causes serious problems such as stability, workers' disease occurrence and job evasion. Silica manufacturers and various research institutes are working to solve the problem of silica scattering, but there is no report on how to solve the fundamental problem. However, the "Silica masterbatch and its manufacturing method" of the Republic of Korea Patent Publication No. 10-0154114 (registered on September 2, 2005), which the applicant has recently registered, improves the processing technology using solid rubber and the loading characteristics of silica. A technique for the production of a high silica content masterbatch has been described that constitutes a chemically treated technique for hazardous chemicals.

       However, the silica masterbatch by the said method has the following problems. First, the above silica master batch manufacturing method is manufactured with rubber processing equipment, which shortens the lifespan of the processing equipment due to silica wear, and incurs additional costs. Second, the time required for binding because the rubber is used as a binder. The longer the productivity, the lower the productivity, and because the third silica is scattered in a large amount of manufacturing process, there is a problem that can not improve the working environment of the manufacturing plant, the fourth silica master batch manufactured by such a manufacturing process than the unit price of silica itself There have been problems that cause the increase in manufacturing costs of the rubber products using the same by more than two times.

       Therefore, the present invention is to solve the above problems, first, by spraying a coating of a mixture of a silane-based coupling agent, a surfactant, a wax, a processing oil and the like as a coating agent in a high speed stirrer capable of uniformly coating the silica surface, In the next step, the binder solution prepared by using latex prepared in liquid form and emulsified liquid adhesive on the coated silica is sprayed on the surface of the binder and bound and discharged to remove moisture to shorten the manufacturing process and manufacturing time, thereby improving productivity. It is an object of the present invention to provide a latex-bound low arsenic silica composition characterized by high and a method for producing the same.

       The silica composition prepared by the above method was able to control the scattering of silica, and it is easy to disperse when applied to rubber compounding, and it can be seen that the processing time can be greatly shortened compared to the recently developed silica masterbatch or scattering silica. Could.

       Hereinafter, the present invention will be described in detail for solving the above problems.

       The present invention relates to a low arsenic silica / latex composition and a method for preparing the same, and more particularly, first, a silica surface is coated with a silica coating so as to easily bind to a latex and an emulsified liquid adhesive, and then the surface is coated. The silica is bound to a binder solution prepared using a latex and an emulsified liquid adhesive to prepare a silica / latex composition, followed by a drying step of removing moisture contained in the latex-bound low arsenic silica composition.

       The composition of the latex bound low arsenic silica composition of the present invention is as follows.

       3 to 15 parts by weight of the silica coating agent was coated with respect to 100 parts by weight of silica, and bound to 80 parts by weight of the coated silica using 80 to 150 parts by weight of a latex-containing binder solution, and then the water content was 5 to 5 at 110 to 150 ° C. It is characterized by drying at 10% by weight.

       The silica coating agent is prepared by mixing 50 to 70% by weight of the silane coupling agent, 10 to 20% by weight of the surfactant, 10 to 20% by weight of the wax, and 10 to 20% by weight of the processing oil. And the binder solution is prepared by mixing 50 to 75% by weight of the latex and 25 to 50% by weight of the emulsified liquid adhesive.

       Hereinafter, the low arsenic silica / latex composition of the present invention will be described in more detail through the following preparation method.

       The latex bound low arsenic silica composition of the present invention

       Iii) preparing a silica coating agent by mixing 50 to 70% by weight of the silane coupling agent, 10 to 20% by weight of surfactant, 10 to 20% by weight of wax, and 10 to 20% by weight of processing oil (silica coating agent manufacturing step);

       Ii) uniformly coating the silica surface by adding 3 to 15 parts by weight of the silica coating agent prepared in step iii) with respect to 100 parts by weight of silica in the sealed high speed stirrer (silica surface coating step);

       Iii) separately preparing a binder solution by mixing 50 to 75% by weight of latex and 25 to 50% by weight of the emulsified liquid adhesive (binder solution manufacturing step);

       Iii) binding 80 to 150 parts by weight of the binder solution prepared in step iv) in a high speed stirrer with respect to 100 parts by weight of silica coated in the closed high speed stirrer of step ii) (silica binding) step);

       Iii) drying the silica / latex composition bound with latex in step iii) at 110 to 150 ° C. at a moisture content of 5 to 10% by weight (drying the silica / latex composition);

        It is manufactured through.

       Step iii) of the present invention is a step of preparing a silica coating agent by mixing 50 to 70% by weight of the silane coupling agent, 10 to 20% by weight of the surfactant, 10 to 20% by weight of the wax, and 10 to 20% by weight of the processing oil. In step ii), the silica coating agent prepared in step iii) is added to 100 parts by weight of silica in a sealed high speed stirrer and sprayed in a range of 60 to 180 seconds at a stirring speed of 300 to 1500 rpm. As a uniform coating step, the silica coating agent enhances the binder effect of the latex and the emulsified liquid adhesive used as the binder.

       It is preferable to mix 50 to 70% by weight of the silane coupling agent, and when the mixing amount exceeds the above range, when applied to rubber compounding, there is no reinforcing effect according to the increase, and it is adhered with an environmentally friendly aqueous-based adhesive. There is a fear that the product is a cause of lowering the adhesive strength, and when the mixing amount is less than the above range, there is a fear that the reinforcement when the rubber compound is applied. And as said silane coupling agent, vinyl silane, such as vinyl triethoxysilane, vinyl trimethoxysilane, vinyl tri (2-methoxyethoxy) silane, 3-methacryloxypropyl trimethoxysilane, 2- ( 3,4-epoxycyclohexyl) ethyltrimethoxysilane, 3-glycidyloxypropylmethyldiethoxysilane, N-2- (aminoethyl) -3-aminopropyltrimethoxysilane, N-2- (amino Ethyl) -3-aminopropylmethyldimethoxysilane, 3-aminopropyltriethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, 3-methaptopfiltrimethoxysilane, 3-chloropropyltri One of methoxysilane and bis (triethoxy siloxane) tetrasulfane can be selected and used.

       The surfactant affects the uniform coating while reducing the amount of the silane coupling agent, and the mixing amount is preferably 10 to 20% by weight. If the mixing amount exceeds the above range, the reinforcement of the silane coupling agent to silica may be reduced. If the mixing amount is less than the above range, it is difficult to uniformly coat the silane coupling agent. Uncoated silica appears in the rubber compound may cause dispersion failure when applied. In addition, the surfactant may be anionic dioctyl sodium sulfosuccinate, benzophenone-9, or cationic ralkonium chloride, stearalkonium fluoride. chloride), nonionic Cocamide MEA, and Modified cocamide DEA.

       The waxes and the processed oils are effective in improving the dispersibility of the finally obtained silica composition and lowering the non-acidic properties, respectively, and the mixing amount thereof is preferably 10 to 20% by weight. When the mixing amount exceeds the above range, the non-acid effect and dispersibility are improved, but the silane coupling agent is relatively decreased, and thus the physical properties of the product may be deteriorated when the finally obtained silica composition is applied to the rubber compound. When the amount of each mixture is less than the above range, when the finally obtained silica composition is applied to the rubber compounding, the amount of scattering of the silica increases, which may make it difficult to achieve the object desired by the present invention. The waxes may be selected from one of PE wax, stearic acid, and polyethylene glycol (PEG). In addition, the processing oil may be a paraffinic system having a viscosity-gravity constant of 0.79 to 0.849, an aromatic system or a viscosity-specific gravity having a viscosity-gravity constant of 0.85 to 0.899. One of the naphthene systems having a viscosity-gravity constant of 0.9 or more can be used.

And in the step ii) it is preferable to uniformly coat the silica surface by adding 3 to 15 parts by weight of the silica coating agent to 100 parts by weight of silica in a sealed high speed stirrer. When the coating amount of the silica coating agent exceeds the coating amount range, it is advantageous to the binding, but when it is applied to the rubber compound, the physical properties may be reduced or cause blooming, and when the coating amount is below the coating amount range, Due to the poor binding properties, there is a fear that the amount of silica scattered when applied to rubber compounding increases.

       And the stirring speed of the high speed stirrer of step ii) is 300 ~ 1500rpm, the stirring time is preferably 60 ~ 180 seconds. If the stirring speed or the stirring time exceeds the above range, the silica may be biased toward the stirrer wall, and uniform coating may be difficult, and if the stirring speed or the stirring time is less than the above range, the coating agent may be There is a fear that a uniform coating will be difficult to shift to the side.

       Thus, the silica coated in step ii) is bound in step iii) using the binder solution prepared in step iii).

       Step iii) of the present invention is to prepare a binder solution by mixing 50 to 75% by weight of the latex and 25 to 50% by weight of the emulsified liquid pressure-sensitive adhesive, using the binder solution prepared in step iii) in step iii). 100 parts by weight of the coated silica obtained in step ii) was injected into a sealed high speed stirrer and sprayed within a stirring time range of 60 to 300 seconds at a stirring speed of 200 to 500 rpm to bind uniformly to latex and The emulsified liquid adhesive has an effect of fundamentally suppressing the scattering of silica.

       It is preferable to mix 50-75 weight% of said rubber latex. When the mixing amount exceeds the above range, it is easy to control the physical properties of the rubber product when the finally obtained silica composition is applied to the rubber compound, but there is a fear that the scattering amount of silica may increase, and the mixing amount is less than the above range. In this case, when the finally obtained silica composition is applied to the rubber compound, the scattering of the silica can be significantly reduced in the processing equipment, but there is a concern that it is difficult to control the physical properties of the rubber product. And the latex is a natural rubber (NR) latex, styrene-butadiene rubber (SBR) latex, nitrile rubber (NBR) latex, liquid isoprene rubber (LIR) latex, ethylene-vinyl acetate (solid content of 40 to 70% by weight) EVA) can be used alone or in combination of two or more. In the case of the binder, if the solid content exceeds 70% by weight, there is a concern that the even coating on the silica may be difficult, and when the solid content is 40% by weight or less, the time is long in the step of removing the moisture of the manufactured silica composition. This may occur.

       The emulsified liquid pressure-sensitive adhesive is preferably mixed 25 to 50% by weight. When the mixing amount exceeds the above range, the application of the finally obtained silica composition to rubber compounding can significantly reduce the amount of scattering in the processing equipment, but it is difficult to control the physical properties of the rubber product, and the mixing amount is less than the above range. In this case, when the finally obtained silica composition is applied to the rubber compounding, it is easy to control the physical properties of the rubber product, but there is a fear that the scattering amount of silica increases in the processing equipment and thus the working environment may not be improved. The emulsified liquid pressure-sensitive adhesive may be used by selecting one of polybutene, liquid isoprene rubber (LIR), liquid ethylene propylene diene rubber having a solid content of 30 to 80% by weight. In the case of the liquid adhesive, if the solids content exceeds 80% by weight, the viscosity is high, so that even coating on the silica may be difficult, and when the solids content is less than 30% by weight, the moisture of the manufactured silica composition is removed. There is a fear that a problem that a long time occurs in the step.

       And in the step iii), the stirring speed of the high speed stirrer is preferably 200 to 500 rpm, and the stirring time is 60 to 300 seconds. If the stirring speed or the stirring time exceeds the above range, the silica is biased toward the stirrer wall, so that uniform binding is difficult, and the binder silica may fall off, and the stirring speed or the stirring time is less than the above range. If there is a possibility that the coated silica is not scattered enough, there is a possibility that the portion that can be in contact with the binder is reduced.

       Step iii) of the present invention is preferably dried at a temperature of 110 ~ 150 ℃ the silica / latex composition prepared through the iii) to iii) step. If the drying temperature is less than 110 ℃ drying time is long, there is a risk that the productivity of the final silica composition is reduced or the design of the drying line may be long, if the drying temperature exceeds 150 ℃ drying time is shortened The productivity of the silica composition is high, reducing the manufacturing cost, but there is a concern that a yellowing phenomenon of the composition and a problem of separating the bound silica may occur.

       And the moisture content of the latex bound low arsenic silica composition is preferably dried to 5 to 10% by weight. When the moisture content of the latex-bound low arsenic silica composition is less than 5% by weight, the drying cost is not only high, but the silica itself contains 5 to 8% by weight of moisture, so drying to 5% by weight or less is not very effective. If it is more than 10% by weight, it takes a long time to remove moisture during processing when applied to the rubber compounding, and the time to vulcanize is long, there is a fear that the productivity of the rubber product is lowered as well as the physical properties of the rubber product.

       Hereinafter, the present invention will be described in detail with reference to Examples, but the present invention is not limited by Examples.

       1. Preparation of Latex Bound Low Ferric Silica Composition

       (Example 1)

       As described in the following Table 1, 70% by weight of the silane coupling agent bis (triethoxysilpropyl) tetrasulfane, 10% by weight of the surfactant comamide MEI, 10% by weight of the polyethylene glycol wax and After preparing 10% by weight of paraffin-based process oil in the processing oil at 40 ° C to prepare a silica coating agent, 100 parts by weight of silica was added to a sealed high-speed stirrer and sprayed 15 parts by weight of the silica coating agent prepared at a stirring speed of 700 rpm for 120 seconds. The coating was uniformly carried out.

       100 parts by weight of the silica coated in this way, as described in the content of [Table 1] below 75% by weight of the natural rubber latex of 50% by weight solids and 25% by weight of the liquid adhesive polybutene emulsified in 50% by weight solids After adding 80 parts by weight of the binder solution, the coated silica at a stirring speed of 300 rpm was stirred for 200 seconds, followed by binding. The silica composition thus prepared was dried in an oven at 130 ° C. for 1 hour to remove moisture, thereby preparing a low arsenic silica composition having a water content of 7 wt% or less.

       (Example 2)

       As described in Table 1 below, 60% by weight of the silane coupling agent bis (triethoxysilpropyl) tetrasulfane, 20% by weight of the surfactant, cocaramide M, 10% by weight of polyethylene glycol, which is a wax, and After preparing 10% by weight of paraffin-based process oil in the processing oil at 40 ° C. to prepare a silica coating material, 100 parts by weight of silica was added to a closed high speed stirrer and sprayed by 10 parts by weight of the silica coating material prepared at a stirring speed of 700 rpm for 100 seconds. The coating was uniformly carried out.

       As described in the following Table 1, based on 100 parts by weight of the silica coated, a binder mixed with 60% by weight of natural rubber latex with a solid content of 50% and 40% by weight of a liquid adhesive polybutene emulsified with a solid content of 50% After adding 108 parts by weight of the solution, the silica coated with a stirring speed of 300rpm was stirred for 220 seconds while binding to bind. The silica composition thus prepared was dried in an oven at 130 ° C. for 1 hour to remove moisture, thereby preparing a low arsenic silica composition having a water content of 7 wt% or less.

       (Example 3)

       As described in Table 1 below, 50% by weight of the silane coupling agent bis (triethoxysilpropyl) tetrasulfane, 20% by weight of a surfactant, cocaramide M, 15% by weight of waxed polyethylene glycol, and processed oil After preparing 15% by weight of the process oil, which is a paraffinic solvent, at 40 ° C. to prepare a silica coating material, 100 parts by weight of silica was added to a sealed high speed stirrer, and then 10 parts by weight of the silica coating material prepared at a stirring speed of 700 rpm was sprayed for 100 seconds. The coating was made.

       As described in the following Table 1, based on 100 parts by weight of the coated silica, a binder mixed with 50% by weight of the natural rubber latex of 50% of the solid content and 50% by weight of the liquid adhesive polybutene emulsified with the solid content of 50% 150 parts by weight of the solution was bound by stirring for 250 seconds while stirring the silica coated silica at a stirring speed of 300rpm. The silica composition thus prepared was dried in an oven at 130 ° C. for 1 hour to remove moisture, thereby preparing a low arsenic silica composition having a water content of 7 wt% or less.

                               TABLE 1

division Example 1 Example 2 Example 3 Silica Coating Agent (wt%) Silane coupling agent ¹⁾ 70 60 50 Surfactant ²⁾ 10 20 20 Wax ³⁾ 10 10 15 Process oil ⁴⁾ 10 10 15 Coated silica (parts by weight) Silica ⁵⁾ 100 100 100 Silica coating 15 10 10 Binder solution (% by weight) Natural rubber latex ⁶⁾ 75 60 50 Emulsified liquid adhesive ⁷⁾ 25 40 50 Bound silica (parts by weight) Coated silica 100 100 100 Binder solution 80 108 150 Time Less than 10 minutes Less than 10 minutes Less than 10 minutes Dust amount during processing none none none  1) Degussa, SI-69 2) Miwon Corp., cocamide MEA 3) Korea Polyol, PEG 40000 4) Unchanged Petroleum, Process Oil P-1 5) Rhodia, Zeosil 155 6) Natural rubber latex 7) Daelim Industrial Co., Ltd. Polybutene

       2. Preparation of Silica Masterbatch

       (Comparative Example 1)

       50% by weight of styrene-butadiene-styrene copolymer (SBR) according to the contents of the following [Table 2] with a silica composition blended through the silica master batch according to the method of the Republic of Korea Patent Publication No. 10-0154114, the applicant has already registered 100 parts by weight of the mixture and 50% by weight of the natural rubber was kneaded at 130 to 150 ° C. for 5 minutes, and then 195 parts by weight of the silica composition prepared according to the contents of [Table 3] was kneaded in the kneader for 30 minutes. A sheet-shaped silica composition was prepared using an open roll mill and a calendar at 80 ° C. The silica masterbatch itself is in the absence of dust, but in the processing process without the wearing of the mask is impossible to work and compared to the composition of the present invention was found to take more than four times the time required to manufacture.

                                   TABLE 2

division Comparative Example 1 Substrate (wt%) Natural rubber ⁴⁾ 50 Styrene-butadiene-styrene copolymer ²⁾ 50 Silica Masterbatch (parts by weight) materials 100 Silica composition 195 Dust amount during processing No work without wearing a mask Required time (minutes) 50  1) Vietnam Namsan, natural rubber (SVR 3L) 2) LG Chem, LG 503

       The silica composition was prepared according to the contents of Table 3 below.

                               TABLE 3

division Comparative Example 1 Silica Composition (wt%) Silica ¹⁾ 77 Coupling agent ²⁾ 5 Activator ³⁾ 5 Process oil ⁴⁾ 23  1) Rhodia, Zeosil 155 2) Degussa, SI-69 3) Polyol Korea, PEG 40000 4) Unchanged petroleum, process oil P-1

       According to the contents of [Table 1] and [Table 2], Examples 1 to 3 had no scattering of silica even in the process of making a silica composition, because the sealed stirrer was used, and the manufacturing process and required compared to Comparative Example 1 The time required was simple, shortened and, above all, improved working conditions. On the other hand, in Comparative Example 1, since the silica master batch is manufactured using the open roll mill and the calender which are the rubber processing apparatus described in the method of Korean Patent Publication No. 10-0154114, the dust scattering of silica is severe, and the manufacturing process and the time required are complicated. It was found that it takes a long time.

       3. Manufacture of rubber sheet

       Examples 4 to 6 and Comparative Example 1 show a rubber sheet prepared according to the contents of the following [Table 4] by using a low silica silicate / latex composition according to the present invention and powder silica according to a conventional silica masterbatch.

       (Examples 4 to 6)

       Examples 4 to 6 are 20 parts by weight of cis-1,4-butadiene rubber (BR), 30 parts by weight of natural rubber (NR), 30 parts by weight of styrene-butadiene rubber (SBR) and prepared in Examples 1 to 3 3 parts by weight of metal oxide, 1 part by weight of stearic acid, 1 part by weight of anti-aging agent, and 0.5 parts by weight of polyethylene glycol are added to each of the silica composition, and the mixture is kneaded at 90 to 120 ° C. for 7 minutes, and a thiazole vulcanization accelerator is added thereto. 1 part by weight, 1 part by weight of thiazole vulcanization accelerator and 0.05 part by weight of thiuram vulcanization accelerator were added and kneaded for 3 minutes, and 1.2 parts by weight of sulfur were added, followed by kneading for 5 minutes in an open roll mill at 70 ° C. (kneading Water constituents are listed in Table 4 below. This was pressed for 6 minutes at 150 ℃, 150 tons press to produce a rubber sheet, respectively.

       (Comparative Example 2)

       20 parts by weight of cis-1,4-butadiene rubber, 50 parts by weight of natural rubber, 30 parts by weight of styrene-butadiene rubber and 30 parts by weight of silica, 3 parts by weight of metal oxide, 1 part by weight of stearic acid, 1 part by weight of antioxidant, polyethylene glycol 0.5 and 1.5 parts by weight of a silane coupling agent were kneaded in a kneader at 90 to 120 ° C. for 20 minutes, 1 part by weight of a thiazole vulcanization accelerator, 1 part by weight of a thiazole vulcanization accelerator, and 0.05 parts by weight of a thiuram vulcanization accelerator. After kneading for 3 minutes, 1.2 parts by weight of sulfur was kneaded in an open roll mill at 70 ° C. for 5 minutes (for the components of the kneaded product, see Table 4 below). This was pressed for 6 minutes at 150 ℃, 150 ton press to prepare a rubber sheet.

                               TABLE 4

matter Usage (part by weight) Example 4 Example 5 Example 6 Comparative Example 2 Butadiene rubber A ¹⁾ 20 20 20 20 Natural rubber B ²⁾ 30 30 30 50 Styrene-butadiene rubber C ³⁾ 30 30 30 30 Silica / latex composition 50 50 50 - Silica ⁴⁾ - - - 30 Coupling Agent ⁵⁾ - - - 1.5 Metal oxide ⁶⁾ 3 3 3 3 Stearic acid ⁷⁾ One One One One Antioxidant ⁸⁾ One One One One Activator ⁹⁾ 0.5 0.5 0.5 0.5 Vulcanization Accelerator A ¹⁰⁾ One One One One Vulcanization Accelerator B ¹¹⁾ One One One One Vulcanization Accelerator C ¹²⁾ 0.05 0.05 0.05 0.05 Sulfur ¹³⁾ 1.2 1.2 1.2 1.2  1) Kumho Petrochemical, KBR 01 2) Batnamsan, SVR 3L 3) Kumho Petrochemical, SBR 1502 4) Rhodia, Zeosil 155 5) Degussa, SI-69 6) Gilcheon, ZnO 7) LG Chemical, St / A 8 ) Bayer, BHT 9) Korea Polyol, PEG 4000 10) Dongyang Steel Chemical, M (Thiazole) 11) Dongyang Steel Chemical, DM (Thiazole) 12) Dongyang Steel Chemical, TS (Thiuram) 13) Miwon Chemical, Sulfur

       In Example 4 was prepared using the silica / latex composition of Example 1, Example 5 was prepared using the silica / latex composition of Example 2, Example 6 is the silica / latex composition of Example 3 It was prepared using.

       4. Property test method

       Rubber sheets prepared according to Examples 4 to 6 and Comparative Example 2 were tested by the following method.

       Hardness: measured using the method of KS M 6518.

       Specific gravity: It was measured using an automatic specific gravity measuring device (model DMA-3) by the method of KS M 6519.

       Tensile strength: measured using the method of KS M 6518.

       Elongation rate was measured using the method of KS M 6518.

       Tear strength was measured using the method of KS M 6518.

       -NBS wear: NBS (National Bureau of standards) wear device was used to measure the wear resistance, and was calculated by the following equation. The measurement method was based on KS M 6625.

-Scattered dust: The scattered dust of this silica composition was collected by measuring the weight of silica scattered on the edges (400cm ² ) around the kneader, which is a processing equipment, during the mixing process when the composition was applied to rubber compounding.

       5. Property test result

       After the comparative tests of Examples 4 to 6 and Comparative Example 2, the results are as shown in Table 5 below.

                                 TABLE 5

division Example 4 Example 5 Example 6 Comparative Example 2 Properties unit Hardness type A 54 52 49 50 importance g / cc 1.10 1.09 1.07 1.07 The tensile strength kg / cm ² 163 156 152 155 Elongation % 670 700 735 700 Tear strength kg / cm 65 63 61 63 Wear Resistance (NBS) % 445 432 410 420 Compounding time min 10 10 10 30 Scattering dust g 0.3 or less ¹⁾ 0.1 or less ¹⁾ Not detected ²⁾ 7.7

1) Small amount scattered but very little compared to powdered silica

   2) It is impossible to collect scattered dust because almost no scattered dust is generated.

       As shown in [Table 5] Examples 4 to 6 shows the physical properties when applied to the rubber compound using a latex-bound low arsenic silica composition prepared through the present invention, using powdered silica as in Comparative Example 2 Compared to the case, it was found that there is almost no change in physical properties, and only the difference in silica content in the latex-bound low arsenic silica composition used. As described above, Examples 4 to 6 may not only be inferior in physical properties to Comparative Example 2, but also shorten the mixing time by 50% or more, thereby contributing to productivity. Particularly, Comparative Example 2 may have scattered dust as shown in the photograph of FIG. While 7.7g was detected, Examples 4 to 6 were able to maintain a comfortable working environment in which no dust was collected because no scattering dust was generated as shown in the photograph of FIG. 2.

       The latex-bound low fugitive silica composition prepared according to the present invention having the above structure reduces silica scattering more when using powdered silica, thereby improving the working environment as well as shortening the processing time for compounding. Could increase. In addition, it can be seen that due to the excellent dispersibility there is no change in physical properties compared to rubber products having the same silica content.

       And since the completion of the present invention was able to solve the scattering of silica is expected to contribute significantly to improve the working environment of the industry using silica in the future.

Claims (10)

       3 to 15 parts by weight of the silica coating agent was coated based on 100 parts by weight of silica, and bound to 80 parts by weight of the coated silica using 80 to 150 parts by weight of a latex-containing binder solution, and then the water content was 5 to 5 at 110 to 150 ° C. A latex bound low arsenic silica composition, characterized in that drying at 10% by weight.        The method of claim 1,       The silica coating agent is a latex-bound low, characterized in that 50 to 70% by weight of the silane coupling agent, 10 to 20% by weight surfactant, 10 to 20% by weight wax, 10 to 20% by weight of the processing oil Fugitive silica composition.        The method of claim 1,        The binder solution is a latex-bound low-acid silica composition, characterized in that the latex-binding low-acid silica composition is prepared by mixing 50 to 75% by weight of the latex and the emulsified liquid adhesive.         The method of claim 2,          The silane coupling agent is a vinylsilane such as vinyltriethoxysilane, vinyltrimethoxysilane, vinyltri (2-methoxyethoxy) silane, 3-methacryloxypropyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 3-glycidyloxypropylmethyldiethoxysilane, N-2- (aminoethyl) -3-aminopropyltrimethoxysilane, N-2- (aminoethyl) 3-Aminopropylmethyldimethoxysilane, 3-aminopropyltriethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, 3-metlabtopfiltrimethoxysilane, 3-chloropropyltrimethoxy A latex-bound low arsenic silica composition, characterized in that one of silane and bis (triethoxysilpropyl) tetrasulfane is selected and used.         The method of claim 2,      The surfactant is anionic dioctyl sodium sulfosuccinate, benzophenone-9, cationic ralkonium chloride, stearalkonium chloride , Latex bound low arsenic silica composition, characterized in that the use of one selected from non-ionic cocamide MEA (Modified cocamide DEA).         The method of claim 2,         The wax is latex bound low arsenic silica composition, characterized in that one selected from PE wax, stearic acid (stearic acid), polyethylene glycol (PEG) used.         The method of claim 2,         The processed oil has a viscosity-specific gravity of 0.79 to 0.849 paraffins (paraffins), aromatic specific gravity of 0.85 to 0.899 ranges or a viscosity specific gravity of more than 0.9 naphthene (naphthene) A latex-bound low arsenic silica composition, characterized in that one of the system is selected and used.        The method of claim 3, wherein        The latex is latex-bound, characterized in that one selected from natural rubber (NR) latex, styrene-butadiene rubber (SBR) latex, nitrile-based rubber (NBR) latex, ethylene-vinylacetate (EVA) emulsion Low Acid Silica Composition.        The method of claim 3, wherein        The liquid pressure-sensitive adhesive latex-bound low arsenic silica composition, characterized in that one selected from high polybutene, liquid isoprene rubber (LIR), liquid ethylene propylene diene rubber.        Iii) preparing a silica coating agent by mixing 50 to 70% by weight of the silane coupling agent, 10 to 20% by weight of surfactant, 10 to 20% by weight of wax, and 10 to 20% by weight of processing oil (silica coating agent manufacturing step);        Ii) uniformly coating the silica surface by adding 3 to 15 parts by weight of the silica coating agent prepared in step iii) with respect to 100 parts by weight of silica in the sealed high speed stirrer (silica surface coating step);        Iii) separately preparing a binder solution by mixing 50 to 75% by weight of latex and 25 to 50% by weight of the emulsified liquid adhesive (binder solution manufacturing step);        Iii) binding 80 to 150 parts by weight of the binder solution prepared in step iv) in a high speed stirrer with respect to 100 parts by weight of silica coated in the closed high speed stirrer of step ii) (silica binding) step);        Iii) drying the silica / latex composition bound with latex in step iii) at 110 to 150 ° C. at a moisture content of 5 to 10% by weight (drying the silica / latex composition); Process for producing a latex bound low arsenic silica composition, characterized in that it is prepared through.

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