CN113896951B - Preparation method of sulfur-containing silane coupling agent with carbon black as carrier - Google Patents
Preparation method of sulfur-containing silane coupling agent with carbon black as carrier Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/548—Silicon-containing compounds containing sulfur
Abstract
The invention discloses a preparation method of a sulfur-containing silane coupling agent with carbon black as a carrier, which belongs to the technical field of chemical industry, and relates to a preparation method of a sulfur-containing silane coupling agent with carbon black as a carrier.
Description
Technical Field
The invention relates to a preparation method of a sulfur-containing silane coupling agent with carbon black as a carrier, belonging to the technical field of chemical industry.
Background
The sulfur-containing silane coupling agent is a special green rubber auxiliary agent, is mainly applied to the tire industry, has a special reinforcing function and an adhesion function for rubber materials, can improve the tear resistance of the rubber materials, reduces abrasion, can reduce the low rolling resistance of the tire, and improves the braking performance of the tire, thereby reducing fuel oil and energy conservation, being a key material indispensable for novel environment-friendly tires, and in addition, the product is also widely applied to the fields of rubber products such as shoe industry, rubber rollers, rubber sundries and the like.
At present, sulfur-containing silane coupling agent products in markets at home and abroad are classified into two types according to forms, one type is a sulfur-containing silane coupling agent liquid product, namely a sulfur-containing silane coupling agent body product, and the other type is a sulfur-containing silane coupling agent product taking carbon black as a carrier, and is commonly called solid silicon, black material sulfur-containing silane products and the like.
The solid sulfur-containing silane product with carbon black as a carrier is more convenient to operate while playing the same function as liquid, the solid silicon is easier to operate by adopting single-package net weight metering, and the single-package feeding of the solid silicon is more convenient than the dropping or pump conveying of liquid silicon; in addition, the effective component silane of the silicon-fixing is dispersed in the carbon black particles, which is more beneficial to the uniform dispersion of the silane and can also effectively prevent the silane from generating hydrolysis self-condensation phenomenon at the initial banburying stage. Therefore, solid sulfur-containing silane products with carbon black as a carrier are very popular among customers.
However, the solid sulfur-containing silane products with carbon black as a carrier also have their own disadvantages compared to liquid silicon products. The moisture in the carbon black can cause hydrolysis of the sulfur-containing silane coupling agent, so that the quality of the sulfur-containing silane coupling agent is influenced, and particularly, the sulfur-containing silane coupling agent is more seriously hydrolyzed along with the longer storage time, so that the quality guarantee period of a solid silicon product is influenced, and the quality guarantee period of the solid silicon product is shorter than that of a liquid silicon product, and the requirements of downstream users cannot be met.
In addition, the carbon black with the conventional specification is used for producing a solid sulfur-containing silane product in a mixing manner, so that the serious agglomeration phenomenon often occurs in the production process, the flowability of materials is influenced, and a pipeline is blocked, so that a production device is often stopped, and the production efficiency and the economic benefit of silicon solidification are influenced.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a sulfur-containing silane coupling agent with carbon black as a carrier, which solves the problems of shelf life and continuous production of the sulfur-containing silane coupling agent with carbon black as the carrier by controlling the quality indexes of the carbon black and the sulfur-containing silane coupling agent, especially the moisture content, pH value and viscosity index of the carbon black and the moisture content and pH value index of the sulfur-containing silane coupling agent before the carbon black and the sulfur-containing silane coupling agent are physically mixed, prolongs the shelf life of the solid silane coupling agent, improves the content of effective components in a solid silicon product, meets the higher quality requirement of downstream users on the solid silicon product, solves the problem of frequent shutdown of a production device, and improves the production efficiency, the field environment and the economic benefit of the solid silicon product.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A method for preparing sulfur-containing silane coupling agent with carbon black as carrier, which physically mixes carbon black and sulfur-containing silane coupling agent, is characterized in that before the carbon black and the sulfur-containing silane coupling agent are physically mixed, the quality indexes of the carbon black and the sulfur-containing silane coupling agent meet the following requirements:
(1) The quality index of the carbon black meets the following requirements:
moisture content: less than or equal to 0.5 percent;
pH value: 7.0-7.5;
viscosity index: qualified;
(2) The quality index of the sulfur-containing silane coupling agent meets the following requirements:
moisture content: less than or equal to 0.012 percent;
pH value: 7.0-8.0;
in the scheme of the invention, the specification of the carbon black is selected according to the requirements of customers. Can be one of series products in national standard GB/T3778 carbon black for rubber. Further, the carbon black is in the form of particles.
In the scheme of the invention, the sulfur-containing silane coupling agent is a polysulfide silane coupling agent, a mercapto silane coupling agent or a thiocarboxylate silane coupling agent. Representative examples include, but are not limited to: bis (3-propyltriethoxysilane coupling agent) polysulfide, bis (3-propyltriethoxysilane coupling agent) disulfide, bis (3-propyltriethoxysilane coupling agent) tetrasulfide, 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-mercaptopropylmethyldimethoxysilane, 3-mercaptopropylmethyldiethoxysilane, 3-mercaptopropylethoxybis (tridecylpentaethylether) silane, 3-mercaptopropyl-2, 2',2 ″ -nitrilotriethoxysilane, 3-mercaptopropylethoxybis (propylhexapolypropylether) silane, 3-hexanoylthio-1-propyltriethoxysilane, 3-octanoylthio-1-propylethoxy (2-methyl-1, 3-propyleneglycol subunit) silane, and the like.
In the scheme of the invention, the carbon black and the sulfur-containing silane coupling agent are mixed by a double-cone rotary mixer, a single-spiral conical mixer or a double-spiral conical mixer.
Further, the carbon black and the sulfur-containing silane coupling agent are physically mixed under the protection of nitrogen.
In the scheme of the invention, the mass ratio of the carbon black to the sulfur-containing silane coupling agent is 1 to 1.5 to 1, further, the mass ratio of the carbon black to the sulfur-containing silane coupling agent is 1 to 1.05 to 1, and preferably, the mass ratio of the carbon black to the sulfur-containing silane coupling agent is 1.
Before the carbon black and the sulfur-containing silane coupling agent are physically mixed, the quality index of the carbon black is controlled to meet the requirement, and preferably, the carbon black raw material meeting the quality index requirement is directly used.
Before the carbon black and the sulfur-containing silane coupling agent are physically mixed, the quality index of the carbon black is controlled to meet the requirement, and preferably, the carbon black raw material is processed to enable each quality index of the carbon black to meet the requirement.
The carbon black has stable structure, other indexes generally do not have obvious changes in the storage period, but the carbon black has rich pore structure, so that the moisture content in the air is easy to absorb, even if the purchased carbon black is in a factory, the moisture content meets the requirement, the longer the carbon black is stored in the factory, the moisture content is increased when the carbon black is reused, and the use requirement cannot be met. Generally, low structure carbon blacks have a slow rate of moisture absorption, increasing the moisture content from 0.5% to 2.0% with storage time, high structure carbon blacks have a fast rate of moisture absorption, and the moisture content can increase from 0.8% to 5.0% with storage time. Therefore, it is preferable that the carbon black raw material is subjected to a moisture removal treatment before the carbon black is physically mixed with the sulfur-containing silane coupling agent so that the moisture content index of the carbon black can meet the requirement.
Before the carbon black and the sulfur-containing silane coupling agent are physically mixed, the carbon black raw material needs to be subjected to moisture removal treatment, and further, the carbon black raw material is subjected to moisture removal treatment in a drying mode.
The invention relates to a preparation method of a sulfur-containing silane coupling agent with carbon black as a carrier, which comprises the following specific steps:
s1: preparing carbon black and a sulfur-containing silane coupling agent, wherein the quality indexes of the carbon black and the sulfur-containing silane coupling agent meet the following requirements:
(1) The quality index of the carbon black meets the following requirements:
pH value: 7.0-7.5;
viscosity index: qualified;
other quality indexes meet the requirements of customers.
(2) The quality index of the sulfur-containing silane coupling agent meets the following requirements:
moisture content: less than or equal to 0.012 percent;
pH value: 7.0-8.0;
other quality indexes meet the requirements of customers.
S2: drying the carbon black to make the moisture content of the dried carbon black less than or equal to 0.5 percent.
S3: and (3) physically mixing the carbon black with the sulfur-containing silane coupling agent.
Further, the carbon black drying and physical mixing are carried out in the same equipment, the equipment has the drying function and the mixing function, and preferably, a double-cone rotary dryer, a single-spiral conical mixing dryer and a double-spiral conical mixing dryer are selected.
Further, the drying of the carbon black, physical mixing, was carried out in different equipment. The carbon black is dried in a drying apparatus, cooled or not after the drying is finished, and then transferred to a mixing apparatus. Preferably, the carbon black is dried in a rotating drum dryer and then transferred to a mixing apparatus.
Further, the carbon black and the sulfur-containing silane coupling agent are physically mixed under the protection of nitrogen.
Before the carbon black and the sulfur-containing silane coupling agent are physically mixed, the quality index of the sulfur-containing silane coupling agent is controlled to meet the requirement, and preferably, the carbon black raw material meeting the quality index requirement is directly used.
Before the carbon black and the sulfur-containing silane coupling agent are physically mixed, the quality index of the sulfur-containing silane coupling agent is controlled to meet the requirement, and preferably, the sulfur-containing silane coupling agent is processed, so that all quality indexes of the sulfur-containing silane coupling agent meet the requirement.
At present, the sulfur-containing silane coupling agent is produced in large industry by a phase transfer catalyst aqueous solution preparation method, so that the sulfur-containing silane coupling agent product inevitably contains water.
Further, the moisture in the sulfur-containing silane coupling agent is removed, preferably by using a water removal agent, which includes but is not limited to: anhydrous sodium sulfate, anhydrous magnesium sulfate, calcium chloride, molecular sieves and the like.
Further, the sulfur-containing silane coupling agent is preferably subjected to water removal by distillation, molecular distillation, blade distillation, or the like.
Further, the pH index of carbon black was measured in accordance with GB/T3780.7.
Furthermore, the moisture content index of the carbon black is measured according to GB/T3780.8.
Further, the measurement of the moisture content index of carbon black was carried out as follows:
weighing quantitative carbon black and an extracting agent, soaking the carbon black in the extracting agent to extract water, measuring the water content in an extracting solution by adopting a Karl Fischer reagent method, simultaneously measuring the water content of a blank sample of the extracting agent, and calculating to obtain the water content in the carbon black. Preferably, the extractant is absolute ethanol. Preferably, the extractant is a sulfur-containing silane coupling agent.
Further, the measurement of the viscosity index of carbon black was carried out by the following steps:
a1 To make a small sample mix of carbon black and sulfur-containing silane coupling agent: drawing a certain amount of representative carbon black sample from the carbon black raw material packaging bag; respectively and quantitatively weighing the carbon black and the sulfur-containing silane coupling agent according to the mass production ratio of the carbon black and the sulfur-containing silane coupling agent, and then physically mixing in a small test;
a2 Pouring out the mixed sample, spreading the sample flatly and placing the sample for 10 minutes;
a3 Observe the appearance of the mixed sample and draw conclusions: if the appearance of the mixed sample has no moist feeling and no agglomeration, the viscosity index of the batch of carbon black is evaluated to be qualified; the batch was evaluated for a "fail" in the viscosity index if the mixed sample was wet in appearance and/or agglomerated.
Other quality indexes of the carbon black are carried out according to the specific provisions of the national standard GB/T3778 carbon black for rubber.
Further, the moisture content of the sulfur-containing silane coupling agent was measured by the Karl Fischer's reagent method.
Further, the pH value of the sulfur-containing silane coupling agent is extracted by an extraction method: measuring a certain amount of sulfur-containing silane coupling agent, adding the sulfur-containing silane coupling agent into a certain amount of water, stirring for a certain time, and measuring the pH value of the supernatant of the aqueous solution by using a pH meter, wherein the pH value displayed by the pH meter is the pH value of the sulfur-containing silane coupling agent.
Other quality indexes of the sulfur-containing silane coupling agent are implemented according to specific regulations of national standards, international standards, enterprise standards, conventional detection methods and the like, such as national standards GB/T30309 polysulfide silane coupling agent, HG/T5090 mercapto silane coupling agent and the like.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) The problem of short shelf life of the silicon-fixing product of the sulfur-containing silane coupling agent with carbon black as a carrier is solved, and compared with the conventional silicon-fixing product, the silicon-fixing product produced by adopting the technical scheme of the invention has the advantages of long shelf life, high content of effective components and low heating decrement index.
(2) The problems that production equipment is shut down, metering cannot be carried out and the like due to material agglomeration in the production process of the silicon-fixing product of the sulfur-containing silane coupling agent taking carbon black as a carrier are solved, and the technical scheme of the invention can be used for continuously producing the silicon-fixing product without pipeline blockage; and the agglomeration phenomenon is avoided, the carbon black and the sulfur-containing silane coupling agent are uniformly mixed, and the uniformity of the product quality is ensured.
(3) By adopting the technical scheme of the invention, after the carbon black and the sulfur-containing silane coupling agent are physically mixed, the low boiling point is not required to be removed by heating so as to control the heating decrement index of the solid silicon product to be qualified. In addition, the moisture content in the carbon black and the sulfur-containing silane coupling agent is controlled before the carbon black and the sulfur-containing silane coupling agent are physically mixed, so that the possibility of hydrolysis and polymerization of the sulfur-containing silane coupling agent serving as an effective component caused by the high moisture content in the raw materials is reduced, the dispersion of the silicon-fixing product in rubber compound is prevented from being influenced by the content reduction of the sulfur-containing silane coupling agent serving as the effective component and the hydrolyzed high polymer of the sulfur-containing silane coupling agent, and the condition that the heating decrement index of the silicon-fixing product is unqualified due to the increase of the content of ethanol generated after the hydrolysis of the sulfur-containing silane coupling agent is avoided.
(4) By adopting the technical scheme of the invention, the moisture content index of the carbon black entering the factory does not need to be controlled strictly,
the moisture of the carbon black raw material can be removed before the carbon black and the sulfur-containing silane coupling agent are physically mixed, so that the moisture content index of the carbon black meets the requirement, and the carbon black raw material can be supplied with more selectivity by adopting the measures; in addition, the problem that the carbon black cannot be used due to the increase of the moisture content caused by the long storage period is avoided, and the special requirement on the storage environment of the carbon black is reduced. Therefore, the technical scheme of the invention is particularly suitable for flexibly scheduling and purchasing carbon black in solid silicon production enterprises, the storage period of the carbon black can be longer, and the storage capacity can be larger. The problem of shutdown of silicon fixation production and the like caused by the influence of high-humidity weather such as plum rain season on the moisture content of carbon black is not worried about.
(5) By adopting the technical scheme of the invention, whether the materials have the phenomenon of agglomeration or dampness is tested in a small scale before the premise of solid silicon mixing production by checking and accepting the viscosity index of the carbon black, so that the blockage in large-scale production is avoided, and the production efficiency is improved.
(6) According to the technical scheme, the pH index of the carbon black is strictly controlled to be 7.0-7.5, and compared with acid carbon black or alkaline carbon black with the pH value higher than 7.5, the carbon black is close to a neutral alkalescent environment, the hydrolysis tendency of the sulfur-containing silane coupling agent as an effective component is reduced, the content of the sulfur-containing silane coupling agent as an effective component is increased, the heating decrement index of a solid silicon product is reduced, and the quality guarantee period of the solid silicon product is prolonged.
(7) According to the technical scheme, the pH index of the sulfur-containing silane coupling agent is strictly controlled to be 7.0-8.0, and compared with the sulfur-containing silane coupling agent with the pH index lower than 7 and with acidity, the quality guarantee period of a solid silicon product produced by the alkalescent sulfur-containing silane coupling agent close to neutrality is longer; the moisture content of the sulfur-containing silane coupling agent is controlled to be less than or equal to 0.012 percent, which is more beneficial to improving the effective content of the sulfur-containing silane coupling agent in the solid silicon product and reducing the heating decrement index of the solid silicon product.
Drawings
FIG. 1 is a flow chart of the present invention as a whole.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; rather than all embodiments, are based on the embodiments of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in a specific case to those of ordinary skill in the art.
The measurement methods in the quality control indexes in the following examples and comparative examples were carried out according to the following specifications, respectively:
measurement method 1: the pH index of the carbon black is determined according to GB/T3780.7.
Measurement method 2: the method for measuring the moisture content index of the carbon black is carried out according to GB/T3780.8, and is the method A; the method is carried out as follows:
weighing 1g of carbon black and 100g of absolute ethyl alcohol, soaking the carbon black for 4h by the absolute ethyl alcohol, then measuring the moisture content in the ethyl alcohol by adopting a Karl Fischer reagent method, simultaneously making the moisture content of an absolute ethyl alcohol blank sample, and calculating to obtain the moisture content in the carbon black.
Measurement method 3: the measurement of the viscosity index of carbon black is carried out according to the following steps:
a1 Small mix sample): extracting a carbon black sample from the carbon black raw material packaging bag; respectively and quantitatively weighing carbon black and a sulfur-containing silane coupling agent sample, and then mixing in a small test; note: the proportion of the carbon black and the sulfur-containing silane coupling agent in a small sample is consistent with that in large-scale production;
a2 Pouring out, spreading and standing the mixed sample for 10 minutes;
a3 Observe the appearance of the mixed sample and draw conclusions: if the appearance of the mixed sample has no moist feeling and no agglomeration, the viscosity index of the batch of carbon black is evaluated to be qualified; the batch was evaluated for a "off-spec" viscosity index if the mixed sample was wet in appearance and/or agglomerated.
Measurement method 4: other quality indexes of the carbon black are carried out according to specific terms of national standard GB/T3778 'carbon black for rubber'.
Measurement method 5: the moisture content of the sulfur-containing silane coupling agent was measured by the Karl Fischer's reagent method.
Measurement method 6: the pH value of the sulfur-containing silane coupling agent is measured by an extraction method, 10g of the sulfur-containing silane coupling agent is weighed and added into 90g of water, after stirring for 2h, the pH value of the supernatant of the aqueous solution is measured by using a pH meter, and the pH value displayed by the pH meter is the pH value of the sulfur-containing silane coupling agent.
Measurement method 7: other quality indexes of the sulfur-containing silane coupling agent are implemented according to specific regulations of national standards, international standards, enterprise standards, conventional detection methods and the like, such as national standards GB/T30309 polysulfide silane coupling agent, HG/T5090 mercapto silane coupling agent and the like.
Example 1
Weighing 2 raw materials, wherein the mass indexes of N330 carbon black and bis (3-propyltriethoxysilane) polysulfide Si17 are respectively as follows:
(1) The detection result of the N330 carbon black quality index is as follows:
moisture content: 0.3%, test method A;
pH value: 7.2;
viscosity index: qualified, and mixing according to a mass ratio of 1;
other quality indexes meet the requirements of national standard GB/T3778 'carbon black for rubber'.
(2) The detection result of the quality index of the bis (3-propyltriethoxysilane) polysulfide Si17 is as follows:
moisture content: 0.009%;
pH value: 7.3;
other quality indexes meet the requirements of GB/T30309 polysulfide silane coupling agent.
The method comprises the following steps of physically mixing N330 carbon black and bis (3-propyltriethoxysilane) polysulfide Si17 in a mass ratio of 1.
The produced solid silicon product is detected according to GB/T30309 polysulfide silane coupling agent. The results are shown in Table 1.
Comparative example 1
In comparison with example 1, the carbon black of comparative example 1 using N330 was the carbon black of example 1 stored for 1 month, and the moisture content increased to 0.7%, and the rest was the same. The results are shown in Table 1.
Comparative example 2
The pH test result of the N330 carbon black used in comparative example 2 was 7.7 as compared with example 1, and the rest was the same. The results are shown in Table 1.
Comparative example 3
The viscosity index test result of the N330 carbon black used in comparative example 3 was failed compared to that of example 1, and the rest was the same. The results are shown in Table 1.
Comparative example 4
In comparison with example 1, comparative example 4 used bis (3-propyltriethoxysilane) polysulfide Si17 whose moisture content was measured was 0.09%, and the rest was the same. The results are shown in Table 1.
Comparative example 5
The pH test result of the bis (3-propyltriethoxysilane) polysulfide Si17 used in comparative example 5 was 6.2, as compared with example 1, and the rest was the same. The results are shown in Table 1.
Example 2
The carbon black of example 2 was stored for 1 month as the carbon black of example 1, the moisture content was increased to 0.7% and the sulfur-containing silane coupling agent was the same as in example 1, as compared with example 1.
The method comprises the following steps of putting N330 carbon black into a double-cone rotary dryer, drying the carbon black to the moisture content of less than 0.5%, spraying bis (3-propyltriethoxysilane) polysulfide Si17 into a mixer in a spraying mode, and physically mixing, wherein the mass ratio of the carbon black to the bis (3-propyltriethoxysilane) polysulfide Si17 is 1.
The produced solid silicon product is detected according to GB/T30309 polysulfide silane coupling agent. The results are shown in Table 1.
TABLE 1 solid silicon product test results
According to the detection results shown in the table 1, it can be seen from the above examples and comparative examples that before the carbon black and the sulfur-containing silane coupling agent are physically mixed, the indexes of moisture, pH and the like of the carbon black and the sulfur-containing silane coupling agent are controlled to meet the quality index requirements, the butanone insoluble matter content of the solid silicon product is lower, which indicates that the content of the sulfur-containing silane coupling agent serving as an active ingredient is higher, the heating decrement index of the solid silicon product is lower, after the solid silicon product is stored for one year, the butanone insoluble matter and the heating decrement index of the solid silicon product are still very low, the quality index requirements of national standard GB/T30309 polysulfide silane coupling agent are met, and no pipeline blockage or agglomeration occurs in the production process, thereby reflecting that the solid silicon product produced by adopting the technical scheme of the invention has longer shelf life, higher content of the active ingredient and lower heating decrement index. From the example 2, it can be seen that, by adopting the technical scheme of the invention, even if the moisture content of the carbon black raw material is relatively high, the carbon black is dried before the carbon black and the sulfur-containing silane coupling agent are physically mixed, so that the quality index of the carbon black meets the control requirement, the produced silicon-fixing product has low butanone insoluble substance content and low heating decrement index, and after being stored for one year, the silicon-fixing product still meets the quality index requirements of national standard GB/T30309 polysulfide silane coupling agent, and has long shelf life.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto; any person skilled in the art is within the technical scope of the present disclosure; the technical scheme and the improved concept of the invention are equally replaced or changed; are intended to be covered by the scope of the present invention.
Claims (9)
1. A method for preparing sulfur-containing silane coupling agent with carbon black as carrier, which physically mixes carbon black and sulfur-containing silane coupling agent, is characterized in that before the carbon black and the sulfur-containing silane coupling agent are physically mixed, the quality indexes of the carbon black and the sulfur-containing silane coupling agent meet the following requirements:
(1) The carbon black quality index meets the following requirements:
moisture content: less than or equal to 0.5 percent;
pH value: 7.0-7.5;
viscosity index: qualified;
(2) The quality index of the sulfur-containing silane coupling agent meets the following requirements:
moisture content: less than or equal to 0.012%;
pH value: 7.0-8.0;
wherein, the viscosity index of the carbon black is measured according to the following steps:
a1 To make a small sample mix of carbon black and sulfur-containing silane coupling agent: extracting a carbon black sample from the carbon black raw material packaging bag; respectively and quantitatively weighing the carbon black and the sulfur-containing silane coupling agent according to the mass production ratio of the carbon black and the sulfur-containing silane coupling agent, and then physically mixing small samples;
a2 Pouring out the mixed sample, flatly paving the sample, and standing the sample for 10 minutes;
a3 Observe the appearance of the mixed sample and draw conclusions: if the appearance of the mixed sample has no moist feeling and no agglomeration, the viscosity index of the batch of carbon black is evaluated to be qualified; the batch was evaluated for a "off-spec" viscosity index if the mixed sample was wet in appearance and/or agglomerated.
2. The method for producing a sulfur-containing silane coupling agent carried by carbon black according to claim 1, wherein said carbon black is in the form of particles.
3. The method according to claim 1, wherein the sulfur-containing silane coupling agent is a polysulfide silane coupling agent, a mercaptosilane coupling agent, or a thiocarboxylate silane coupling agent.
4. The method according to claim 1, wherein the carbon black is mixed with the sulfur-containing silane coupling agent by means of a double-cone rotary mixer, a single-screw conical mixer or a twin-screw conical mixer.
5. The method for preparing the sulfur-containing silane coupling agent using carbon black as a carrier according to claim 1, wherein the mass ratio of the carbon black to the sulfur-containing silane coupling agent is 1 to 1.5.
6. The method of claim 1, wherein the carbon black is subjected to a moisture removal treatment before the carbon black is physically mixed with the sulfur-containing silane coupling agent, and further wherein the carbon black is subjected to a moisture removal treatment and dried.
7. The method for preparing the sulfur-containing silane coupling agent with carbon black as a carrier according to claim 1, is characterized by comprising the following steps:
s1: preparing carbon black and a sulfur-containing silane coupling agent, wherein the quality indexes of the carbon black and the sulfur-containing silane coupling agent meet the following requirements:
(1) The carbon black quality index meets the following requirements:
pH value: 7.0-7.5;
viscosity index: qualified;
(2) The quality index of the sulfur-containing silane coupling agent meets the following requirements:
moisture content: less than or equal to 0.012%;
pH value: 7.0-8.0
S2: drying the carbon black to ensure that the moisture content of the dried carbon black is less than or equal to 0.5 percent;
s3: physical mixing, namely physically mixing the carbon black with a sulfur-containing silane coupling agent;
wherein, the viscosity index of the carbon black is measured according to the following steps:
a1 To make a small sample mix of carbon black and sulfur-containing silane coupling agent: extracting a carbon black sample from the carbon black raw material packaging bag; respectively and quantitatively weighing the carbon black and the sulfur-containing silane coupling agent according to the mass production ratio of the carbon black and the sulfur-containing silane coupling agent, and then physically mixing in a small test;
a2 Pouring out the mixed sample, spreading the sample flatly and placing the sample for 10 minutes;
a3 Observe the appearance of the mixed sample and draw conclusions: if the appearance of the mixed sample has no moist feeling and no agglomeration, the viscosity index of the batch of carbon black is evaluated to be qualified; the batch was evaluated for a "fail" in the viscosity index if the mixed sample was wet in appearance and/or agglomerated.
8. The method for preparing the sulfur-containing silane coupling agent with carbon black as a carrier according to claim 1 or 7, wherein the pH value of the sulfur-containing silane coupling agent is obtained by adopting an extraction method: measuring a certain amount of sulfur-containing silane coupling agent, adding the sulfur-containing silane coupling agent into a certain amount of water, stirring for a certain time, and measuring the pH value of the supernatant of the water solution by using a pH meter, wherein the pH value displayed by the pH meter is the pH value of the sulfur-containing silane coupling agent.
9. The method according to claim 7, wherein the drying of the carbon black and the physical mixing are performed in the same apparatus, which has both drying and mixing functions, and is a double-cone rotary dryer, a single-spiral conical mixing dryer, or a double-spiral conical mixing dryer.
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| JP2008120951A (en) * | 2006-11-14 | 2008-05-29 | Sumitomo Rubber Ind Ltd | Production method of surface-treated carbon black |
| CN101555363A (en) * | 2009-04-30 | 2009-10-14 | 上海大学 | Method for reinforcing performance of tread rubber of lorry tyre by resin acceptor modified white carbon black |
| JP2018095704A (en) * | 2016-12-09 | 2018-06-21 | 精工化学株式会社 | Silane coupling agent composition and compounding agent for rubber |
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| EP1256595A1 (en) * | 2001-05-10 | 2002-11-13 | Sika AG, vorm. Kaspar Winkler & Co. | Adhesive filled with surface-treated chalk and carbon black |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2008120951A (en) * | 2006-11-14 | 2008-05-29 | Sumitomo Rubber Ind Ltd | Production method of surface-treated carbon black |
| CN101555363A (en) * | 2009-04-30 | 2009-10-14 | 上海大学 | Method for reinforcing performance of tread rubber of lorry tyre by resin acceptor modified white carbon black |
| JP2018095704A (en) * | 2016-12-09 | 2018-06-21 | 精工化学株式会社 | Silane coupling agent composition and compounding agent for rubber |
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| "除水工艺疏水改性白炭黑及对硅橡胶力学性能";石大立 等;《广东化工》;20170915;第44卷(第355期);第20,29-31页 * |
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