CN113004702B - Silicone rubber compound and preparation method thereof - Google Patents
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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Abstract
The application belongs to the technical field of silicon rubber. The application provides a silicone rubber compound and a preparation method thereof. The silicone rubber compound comprises silicone rubber, filler, a structural control agent and a release agent. By compounding and using the fillers with different specific surface areas, the problem of powder eating of raw rubber in the preparation of the silicone rubber by a continuous production process can be effectively solved, excessive structurization in the preparation process is avoided, and the pre-kneading time is effectively shortened. By adding the structure control agent and the release agent, the technical problems of fast product structure and slow vulcanization of an automatic production line can be effectively improved. The silicone rubber compound is beneficial to improving the production efficiency, and has excellent physical properties such as hardness, tear resistance, tensile strength and elongation.
Description
Technical Field
The application belongs to the technical field of silicone rubber, and particularly relates to a silicone rubber compound and a preparation method thereof.
Background
The silicone rubber compound has excellent heat resistance, cold resistance, weather resistance, dielectricity, ozone resistance, atmospheric aging resistance and other performances, is widely applied to various industries such as electronics, electrical appliances, electric power, communication, automobiles, aviation and the like and various specific occasions, and the demand of the silicone rubber compound is steadily increased year by year. The traditional mixing type silicon rubber is generally configured on a general rubber mixing mill, and the industrial production mostly adopts a batch method production process and is carried out in a kneader or a closed mixing mill, namely, raw silicon rubber, filler and a structural control agent are processed into a mass in the kneader and then are processed for a period of time in the kneader under the protection of nitrogen or under the reduced pressure. Because the space of the kneading machine and the closed mixing mill is limited, powder needs to be put in batches, longer mixing time is needed for uniform mixing of the raw materials and heat treatment, and finished products are obtained by open mixing and filtering after vacuumizing, so that the method has the advantages of multiple working procedures, long process time, low productivity in unit time and great pollution to the field environment.
The continuous production process has high production efficiency, and is characterized in that the raw rubber, the filler and the structural control agent are stirred and mixed uniformly at a high speed and then continuously enter a screw extruder for high-speed shearing heat treatment to obtain the silicone rubber compound. However, the continuous production process is generally high in yield, short in kneading time, easy to cause insufficient wettability of the rubber compound, easy to structure in the storage process and influence the service performance.
Disclosure of Invention
In view of the above, the application provides a silicone rubber compound and a preparation method thereof, which solve the defects of the existing continuous production process for preparing the silicone rubber compound and obtain the silicone rubber compound with excellent performance.
The specific technical scheme of the application is as follows:
a silicone rubber compound comprises the following components: silicone rubber, filler, structured control agent and release agent;
the filler comprises a first filler and a second filler, wherein the specific surface area of the first filler is 130-170m 2 The specific surface area of the second filler is 190-250m 2 /g。
In the application, the filler with different specific surface areas is compounded for use, so that the problem of powder eating of raw rubber in the preparation of the silicone rubber by a continuous production process can be effectively solved, excessive structurization in the preparation process is avoided, and the pre-kneading time is effectively shortened. By adding the structure control agent and the release agent, the technical problems of fast product structuring and slow vulcanization of the product in the automatic production line can be effectively improved. The silicone rubber compound is beneficial to improving the production efficiency, and has excellent physical properties such as hardness, tear resistance, tensile strength and elongation.
Preferably, the silicone rubber comprises a first silicone rubber, and the vinyl content of the first silicone rubber is 0.23% -3.0%.
In the application, the content of the vinyl is adjusted, so that the silicon rubber compound has excellent physical property, demolding property and electrical property, especially the tearing strength of the silicon rubber can be improved, and different requirements for the performance of the compound are met.
Preferably, the silicone rubber further comprises a second silicone rubber, and the vinyl content of the second silicone rubber is 0.03-0.05%.
Preferably, the mass ratio of the first silicon rubber to the second silicon rubber is (6-7): (0-2), wherein the mass ratio of the first filler to the second filler is 2: (3-5).
Preferably, the silicone rubber is methyl vinyl silicone rubber, and the molecular weight of the silicone rubber is 550,000-700,000.
Preferably, the filler is selected from precipitated silica or fumed silica.
Preferably, the structural control agent is selected from more than two of hydroxyl-terminated polydimethylsiloxane, alkoxy silane and low molecular polysiloxane;
the viscosity of the hydroxyl-terminated polydimethylsiloxane is 20-100mPa.s, and the viscosity of the alkoxysilane or the low-molecular polysiloxane is 1-10mPa.s.
In the application, the structural control agent is prepared by compounding the structural control agents with different active groups and different high and low viscosities, so that the defects of product stickiness and poor physical properties caused by the adoption of a single structural control agent can be effectively overcome, the structural condition of the sizing material is improved, and the physical properties such as the tearing strength of the sizing material are improved.
Preferably, the structural control agent comprises hydroxyl-terminated polydimethylsiloxane and alkoxy silane;
the mass ratio of the hydroxyl-terminated polydimethylsiloxane to the alkoxy silane is (0.8-1): 2.
preferably, the release agent includes polymethylhydrosiloxane or vinyl silicone oil, stearic acid, zinc stearate, and methyl vinyl silicone rubber.
Preferably, the methyl vinyl silicone rubber in the release agent has a vinyl content of 0.05% and a molecular weight of 600,000.
Preferably, the release agent comprises 0.3-0.6 part of polymethylhydrosiloxane or vinyl silicone oil, 0.2-0.3 part of stearic acid, 0.1-0.2 part of zinc stearate, 0-0.05 part of blue paste and 100 parts of methyl vinyl silicone rubber in parts by mass.
Preferably, the composition comprises the following components in parts by weight: 30-70 parts of silicon rubber, 20-45 parts of filler, 2-5 parts of structural control agent and 4-10 parts of release agent.
In the application, the filler content is increased and the silicon rubber content is reduced, so that the silicon rubber compound with the same hardness specification and excellent performance can be produced, and the win-win purpose of shortening the process time and reducing the cost is achieved.
The application also provides a preparation method of the silicone rubber compound, which comprises the following steps: the silicone rubber, the filler, the structural control agent and the release agent are premixed, heated, kneaded into a mass and then extruded by a screw to obtain the silicone rubber compound.
Preferably, the temperature of the premixing is 120-150 ℃, and the time is 20-30 min;
the heating kneading temperature is 160-170 ℃, and the vacuum degree is less than-0.09 MPa.
In summary, the present application provides a silicone rubber compound and a method for preparing the same. The silicone rubber compound comprises silicone rubber, filler, a structural control agent and a release agent. By compounding and using the fillers with different specific surface areas, the problem of powder eating of raw rubber in the preparation of the silicone rubber by a continuous production process can be effectively solved, excessive structurization in the preparation process is avoided, and the pre-kneading time is effectively shortened. By adding the structure control agent and the release agent, the technical problems of fast product structuring and slow vulcanization of the product in the automatic production line can be effectively improved. The silicone rubber compound is beneficial to improving the production efficiency, and has excellent physical properties such as hardness, tear resistance, tensile strength and elongation.
Detailed Description
In order to make the objects, features and advantages of the present application more obvious and understandable, the technical solutions in the embodiments of the present application are clearly and completely described, and it is obvious that the embodiments described below are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The raw materials and reagents used in the examples of the present application are commercially available products. The preparation method of the release agent in the embodiment of the application is that 0.3 part of polymethylhydrosiloxane, 0.1 part of vinyl silicone oil, 0.2 part of stearic acid, 0.2 part of zinc stearate, 0.05 part of blue paste and 100 parts of methyl vinyl silicone rubber are uniformly stirred in a kneader at 80 ℃, and the stirring time is about 20min.
Example 1
Respectively adding 48 parts by weight of methyl vinyl silicone rubber with the vinyl content of 0.05 percent and the molecular weight of 60 ten thousand, 5 parts by weight of methyl vinyl silicone rubber with the vinyl content of 3.0 percent and the molecular weight of 62 ten thousand into a metering tank, uniformly mixing in a raw rubber premixing tank, 23 parts by weight of methyl vinyl silicone rubber with the specific surface area of 160m 2 Precipitated silica in a proportion of 16 parts by weight, with a specific surface area of 220m 2 And mixing the precipitated white carbon black per gram in a powder filler premixing tank, mixing 4 parts of release agent in an auxiliary agent premixing tank, and mixing 2 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 30mPa.s and 2 parts of methoxysilane with the viscosity of 5mPa.s in an oil material premixing tank for later use.
And (3) feeding the uniformly mixed materials into a group of double-screw premixers through a metering tank, setting the frequency to be 25Hz and the temperature to be 120 ℃, wherein the process is about 30min, then feeding the materials into a group of heat treatment kneading machines at the rear section, setting the rotating speed to be 30r/min and the temperature to be 160 ℃, and vacuumizing to be 0.09MPa, wherein the process is about 30min. After 200 mesh filtration, the mixture was cooled (temperature about 50 ℃ C.) and discharged to obtain sample 1. The whole production process takes about 70min, and the yield is 1000kg/h.
Taking the prepared sample 1 to perform mechanical property test according to a conventional method, and performing vulcanization time test, wherein the used vulcanizing agent is 2,5-dimethyl-2,5-di-tert-butyl peroxy hexane, the mass ratio of the material to the vulcanizing agent is 100, and the vulcanization condition is 170 ℃ and 5min. The results of the performance testing of sample 1 are shown in table 1.
Example 2
34 parts by weight of methyl vinyl silicone rubber with 0.05 percent of vinyl content and 59 ten thousand of molecular weight and 31 parts by weight of methyl vinyl silicone rubber with 0.23 percent of vinyl content and 58 ten thousand of molecular weight are respectively put into a metering tankMixing the materials evenly in a glue premixing tank, 16 parts of the mixture has the specific surface area of 170m 2 Precipitated silica in a proportion of 13 parts by weight, the specific surface area of which is 250m 2 The precipitated white carbon black/g is uniformly mixed in a powder filler premixing tank, 4 parts of release agent is uniformly mixed in an auxiliary agent premixing tank, and 0.7 part of hydroxyl-terminated polydimethylsiloxane with the viscosity of 32mPa.s and 1.3 parts of methoxysilane with the viscosity of 9mPa.s are uniformly mixed in an oil material premixing tank for later use.
And (3) feeding the uniformly mixed materials into a group of double-screw premixers through a metering tank, setting the frequency to be 25Hz and the temperature to be 120 ℃, wherein the process is about 20min, then feeding the materials into a group of heat treatment kneading machines at the rear section, setting the rotating speed to be 30r/min and the temperature to be 160 ℃, and vacuumizing to be 0.09MPa, wherein the process is about 30min. After 200 mesh filtration, the mixture was cooled (at about 50 ℃ C.) and discharged to obtain sample 2. The whole production process takes about 60min, and the yield is 1200kg/h.
Taking the prepared sample 2 to perform mechanical property test according to a conventional method, and performing vulcanization time test, wherein the used vulcanizing agent is 2,5-dimethyl-2,5-di-tert-butyl peroxy hexane, the mass ratio of the materials to the vulcanizing agent is 100, and the vulcanization condition is 170 ℃ and 5min. The results of the performance testing of sample 2 are shown in table 1.
Example 3
According to parts by weight, 66 parts of methyl vinyl silicone rubber with 0.04 percent of vinyl content and 61 ten thousand of molecular weight and 2 parts of methyl vinyl silicone rubber with 1.0 percent of vinyl content and 62 ten thousand of molecular weight are respectively put into a metering tank and are uniformly mixed in a raw rubber premixing tank, and 14 parts of methyl vinyl silicone rubber with 150m specific surface area 2 Precipitated silica in a proportion of 10 parts by weight, with a specific surface area of 210m 2 The precipitated silica/g is uniformly mixed in a powder filler premixing tank, 5.8 parts of release agent is uniformly mixed in an auxiliary agent premixing tank, and 1 part of hydroxyl-terminated polydimethylsiloxane with the viscosity of 32mPa.s and 1.2 parts of methoxysilane with the viscosity of 6mPa.s are uniformly mixed in an oil material premixing tank for later use.
And (3) feeding the uniformly mixed materials into a group of double-screw premixers through a metering tank, setting the frequency to be 25Hz and the temperature to be 120 ℃, wherein the process is about 20min, then feeding the materials into a group of heat treatment kneaders at the rear section, setting the rotating speed to be 30r/min and the temperature to be 160 ℃, and vacuumizing to be 0.09MPa, wherein the process is about 20min. After 200 mesh filtration, the mixture was cooled (at about 50 ℃ C.) and discharged to obtain sample 3. The whole production process takes about 60min, and the yield is 1300kg/h.
And (3) taking the prepared sample 3 to perform mechanical property test according to a conventional method, and performing vulcanization time test, wherein the used vulcanizing agent is 2,5-dimethyl-2,5-di-tert-butyl peroxy hexane, the mass ratio of the material to the vulcanizing agent is 100, and the vulcanization condition is 170 ℃ and 5min. The results of the performance test of sample 3 are shown in table 1.
Example 4
Respectively adding 63 parts by weight of methyl vinyl silicone rubber with the vinyl content of 0.26 percent and the molecular weight of 63 ten thousand into a metering tank, uniformly mixing in a raw rubber premixing tank, and 16 parts by weight of methyl vinyl silicone rubber with the specific surface area of 150m 2 Precipitated silica in g, 12 parts specific surface area 198m 2 And mixing precipitated white carbon black per gram in a powder filler premixing tank, mixing 6 parts of release agent in an auxiliary agent premixing tank, and mixing 1.5 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 25mPa.s and 1.5 parts of methoxysilane with the viscosity of 7mPa.s in an oil material premixing tank for later use.
And (3) feeding the uniformly mixed materials into a group of double-screw premixers through a metering tank, setting the frequency to be 25Hz and the temperature to be 120 ℃, wherein the process is about 20min, then feeding the materials into a group of heat treatment kneading machines at the rear section, setting the rotating speed to be 30r/min and the temperature to be 160 ℃, and vacuumizing to be 0.09MPa, wherein the process is about 30min. After 200 mesh filtration, the mixture was cooled (temperature about 50 ℃ C.) and discharged to obtain sample 4. The whole production process takes about 60min, and the yield is 1300kg/h.
And (3) taking the prepared sample 4 to perform mechanical property test according to a conventional method, and performing vulcanization time test, wherein the used vulcanizing agent is 2,5-dimethyl-2,5-di-tert-butyl peroxy hexane, the mass ratio of the material to the vulcanizing agent is 100, and the vulcanization condition is 170 ℃ and 5min. The results of the performance testing of sample 4 are shown in table 1.
Comparative example 1
Respectively adding 48 parts by weight of methyl vinyl silicone rubber with the vinyl content of 0.05 percent and the molecular weight of 60 ten thousand, 5 parts by weight of methyl vinyl silicone rubber with the vinyl content of 3.0 percent and the molecular weight of 62 ten thousand into a metering tank, uniformly mixing in a raw rubber premixing tank, 39 parts by weight of methyl vinyl silicone rubber with the specific surface area of 220m 2 The precipitated white carbon black is put in a powder filler premixing tankAnd (2) uniformly mixing, namely uniformly mixing 4 parts of release agent in an additive premixing tank, and uniformly mixing 2 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 30mPa.s and 2 parts of methoxysilane with the viscosity of 5mPa.s in an oil premixing tank for later use.
And (3) feeding the uniformly mixed materials into a group of double-screw premixers through a metering tank, setting the frequency to be 25Hz and the temperature to be 120 ℃, wherein the process is about 50min, then feeding the materials into a group of heat treatment kneading machines at the rear section, setting the rotating speed to be 30r/min and the temperature to be 160 ℃, and vacuumizing to be 0.09MPa, wherein the process is about 30min. After 200 mesh filtration, the mixture was cooled (temperature about 50 ℃ C.) and discharged to obtain sample 5. The whole production process takes about 90min, and the yield is 1000kg/h.
Taking the prepared sample 5 to perform mechanical property test according to a conventional method, and performing vulcanization time test, wherein the used vulcanizing agent is 2,5-dimethyl-2,5-di-tert-butyl peroxy hexane, the mass ratio of the material to the vulcanizing agent is 100, and the vulcanization condition is 170 ℃ and 5min. The results of the performance test of sample 5 are shown in table 1.
Comparative example 2
Respectively adding 48 parts by weight of methyl vinyl silicone rubber with the vinyl content of 0.05 percent and the molecular weight of 60 ten thousand, 5 parts by weight of methyl vinyl silicone rubber with the vinyl content of 3.0 percent and the molecular weight of 62 ten thousand into a metering tank, uniformly mixing in a raw rubber premixing tank, 23 parts by weight of methyl vinyl silicone rubber with the specific surface area of 160m 2 Precipitated silica in a proportion of 16 parts by weight, with a specific surface area of 220m 2 And mixing the precipitated white carbon black per gram in a powder filler premixing tank, mixing 4 parts of release agent in an auxiliary agent premixing tank, and mixing 4 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 30mPa.s and an oil material premixing tank for later use.
And (3) feeding the uniformly mixed materials into a group of double-screw premixers through a metering tank, setting the frequency to be 25Hz and the temperature to be 120 ℃, wherein the process is about 50min, then feeding the materials into a group of heat treatment kneading machines at the rear section, setting the rotating speed to be 30r/min and the temperature to be 160 ℃, and vacuumizing to be 0.09MPa, wherein the process is about 30min. After 200 mesh filtration, the mixture was cooled (at a temperature of about 50 ℃) and discharged to obtain sample 6. The whole production process takes about 90min, and the yield is 1000kg/h.
And (3) taking the prepared sample 6 to perform mechanical property test according to a conventional method, and performing vulcanization time test, wherein the used vulcanizing agent is 2,5-dimethyl-2,5-di-tert-butyl peroxy hexane, the mass ratio of the material to the vulcanizing agent is 100, and the vulcanization condition is 170 ℃ and 5min. The results of the performance test of sample 6 are shown in table 1.
TABLE 1 results of performance test of products obtained in examples 1 to 4 and comparative examples 1 to 2
Table 1 shows that the silicone rubber in the rubber compound has a vinyl content of 0.23% to 3.0% and the specific surface area of the first filler is 130 to 170m 2 Per g, the specific surface area of the second filler is 190 to 250m 2 And/g, when the structural control agent is compounded by siloxane with the viscosity of 20-100mPa.s and the viscosity of 1-10mPa.s, the prepared rubber compound can keep good hardness, tensile strength, elongation and tearing strength, can effectively solve the problem of powder eating of raw rubber in the silicone rubber prepared by a continuous production process, improves the technical problems of faster product structure and slow curing of product vulcanization in an automatic production line, has excellent plasticity, effectively shortens the pre-kneading time, and can reach 1300kg/h in 60min yield, thereby greatly improving the production efficiency. Meanwhile, when the silicone rubber in examples 1-2 is compounded by the first silicone rubber and the second silicone rubber with vinyl contents of 0.23% -3.0% and 0.03-0.05%, the tear strength and plasticity of the prepared sample are improved compared with those of examples 3-4.
By comparing example 1 and comparative examples 1 to 2, when only a filler of a specific surface area is used in the rubber compound or only a siloxane of a viscosity is used as a structural control agent, the tensile strength of the sample is obviously defective, the disqualification of the rubber sample after rubber mixing seriously affects the usability, and the rubber compound requires a longer production time on the premise of achieving the same yield.
The above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
Claims (4)
1. A silicone rubber compound is characterized by comprising silicone rubber, a filler, a structural control agent and a release agent;
the silicone rubber comprises a first methyl vinyl silicone rubber and a second methyl vinyl silicone rubber, wherein the vinyl content of the first methyl vinyl silicone rubber is 0.23% -3.0%, and the vinyl content of the second methyl vinyl silicone rubber is 0.04% -0.05%;
the molecular weight of the first methyl vinyl silicone rubber is 58-62 ten thousand, and the molecular weight of the second methyl vinyl silicone rubber is 59-61 ten thousand;
the filler comprises first precipitated white carbon black and second precipitated white carbon black, and the specific surface area of the first precipitated white carbon black is 150-170m 2 The specific surface area of the second precipitated silica is 210-250m 2 /g；
The structural control agent is selected from hydroxyl-terminated polydimethylsiloxane and methoxysilane; the viscosity of the hydroxyl-terminated polydimethylsiloxane is 30-32mPa.s, and the viscosity of the methoxysilane is 5-9mPa.s;
the coating comprises, by weight, 5 parts of first methyl vinyl silicone rubber, 48 parts of second dimethyl vinyl silicone rubber, 23 parts of first precipitated white carbon black, 16 parts of second precipitated white carbon black, 2 parts of hydroxyl-terminated polydimethylsiloxane, 2 parts of methoxysilane and 4 parts of a release agent;
or the coating consists of 31 parts of first methyl vinyl silicone rubber, 34 parts of second dimethyl vinyl silicone rubber, 16 parts of first precipitated white carbon black, 13 parts of second precipitated white carbon black, 0.7 part of hydroxyl-terminated polydimethylsiloxane, 1.3 parts of methoxysilane and 4 parts of release agent in parts by weight;
or 2 parts of first methyl vinyl silicone rubber, 66 parts of second dimethyl vinyl silicone rubber, 14 parts of first precipitated white carbon black, 10 parts of second precipitated white carbon black, 1 part of hydroxyl-terminated polydimethylsiloxane, 1.2 parts of methoxysilane and 5.8 parts of a release agent;
each part of the release agent is prepared from 0.3 part of polymethylhydrosiloxane, 0.1 part of vinyl silicone oil, 0.2 part of stearic acid, 0.2 part of zinc stearate, 0.05 part of blue paste and 100 parts of methyl vinyl silicone rubber.
2. A silicone rubber compound according to claim 1, characterized in that the precipitated silica is replaced by fumed silica.
3. A method for preparing a silicone rubber compound according to any one of claims 1 to 2, characterized by comprising the steps of: the silicone rubber, the filler, the structural control agent and the release agent are premixed, heated, kneaded into a mass and then extruded by a screw to obtain the silicone rubber compound.
4. The method according to claim 3, wherein the temperature of the pre-mixing is 120-150 ℃ and the time is 20-30 min;
the heating kneading temperature is 160-170 ℃, and the vacuum degree is less than-0.09 MPa.
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