CN110540753A - low-temperature-resistant silicone rubber and preparation process thereof - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
- B29C35/0805—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/392—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing sulfur
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
- B29C35/0805—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
- B29C2035/0855—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation using microwave
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
the invention discloses low-temperature-resistant silicone rubber and a preparation process thereof, and the prepared low-temperature-resistant rubber comprises the following components in parts by mass: 80-100 parts of modified methyl vinyl silica gel, 40-50 parts of white carbon black, 5-10 parts of graphene oxide, 3-5 parts of white oil, 1-3 parts of zinc stearate, 10-20 parts of organic peroxide, 1-5 parts of vulcanization aid and 0.5-1 part of composite additive, and the low-temperature resistant rubber is prepared by mixing, remixing and vulcanizing.
Description
Technical Field
the invention relates to the technical field of rubber preparation, in particular to low-temperature-resistant silicone rubber and a preparation process thereof.
background
With the continuous development of silicone rubber, people put forward higher and higher requirements on the performance of silicone rubber, so more and more scientific researchers hope to obtain silicone rubber with more excellent performance by a modification means while ensuring the original excellent characteristics of the silicone rubber, and the silicone rubber has excellent performance and a series of defects to be improved urgently, such as poor mechanical properties, easy crystallization at low temperature, poor hydrophilicity and the like, and limits the application range.
In the prior art, methyl vinyl silica gel is used as raw rubber to prepare low-temperature-resistant rubber, but the prepared low-temperature-resistant rubber has poor mechanical property and cannot be compatible with the rubber.
Disclosure of Invention
In order to solve the problems, the invention provides low-temperature-resistant silicone rubber and a preparation process thereof.
The invention provides low-temperature-resistant silicone rubber which comprises the following components in parts by weight: 80-100 parts of modified methyl vinyl silica gel, 40-50 parts of white carbon black, 5-10 parts of graphene oxide, 3-5 parts of white oil, 1-3 parts of zinc stearate, 10-20 parts of organic peroxide, 1-5 parts of vulcanization aid and 0.5-1 part of composite additive.
Preferably, the complex additive comprises zinc oxide, 2-mercaptobenzimidazole and dioctyl adipate.
Preferably, the organic peroxide comprises benzoyl peroxide.
Preferably, the vulcanization aid comprises, for example, triallyl cyanurate, triallyl isocyanurate.
Preferably, the preparation method of the modified methyl vinyl silica gel comprises the following steps: mixing the methyl vinyl silica gel, thioglycollic acid and a photocatalyst, and carrying out a mercapto-alkenyl click chemical reaction under the excitation of ultraviolet light to obtain the modified methyl vinyl silica gel.
preferably, the feeding molar ratio of the methyl vinyl silica gel to the thioglycolic acid is 1: 1.5, based on the vinyl group in the methylvinyl silica gel as 1.
Preferably, the preparation method of the low temperature resistant silica gel comprises the following steps: s1, mixing, namely mixing modified methyl vinyl silica gel with zinc stearate, adding a uniformly dispersed graphene oxide organic solution, ultrasonically stirring, evaporating an organic solvent, adding white carbon black, white oil and a composite additive by 3-4 times, performing heat treatment at 60-90 ℃ for 10-30min, vacuumizing, discharging glue after 20-40 min, thinly passing the glue stock through an open rubber mixing mill for 2-4 times, and filtering in a rubber filter to obtain a clean and impurity-free glue stock; s2, remilling, heating to restore the plasticity of the rubber material obtained in the S1, adding organic peroxide and an auxiliary crosslinking agent, thinly passing for 10-15 times, and rolling and discharging; s3, vulcanizing, namely vulcanizing the rubber material obtained in the step S2 by using microwave steam to obtain the low-temperature-resistant rubber.
preferably, the vulcanization temperature of the microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20 min.
the traditional silicon rubber has the advantages that the molecular chain flexibility is large, the intermolecular force is low, the glass transition temperature is low and is about-128 ℃, but the molecular chain structure of the silicon rubber is regular, the crystallization phenomenon is easy to occur at low temperature, the thioglycolic acid group is introduced on the side chain, and the polar functional group is introduced into the side chain of the free radical reaction through the click chemical reaction, so that the regularity of the rubber molecular chain is damaged, the glass transition temperature Tg of the silicon rubber is obviously improved, and the low temperature resistance is stronger, and the reasons are as follows: after the thioglycollic acid is grafted, the regularity and symmetry of a molecular chain are destroyed, so that the internal rotation of the molecular chain is hindered, and the movement of the molecular chain is inhibited; carboxyl in thioglycollic acid is a polar group, and the polar group introduced into the side chain increases the interaction force between molecular chain segments and also inhibits the movement of the chain segments; the carboxyl group forms a hydrogen bond, the Tg of the silica gel is increased, the molecular chain of the silicone rubber before modification is nonpolar, the interaction force with the polar nano filler is small, and meanwhile, the main chain of the silicone rubber molecule in the rubber compound and the hydroxyl on the surface of the filler form the hydrogen bond, so that the rubber compound is easy to structure, but the modified silicone rubber has the carboxyl polar group, so that the interface interaction force between the silica gel and the filler is improved, the Payne effect is effectively reduced, the mechanical strength is improved, and the surface hydrophilicity is also improved due to the carboxyl group.
In the scheme, the adding amount of thioglycolic acid needs to be strictly controlled, when the thioglycolic acid with the molar weight of 1:1 is added, the silica gel generates obvious crosslinking phenomenon and brings serious influence on the subsequent processing of the silica gel, and the reason for analyzing the crosslinking phenomenon is that the crosslinking phenomenon is inhibited by adding excessive thioglycolic acid because the mercapto-alkene reaction is an active free radical reaction and the double bond free radicals generated by the attack of the free radicals on double bonds generate coupling crosslinking. When the mercapto reagent is excessive, the side reactions such as main chain degradation are serious because the silica gel main chain is not acid-resistant, and the molar ratio of the double bond to the thioglycolic acid is finally determined to be 1:3 by comprehensively considering various factors.
In order to improve the crosslinking efficiency of peroxide, accelerate the vulcanization speed, reduce the decomposition temperature of the peroxide and maintain the excellent performance of vulcanized rubber, the proposal uses vulcanization aids triallyl cyanurate and triallyl isocyanurate to vulcanize the rubber, the molecules of the vulcanization aids contain 2 or more unsaturated groups, in the presence of free radicals, these unsaturated groups can polymerize to form resin-like reinforcing materials, the elastic modulus of the rubber material is increased to a greater degree than that of the rubber material which is singly used with peroxide, the coagent is polymerized to form the multi-branched resin reinforced filler under the condition of the existence of free radicals or the coagent reacts with the free radicals of the polymer to form the branched chain of the polymer, the vulcanizing assistant and the vulcanizing agent benzoyl peroxide form a composite combination simultaneously containing a peroxide nuclear-assisted crosslinking function, so that the defect of generating a odorous byproduct when the vulcanizing assistant and the vulcanizing agent benzoyl peroxide are used alone is overcome, and the solubility and the dynamic performance of the peroxide are improved.
The acidic substance can catalyze the decomposition of the peroxide to influence the homolytic cracking of the peroxide, the reaction temperature is lower than the homolytic cracking temperature, free radicals required by crosslinking are not generated, the silica gel structure of the scheme contains carboxyl, in order to not influence the crosslinking, metal oxide ZnO is added to improve the alkalinity of the sizing material, 2-mercapto benzimidazole with small influence on the crosslinking is provided as an anti-aging agent, and dioctyl adipate is provided as a cold-resistant plasticizer to improve the cold resistance of the product.
The white oil is added to inhibit the structuring of the filler white carbon black to the silicone rubber, and the principle is to physically isolate the white carbon black from the white oil.
in the preparation process, the graphene oxide is introduced by an in-situ intercalation method in the mixing process, so that the graphene oxide and modified methyl vinyl silica gel molecules are mutually crossed and compounded, the interlayer spacing of the graphene oxide is increased due to a large number of oxygen-containing groups on the graphene oxide, and the compatibility with an organic solvent is increased, so that the graphene oxide in the composite material realizes stable dispersion of few layers or even single layer, the agglomeration phenomenon is not generated, the interface bonding effect of the graphene oxide and a silica gel matrix is enhanced, the molecular chain movement of the silica gel is influenced, the glass transition temperature of the silica gel is slightly improved, and the mechanical property of the silica gel is favorably improved; because the organosilicon rubber can be hardened and the elongation at break is reduced when being heated in air, but can be softened due to the degradation of siloxane polymer when being heated in a sealing way, and the service life of the organosilicon rubber under the sealing condition is shorter than that of air, the scheme adopts microwave steam vulcanization, overcomes the defect of slow heat transfer of hot air, and has short vulcanization time, difficult aging, thorough vulcanization and no byproduct; and the micromolecule low-boiling-point substances are removed by vacuum in the mixing process.
Compared with the prior art, the beneficial effect of this scheme is as follows:
1. Thioglycollic acid groups are introduced on side chains, and polar functional groups are introduced on side chains through a free radical reaction through a click chemical reaction, so that the regularity of rubber molecular chains is damaged, the glass transition temperature Tg of the silicone rubber is obviously improved, and the low-temperature resistance is stronger;
2. The vulcanization auxiliary agent and the vulcanizing agent benzoyl peroxide form a composite combination simultaneously containing a peroxide nuclear-assisted crosslinking function, so that the vulcanization speed is accelerated, the peroxide decomposition temperature is reduced, and the excellent performance of vulcanized rubber is maintained;
3. The metal oxide ZnO is used for improving the alkalinity of rubber materials, 2-mercaptobenzimidazole with small influence on crosslinking is provided as an anti-aging agent, dioctyl adipate is provided as a cold-resistant plasticizer to improve the cold resistance of products, and white oil is added to inhibit the filler white carbon black from structuring the silicon rubber;
4. The graphene oxide is introduced by an in-situ intercalation method, so that the graphene oxide and modified methyl vinyl silica gel molecules are mutually crossed and compounded, the interface bonding effect of the graphene oxide and a silica gel matrix is enhanced, the molecular chain movement of the silica gel is influenced, the glass transition temperature of the silica gel is increased, and the mechanical property of the silica gel is favorably improved;
5. microwave steam vulcanization is adopted, the defect of slow heat transfer of hot air is overcome, the vulcanization time is short, the aging is not easy, the vulcanization is thorough, and byproducts are not produced; and in the mixing process, small molecular low-boiling-point substances and mechanical bubbles are removed by using vacuum.
Drawings
FIG. 1 shows the results of mechanical property measurements of low temperature resistant rubbers prepared in examples 2 to 4;
FIG. 2 is a DSC spectrum of the low temperature resistant rubber prepared in example 2.
Detailed Description
The following is a detailed description of the embodiments of the present invention with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
preparing modified methyl vinyl silica gel: weighing 5g of methyl vinyl silica gel into a 150ml conical flask, adding 50ml of tetrahydrofuran, stirring until the mixture is fully dissolved, adding mercaptopropionic acid according to the molar ratio of vinyl to mercapto of 1:1.3, simultaneously adding 1wt% of photocatalyst DMPA, stirring until the mixture is fully mixed, placing the mixture under ultraviolet light to initiate a mercapto-alkene click chemical reaction, and after the reaction is finished, carrying out rotary evaporation on the tetrahydrofuran to obtain the modified methyl vinyl.
Example 2
Preparing low-temperature-resistant rubber:
S1, mixing: kneading 80g of modified methyl vinyl silica gel and 1g of zinc stearate as a release agent in a vacuum kneader for 3-5 minutes, firstly adding 5g of graphene oxide into tetrahydrofuran as an organic solvent, performing ultrasonic treatment for 5 minutes to form uniform and stable dispersion liquid, then adding the dispersion liquid into the kneaded silica gel, continuing to perform ultrasonic stirring, gathering the modified methyl vinyl silica gel into a graphene oxide lamellar structure in an intercalation form, ensuring the entropy balance of a system by continuously desorbing solvent molecules, finally forming a stable intercalation structure, removing the solvent by rotary evaporation to obtain a graphene oxide/rubber composite material, adding 40g of white carbon black, 3g of white oil, 0.1g of zinc oxide, 0.2g of 2-mercaptobenzimidazole, 0.1g of dioctyl adipate and uniformly stirring and mixing at the speed of 10-50 r/min for 4 times, performing heat treatment for 10-30 minutes at the temperature of 60-90 ℃, then vacuumizing to-0.07-0.05 Mpa for 30-60 minutes, discharging the rubber, thinly passing the rubber on an open rubber mixing mill for 3-5 times, and filtering on a rubber filter to obtain the clean rubber without impurities;
S2, remilling: heating to restore plasticity of the silicone rubber, when the rubber material becomes soft and smooth, adding 10g of benzoyl peroxide and 1g of triallyl cyanurate, performing thin passing for 8-10 times, and rolling and discharging;
S3, vulcanization: adjusting the conditions that the vulcanization temperature of microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20min, and vulcanizing the colloid to obtain the low-temperature resistant rubber.
Example 3
Preparing low-temperature-resistant rubber:
S1, mixing: kneading 100g of modified methyl vinyl silica gel and 3g of release agent zinc stearate in a vacuum kneader for 3-5 minutes, firstly adding 10g of graphene oxide into organic solvent tetrahydrofuran, performing ultrasonic treatment for 5 minutes to form uniform and stable dispersion liquid, then adding the dispersion liquid into the kneaded silica gel, continuing to perform ultrasonic stirring, gathering the modified methyl vinyl silica gel into a graphene oxide lamellar structure in an intercalation form, ensuring the entropy balance of a system by continuously desorbing solvent molecules, finally forming a stable intercalation structure, removing the solvent through rotary evaporation to obtain a graphene oxide/rubber composite material, adding 50g of white carbon black, 5g of white oil, 0.2g of zinc oxide, 0.4g of 2-mercaptobenzimidazole, 0.4g of dioctyl adipate and 10-50 r/min for 4 times, uniformly stirring and mixing, performing heat treatment for 10-30 minutes at the temperature of 60-90 ℃, then vacuumizing to-0.07-0.05 Mpa for 30-60 minutes, discharging the rubber, thinly passing the rubber on an open rubber mixing mill for 3-5 times, and filtering on a rubber filter to obtain the clean rubber without impurities;
S2, remilling: heating to restore plasticity of the silicone rubber, when the rubber material becomes soft and smooth, adding 20g of benzoyl peroxide and 5g of triallyl cyanurate, performing thin passing for 8-10 times, and rolling and discharging;
S3, vulcanization: adjusting the conditions that the vulcanization temperature of microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20min, and vulcanizing the colloid to obtain the low-temperature resistant rubber.
Example 4
Preparing low-temperature-resistant rubber:
s1, mixing: kneading 80g of modified methyl vinyl silica gel and 2g of zinc stearate as a release agent in a vacuum kneader for 3-5 minutes, firstly adding 8g of graphene oxide into tetrahydrofuran as an organic solvent, performing ultrasonic treatment for 5 minutes to form uniform and stable dispersion liquid, then adding the dispersion liquid into the kneaded silica gel, continuing to perform ultrasonic stirring, gathering the modified methyl vinyl silica gel into a graphene oxide lamellar structure in an intercalation form, ensuring the entropy balance of a system by continuously desorbing solvent molecules, finally forming a stable intercalation structure, removing the solvent by rotary evaporation to obtain a graphene oxide/rubber composite material, adding 45g of white carbon black, 4g of white oil, 0.2g of zinc oxide, 0.3g of 2-mercaptobenzimidazole, 0.3g of dioctyl adipate and uniformly stirring and mixing at the speed of 10-50 r/min for 4 times, performing heat treatment for 10-30 minutes at the temperature of 60-90 ℃, then vacuumizing to-0.07-0.05 Mpa for 30-60 minutes, discharging the rubber, thinly passing the rubber on an open rubber mixing mill for 3-5 times, and filtering on a rubber filter to obtain the clean rubber without impurities;
S2, remilling: heating to recover the plasticity of the silicone rubber, when the rubber material becomes soft and smooth, adding 15g of benzoyl peroxide and 2g of triallyl cyanurate, performing thin passing for 8-10 times, and rolling and discharging;
S3, vulcanization: adjusting the conditions that the vulcanization temperature of microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20min, and vulcanizing the colloid to obtain the low-temperature resistant rubber.
Example 5
Preparing low-temperature-resistant rubber:
S1, mixing: kneading 80g of methyl vinyl silica gel and 2g of release agent zinc stearate in a vacuum kneader for 3-5 minutes, adding 45g of white carbon black and 4g of white oil by 4 times, stirring and mixing uniformly at 10-50 r/min, then carrying out heat treatment for 10-30 minutes at 60-90 ℃, then vacuumizing to-0.07-0.05 Mpa, discharging the gel after vacuumizing for 30-60 minutes, then thinly passing the gel on an open rubber mixing mill for 3-5 times, and then filtering on a rubber filter to obtain a clean and impurity-free gel;
S2, remilling: heating to recover the plasticity of the silicone rubber, when the rubber material becomes soft and smooth, adding 15g of benzoyl peroxide and 2g of triallyl cyanurate, performing thin passing for 8-10 times, and rolling and discharging;
s3, vulcanization: adjusting the conditions that the vulcanization temperature of microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20min, and vulcanizing the colloid to obtain the low-temperature resistant rubber.
Example 6
the mechanical property of the low-temperature resistant rubber prepared by the scheme is detected, the result is shown in figure 1, the mechanical property is good, and the DSC analysis is carried out on the prepared low-temperature resistant rubber, the result is shown in figure 2, which shows that the low-temperature resistant rubber is not crystallized at low temperature and has strong low-temperature resistance.
The above mentioned matters are not related, and all the matters are applicable to the prior art.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (8)
1. the low-temperature-resistant silicone rubber is characterized by comprising the following components in parts by weight: 80-100 parts of modified methyl vinyl silica gel, 40-50 parts of white carbon black, 5-10 parts of graphene oxide, 3-5 parts of white oil, 1-3 parts of zinc stearate, 10-20 parts of organic peroxide, 1-5 parts of vulcanization aid and 0.5-1 part of composite additive.
2. the low temperature resistant silicone rubber according to claim 1, wherein the complex additive comprises zinc oxide, 2-mercaptophenylimidazole, and dioctyl adipate.
3. The low temperature resistant silicone rubber according to claim 1, wherein the organic peroxide comprises benzoyl peroxide.
4. the low temperature resistant silicone rubber according to claim 1, wherein the vulcanization aid comprises one or more of triallyl cyanurate and triallyl isocyanurate.
5. The low temperature resistant silicone rubber according to claim 1, wherein the preparation method of the modified methyl vinyl silicone rubber comprises the following steps: mixing the methyl vinyl silica gel, thioglycollic acid and a photocatalyst, and carrying out a mercapto-alkenyl click chemical reaction under the excitation of ultraviolet light to obtain the modified methyl vinyl silica gel.
6. The low-temperature-resistant silicone rubber according to claim 5, wherein the molar ratio of methyl vinyl silica gel to thioglycolic acid is 1:1.3, based on the vinyl group in the methyl vinyl silica gel as 1.
7. The preparation process of the low-temperature-resistant silicone rubber according to claim 1, wherein the preparation method of the low-temperature-resistant silicone rubber comprises the following steps: s1, mixing, namely mixing modified methyl vinyl silica gel with zinc stearate, adding a uniformly dispersed graphene oxide organic solution, ultrasonically stirring, evaporating an organic solvent, adding white carbon black, white oil and a composite additive by 3-4 times, performing heat treatment at 60-90 ℃ for 10-30min, vacuumizing, discharging glue after 20-40 min, thinly passing the glue stock through an open rubber mixing mill for 2-4 times, and filtering in a rubber filter to obtain a clean and impurity-free glue stock; s2, remilling, heating to restore the plasticity of the rubber material obtained in the S1, adding organic peroxide and an auxiliary crosslinking agent, thinly passing for 10-15 times, and rolling and discharging; s3, vulcanizing, namely vulcanizing the rubber material obtained in the step S2 by using microwave steam to obtain the low-temperature-resistant rubber.
8. The preparation process of low temperature resistant silicone rubber as claimed in claim 7, wherein the vulcanization temperature of the microwave steam vulcanization is 120-.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115785577A (en) * | 2022-12-07 | 2023-03-14 | 台州兴宇新材料有限公司 | Rubber composition, preparation method thereof and sealing strip |
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Application publication date: 20191206 |