CN116285365A - Foaming conductive silicon rubber and preparation method thereof - Google Patents
Foaming conductive silicon rubber and preparation method thereof Download PDFInfo
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- CN116285365A CN116285365A CN202310327955.7A CN202310327955A CN116285365A CN 116285365 A CN116285365 A CN 116285365A CN 202310327955 A CN202310327955 A CN 202310327955A CN 116285365 A CN116285365 A CN 116285365A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 99
- 238000005187 foaming Methods 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000004945 silicone rubber Substances 0.000 claims abstract description 77
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229920001971 elastomer Polymers 0.000 claims abstract description 53
- -1 methyl vinyl Chemical group 0.000 claims abstract description 53
- 239000005060 rubber Substances 0.000 claims abstract description 53
- 239000011231 conductive filler Substances 0.000 claims abstract description 47
- 239000004088 foaming agent Substances 0.000 claims abstract description 36
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 36
- 238000004073 vulcanization Methods 0.000 claims abstract description 29
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims description 60
- 239000003795 chemical substances by application Substances 0.000 claims description 59
- 229920002545 silicone oil Polymers 0.000 claims description 42
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 33
- 239000003112 inhibitor Substances 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 239000003431 cross linking reagent Substances 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 15
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 14
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 9
- 229920002554 vinyl polymer Polymers 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 150000004684 trihydrates Chemical class 0.000 claims description 5
- 229940037003 alum Drugs 0.000 claims description 3
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 claims description 3
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 2
- MQRJBSHKWOFOGF-UHFFFAOYSA-L disodium;carbonate;hydrate Chemical compound O.[Na+].[Na+].[O-]C([O-])=O MQRJBSHKWOFOGF-UHFFFAOYSA-L 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- HJFRLXPEVRXBQZ-UHFFFAOYSA-N pent-3-yn-2-ol Chemical compound CC#CC(C)O HJFRLXPEVRXBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 229910002027 silica gel Inorganic materials 0.000 description 5
- 239000000741 silica gel Substances 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 229910002011 hydrophilic fumed silica Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- UOCIZHQMWNPGEN-UHFFFAOYSA-N dialuminum;oxygen(2-);trihydrate Chemical group O.O.O.[O-2].[O-2].[O-2].[Al+3].[Al+3] UOCIZHQMWNPGEN-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- NBOCQTNZUPTTEI-UHFFFAOYSA-N 4-[4-(hydrazinesulfonyl)phenoxy]benzenesulfonohydrazide Chemical compound C1=CC(S(=O)(=O)NN)=CC=C1OC1=CC=C(S(=O)(=O)NN)C=C1 NBOCQTNZUPTTEI-UHFFFAOYSA-N 0.000 description 1
- 239000004156 Azodicarbonamide Substances 0.000 description 1
- 239000004604 Blowing Agent Substances 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- DDCDEKHXBABHHI-UHFFFAOYSA-N acetylene cyclohexanol Chemical group C1(CCCCC1)O.C#C DDCDEKHXBABHHI-UHFFFAOYSA-N 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 description 1
- 235000019399 azodicarbonamide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229940042795 hydrazides for tuberculosis treatment Drugs 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000002832 nitroso derivatives Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
Abstract
The invention relates to the technical field of silicon rubber, in particular to foaming conductive silicon rubber and a preparation method thereof, wherein the foaming conductive silicon rubber comprises the following raw materials in parts by weight: 90-110 parts of methyl vinyl organosilicon raw rubber, 15-25 parts of modified conductive filler, 0-15 parts of reinforcing filler, 1-5 parts of dispersing aid, 2-5 parts of platinum vulcanization system and 2-8 parts of foaming agent. The foaming conductive silicone rubber carries out surface modification on the conductive filler, so that the compatibility of the conductive filler and methyl vinyl organosilicon raw rubber is increased, and the conductive silicone rubber has high conductivity; the vulcanization rate and the foaming degree of the conductive silicone rubber base rubber are improved to a certain extent, so that the foamed conductive silicone rubber has excellent properties of high hardness and uniform foaming; the addition amount and the proportion of each raw material are strictly controlled, so that the two processes of foaming conductive silicon rubber crosslinking and foaming fully react to form a dense crosslinking network, and the foaming is uniform, so that the foaming conductive silicon rubber with high hardness and low density is prepared.
Description
Technical Field
The invention relates to the technical field of silicon rubber, in particular to foaming conductive silicon rubber and a preparation method thereof.
Background
Typically silicone rubber foams, the blowing agents selected fall into two categories: organic foaming agents and inorganic foaming agents. The organic foaming agent includes azo compounds, sulfonyl hydrazides, nitroso compounds, etc., such as: AC (azodicarbonamide), OBSH (4, 4' -oxybisbenzenesulfonyl hydrazide) and the like, and the decomposition products of the organic foaming agents contain substances such as amines, benzene rings and the like, have odor and are not environment-friendly; the inorganic foaming agent comprises sodium bicarbonate, ammonium chloride, sodium carbonate and the like, and the inorganic foaming agent has small foaming amount and limited application. In recent years, a thermoplastic expandable foaming microsphere is also used as a foaming agent in the market, which is a polymer particle with a typical core-shell structure by taking a thermoplastic polymer as a shell layer and a foaming agent (low-boiling alkane or other compounds) as a core, wherein the foaming agent has poor compatibility with silicone rubber, and the prepared product has the advantages of unsmooth surface, obvious granular feel, difficult color mixing and poor thermal stability.
The above-mentioned foaming agents, although being used in the foaming conductive silicone rubber molded using the bis-dipentaerythritol, are not completely used in the extrusion type foaming conductive silicone rubber. Further, the main component and decomposition products of the foaming agent are relatively complex, and the inclusion of a substance that inhibits platinum vulcanization can poison platinum and cause the vulcanized product to be unripe.
Disclosure of Invention
In view of the above, the present invention aims to overcome the problems of the prior art and provide a foamed conductive silicone rubber which has excellent properties of high conductivity, high hardness and uniform foaming, and can be molded by compression molding or extruded.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
the invention provides foaming conductive silicon rubber, which comprises the following raw materials in parts by weight:
90-110 parts of methyl vinyl organosilicon raw rubber;
15-25 parts of modified conductive filler;
0-15 parts of reinforcing filler;
1-5 parts of dispersing auxiliary;
2-5 parts of a platinum vulcanization system;
2-8 parts of foaming agent.
Preferably, the molecular weight of the methyl vinyl organosilicon raw rubber is 55-65 ten thousand, the vinyl content of the methyl vinyl organosilicon raw rubber is 0.05-0.5%, the surface of the modified conductive filler is modified by high-content hydroxyl silicone oil, and the hydroxyl content of the high-content hydroxyl silicone oil is 5-10%. The conductive filler is subjected to surface modification by utilizing the high-content hydroxyl silicone oil, so that on one hand, the compatibility of the conductive filler and methyl vinyl organosilicon raw rubber can be increased, the condition of sticking a mold is prevented, the foamed conductive silicone rubber has high conductivity, and on the other hand, the vulcanization rate and the foaming degree of the conductive silicone rubber base rubber can be improved, and the foamed conductive silicone rubber has excellent properties of high hardness and uniform foaming.
Preferably, the modified conductive filler is at least one of conductive metal powder, acetylene conductive carbon black, conductive carbon nanotubes or graphene, the reinforcing filler is hydrophilic gas-phase white carbon black, the dispersing aid is methyl silicone oil, and the foaming agent is at least one of alumina trihydrate, copper sulfate pentahydrate, sodium carbonate hydrate or alum. The conductive carbon nano-tube or graphene has large specific surface area, is unfavorable for modifying the surfaces of the conductive carbon nano-tube or graphene by high-content hydroxyl silicone oil, and is additionally added with hydrophilic fumed silica as a reinforcing filler, wherein the surface of the hydrophilic fumed silica contains hydrophilic groups, so that the reinforcing effect is good, the vulcanization condition of the conductive silicone rubber base rubber can be effectively improved, and the conductive silicone rubber has excellent performance of high hardness.
Preferably, the platinum vulcanization system comprises a vulcanizing agent A and a vulcanizing agent B, wherein the vulcanizing agent A is a platinum catalyst.
Preferably, the weight part ratio of the vulcanizing agent A to the vulcanizing agent B is 0.5-2:1.5-3. And controlling the weight part ratio of the vulcanizing agent A to the vulcanizing agent B within the range, adding excessive hydrogen-containing silicone oil, and utilizing the excessive hydrogen atoms to react with water molecules in the foaming agent to generate hydrogen for discharging so as to generate bubbles.
Preferably, the vulcanizing agent B consists of a cross-linking agent and an inhibitor, wherein the cross-linking agent is hydrogen-containing silicone oil, and the inhibitor is at least one of ethynyl cyclohexanol, 1-methylbutynol or methyl maleate. The platinum catalyst, the cross-linking agent and the inhibitor form a vulcanization system, and under the catalysis of the platinum catalyst, the hydrogen atoms in the hydrogen-containing silicone oil and the vinyl in the methyl vinyl organosilicon raw rubber undergo an addition reaction to form a cross-linked network to complete vulcanization.
Preferably, the molar ratio of hydrogen atoms to vinyl groups in the hydrogen-containing silicone oil is 1.5-5:1. In the system, the mole ratio of the hydrogen atoms and vinyl groups of the hydrogen-containing silicone oil can influence the foaming effect of the foaming material, and the optimal foaming effect can be ensured by controlling the dosage ratio; the molar ratio is too low, gas cannot be generated, the foaming amount is too low, the molar ratio is too high, gas is generated too much, and the foaming is uneven.
Preferably, the inhibitor is used in an amount of 0.05 to 0.2%. The dosage of the inhibitor is controlled within the range, so that the vulcanization speed can be effectively controlled, and the condition of scorching or dead materials caused by the too high vulcanization speed is prevented.
The invention also provides a preparation method of the foaming conductive silicon rubber, which is suitable for molding and extrusion molding of the foaming conductive silicon rubber, has good performances of high conductivity and uniform foaming, does not generate harmful substances in the preparation process, and is environment-friendly and energy-saving.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
the preparation method of the foaming conductive silicone rubber comprises the following steps: the method comprises the following steps:
(1) Mixing and stirring the conductive filler and the high-content hydroxyl silicone oil, heating to a certain temperature, stirring at a constant temperature, and vacuumizing after stirring to obtain a modified conductive filler;
(2) Mixing methyl vinyl organosilicon raw rubber, modified conductive filler, reinforcing filler and dispersing aid according to parts by weight to prepare conductive silicone rubber base rubber for later use;
(3) Dividing the conductive silicone rubber base into A, B two equal parts, adding vulcanizing agent A into equal parts A, adding vulcanizing agent B into equal parts B, uniformly mixing the two equal parts of systems, and blending the mixed systems;
(4) And adding a foaming agent into the well-mixed blend, and uniformly mixing to prepare the foaming conductive silicone rubber.
The vulcanizing agent A is added into the conductive silicone rubber base adhesive A equal part, the vulcanizing agent B is added into the conductive silicone rubber base adhesive B equal part, and A, B equal part systems are mixed again when being used, so that on one hand, the situation that if a platinum catalyst and an inhibitor exist in one system at the same time, the poisoning failure of the platinum catalyst can occur can be prevented, and on the other hand, the platinum and hydrogen-containing silicone oil are separated to prevent the glue from being subjected to crosslinking reaction in advance, so that the situation that the glue is burnt and dead due to too fast reaction can be prevented.
Preferably, the constant temperature of the step (1) is 145-150 ℃, the constant temperature stirring time is 1.5-2h, the vacuumizing time is 25-30min, and the vacuum degree is- (0.03-0.02) MPa; the mixing temperature in the mixing process of the steps (2) - (3) is 20-26 ℃, and the mixing time is 10-20min. The mixing temperature is strictly controlled in the range, the temperature is too low, the A, B vulcanization system can be unevenly dispersed, the temperature is too high, the activity of the platinum catalyst is increased, the inhibitor is easy to volatilize and lose, and the sizing material is easy to burn.
Compared with the prior art, the invention has the beneficial effects that:
1. the foaming conductive silicone rubber disclosed by the invention has the advantages that the high-content hydroxyl silicone oil is used for carrying out surface modification on the conductive filler, so that on one hand, the compatibility of the conductive filler and methyl vinyl organic silicone rubber can be increased, the situation of sticking a mold is prevented, the foaming conductive silicone rubber has high conductivity, on the other hand, the vulcanization rate and the foaming degree of the conductive silicone rubber base rubber can be improved, and the foaming conductive silicone rubber has excellent performances of high hardness and uniform foaming;
2. the addition amount of various raw materials is strictly controlled, and a certain proportion exists between the raw material consumption, so that the prepared foaming conductive silicone rubber is ensured to be uniformly foamed, and the foaming conductive silicone rubber can be molded by compression and extruded;
3. in the preparation process of the foaming conductive silicone rubber, the conductive silicone rubber base rubber is divided into A, B equal parts, vulcanizing agent A and vulcanizing agent B are respectively added and then blended, so that the situation that if a platinum catalyst and an inhibitor exist in one system at the same time, the platinum catalyst is poisoned and loses efficacy can be prevented, and on the other hand, the situation that the rubber material is subjected to crosslinking reaction in advance and the rubber material is burnt and dead due to too fast reaction can be prevented;
4. the mixing temperature is strictly controlled in the preparation process of the foaming conductive silicon rubber, so that the situation of abnormal vulcanization can be avoided.
Detailed Description
The present invention is further illustrated below in conjunction with examples, which are not intended to limit the scope of the invention, in order to facilitate understanding of those skilled in the art.
Example 1
The foaming conductive silicone rubber comprises the following raw materials in parts by weight:
100 parts of methyl vinyl organosilicon raw rubber;
25 parts of modified conductive filler;
2 parts of reinforcing filler;
2 parts of dispersing auxiliary;
2.1 parts of platinum vulcanization system;
5 parts of foaming agent.
The methyl vinyl organosilicon raw rubber has a molecular weight of 60 ten thousand, the vinyl content of the methyl vinyl organosilicon raw rubber is 0.25%, the modified conductive filler is acetylene conductive carbon black, the surface of the acetylene conductive carbon black is modified by high-content hydroxyl silicone oil, the hydroxyl content of the high-content hydroxyl silicone oil is 8%, the reinforcing filler is hydrophilic gas-phase white carbon black, the dispersing aid is methyl silicone oil, the platinum vulcanization system consists of a vulcanizing agent A and a vulcanizing agent B according to a weight ratio of 0.5:1.6, the vulcanizing agent A is a platinum catalyst, the vulcanizing agent B consists of a crosslinking agent and an inhibitor according to a weight ratio of 1.5:0.1, the crosslinking agent is hydrogen-containing silicone oil, the inhibitor is ethynyl cyclohexanol, and the foaming agent is aluminum oxide trihydrate.
The foaming conductive silicon rubber is prepared through the following steps:
(1) Mixing and stirring the conductive filler and the high-content hydroxyl silicone oil, heating to 150 ℃, stirring for 2 hours at constant temperature, and vacuumizing for 30 minutes under the condition that the vacuum degree is-0.03 MPa after stirring to obtain modified conductive silica gel;
(2) Mixing methyl vinyl organosilicon raw rubber, modified conductive filler, reinforcing filler and dispersing aid for 10min at 25 ℃ according to parts by weight to prepare conductive silicone rubber base rubber for later use;
(3) Dividing the conductive silicone rubber base into A, B two equal parts, adding vulcanizing agent A into equal parts A, adding vulcanizing agent B into equal parts B, mixing the two equal parts at 25 ℃ for 10min, and blending the mixed systems after uniform mixing;
(4) And adding a foaming agent into the well-mixed blend, mixing for 10min at 25 ℃, and uniformly mixing to prepare the foaming conductive silicone rubber.
Example 2
The foaming conductive silicone rubber comprises the following raw materials in parts by weight:
95 parts of methyl vinyl organosilicon raw rubber;
15 parts of modified conductive filler;
2 parts of dispersing auxiliary;
3.15 parts of platinum vulcanization system;
8 parts of foaming agent.
The methyl vinyl organosilicon raw rubber has a molecular weight of 55 ten thousand, the vinyl content of the methyl vinyl organosilicon raw rubber is 0.3%, the modified conductive filler consists of a conductive carbon nano tube and acetylene conductive carbon black according to a weight part ratio of 5:10, the surfaces of the conductive carbon nano tube and the acetylene conductive carbon black are modified by high-content hydroxyl silicone oil, the hydroxyl content of the high-content hydroxyl silicone oil is 10%, the dispersing aid is methyl silicone oil, the platinum vulcanizing system consists of a vulcanizing agent A and a vulcanizing agent B according to a weight part ratio of 1:2.15, the vulcanizing agent A is a platinum vulcanizing agent, the vulcanizing agent B consists of a crosslinking agent and an inhibitor according to a weight part ratio of 2:0.15, the crosslinking agent is hydrogen-containing silicone oil, the inhibitor is 1-methylbutinol, and the foaming agent is anhydrous copper sulfate.
The foaming conductive silicon rubber is prepared through the following steps:
(1) Mixing and stirring the conductive filler and the high-content hydroxyl silicone oil, heating to 150 ℃, stirring for 2 hours at constant temperature, and vacuumizing for 30 minutes under the condition that the vacuum degree is-0.03 MPa after stirring to obtain modified conductive silica gel;
(2) Mixing methyl vinyl organosilicon raw rubber, modified conductive filler and dispersing auxiliary agent according to parts by weight for 15min at 24 ℃ to prepare conductive silicone rubber base rubber for later use;
(3) Dividing the conductive silicone rubber base into A, B two equal parts, adding vulcanizing agent A into equal parts A, adding vulcanizing agent B into equal parts B, mixing the two equal parts at 24 ℃ for 15min, and blending the mixed systems after uniform mixing;
(4) And adding a foaming agent into the well-mixed blend, mixing for 15min at 24 ℃, and uniformly mixing to prepare the foaming conductive silicone rubber.
Example 3
The foaming conductive silicone rubber comprises the following raw materials in parts by weight:
105 parts of methyl vinyl organosilicon raw rubber;
18 parts of modified conductive filler;
5 parts of reinforcing filler;
5 parts of dispersing auxiliary;
3.2 parts of a platinum vulcanization system;
8 parts of foaming agent.
The methyl vinyl organosilicon raw rubber has a molecular weight of 60 ten thousand, the vinyl content of the methyl vinyl organosilicon raw rubber is 0.38%, the modified conductive filler consists of graphene and acetylene conductive carbon black according to a weight part ratio of 8:10, the surfaces of the graphene and the acetylene conductive carbon black are modified by high-content hydroxyl silicone oil, the hydroxyl content of the high-content hydroxyl silicone oil is 5%, the reinforcing filler is hydrophilic gas-phase white carbon black, the dispersing auxiliary agent is methyl silicone oil, the platinum vulcanization system consists of a vulcanizing agent A and a vulcanizing agent B according to a weight part ratio of 1:2.2, the vulcanizing agent A is a platinum catalyst, the vulcanizing agent B consists of a crosslinking agent and an inhibitor according to a weight part ratio of 2:0.2, the crosslinking agent is hydrogen-containing silicone oil, the inhibitor is methyl maleate, and the foaming agent is alum.
The foaming conductive silicon rubber is prepared through the following steps:
(1) Mixing and stirring the conductive filler and the high-content hydroxyl silicone oil, heating to 150 ℃, stirring for 2 hours at constant temperature, and vacuumizing for 30 minutes under the condition that the vacuum degree is-0.03 MPa after stirring to obtain modified conductive silica gel;
(2) Mixing methyl vinyl organosilicon raw rubber, modified conductive filler, reinforcing filler and dispersing aid for 13min at 23 ℃ according to parts by weight to prepare conductive silicone rubber base rubber for later use;
(3) Dividing the conductive silicone rubber base into A, B two equal parts, adding vulcanizing agent A into equal parts A, adding vulcanizing agent B into equal parts B, mixing the two equal parts at 23 ℃ for 13min, and blending the mixed systems after uniform mixing;
(4) And adding a foaming agent into the well-mixed blend, mixing for 13min at the temperature of 23 ℃, and uniformly mixing to prepare the foaming conductive silicone rubber.
Comparative example 1
The foaming conductive silicone rubber comprises the following raw materials in parts by weight:
100 parts of methyl vinyl organosilicon raw rubber;
25 parts of modified conductive filler;
2 parts of reinforcing filler;
2 parts of dispersing auxiliary;
10.7 parts of platinum vulcanization system;
5 parts of foaming agent.
The methyl vinyl organosilicon raw rubber has a molecular weight of 60 ten thousand, the vinyl content of the methyl vinyl organosilicon raw rubber is 0.25%, the modified conductive filler is acetylene conductive carbon black, the surface of the acetylene conductive carbon black is modified by high-content hydroxyl silicone oil, the hydroxyl content of the high-content hydroxyl silicone oil is 8%, the reinforcing filler is hydrophilic gas-phase white carbon black, the dispersing aid is methyl silicone oil, the platinum vulcanization system consists of a vulcanizing agent A and a vulcanizing agent B according to a weight ratio of 0.5:10.2, the vulcanizing agent A is a platinum catalyst, the vulcanizing agent B consists of a crosslinking agent and an inhibitor according to a weight ratio of 10:0.2, the crosslinking agent is hydrogen-containing silicone oil, the inhibitor is ethynyl cyclohexanol, and the foaming agent is alumina trihydrate.
The foaming conductive silicon rubber is prepared through the following steps:
(1) Mixing and stirring the conductive filler and the high-content hydroxyl silicone oil, heating to 150 ℃, stirring for 2 hours at constant temperature, and vacuumizing for 30 minutes under the condition that the vacuum degree is-0.03 MPa after stirring to obtain modified conductive silica gel;
(2) Mixing methyl vinyl organosilicon raw rubber, modified conductive filler, reinforcing filler and dispersing aid for 10min at 25 ℃ according to parts by weight to prepare conductive silicone rubber base rubber for later use;
(3) Dividing the conductive silicone rubber base into A, B two equal parts, adding vulcanizing agent A into equal parts A, adding vulcanizing agent B into equal parts B, mixing the two equal parts at 25 ℃ for 10min, and blending the mixed systems after uniform mixing;
(4) And adding a foaming agent into the well-mixed blend, mixing for 10min at 25 ℃, and uniformly mixing to prepare the foaming conductive silicone rubber.
Comparative example 2
The foaming conductive silicone rubber comprises the following raw materials in parts by weight:
100 parts of methyl vinyl organosilicon raw rubber;
25 parts of modified conductive filler;
2 parts of dispersing auxiliary;
2.1 parts of platinum vulcanization system;
5 parts of foaming agent.
The methyl vinyl organosilicon raw rubber has a molecular weight of 60 ten thousand, the vinyl content of the methyl vinyl organosilicon raw rubber is 0.25%, the modified conductive filler is acetylene conductive carbon black, the surface of the acetylene conductive carbon black is modified by high-content hydroxyl silicone oil, the hydroxyl content of the high-content hydroxyl silicone oil is 8%, the dispersing aid is methyl silicone oil, the platinum vulcanization system consists of a vulcanizing agent A and a vulcanizing agent B according to a weight ratio of 0.5:1.6, the vulcanizing agent A is a platinum catalyst, the vulcanizing agent B consists of a cross-linking agent and an inhibitor according to a weight ratio of 1.5:0.1, the cross-linking agent is hydrogen-containing silicone oil, the inhibitor is acetylene cyclohexanol, and the foaming agent is alumina trihydrate.
The foaming conductive silicon rubber is prepared through the following steps:
(1) Mixing and stirring the conductive filler and the high-content hydroxyl silicone oil, heating to 150 ℃, stirring for 2 hours at constant temperature, and vacuumizing for 30 minutes under the condition that the vacuum degree is-0.03 MPa after stirring to obtain modified conductive silica gel;
(2) Mixing methyl vinyl organosilicon raw rubber, modified conductive filler and dispersing auxiliary agent according to parts by weight for 10min at 25 ℃ to prepare conductive silicone rubber base rubber for later use;
(3) Dividing the conductive silicone rubber base into A, B two equal parts, adding vulcanizing agent A into equal parts A, adding vulcanizing agent B into equal parts B, mixing the two equal parts at 25 ℃ for 10min, and blending the mixed systems after uniform mixing;
(4) And adding a foaming agent into the well-mixed blend, mixing for 10min at 25 ℃, and uniformly mixing to prepare the foaming conductive silicone rubber.
Comparative example 3
The foaming conductive silicone rubber comprises the following raw materials in parts by weight:
100 parts of methyl vinyl organosilicon raw rubber;
25 parts of conductive filler acetylene conductive carbon black;
2 parts of reinforcing filler hydrophilic gas phase white carbon black;
2 parts of dispersing auxiliary methyl silicone oil;
2.1 parts of platinum vulcanization system;
0.5 part of platinum catalyst;
1.5 parts of hydrogen silicone oil;
0.1 parts of ethynyl cyclohexanol;
alumina trihydrate 5 parts.
The methyl vinyl organosilicon raw rubber has a molecular weight of 60 ten thousand, the vinyl content of the methyl vinyl organosilicon raw rubber is 0.25%, the conductive filler is acetylene conductive carbon black, the reinforcing filler is hydrophilic gas-phase white carbon black, the dispersing aid is methyl silicone oil, the platinum vulcanization system consists of a vulcanizing agent A and a vulcanizing agent B according to a weight part ratio of 0.5:1.6, the vulcanizing agent A is a platinum catalyst, the vulcanizing agent B consists of a cross-linking agent and an inhibitor according to a weight part ratio of 1.5:0.1, the cross-linking agent is hydrogen-containing silicone oil, the inhibitor is ethynyl cyclohexanol, and the foaming agent is aluminum oxide trihydrate.
The foaming conductive silicon rubber is prepared through the following steps:
(1) Mixing methyl vinyl organosilicon raw rubber, conductive filler, reinforcing filler and dispersing auxiliary agent for 10min at 25 ℃ according to parts by weight to prepare conductive silicone rubber base rubber for later use;
(2) Dividing the conductive silicone rubber base into A, B two equal parts, adding vulcanizing agent A into equal parts A, adding vulcanizing agent B into equal parts B, mixing the two equal parts at 25 ℃ for 10min, and blending the mixed systems after uniform mixing;
(3) And adding a foaming agent into the well-mixed blend, mixing for 10min at 25 ℃, and uniformly mixing to prepare the foaming conductive silicone rubber.
The foaming conductive silicone rubbers prepared in the examples 1-3 and the comparative examples 1-3 were subjected to multiple groups of sampling and detection, and the results are shown in the following table:
from the above results, the foaming conductive silicone rubber of the invention utilizes high-content hydroxyl silicone oil to carry out surface modification on the conductive filler, so that the compatibility of the conductive filler and methyl vinyl organosilicon raw rubber is increased, and the conductive silicone rubber has high conductivity; the vulcanization rate and the foaming degree of the conductive silicone rubber base rubber are improved to a certain extent, so that the prepared foaming conductive silicone rubber has excellent properties of high hardness and uniform foaming; the addition amount and the proportion of each raw material are strictly controlled, so that the two processes of foaming conductive silicone rubber crosslinking and foaming fully react to form a dense crosslinking network, and foaming is uniform, thus preparing the foaming conductive silicone rubber with high hardness and low density.
Compared with example 1, in the process of preparing the foaming conductive silicon rubber by adding excessive hydrogen-containing silicone oil in comparative example 1, the vulcanization speed is too high, so that the prepared foaming conductive silicon rubber has less and uneven foaming, too high density, too high and uneven surface resistance and poor conductive effect.
Compared with example 1, in comparative example 2, no hydrophilic fumed silica was added, and in the process of preparing the foamed conductive silicone rubber, the vulcanization speed was slower, resulting in a decrease in hardness of the foamed conductive silicone rubber prepared.
Compared with example 1, the conductive filler added in comparative example 3 is not subjected to surface modification, in the process of preparing the foamed conductive silicone rubber, the dispersibility of the conductive filler and methyl vinyl silicone rubber is poor, the conductive filler cannot provide hydroxyl groups to react with hydrogen-containing silicone oil, bubbles are generated, and the prepared foamed conductive silicone rubber is uneven in foaming and too high in density.
The foregoing has described in detail the technical solutions provided by the embodiments of the present invention, and specific examples have been applied to illustrate the principles and implementations of the embodiments of the present invention, where the above description of the embodiments is only suitable for helping to understand the principles of the embodiments of the present invention; meanwhile, as for those skilled in the art, according to the embodiments of the present invention, there are variations in the specific embodiments and the application scope, and the present description should not be construed as limiting the present invention.
Claims (10)
1. The foaming conductive silicone rubber is characterized in that: the material comprises the following raw materials in parts by weight:
90-110 parts of methyl vinyl organosilicon raw rubber;
15-25 parts of modified conductive filler;
0-15 parts of reinforcing filler;
1-5 parts of dispersing auxiliary;
2-5 parts of a platinum vulcanization system;
2-8 parts of foaming agent.
2. The foamed electrically conductive silicone rubber of claim 1, wherein: the molecular weight of the methyl vinyl organosilicon raw rubber is 55-65 ten thousand, the vinyl content of the methyl vinyl organosilicon raw rubber is 0.05-0.5%, the surface of the modified conductive filler is modified by high-content hydroxyl silicone oil, and the hydroxyl content of the high-content hydroxyl silicone oil is 5-10%.
3. The foamed electrically conductive silicone rubber of claim 1, wherein: the modified conductive filler is at least one of conductive metal powder, acetylene conductive carbon black, conductive carbon nano-tubes or graphene; the reinforcing filler is hydrophilic gas-phase white carbon black; the dispersing aid is methyl silicone oil; the foaming agent is at least one of alumina trihydrate, copper sulfate pentahydrate, sodium carbonate hydrate or alum.
4. The foamed electrically conductive silicone rubber of claim 1, wherein: the platinum vulcanizing system comprises a vulcanizing agent A and a vulcanizing agent B, wherein the vulcanizing agent A is a platinum catalyst.
5. The foamed electrically conductive silicone rubber of claim 4, wherein: the weight part ratio of the vulcanizing agent A to the vulcanizing agent B is 0.5-2:1.5-3.
6. The foamed electrically conductive silicone rubber of claim 4, wherein: the vulcanizing agent B consists of a cross-linking agent and an inhibitor, wherein the cross-linking agent is hydrogen-containing silicone oil, and the inhibitor is at least one of ethynyl cyclohexanol, 1-methylbutynol or methyl maleate.
7. The foamed electrically conductive silicone rubber of claim 6, wherein: the molar ratio of the hydrogen atoms to the vinyl groups in the hydrogen-containing silicone oil is 1.5-5:1.
8. The foamed electrically conductive silicone rubber of claim 5, wherein: the inhibitor is used in an amount of 0.05-0.2%.
9. A method for preparing the foamed conductive silicone rubber as set forth in any one of claims 4 to 8, characterized in that: the method comprises the following steps:
(1) Mixing and stirring the conductive filler and the high-content hydroxyl silicone oil, heating to a certain temperature, stirring at a constant temperature, and vacuumizing after stirring to obtain a modified conductive filler;
(2) Mixing methyl vinyl organosilicon raw rubber, modified conductive filler, reinforcing filler and dispersing aid according to parts by weight to prepare conductive silicone rubber base rubber for later use;
(3) Dividing the conductive silicone rubber base into A, B two equal parts, adding vulcanizing agent A into equal parts A, adding vulcanizing agent B into equal parts B, uniformly mixing the two equal parts of systems, and blending the mixed systems;
(4) And adding a foaming agent into the well-mixed blend, and uniformly mixing to prepare the foaming conductive silicone rubber.
10. The method for preparing the foamed conductive silicone rubber according to claim 9, wherein the method comprises the following steps: the constant temperature of the step (1) is 145-150 ℃, the constant temperature stirring time is 1.5-2h, the vacuumizing time is 25-30min, and the vacuum degree is- (0.03-0.02) MPa; the mixing temperature in the mixing process of the steps (2) - (4) is 20-26 ℃, and the mixing time is 10-20min.
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