CN114874629A - Preparation method of novel inorganic fullerene nano silicon rubber material - Google Patents
Preparation method of novel inorganic fullerene nano silicon rubber material Download PDFInfo
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 46
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 21
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920001971 elastomer Polymers 0.000 claims abstract description 39
- 239000005060 rubber Substances 0.000 claims abstract description 39
- 238000004073 vulcanization Methods 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000003490 calendering Methods 0.000 claims abstract description 17
- 239000000654 additive Substances 0.000 claims abstract description 15
- 238000001125 extrusion Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 229920005560 fluorosilicone rubber Polymers 0.000 claims abstract description 4
- 238000005187 foaming Methods 0.000 claims abstract description 4
- 239000000295 fuel oil Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- 239000004945 silicone rubber Substances 0.000 claims description 17
- 239000012763 reinforcing filler Substances 0.000 claims description 14
- 239000012744 reinforcing agent Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000004088 foaming agent Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000003086 colorant Substances 0.000 claims description 5
- 229910021485 fumed silica Inorganic materials 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 230000000704 physical effect Effects 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 1
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract 2
- 239000006229 carbon black Substances 0.000 description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 230000032683 aging Effects 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- 239000004636 vulcanized rubber Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000004513 sizing Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 150000001451 organic peroxides Chemical class 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 235000010215 titanium dioxide Nutrition 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 239000004156 Azodicarbonamide Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MWRWFPQBGSZWNV-UHFFFAOYSA-N Dinitrosopentamethylenetetramine Chemical compound C1N2CN(N=O)CN1CN(N=O)C2 MWRWFPQBGSZWNV-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- ANBLKISCTWYEIH-UHFFFAOYSA-N [Cd++].[O-][O-] Chemical compound [Cd++].[O-][O-] ANBLKISCTWYEIH-UHFFFAOYSA-N 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
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- -1 boric acid ester Chemical class 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- MNFGEHQPOWJJBH-UHFFFAOYSA-N diethoxy-methyl-phenylsilane Chemical compound CCO[Si](C)(OCC)C1=CC=CC=C1 MNFGEHQPOWJJBH-UHFFFAOYSA-N 0.000 description 1
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 description 1
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 235000013799 ultramarine blue Nutrition 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- 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
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
-
- 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
- C08J9/10—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 developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
-
- 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
- C08J9/10—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 developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/107—Nitroso compounds
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- 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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- 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
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- 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
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- 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
- C08J2383/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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Abstract
The invention relates to the technical field of preparation of rubber materials, and provides a preparation method of a novel inorganic fullerene nano-silicon rubber material, which is used for tracing the source, fundamentally controlling the performance of silicon rubber, presenting the comprehensive characteristics of the novel inorganic fullerene nano-silicon rubber material by strictly controlling each flow, being suitable for application in more fields, and mainly comprising the following steps: the production method comprises the steps of raw rubber selection, mixing and stirring in a metering matching manner, banbury mixer mixing processing, extruder extrusion processing, calender calendering processing, multi-stage vulcanization processing and foaming forming processing, wherein different rubber raw materials can be selected according to the use temperature requirement, a silicon rubber product with the use temperature requirement of-70-250 ℃ is adopted, vinyl silicon rubber is adopted, a silicon rubber product with the use temperature requirement of-90-300 ℃ is adopted, low-phenyl silicon rubber is adopted, when the product requires high and low temperature resistance and fuel oil or solvent resistance, fluorosilicone rubber is adopted, and an additive is put into the raw rubber in the metering matching manner during mixing and stirring.
Description
Technical Field
The invention relates to the technical field of preparation of rubber materials, in particular to a preparation method of a novel inorganic fullerene nano-silicon rubber material.
Background
It is known that silicone rubber is a polymeric elastic material with both inorganic and organic properties, the main chain of the molecule is composed of silicon atoms and oxygen atoms (Si-O-Si), and the side chains are hydrocarbon or substituted hydrocarbon organic groups connected with the silicon atoms, such groups can be methyl, unsaturated vinyl (the mole fraction is generally not more than 01005) or other organic groups.
The silicon rubber is developed in the 40 th century, the earliest studied variety abroad is dimethyl silicon rubber, Dow Corning company and general electric company in the United states are respectively put into production before and after 1944, China successfully studies and puts into industrial production in the initial 60 th year, the countries producing the silicon rubber at present also have more than 1000 varieties of brands in the United states, British, Japan, Germany and the like besides China, along with the development of silicon rubber industry, the variety of the silicon rubber is more and more abundant, and the novel inorganic fullerene nano silicon rubber material is one of novel silicon rubber materials, and is applied to various fields due to the excellent heat aging resistance and weather aging resistance, and the softness and the elasticity while resisting ultraviolet and ozone erosion.
Although the prior art scheme can realize the preparation of novel inorganic fullerene nano-silicon rubber materials, along with the further expansion of the application field and the research on nano-materials, the requirement of novel silicon rubber materials with higher performance is increasingly exposed, and how to further improve the performance of the novel inorganic fullerene nano-silicon rubber materials and better production becomes one of the current hot topics.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of a novel inorganic fullerene nano silicon rubber material, which is traced to the source, fundamentally controls the performance of silicon rubber, presents the comprehensive characteristics of the novel inorganic fullerene nano silicon rubber material by strictly controlling each flow, and is suitable for application in more fields.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a novel inorganic fullerene nano-silicon rubber material mainly comprises the following steps:
(1) selecting raw rubber;
(2) mixing the materials in a metering and matching manner;
(3) mixing and processing by an internal mixer;
(4) extruding and processing by an extruder;
(5) calendering by a calender;
(6) a multi-stage vulcanization process;
(7) and (5) foaming and forming.
On the basis of the scheme, different rubber raw materials can be selected according to the use temperature requirement, a silicon rubber product with the use temperature requirement of-70-250 ℃ is adopted, vinyl silicon rubber is adopted, a silicon rubber product with the use temperature requirement of-90-300 ℃ is adopted, low-phenyl silicon rubber is adopted, and when the product requires high and low temperature resistance and fuel oil or solvent resistance, fluorosilicone rubber is adopted.
Preferably on the basis of the scheme, when the materials are mixed in a metering and matching way, additives are added, wherein the additives comprise a vulcanizing agent, a reinforcing agent, an auxiliary agent, a heat-resistant additive, a coloring agent and a foaming agent, and the weight ratio of the crude rubber to the six additives is 10 to (0.5-1) to (1-2) to (0.5-1).
Further on the basis of the foregoing scheme, the internal mixer mixing process should be noted that: firstly, the processing process is kept clean, and other rubber, oil stain or impurities cannot be mixed, otherwise, the vulcanization and the performance of the silicon rubber are influenced; secondly, the mixing time is 7-17 min during mixing, when the charging coefficient is 0.84, the mixing can be normally carried out by adopting a p160mm open mill, the discharging temperature is related to the type of the reinforcing filler, and when the weak reinforcing filler and the precipitated silica are adopted, the discharging temperature is below 55 ℃; when the fumed silica is used, the binder removal temperature is about 75 ℃.
On the basis of the scheme, in the extrusion processing process of the extruder, a single-thread screw rod with the diameter of 35 mm or 70mm is generally used, the length-diameter ratio is (10-12) to 1, the effect is good, the low temperature is kept as much as possible during extrusion, and the temperature is preferably not higher than 4.3 ℃, so that cooling water needs to be introduced into a machine barrel and the screw rod, a 90-150-mesh filter screen can be additionally arranged on a product with higher quality requirement near the machine head part, so that impurities in rubber materials are removed, and the extrusion quality is improved.
On the basis of the scheme, the calender is used for calendering, a vertical three-roller calender is adopted for the calender, when the calender is used for production, a middle roller is fixed, the rotation speed of the middle roller is higher than that of an upper roller, the speed ratio is (1.15-1.45): 1, the rotation speed of a lower roller is the same as that of the middle roller, when the calender is started, the temperature of the upper roller is 50 ℃, the middle roller is kept at room temperature, the lower roller is cooled by cooling water, the calendering speed is generally 60-300 cm/min, and the speed is not too high, the roller distance (the middle roller and the lower roller) is adjusted at a low speed firstly to ensure a certain calendering thickness, and then the speed is increased to a normal speed for continuous operation.
As a further aspect of the above scheme, the multi-stage vulcanization processing is performed by two stages, wherein the first stage vulcanization is performed under pressure or normal pressure for heating and setting, the first stage vulcanization temperature is 110-130 ℃, the vulcanization time is 12-20 minutes, the second stage vulcanization is performed in an oven at a high temperature, so as to further stabilize various physical properties, the vulcanization temperature is 220-230 ℃, and the vulcanization time is 3-5 minutes.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of a novel inorganic fullerene nano-silicon rubber material, which has the following beneficial effects:
according to the invention, the properties of the silicon rubber are fundamentally controlled by controlling the selection of raw rubber and tracing the source, the processing time of each process section is refined by strictly controlling each process, and the comprehensive characteristics of the novel inorganic fullerene nano silicon rubber material are better presented, so that the novel inorganic fullerene nano silicon rubber material can be better suitable for application in more fields.
Detailed Description
Examples
A preparation method of a novel inorganic fullerene nano-silicon rubber material mainly comprises the following steps:
(1) selecting raw rubber: the raw rubber can be selected from different rubber raw materials according to the use temperature requirement, a silicon rubber product with the use temperature requirement of-70-250 ℃ is adopted, vinyl silicon rubber is adopted, a silicon rubber product with the use temperature requirement of-90-300 ℃ is adopted, low-phenyl silicon rubber is adopted, and when the product requires high and low temperature resistance and fuel oil or solvent resistance, fluorosilicone rubber is adopted.
(2) Mixing materials by metering and matching: when the materials are mixed in a metering and matching manner, additives are put in, wherein the additives comprise a vulcanizing agent, a reinforcing agent, an auxiliary agent, a heat-resistant additive, a coloring agent and a foaming agent, and the weight ratio of the raw rubber to the six additives is 10 to (0.5-1) to (1-2) to (0.5-1).
A vulcanizing agent
Vulcanizing agents used for heat-vulcanized silicone rubbers mainly include organic peroxides, aliphatic azo compounds, inorganic compounds, high-energy rays, and the like, and among them, organic peroxides are most commonly used because organic peroxides are generally stable at room temperature, but rapidly decompose to generate radicals at a higher vulcanization temperature, thereby causing crosslinking of silicone rubbers.
The B reinforcing filler can be classified into a reinforcing filler and a weak reinforcing filler according to the difference of the reinforcing effect, the particle diameter of the former is 10-50 nm, the specific surface area is 70-400 m 2 The reinforcing effect is better, the particle diameter of the reinforcing agent is 300-1000 nm, and the specific surface area of the reinforcing agent is largerAt 30m 2 The ratio of the carbon atoms to the carbon atoms is less than g.
The reinforcing filler is mainly synthetic silicon dioxide, also called white carbon black, which can be divided into gas phase white carbon black and precipitation white carbon black, the gas phase white carbon black is one of the most commonly used reinforcing agents for silicone rubber, the vulcanized rubber of the rubber material reinforced by the reinforcing filler has high mechanical strength and good electrical property, and the reinforcing filler can be used together with other reinforcing agents or weak reinforcing agents to prepare rubber materials with different use requirements.
Compared with silicone rubber reinforced by white carbon black prepared by a gas phase method, the rubber reinforced by the white carbon black prepared by a precipitation method has slightly low mechanical strength, poorer dielectric properties (especially the dielectric properties after being damped), better heat aging resistance and low cost of rubber compound, and when the requirement on the mechanical strength of a product is not high, the white carbon black prepared by the precipitation method can be used independently or can be used together with the white carbon black prepared by the gas phase method.
The treated white carbon black is used as reinforcing agent, the mechanical strength of the rubber material is higher, the mixing and remixing process performance is good, and the transparency of vulcanized rubber is good, so that the rubber material is widely used in medical products.
The weak reinforcing filler can also be called as inert filler, has little reinforcing effect on silicon rubber, is not used in silicon rubber alone but used together with white carbon black to adjust the hardness of the silicon rubber, improve the technological property of rubber and the oil resistance and solvent resistance of vulcanized rubber and reduce the cost of the rubber, and the commonly used weak reinforcing agent comprises diatomite, quartz powder, zinc oxide, ferric oxide, titanium dioxide, silicic acid, calcium carbonate and the like.
C auxiliary agent
Silicone rubber compounds reinforced with fumed silica tend to become hard, have a reduced plasticity value and gradually lose processing properties, which is called a "structuring" effect, and compounding agents added to prevent or reduce this "structuring" tendency are called "structure-controlling agents", which are generally low-molecular organosilicon compounds containing hydroxyl or boron atoms, commonly used are diphenylsilanediol, methylphenyldiethoxysilane, tetramethylethylenedioxydimethylsilane, low-molecular hydroxysilicone oils, silazanes and the like.
D Heat-resistant additive
The hot air aging performance of the silicone rubber can be greatly improved by adding certain metal oxides or salts thereof and organic compounds of certain elements, wherein the most common metal oxide is ferric oxide, the common usage amount is 3-5 parts, other metal oxides such as manganese, zinc, nickel, copper and the like also have similar effects, a small amount (less than 1 part) of spray carbon black is added to play a role in improving the heat resistance, and the hot air aging is usually carried out within the temperature range of 250-300 ℃ to show the effects of the additives.
E colorant
Common colorants for silicone rubber are as follows:
red color of iron oxide (ferric oxide)
Yellow of cadmium yellow (cadmium dioxide)
Chrome green (chromium oxide) green
Black color of carbon black
Titanium white (titanium dioxide) white
Ultramarine blue color
F foaming agent
A foaming agent is required to be added when a silicone rubber sponge product is prepared, the commonly used foaming agent of the silicone rubber comprises N, N2 dinitrosopentamethylenetetramine, azodicarbonamide and the like, a small amount (generally less than 1 part) of tetrafluoroethylene powder is added into a rubber sizing material, the calendering process performance and the film forming performance of the sizing material can be improved, the tearing strength of vulcanized rubber is improved, boric acid ester and a boron-containing compound can enable the vulcanized rubber of the silicone rubber to have self-adhesiveness, when the rubber is reinforced by adopting fumed silica with a large specific surface area, a small amount (3-5 parts, the vinyl mass fraction is generally about 0.10) of high vinyl silicone oil is added, the tearing resistance of the sizing material can be improved to 30-50 kN/m after vulcanization, and the commonly used formula of the vinyl silicone rubber and the fluororubber and the physical properties of the sizing material are obtained.
(3) An internal mixer mixing process, wherein the internal mixer mixing process is as follows: firstly, the processing process is kept clean, and other rubber, oil stain or impurities cannot be mixed, otherwise, the vulcanization and the performance of the silicon rubber are influenced; secondly, the mixing time is 7-17 min during mixing, when the charging coefficient is 0.84, the mixing can be normally carried out by adopting a p160mm open mill, the discharging temperature is related to the type of the reinforcing filler, and when the weak reinforcing filler and the precipitated silica are adopted, the discharging temperature is below 55 ℃; when the fumed silica is used, the binder removal temperature is about 75 ℃.
(4) And (2) extruding and processing by using an extruder, wherein a single-thread screw rod with the diameter of 35 mm or 70mm is generally used in the extruding and processing process of the extruder, the length-diameter ratio is (10-12) to 1, the effect is better, the low temperature is kept as far as possible during extruding, and the temperature is preferably not higher than 4.3 ℃, so that cooling water needs to be introduced into a machine barrel and the screw rod, a filter screen with 90-150 meshes can be additionally arranged near the machine head part of a product with higher quality requirement, so that impurities in the rubber material are removed, and the extruding quality is improved.
(5) The method comprises the steps of calendering by a calender, wherein the calender adopts a vertical three-roller calender, when the calender is used for production, a middle roller is fixed, the rotation speed of the middle roller is higher than that of an upper roller, the speed ratio is (1.15-1.45): 1, the rotation speed of a lower roller is the same as that of the middle roller, when the calender is started, the temperature of the upper roller is 50 ℃, the temperature of the middle roller is kept at room temperature, the temperature of the lower roller is kept at room temperature, the lower roller is cooled by cooling water, the calendering speed is generally 60-300 cm/min, the speed is not too fast, the roller distance (the middle roller and the lower roller) is adjusted at a low speed to ensure a certain calendering thickness, then the roller is continuously operated at a normal speed, the degree of the rubber material used for calendering must be correctly controlled, the rubber material is preferably not fully rewound on a rubber refining machine, enough remill is obtained in the process of calendering, so that the rubber material is prevented from being stuck to the roller due to the excessive remill in the calendering process, the formula of the rubber material also has a certain influence on the calendering, the rubber material adopting the reinforcing filler has better calendering process performance.
(6) And (2) multi-stage vulcanization processing, wherein the vulcanization is carried out in two stages, the first-stage vulcanization is carried out under pressurization or normal pressure for heating and shaping, the first-stage vulcanization temperature is 110-130 ℃, the vulcanization time is 12-20 minutes, the second-stage vulcanization is carried out in an oven at a high temperature, so that various physical properties are further stabilized, the vulcanization temperature is 220-230 ℃, and the vulcanization time is 3-5 minutes.
(7) And (5) foaming and forming.
Claims (7)
1. A preparation method of a novel inorganic fullerene nano-silicon rubber material is characterized by mainly comprising the following steps:
(1) selecting raw rubber;
(2) mixing materials by metering and matching;
(3) mixing and processing by an internal mixer;
(4) extruding and processing by an extruder;
(5) calendering by a calender;
(6) a multi-stage vulcanization process;
(7) and (5) foaming and forming.
2. The preparation method of the novel inorganic fullerene nano-silicon rubber material as claimed in claim 1, wherein the raw rubber is selected from different rubber raw materials according to the use temperature requirement, the use temperature requirement is-70-250 ℃, the silicone rubber product is vinyl silicone rubber, the use temperature requirement is-90-300 ℃, the low phenyl silicone rubber is adopted, and when the product requires high and low temperature resistance and fuel oil or solvent resistance, the fluorosilicone rubber is adopted.
3. The method for preparing a novel inorganic fullerene nano-silicone rubber material as claimed in claim 2, wherein additives are added during the metering, mixing and mixing, wherein the additives comprise a vulcanizing agent, a reinforcing agent, an auxiliary agent, a heat-resistant additive, a coloring agent and a foaming agent, and the weight ratio of the raw rubber to the six additives is 10: 0.5-1: 1-2: 0.5-1.
4. The method for preparing a novel inorganic fullerene nano-silicone rubber material as claimed in claim 3, wherein the internal mixer mixing process is carried out by taking into account: firstly, the processing process is kept clean, and other rubber, oil stain or impurities cannot be mixed, otherwise, the vulcanization and the performance of the silicon rubber are influenced; secondly, the mixing time is 7-17 min during mixing, when the charging coefficient is 0.84, the mixing can be normally carried out by adopting a p160mm open mill, the discharging temperature is related to the type of the reinforcing filler, and when the weak reinforcing filler and the precipitated silica are adopted, the discharging temperature is below 55 ℃; when the fumed silica is used, the binder removal temperature is about 75 ℃.
5. The method for preparing a novel inorganic fullerene nano-silicone rubber material as claimed in claim 4, wherein the extruder in the extrusion process of the extruder is a single-thread screw with diameter of 35 mm or 70mm, the length-diameter ratio is (10-12) to 1, the effect is good, the low temperature is kept as low as possible during extrusion, preferably not more than 4.3 ℃, so that cooling water is introduced into both a cylinder and the screw, and a 90-150 mesh filter screen can be additionally arranged near the head part of the extruder for products with high quality requirements, so as to remove impurities in the rubber material and improve the extrusion quality.
6. The method as claimed in claim 5, wherein the calender is a vertical three-roll calender, and when the calender is used for production, the middle roll is fixed, the rotation speed of the middle roll is faster than that of the upper roll, the speed ratio is (1.15-1.45): 1, the rotation speed of the lower roll is the same as that of the middle roll, when the calender is started, the temperature of the upper roll is 50 ℃, the middle roll is kept at room temperature, the lower roll is cooled by cooling water, the calendering speed is generally 60-300 cm/min, and the lower roll is not too fast, the roll distance (the middle and lower rolls) is adjusted at a low speed to ensure a certain calendering thickness, and then the speed is increased to normal speed for continuous operation.
7. The preparation method of the novel inorganic fullerene nano-silicone rubber material as claimed in claim 6, wherein the multi-stage vulcanization processing is carried out in two stages, wherein the first stage vulcanization is carried out under pressure or normal pressure for heating and shaping, the first stage vulcanization temperature is 110-130 ℃, the vulcanization time is 12-20 minutes, the second stage vulcanization is carried out in an oven at high temperature, so as to further stabilize various physical properties, the vulcanization temperature is 220-230 ℃, and the vulcanization time is 3-5 minutes.
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| CN1673280A (en) * | 2004-03-22 | 2005-09-28 | 徐英强 | Making process silicone rubber sponge backing board |
| CN103042646A (en) * | 2013-01-16 | 2013-04-17 | 桂林裕天新材料有限公司 | Process for fabricating thermal conductive silica gel sheets |
| WO2018130194A1 (en) * | 2017-01-13 | 2018-07-19 | 杭州星庐科技有限公司 | Rubber composite, processing method, rubber products applying composite, and manufacturing method |
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|---|---|---|---|---|
| CN1673280A (en) * | 2004-03-22 | 2005-09-28 | 徐英强 | Making process silicone rubber sponge backing board |
| CN103042646A (en) * | 2013-01-16 | 2013-04-17 | 桂林裕天新材料有限公司 | Process for fabricating thermal conductive silica gel sheets |
| WO2018130194A1 (en) * | 2017-01-13 | 2018-07-19 | 杭州星庐科技有限公司 | Rubber composite, processing method, rubber products applying composite, and manufacturing method |
| CN109825085A (en) * | 2018-12-29 | 2019-05-31 | 易宝（福建）高分子材料股份公司 | A kind of environmental protection flame retardant thermal contraction silicon rubber closed pore molding high temperature second time of foaming material resistant to high temperatures and preparation method thereof |
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