CN112063181A - Mixing silicone rubber and preparation method thereof - Google Patents
Mixing silicone rubber and preparation method thereof Download PDFInfo
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- CN112063181A CN112063181A CN202010989994.XA CN202010989994A CN112063181A CN 112063181 A CN112063181 A CN 112063181A CN 202010989994 A CN202010989994 A CN 202010989994A CN 112063181 A CN112063181 A CN 112063181A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 106
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 96
- 238000002156 mixing Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000003063 flame retardant Substances 0.000 claims abstract description 42
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 40
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 39
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 34
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 239000007822 coupling agent Substances 0.000 claims abstract description 20
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- -1 triazole compound Chemical class 0.000 claims abstract description 16
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 14
- 239000000194 fatty acid Substances 0.000 claims abstract description 14
- 229930195729 fatty acid Natural products 0.000 claims abstract description 14
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 14
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 13
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 13
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 12
- 229920001971 elastomer Polymers 0.000 claims description 23
- 239000005060 rubber Substances 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 238000004898 kneading Methods 0.000 claims description 5
- 229920002545 silicone oil Polymers 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004513 sizing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 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 claims description 2
- 229920000548 poly(silane) polymer Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 9
- 230000009286 beneficial effect Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- IYAZLDLPUNDVAG-UHFFFAOYSA-N 2-(benzotriazol-2-yl)-4-(2,4,4-trimethylpentan-2-yl)phenol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 IYAZLDLPUNDVAG-UHFFFAOYSA-N 0.000 description 4
- 235000021355 Stearic acid Nutrition 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
- 239000008117 stearic acid Substances 0.000 description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910052809 inorganic oxide Inorganic materials 0.000 description 3
- 239000006082 mold release agent Substances 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 239000005639 Lauric acid Substances 0.000 description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 2
- 239000012964 benzotriazole Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 229940125904 compound 1 Drugs 0.000 description 1
- 229940125782 compound 2 Drugs 0.000 description 1
- 229940126214 compound 3 Drugs 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
Abstract
The invention belongs to the technical field of silicone rubber, and particularly relates to mixed silicone rubber which comprises the following components in parts by mass: 20-100 parts of methyl vinyl silicone rubber, 10-900 parts of vinyl-terminated polymethyl vinyl silicone rubber, 20-800 parts of fumed silica, 0.5-50 parts of platinum flame retardant, 0.3-50 parts of fatty acid, 1-80 parts of structural control agent, 0.1-10 parts of release agent, 0.1-50 parts of ammonium carbonate, 0.3-50 parts of triazole compound, 0.1-30 parts of nano titanium dioxide, 0.1-20 parts of coupling agent and 0.1-30 parts of zinc borate. In addition, the invention also provides a preparation method of the mixing silicone rubber. Compared with the prior art, the mixed silicon rubber has high transparency and high strength, and reaches the flame-retardant safety level.
Description
Technical Field
The invention belongs to the technical field of silicone rubber, and particularly relates to mixed silicone rubber and a preparation method thereof.
Background
The organosilicon mixed silicone rubber is prepared by adding a reinforcing material and other additives on the basis of raw rubber, kneading and mixing the raw rubber to prepare mixed rubber, and then processing, crosslinking and curing the mixed rubber by processes such as mould pressing/extrusion/calendering and the like to prepare various silicone rubber products, and is an organosilicon high polymer material with the most extensive application. However, the organosilicon high molecular material is easy to burn, which is not favorable for the safe, environment-friendly and sustainable development.
The traditional organic silicon flame-retardant rubber compound achieves the flame-retardant effect by adding a large amount of inorganic flame retardants such as aluminum hydroxide and the like or organic nitrogen-phosphorus flame retardants, so that the traditional flame-retardant rubber compound (in white and other colors) loses the natural color transparency of organic silicon, subsequent adjustment processes such as color mixing and dyeing and the like are influenced, the traditional flame-retardant rubber compound is not beneficial to wide expansion of application, flame-retardant silicon rubber is further not beneficial to wide popularization, the popularization of high polymer materials in the aspect of safe flame retardance is hindered, and the requirements of the state on safe, environment-friendly and sustainable development of the high polymer materials are;
therefore, transparent flame-retardant rubber compound appears in the market, and although the transparency of the transparent flame-retardant rubber compound is greatly improved compared with that of the traditional organic silicon flame retardant, part of the transparent flame-retardant rubber compound still cannot reach the flame-retardant safety level of the rubber compound; some parts of the silicone rubber products reach the safety level by adding halogen flame retardant, but are not beneficial to environmental protection, and some parts of the silicone rubber products are not high in mechanical strength and are not beneficial to wide application in downstream silicone rubber product industries.
Disclosure of Invention
One of the objects of the present invention is: aiming at the defects of the prior art, the provided mixed silicone rubber has high transparency and high strength and can reach the flame-retardant safety level.
In order to achieve the purpose, the invention adopts the following technical scheme:
the mixing silicone rubber comprises the following components in parts by mass: 20-100 parts of methyl vinyl silicone rubber, 10-900 parts of vinyl-terminated polymethyl vinyl silicone rubber, 20-800 parts of fumed silica, 0.5-50 parts of platinum flame retardant, 0.3-50 parts of fatty acid, 1-80 parts of structural control agent, 0.1-10 parts of release agent, 0.1-50 parts of ammonium carbonate, 0.3-50 parts of triazole compound, 0.1-30 parts of nano titanium dioxide, 0.1-20 parts of coupling agent and 0.1-30 parts of zinc borate.
As an improvement of the mixed silicone rubber, the average molecular weight of the methyl vinyl silicone rubber is 40-80 ten thousand, wherein the mass percentage of vinyl is 0.03-8%.
As an improvement of the mixed silicone rubber, the average molecular weight of the vinyl-terminated polymethyl vinyl silicone rubber is 40-80 ten thousand, wherein the mass percentage of vinyl is 0.03-8%.
As an improvement of the mixing silicone rubber, the specific surface area of the fumed silica is 100-400 m2/g。
As an improvement of the mixed silicone rubber of the invention, the platinum flame retardant comprises at least one of chloroplatinic acid and a platinum complex.
In the improved mixed silicone rubber, the fatty acid comprises at least one of aliphatic hydrocarbon carboxylic acids with 10-18 carbon atoms. Such as stearic acid, lauric acid, and the like.
As an improvement of the mixing silicon rubber, the structural control agent comprises at least one of hydroxyl silicone oil, diphenyl silanediol, alkoxy silane, low-molecular polysilane and silazane.
As an improvement of the mixing silicon rubber, the triazole compound comprises at least one of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole and benzotriazole.
As an improvement of the mixed silicone rubber of the present invention, the release agent is a stearate-based release agent such as zinc stearate; the coupling agent is an organosilicon coupling agent or a titanate coupling agent, such as organosilicon coupling agent 171.
As an improvement of the mixed silicone rubber, the particle size D50 of the nano titanium dioxide is 15-25 nm. Preferably, the particle size D50 of the nano titanium dioxide is 20 nm.
The second purpose of the invention is: the preparation method of the mixed silicone rubber comprises the following steps:
adding methyl vinyl silicone rubber, vinyl-terminated polymethyl vinyl silicone rubber, fumed silica, a structural control agent and a release agent into a kneader according to parts by mass, kneading for 1-4 h at 130-200 ℃, and discharging to obtain a sizing material A; preferably, kneading at 150-170 ℃ for 2-3 h;
naturally cooling the rubber material A to 25 ℃, and standing for 24h at 25 ℃;
adding the rubber material A, a platinum flame retardant, fatty acid, ammonium carbonate, a triazole compound, nano titanium dioxide, a coupling agent and zinc borate into a kneader, heating to 100 ℃, stirring for 1.5 hours, and discharging to obtain the mixed silicone rubber.
Compared with the prior art, the invention at least has the following beneficial effects:
1) in the invention, two crude rubbers of methyl vinyl silicone rubber and vinyl-terminated polymethyl vinyl silicone rubber are compounded to form a stronger ethylene crosslinking network, so that the mixed silicone rubber has stronger mechanical strength.
2) Compared with the traditional precipitation-process white carbon black, the gas-phase white carbon black has stronger mechanical complementary performance, can assist two raw rubbers of methyl vinyl silicone rubber and vinyl-terminated polymethyl vinyl silicone rubber to reinforce, and further improves the mechanical performance of the mixed silicone rubber; in addition, the coupling agent and the white carbon black prepared by the gas phase method are subjected to chemical reaction to form a chemical bond, so that the physical properties of the mixed silicon rubber are greatly improved; the structural control agent and the white carbon black prepared by the gas phase method are subjected to chemical reaction to form a chemical bond, so that the silicon rubber is prevented from being structured, and the mechanical property of the silicon rubber is prevented from being reduced.
3) In the invention, a platinum flame retardant is adopted instead of a halogen flame retardant or an inorganic oxide flame retardant, which can pass the ROHS test and does not influence the transparency of the mixed silicon rubber; in addition, the fatty acid, the ammonium carbonate and the triazole compound play a role in assisting flame retardance and further improving flame retardance, and the zinc borate plays a role in increasing transparency, so that the mixed silicone rubber is high in transparency and reaches a flame-retardant safety level.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the embodiments of the present invention are not limited thereto.
Example 1
The mixing silicone rubber comprises the following components in parts by mass: 20 parts of methyl vinyl silicone rubber, 80 parts of vinyl-terminated polymethyl vinyl silicone rubber, 40 parts of fumed silica, 1.5 parts of chloroplatinic acid (platinum flame retardant), 35 parts of stearic acid (fatty acid), 3.5 parts of hydroxy silicone oil (structural control agent), 0.5 part of zinc stearate (mold release agent), 2 parts of ammonium carbonate, 40 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole (triazole compound), 0.8 part of nano titanium dioxide, 1 part of organosilicon coupling agent 171 (coupling agent) and 0.9 part of zinc borate. Wherein the average molecular weight of the methyl vinyl silicone rubber is 40-80 ten thousand, and the mass percentage of the vinyl is 4%; the average molecular weight of the vinyl-terminated polymethyl vinyl silicone rubber is 40-80 ten thousand, and the mass percentage of the vinyl is 4%; the specific surface area of the fumed silica is 100-400 m2(ii) in terms of/g. The particle size D50 of the nano titanium dioxide is 20 nm. Ammonium carbonate and zinc borate are of more than industrial purity.
The preparation method of the mixed silicone rubber comprises the following steps:
1) adding methyl vinyl silicone rubber, vinyl-terminated polymethyl vinyl silicone rubber, fumed silica, a structural control agent and a release agent into a kneader according to parts by mass, kneading for 1-4 h at 130-200 ℃, and discharging to obtain a sizing material A;
2) naturally cooling the rubber material A to 25 ℃, and standing for 24h at 25 ℃;
3) adding the rubber material A obtained in the step 2), a platinum flame retardant, fatty acid, ammonium carbonate, a triazole compound, nano titanium dioxide, a coupling agent and zinc borate into a kneader, heating to 100 ℃, stirring for 1.5h, and discharging to obtain the mixed silicone rubber.
Example 2
The difference from example 1 is:
the mixed silicone rubber of the embodiment comprises the following components in parts by mass: 20 parts of methyl vinyl silicone rubber, 90 parts of vinyl-terminated polymethyl vinyl silicone rubber, 45 parts of fumed silica, 2 parts of chloroplatinic acid (platinum flame retardant), 35 parts of lauric acid (fatty acid), 4 parts of hydroxy silicone oil (structural control agent), 0.5 part of zinc stearate (mold release agent), 2 parts of ammonium carbonate, 35 parts of benzotriazole (triazole compound), 0.9 part of nano titanium dioxide, 1 part of organosilicon coupling agent 172 (coupling agent) and 1 part of zinc borate.
The rest is the same as embodiment 1, and the description is omitted here.
Example 3
The difference from example 1 is:
the mixed silicone rubber of the embodiment comprises the following components in parts by mass: 20 parts of methyl vinyl silicone rubber, 100 parts of vinyl-terminated polymethyl vinyl silicone rubber, 50 parts of fumed silica, 2 parts of chloroplatinic acid (platinum flame retardant), 30 parts of stearic acid (fatty acid), 4.5 parts of hydroxy silicone oil (structural control agent), 0.6 part of zinc stearate (mold release agent), 2.2 parts of ammonium carbonate, 35 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole (triazole compound), 0.1-30 parts of nano titanium dioxide, 1 part of organosilicon coupling agent 171 (coupling agent) and 1.2 parts of zinc borate.
The rest is the same as embodiment 1, and the description is omitted here.
Example 4
The difference from example 1 is:
the mass percentage of vinyl in the methyl vinyl silicone rubber is 0.03 percent; the mass percentage of vinyl in the vinyl-terminated polymethyl vinyl silicone rubber is 4 percent.
The rest is the same as embodiment 1, and the description is omitted here.
Example 5
The difference from example 1 is:
the mass percentage of vinyl in the methyl vinyl silicone rubber is 4 percent; the mass percentage of vinyl in the vinyl-terminated polymethyl vinyl silicone rubber is 0.03 percent.
The rest is the same as embodiment 1, and the description is omitted here.
Example 6
The difference from example 1 is:
the mass percentage of vinyl in the methyl vinyl silicone rubber is 4 percent; the mass percentage of vinyl in the vinyl-terminated polymethyl vinyl silicone rubber is 8 percent.
The rest is the same as embodiment 1, and the description is omitted here.
Example 7
The difference from example 1 is:
the mass percentage of vinyl in the methyl vinyl silicone rubber is 8 percent; the mass percentage of vinyl in the vinyl-terminated polymethyl vinyl silicone rubber is 4 percent.
The rest is the same as embodiment 1, and the description is omitted here.
Example 8
The difference from example 1 is:
the mass percentage of vinyl in the methyl vinyl silicone rubber is 0.03 percent; the mass percentage of vinyl in the vinyl-terminated polymethyl vinyl silicone rubber is 8 percent.
The rest is the same as embodiment 1, and the description is omitted here.
Example 9
The difference from example 1 is:
the mass percentage of vinyl in the methyl vinyl silicone rubber is 8 percent; the mass percentage of vinyl in the vinyl-terminated polymethyl vinyl silicone rubber is 0.03 percent.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 1
The difference from example 1 is:
no vinyl terminated polymethylvinylsiloxane rubber was added.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 2
The difference from example 1 is:
the flame retardant is a halogen flame retardant.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 3
The difference from example 1 is:
the flame retardant is an inorganic oxide flame retardant.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 4
The difference from example 1 is:
stearic acid (fatty acid), ammonium carbonate and 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole (triazole-based compound) were not added.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 5
The difference from example 1 is:
no zinc borate was added.
The rest is the same as embodiment 1, and the description is omitted here.
Performance testing
The silicone rubber compounds obtained in examples 1 to 9 and comparative examples 1 to 5, and commercial compound 1 (non-transparent), compound 2 (transparent) and compound 3 (transparent) were subjected to performance tests, and the results are shown in table 1.
TABLE 1 test results
As can be seen from the test results of table 1:
1) as can be seen by comparing examples 1-9 with comparative examples 1-5 and rubber mixtures 1-3, the mixed silicone rubber prepared by the formula provided by the invention is transparent in appearance, the flame retardant grade can reach 94VO, and the mechanical strength can be more than twice that of other silicone rubbers through ROHS.
2) As can be seen from the comparison of examples and comparative example 1, when the system contains only one raw rubber of methyl vinyl silicone rubber, the mechanical strength of the prepared mixed silicone rubber is poor, and when the system adopts two raw rubbers of methyl vinyl silicone rubber and vinyl-terminated polymethyl vinyl silicone rubber, the mechanical strength of the obtained mixed silicone rubber is greatly improved. The reason is that the methyl vinyl silicone rubber and the vinyl-terminated polymethyl vinyl silicone rubber are compounded to form a stronger ethylene crosslinking network, so that the mechanical strength of the mixed silicone rubber is improved. In particular, the compounded silicone rubber obtained in example 1 was the most excellent in mechanical strength.
3) Compared with halogen flame retardants and inorganic oxide flame retardants, the platinum flame retardant used in the invention can reach a flame retardant rating of 94VO, and can pass ROHS test, so that the platinum flame retardant has environmental protection and safety, and the platinum flame retardant does not affect the color of the mixed silicone rubber, so that the mixed silicone rubber can keep natural color and transparency.
4) As can be seen from the comparison between the examples and the comparative example 4, when the fatty acid, the ammonium carbonate and the triazole compound are also added into the formula, the oxygen index of the prepared mixed silicon rubber is higher, which shows that the flame retardant effect is better, because the three materials play a role in assisting flame retardance, thereby further improving the flame retardant property.
5) As can be seen from the comparison of examples and comparative example 5, when zinc borate was further added to the formulation, the resulting compounded silicone rubber was more transparent, indicating that it had an effect of increasing transparency.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. The mixing silicone rubber is characterized by comprising the following components in parts by mass: 20-100 parts of methyl vinyl silicone rubber, 10-900 parts of vinyl-terminated polymethyl vinyl silicone rubber, 20-800 parts of fumed silica, 0.5-50 parts of platinum flame retardant, 0.3-50 parts of fatty acid, 1-80 parts of structural control agent, 0.1-10 parts of release agent, 0.1-50 parts of ammonium carbonate, 0.3-50 parts of triazole compound, 0.1-30 parts of nano titanium dioxide, 0.1-20 parts of coupling agent and 0.1-30 parts of zinc borate.
2. The mixing silicone rubber according to claim 1, wherein the average molecular weight of the methyl vinyl silicone rubber is 40 to 80 ten thousand, and the mass percentage of vinyl groups is 0.03 to 8%.
3. The mixing silicone rubber according to claim 1, wherein the average molecular weight of the vinyl-terminated polymethylvinyl silicone rubber is 40 to 80 ten thousand, and the mass percentage of vinyl is 0.03 to 8%.
4. The mixing silicone rubber according to claim 1, wherein the fumed silica has a specific surface area of 100 to 400m2/g。
5. The compounded silicone rubber according to claim 1, wherein the platinum flame retardant comprises at least one of chloroplatinic acid and a platinum complex.
6. The compounded silicone rubber according to claim 1, wherein the fatty acid comprises at least one of aliphatic hydrocarbon carboxylic acids having 10 to 18 carbon atoms.
7. The compounded silicone rubber according to claim 1, wherein the structural control agent comprises at least one of a hydroxy silicone oil, a diphenylsilanediol, an alkoxysilane, a low molecular polysilane, and a silazane.
8. The compounded silicone rubber according to claim 1, wherein the release agent is a stearate-based release agent, and the coupling agent is an organosilicon coupling agent or a titanate coupling agent.
9. The mixed silicone rubber according to claim 1, wherein the particle diameter D50 of the nano titanium dioxide is 15 to 25 nm.
10. A method for producing the mixed silicone rubber according to any one of claims 1 to 9, characterized by comprising the steps of:
adding methyl vinyl silicone rubber, vinyl-terminated polymethyl vinyl silicone rubber, fumed silica, a structural control agent and a release agent into a kneader according to parts by mass, kneading for 1-4 h at 130-200 ℃, and discharging to obtain a sizing material A;
naturally cooling the rubber material A to 25 ℃, and standing for 24h at 25 ℃;
adding the rubber material A, a platinum flame retardant, fatty acid, ammonium carbonate, a triazole compound, nano titanium dioxide, a coupling agent and zinc borate into a kneader, heating to 100 ℃, stirring for 1.5 hours, and discharging to obtain the mixed silicone rubber.
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