CN115246990B - Double-component addition type room temperature vulcanization mold silicon rubber and preparation method thereof - Google Patents
Double-component addition type room temperature vulcanization mold silicon rubber and preparation method thereof Download PDFInfo
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- CN115246990B CN115246990B CN202110460005.2A CN202110460005A CN115246990B CN 115246990 B CN115246990 B CN 115246990B CN 202110460005 A CN202110460005 A CN 202110460005A CN 115246990 B CN115246990 B CN 115246990B
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 238000004073 vulcanization Methods 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 93
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 74
- 239000000945 filler Substances 0.000 claims abstract description 70
- 239000004945 silicone rubber Substances 0.000 claims abstract description 53
- 229920005601 base polymer Polymers 0.000 claims abstract description 48
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000002156 mixing Methods 0.000 claims abstract description 44
- 229910000077 silane Inorganic materials 0.000 claims abstract description 44
- 239000003112 inhibitor Substances 0.000 claims abstract description 41
- 239000001257 hydrogen Substances 0.000 claims abstract description 40
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 40
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229920002545 silicone oil Polymers 0.000 claims abstract description 38
- 239000003085 diluting agent Substances 0.000 claims abstract description 37
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- -1 polysiloxane Polymers 0.000 claims description 39
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 36
- 229920001296 polysiloxane Polymers 0.000 claims description 35
- 229920002554 vinyl polymer Polymers 0.000 claims description 34
- 229920001971 elastomer Polymers 0.000 claims description 32
- 239000005060 rubber Substances 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 28
- 239000003292 glue Substances 0.000 claims description 20
- 238000004898 kneading Methods 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 19
- 229910021485 fumed silica Inorganic materials 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 18
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 16
- 239000013522 chelant Substances 0.000 claims description 15
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 11
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 239000000378 calcium silicate Substances 0.000 claims description 7
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 7
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical group [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 6
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 5
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 150000004687 hexahydrates Chemical class 0.000 claims description 2
- BHKICDZVEDYKMW-UHFFFAOYSA-N 4-ethenyl-2,2,6,6-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C[Si]1(O[SiH2]O[Si](O[SiH](O1)C=C)(C)C)C BHKICDZVEDYKMW-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 12
- 230000007306 turnover Effects 0.000 abstract description 7
- 229920002635 polyurethane Polymers 0.000 abstract description 6
- 239000004814 polyurethane Substances 0.000 abstract description 6
- 229920006305 unsaturated polyester Polymers 0.000 abstract description 4
- 239000002585 base Substances 0.000 description 50
- 230000000052 comparative effect Effects 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 7
- 229910002026 crystalline silica Inorganic materials 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical group C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- WRXCBRHBHGNNQA-UHFFFAOYSA-N (2,4-dichlorobenzoyl) 2,4-dichlorobenzenecarboperoxoate Chemical group ClC1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1Cl WRXCBRHBHGNNQA-UHFFFAOYSA-N 0.000 description 1
- WZJUBBHODHNQPW-UHFFFAOYSA-N 2,4,6,8-tetramethyl-1,3,5,7,2$l^{3},4$l^{3},6$l^{3},8$l^{3}-tetraoxatetrasilocane Chemical compound C[Si]1O[Si](C)O[Si](C)O[Si](C)O1 WZJUBBHODHNQPW-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 241000505722 Uraria Species 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- FSIJKGMIQTVTNP-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C=C)C=C FSIJKGMIQTVTNP-UHFFFAOYSA-N 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 239000012975 dibutyltin dilaurate Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002023 wood Substances 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
-
- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a double-component addition type room temperature vulcanization mold silicon rubber and a preparation method thereof, wherein the double-component addition type room temperature vulcanization mold silicon rubber is prepared by preparing a component A and a component B by mixing the component A and the component B according to the mass ratio of 10:1-1:1; a component: base polymer, reinforcing filler, heavy filler, silane treating agent, diluent, platinum catalyst, inhibitor and viscosity increase control agent; and the component B comprises the following components: base polymer, reinforcing filler, heavy filler, silane treating agent, hydrogen-containing silicone oil, diluent, inhibitor, color paste and viscosity increase control agent. The silicone rubber has excellent fluidity within 2 hours at room temperature, can be vulcanized and molded within 8-12 hours, has good operability, high mold turnover frequency, average turnover frequency of more than 120 times, and simple and convenient operation, is suitable for preparing molds of turnover mold materials such as unsaturated polyester, polyurethane and the like, and particularly can prepare large-sized molds.
Description
Technical Field
The invention relates to a mold rubber, in particular to a double-component addition type room temperature vulcanization mold silicon rubber and a preparation method thereof, which are suitable for preparing molds of unsaturated polyester, polyurethane and other mold turning materials, and belong to the technical field of liquid silicon rubber.
Background
With the improvement of living standard, the demand of people for decorative materials is also increasing. At present, large-scale decorative materials with various complex patterns are cast by adopting polyurethane hard foam and the like for high-grade building decoration, and the requirements of good mold stripping performance, high dimensional accuracy and multiple mold turnover times are met. The silicon rubber preparation mold has the characteristics of convenient operation, low cost, easy demolding and the like, can replace the traditional wood and metal molds, and is widely applied to reproduction of artware and building ornaments. The silicon rubber of the addition type die does not release low molecular substances during vulcanization, and has the advantages of low shrinkage rate after molding, high dimensional stability, deep vulcanization and the like, and is widely applied to the field of precision dies. The relevant situation of the existing mold silicone rubber can be further understood by the following patent documents:
patent CN 201510485805.4 discloses an acid and alkali resistant die silicone rubber, which adopts a polysulfide vulcanization system, wherein the vulcanizing agent is 2, 4-dichloro benzoyl peroxide, and the prepared die silicone rubber has better acid and alkali resistance and is suitable for acidic or alkaline working occasions. Patent CN201010231638.8 discloses a kind of transparent high temperature resistant rubber compound for silicon rubber mould, which is used for producing mould used for high grade alloy ornaments. Both the two kinds of silicon rubber are peroxide vulcanized high-temperature rubber compounds, and the silicon rubber needs to be vulcanized and formed under high-temperature and high-pressure conditions.
Patent CN 201510485836.X discloses a tear-resistant mold silicone rubber, which adopts modified uraria to improve the tear strength, adopts tetraethoxysilane as a cross-linking agent, di-tert-butyl peroxide as a vulcanizing agent and dibutyltin dilaurate as an accelerator, wherein the vulcanizing agent and the accelerator in the room temperature vulcanizing mold silicone rubber are non-environment-friendly materials, and the operability and the service life of the mold are not described.
Patent CN201510083787.7 discloses a silicone rubber for injection molding two-component addition mold, which has long operation time and rapid vulcanization at high temperature, and is used for preparing a mold for artificial jewelry for decoration, and the mold turnover frequency is high. The liquid injection molding die for molding the silicone rubber requires equipment heating, and is not suitable for producing a die with a large size.
Therefore, the room temperature vulcanized mold silicone rubber which has longer operable time and is cured quickly at room temperature is not reported in the prior art, and the common mold silicone rubber on the market has shorter service life when large polyurethane hard foam materials are copied, the average copying time is about 80 times, and the mold is seriously damaged and can only be scrapped.
Disclosure of Invention
The invention aims to solve the technical problems, and provides a double-component addition type room temperature vulcanizing mold silicon rubber, which is characterized in that heavy filler, viscosity increase control, silane treating agent and the like are introduced into the existing double-component silicon rubber formula, so that the service life of the mold is obviously prolonged, the average reproduction time can reach more than 120 times, the mold rubber has good operability, low mold shrinkage, high simulation rate of a reproduction model and high dimensional accuracy, and is suitable for preparing molds of unsaturated polyester, polyurethane and other mold turnover materials, and particularly large-sized molds can be prepared.
The invention further aims to provide a preparation method of the double-component addition type room temperature vulcanization mold silicon rubber, which does not need heating equipment, can be molded through room temperature vulcanization, is simple and convenient to operate, improves the production efficiency of rubber materials, and is easy for mass production and preparation of large-scale molds.
The aim of the invention is achieved by the following technical scheme:
the double-component addition type room temperature vulcanization mold silicone rubber is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 10:1-1:1 to prepare the mold silicone rubber;
a component: 100 parts of base polymer, 15-30 parts of reinforcing filler, 10-40 parts of heavy filler, 5-20 parts of silane treating agent, 1-50 parts of diluent, 0.1-3 parts of platinum catalyst, 0.02-3 parts of inhibitor and 0.01-1 part of viscosity increase control agent;
and the component B comprises the following components: 100 parts of base polymer, 15-30 parts of reinforcing filler, 0-40 parts of heavy filler, 5-20 parts of silane treating agent, 40-120 parts of hydrogen-containing silicone oil, 0-40 parts of diluent, 0-3 parts of inhibitor, 0-3 parts of color paste and 0.01-1 part of viscosity increase control agent.
In the present invention, the base polymer is selected from linear vinyl-terminated polysiloxanes having a vinyl content (mass percent) of 0.1 to 0.25%, preferably 0.25%.
In the invention, the reinforcing filler is fumed silica, and the specific surface area is 100-400 g/cm 3 Preferably 200g/cm 3 。
In the present invention, the heavy filler is selected from crystalline silica micropowder, talc or a silicate, and has an average particle diameter of 0.5 to 20. Mu.m, preferably 2 to 10. Mu.m, and more preferably 4. Mu.m; among them, calcium silicate is preferable.
In the invention, the silane treating agent is at least one selected from methyltriethoxysilane, vinyltriethoxysilane, methyltrimethoxysilane, hexamethyldisilazane, hydroxyl silicone oil and divinyl tetramethyl silazane, or a mixture of the two.
In the invention, the diluent is methyl silicone oil or vinyl-terminated silicone oil or a mixture of the methyl silicone oil and the vinyl-terminated silicone oil; the viscosity is 30 to 8000 mPas, preferably 30 to 3000 mPas, more preferably 30 to 500 mPas.
In the invention, the inhibitor is at least one selected from 2-methyl-3-butynyl-2 alcohol, 3-methyl-1-hexynyl-3-alcohol, tetramethyl divinyl disiloxane, tetramethyl cyclotetrasiloxane, vinyl methyl mixed ring and polyvinyl linear polysiloxane; the formula of the polyvinyl linear polysiloxane is R (CH) 3 ) 2 SiO-[Si(CH 3 ) 2 O] m -[Si(CH 3 )（CH 2 =CH-）O] n -Si-R (CH 3 ) 2 Wherein R is-CH 3 Or-ch=ch 2 ，m=0～50，n=10～50。
In the invention, the platinum catalyst is selected from at least one of alcohol modified chloroplatinic acid, chloroplatinic acid hexahydrate and chelate of three compounds; the chelate includes: platinum chelate of olefin, platinum chelate of carbonyl, platinum chelate of alkenyl siloxane, platinum chelate of organopolysiloxane; such as chelate of chloroplatinic acid and 1, 3-divinyl tetramethyl disiloxane, and platinum content of 500-15000 ppm.
In the invention, the hydrogen content of the hydrogen-containing silicone oil is 0.2 to 0.9 weight percent.
In the present invention, the viscosity build-up control agent is selected from the group consisting of compounds having the formula (CH) 3 ) 3 Si-O-[Si(CH 3 ) 2 O] m A monohydroxy-terminated polysiloxane having the formula H, m=0 to 100, or ho—si (CH) 2 )-O-[Si(CH 3 ) 2 ] n OH, n=1 to 100;
a preparation method of a double-component addition type room temperature vulcanization mold silicon rubber comprises the following steps:
(1) Preparation of reinforcing filler base adhesive
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, adding a reinforcing filler in batches after uniformly mixing, slowly heating to 60-120 ℃ after uniformly mixing, heating to 120-160 ℃ after kneading for 1-2 hours, vacuumizing to the vacuum degree of minus 0.06-minus 0.09MPa, continuously kneading for 2-4 hours, and cooling to obtain the reinforcing filler base adhesive;
(2) Preparation of heavy filler base gum
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, adding a heavy filler after uniformly mixing, kneading for 1-2 hours, heating to 80-150 ℃, vacuumizing to the vacuum degree of-0.06-0.009 MPa, continuously kneading for 2-4 hours, and cooling to obtain the heavy filler base rubber;
(3) Preparation of component A
Weighing reinforcing filler base glue, heavy filler base glue, a diluent, an inhibitor, a platinum catalyst and a viscosity increase control agent according to a formula, and stirring in a planetary stirrer for 20-30 minutes at normal temperature to obtain a component A;
(4) Preparation of component B
Weighing reinforcing filler base glue, heavy filler base glue, diluent, inhibitor, hydrogen-containing silicone oil, viscosity increase control agent and color paste according to the formula, and stirring in a planetary stirrer for 20-30 minutes at normal temperature to obtain a component B;
(5) Mixing of the Components
Mixing the component A and the component B according to the mass ratio of 10:1-1:1, and vacuumizing and defoaming to obtain the die silicone rubber.
Compared with the prior art, the invention has the following advantages:
(1) The basic polymer, the diluent, the inhibitor and the viscosity increase control agent in the formula of the invention respectively select polysiloxane with different structures, and the centralized cross-linked network structure formed by the polysiloxane can effectively improve the elongation at break and the tearing strength of the silicone rubber of the die, and endow the die with excellent strength and demolding performance, and is not easy to damage when in use.
(2) In general, the mold silicone rubber adopts a white carbon black reinforcing system, and the introduction of heavy filler can obviously reduce the mechanical property of the mold silicone rubber. However, the invention can maintain better mechanical property by adding the heavy filler of crystal silicon micropowder, talcum powder or calcium silicate and carrying out surface treatment, can effectively reduce the infiltration and corrosion of unsaturated resin to the silicon rubber, improve the solvent resistance of the silicon rubber, and achieve the purpose of prolonging the service life of the silicon rubber mold, namely the prepared mold has high service life.
(3) Because a large amount of hydroxyl groups remain on the surface of the white carbon black in the silicone rubber, hydrogen bonds are easily formed between the hydroxyl groups or between the hydroxyl groups on the surface of the white carbon black and the cross-linking agent, and the viscosity of the AB rubber material is excessively fast increased after the AB rubber material is mixed. According to the invention, by adding the viscosity increase control agent, the hydroxyl of the viscosity increase control agent and the hydroxyl on the surface of the white carbon black act to form hydrogen bond or Van der Waals force, so that the reaction can be avoided, the viscosity increase speed of the mixed sizing material is reduced, the operable time of the die silicone rubber is prolonged, and the die silicone rubber can be cured in 6-12 hours.
(4) The invention prepares the reinforced filler base rubber and the heavy filler base rubber, can uniformly add the two fillers into A, B components, and then prepares the die silicone rubber by mixing.
(5) The mixing A, B of the components of the room temperature vulcanization mold silicone rubber can be completed only by conventional mixing equipment. No toxic and harmful substances, no special equipment in the production process and no toxic solvent. The curing and forming process does not need an additional heating and heating device, the construction process is simple and quick, the production efficiency of the sizing material is improved, and the large-scale production and the preparation of the large-scale mold are easy.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
The embodiment relates to a double-component addition type room temperature vulcanization mold silicon rubber, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 10:1;
a component: 100 parts of base polymer, 30 parts of reinforcing filler, 30 parts of heavy filler, 5 parts of silane treating agent, 5 parts of diluent, 0.2 part of platinum catalyst, 0.1 part of inhibitor and 0.1 part of viscosity increase control agent;
and the component B comprises the following components: 100 parts of base polymer, 30 parts of reinforcing filler, 5 parts of silane treating agent, 50 parts of hydrogen-containing silicone oil, 1 part of inhibitor and 0.1 part of viscosity increase control agent;
wherein,,
the base polymer was a linear vinyl terminated polysiloxane having a vinyl content (mass percent) of 0.25%;
the reinforcing filler has a specific surface area of 200m 2 Fumed silica/g;
the heavy filler is crystalline silica micropowder with an average particle diameter of 4 mu m;
the silane treating agent is hexamethyldisilazane;
the diluent is methyl silicone oil with the viscosity of 30 mpa.s;
the platinum catalyst is chelate of chloroplatinic acid and 1, 3-divinyl tetramethyl disiloxane, and the platinum content is 5000ppm;
the inhibitor is polyvinyl linear polysiloxane; the polyvinyl linear polysiloxane has the formula (CH) 3 ) 3 SiO- [Si(CH 3 )（CH 2 =CH-）O] n -Si-(CH 3 ) 3 ，n=10～50；
The viscosity build-up control agent is a linear hydroxyl terminated polysiloxane of the formula HO (CH) 3 ) 2 Si-O-[Si(CH 3 ) 2 O] m H，m=15～30；
The hydrogen content of the hydrogen-containing silicone oil is 0.6wt%.
In order to achieve the uniform addition of the reinforcing filler and the heavy filler, the invention prepares the reinforcing filler base rubber and the heavy filler base rubber, then prepares the component A and the component B separately, and then mixes the component A and the component B according to the mass ratio of 10:1 to obtain the die silicone rubber.
The specific preparation method of the die silicone rubber comprises the following steps:
(1) Preparation of reinforcing filler base adhesive
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, adding a reinforcing filler in batches after uniformly mixing, slowly heating to 100 ℃ after uniformly mixing, heating to 140 ℃ after kneading for 1h, vacuumizing to the vacuum degree of-0.06 MPa, continuously kneading for 2 hours, and cooling to obtain a reinforcing filler base rubber;
(2) Preparation of heavy filler base gum
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, uniformly mixing, adding a heavy filler, kneading for 1h, heating to 80 ℃, vacuumizing to the vacuum degree of-0.06 MPa, continuously kneading for 2h, and cooling to obtain a heavy filler base adhesive;
(3) Preparation of component A
Weighing reinforcing filler base glue, heavy filler base glue, a diluent, an inhibitor, a platinum catalyst and a viscosity increase control agent according to a formula, and stirring in a planetary stirrer for 20 minutes at normal temperature to obtain a component A;
(4) Preparation of component B
Weighing reinforcing filler base glue, heavy filler base glue, inhibitor, hydrogen-containing silicone oil and viscosity increase control agent according to the formula, and stirring in a planetary stirrer for 20 minutes at normal temperature to obtain a component B;
(5) Mixing of the Components
And mixing the component A and the component B according to the mass ratio of 10:1, and vacuumizing and defoaming to obtain the die silicone rubber I.
Example 2
The embodiment relates to a double-component addition type room temperature vulcanization mold silicon rubber, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 10:1;
a component: 100 parts of base polymer, 30 parts of reinforcing filler, 10 parts of heavy filler, 10 parts of silane treating agent, 20 parts of diluent, 0.1 part of platinum catalyst, 0.05 part of inhibitor and 0.3 part of viscosity increase control agent;
and the component B comprises the following components: 100 parts of base polymer, 30 parts of reinforcing filler, 120 parts of hydrogen-containing silicone oil, 0.3 part of inhibitor, 2 parts of iron oxide red paste and 0.3 part of viscosity increase control agent;
wherein,,
the base polymer was a linear vinyl terminated polysiloxane having a vinyl content (mass percent) of 0.25%;
the reinforcing filler has a specific surface area of 200m 2 Fumed silica/g;
the heavy filler is crystalline silica micropowder with an average particle diameter of 2 mu m;
the silane treating agent is a mixture of hexamethyldisilazane and methyltrimethoxysilane, and the mixing ratio is 9:1;
the diluent is methyl silicone oil with the viscosity of 300 mpa.s;
the platinum catalyst is chloroplatinic acid isopropanol solution, and the platinum content is 8000ppm;
the inhibitor is tetravinyl tetramethyl cyclotetrasiloxane;
the viscosity build-up control agent is a monohydroxy-terminated polysiloxane having the formula (CH) 3 ) 3 Si-O-[Si(CH 3 ) 2 O] m H，m=0～15；
The hydrogen content of the hydrogen-containing silicone oil is 0.2wt%.
In order to achieve the uniform addition of the reinforcing filler and the heavy filler, the invention firstly prepares the reinforcing filler base rubber and the heavy filler base rubber, then separately prepares the component A and the component B, and then mixes the component A and the component B according to the mass ratio of 10:1 to obtain the die silicone rubber II, and the specific preparation method is the same as that of the example 1.
Example 3
The embodiment relates to a double-component addition type room temperature vulcanization mold silicon rubber, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 10:1;
a component: 100 parts of base polymer, 15 parts of reinforcing filler, 40 parts of heavy filler, 5 parts of silane treating agent, 5 parts of diluent, 3 parts of platinum catalyst, 0.02 part of inhibitor and 0.01 part of viscosity increase control agent;
and the component B comprises the following components: 100 parts of base polymer, 30 parts of reinforcing filler, 15 parts of heavy filler, 5 parts of silane treating agent, 60 parts of hydrogen-containing silicone oil, 10 parts of diluent, 0.02 part of inhibitor and 0.01 part of viscosity increase control agent;
wherein,,
the base polymer was a linear vinyl terminated polysiloxane having a vinyl content (mass percent) of 0.25%;
the reinforcing filler has a specific surface area of 400m 2 Fumed silica/g;
the heavy filler is talcum powder with an average particle size of 2 mu m;
the silane treating agent is a mixture of hexamethyldisilazane and methyltriethoxysilane, and the mixing ratio is 9:1;
the diluent is vinyl-terminated silicone oil with the viscosity of 100 mpa.s;
the platinum catalyst is chloroplatinic acid isopropanol solution, and the platinum content is 500ppm;
the inhibitor is 2-methyl-3-butynyl-2 alcohol;
the viscosity increase control agent is a dihydroxy terminated polysiloxane with the molecular formula HO- [ Si (CH) 2 ) 2 -O] n -Si(CH 3 ) 2 OH，n=20～100；
The hydrogen-containing silicone oil contains 0.6wt% of hydrogen.
The reinforcing filler and the heavy filler are respectively prepared into reinforcing filler base rubber and heavy filler base rubber with a base polymer, then the reinforcing filler base rubber and the heavy filler base rubber are mixed with other raw materials under stirring to prepare a component A and a component B, and finally the component A and the component B are mixed according to the mass ratio of 10:1 to obtain the die silicone rubber.
The specific preparation method of the die silicone rubber comprises the following steps:
(1) Preparation of reinforcing filler base adhesive
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, adding a reinforcing filler in batches after uniformly mixing, slowly heating to 60 ℃ after uniformly mixing, heating to 120 ℃ after kneading for 2 hours, vacuumizing to the vacuum degree of-0.09 MPa, continuously kneading for 4 hours, and cooling to obtain a reinforcing filler base rubber;
(2) Preparation of heavy filler base gum
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, uniformly mixing, adding a heavy filler, kneading for 2 hours, heating to 150 ℃, vacuumizing to the vacuum degree of-0.09 MPa, continuously kneading for 4 hours, and cooling to obtain a heavy filler base adhesive;
(3) Preparation of component A
Weighing reinforcing filler base glue, heavy filler base glue, a diluent, an inhibitor, a platinum catalyst and a viscosity increase control agent according to a formula, and stirring in a planetary stirrer for 30 minutes at normal temperature to obtain a component A;
(4) Preparation of component B
Weighing reinforcing filler base glue, heavy filler base glue, a diluent, an inhibitor, hydrogen-containing silicone oil and a viscosity increase control agent according to a formula, and stirring in a planetary stirrer for 30 minutes at normal temperature to obtain a component B;
(5) Mixing of the Components
And mixing the component A and the component B according to the mass ratio of 10:1, and vacuumizing and defoaming to obtain the die silicon rubber III.
Example 4
The embodiment relates to a double-component addition type room temperature vulcanization mold silicon rubber, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 1:1;
a component: 100 parts of base polymer, 20 parts of reinforcing filler, 40 parts of heavy filler, 20 parts of silane treating agent, 1 part of diluent, 0.1 part of platinum catalyst, 0.02 part of inhibitor and 1 part of viscosity increase control agent;
and the component B comprises the following components: 100 parts of base polymer, 15 parts of reinforcing filler, 40 parts of heavy filler, 20 parts of silane treating agent, 40 parts of hydrogen-containing silicone oil, 40 parts of diluent and 0.5 part of viscosity increase control agent;
wherein,,
the base polymer was a linear vinyl terminated polysiloxane having a vinyl content (mass percent) of 0.25%;
the reinforcing filler has a specific surface area of 400m 2 Fumed silica/g;
the heavy filler is calcium silicate with an average particle size of 10 mu m;
the silane treating agent is a mixture of hexamethyldisilazane and methyltrimethoxysilane, and the mixing ratio of the hexamethyldisilazane to methyltrimethoxysilane is 8:2;
the diluent is methyl silicone oil with the viscosity of 500 mPas;
the platinum catalyst is chelate of chloroplatinic acid and beta-diketone, and the platinum content is 15000ppm;
the inhibitor is 3-methyl-1-hexynyl-3-ol;
the viscosity build-up control agent is a monohydroxy-terminated polysiloxane having the formula (CH) 3 ) 3 Si-O-[Si(CH 3 ) 2 O] m H，m=20～40；
The hydrogen content of the hydrogen-containing silicone oil is 0.9wt%.
The reinforcing filler and the heavy filler are respectively prepared into reinforcing filler base rubber and heavy filler base rubber with a base polymer, then the reinforcing filler base rubber and the heavy filler base rubber are mixed with other raw materials under stirring to prepare a component A and a component B, and finally the component A and the component B are mixed according to the mass ratio of 1:1 to obtain the die silicone rubber.
The specific preparation method of the die silicone rubber comprises the following steps:
(1) Preparation of reinforcing filler base adhesive
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, adding a reinforcing filler in batches after uniformly mixing, slowly heating to 120 ℃ after uniformly mixing, heating to 160 ℃ after kneading for 1h, vacuumizing to the vacuum degree of-0.08 MPa, continuously kneading for 3 hours, and cooling to obtain a reinforcing filler base rubber;
(2) Preparation of heavy filler base gum
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, uniformly mixing, adding a heavy filler, kneading for 1.5h, heating to 100 ℃, vacuumizing to the vacuum degree of-0.08 MPa, continuously kneading for 2 hours, and cooling to obtain a heavy filler base adhesive;
(3) Preparation of component A
Weighing reinforcing filler base glue, heavy filler base glue, a diluent, an inhibitor, a platinum catalyst and a viscosity increase control agent according to a formula, and stirring in a planetary stirrer for 25 minutes at normal temperature to obtain a component A;
(4) Preparation of component B
Weighing reinforcing filler base glue, heavy filler base glue, a diluent, hydrogen-containing silicone oil and a viscosity increase control agent according to a formula, and stirring in a planetary stirrer for 25 minutes at normal temperature to obtain a component B;
(5) Mixing of the Components
And mixing the component A and the component B according to the mass ratio of 1:1, and vacuumizing and defoaming to obtain the die silicone rubber IV.
Example 5
The embodiment relates to a double-component addition type room temperature vulcanizing mold silicon rubber, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 8:1 to prepare a mold silicon rubber V, wherein the specific preparation method is the same as that of the embodiment 1.
A component: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 300m 2 Per gram of fumed silica), 25 parts of heavy filler (calcium silicate having an average particle diameter of 1 μm), 35 parts of silane treating agent (mixture of hexamethyldisilazane and hydroxy silicone oil 10:2), 18 parts of diluent (mixture of methyl silicone oil and vinyl terminated silicone oil, viscosity 300mpa·s), 50 parts of viscosity growth controlling agent (molecular formula (CH) 3 ) 3 Si-O-[Si(CH 3 ) 2 O] m H, m=30 to 100), 0.5 part, 2 parts of platinum catalyst (alcohol modified chloroplatinic acid with platinum content of 1000 ppm), 1 part of inhibitor (tetravinyl tetramethyl cyclotetrasiloxane);
and the component B comprises the following components: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 300m 2 Per gram of fumed silica), 10 parts of a silane treating agent (mixture of divinyl tetramethylsilazane and hydroxy silicone oil, mixing ratio 1:9), 80 parts of hydrogen-containing silicone oil (hydrogen content 0.5 wt.%) and a viscosity growth controlling agent (molecular formula (CH) 3 ) 3 Si-O-[Si(CH 3 ) 2 O] m H, m=30 to 100) 1 part.
Example 6
The embodiment relates to a double-component addition type room temperature vulcanizing mold silicon rubber, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 6:1 to prepare the mold silicon rubber VI, wherein the specific preparation method is the same as that of the embodiment 1.
A component: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area of 200m 2 30 parts per g of fumed silica), 25 parts of heavy filler (crystalline silica micropowder with an average particle diameter of 15 μm), 20 parts of silane treatment agent (mixture of methyltriethoxysilane and vinyltriethoxysilane in a ratio of 9:1), and diluent (methyl silicone oil, viscosity)80 mPa.s) 5 parts, a viscosity build control agent (molecular formula HO-Si (CH) 2 )-O-[Si(CH 3 ) 2 ] m OH, m=5 to 10), 3 parts of platinum catalyst (chloroplatinic acid and a mixture of chloroplatinic acid and chelate of 1, 3-divinyl tetramethyl disiloxane, platinum content 15000 ppm), 0.1 parts of inhibitor (vinylmethyl mixed ring);
and the component B comprises the following components: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 100m 2 15 parts of per gram of fumed silica), 5 parts of silane treating agent (hexamethyldisilazane), 60 parts of hydrogen-containing silicone oil (hydrogen content is 0.8 wt%) 0.5 parts of inhibitor (vinylmethyl mixed ring), 1 part of pigment paste, and a viscosity increase control agent (with a molecular formula of HO-Si (CH) 2 )-O-[Si(CH 3 ) 2 ] m OH, m=5 to 10) 3 parts.
Example 7
The embodiment relates to a double-component addition type room temperature vulcanization mold silicon rubber, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 3:1 to prepare a mold silicon rubber VII, wherein the specific preparation method is the same as that of the embodiment 1.
A component: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area of 250m 2 30 parts per g of fumed silica), 40 parts of heavy filler (talcum powder with an average particle size of 4 mu m), 15 parts of silane treating agent (mixture of hexamethyldisilazane and methyltrimethoxysilane in a ratio of 9:1), 40 parts of diluent (ethyl silicone oil, viscosity of 500 mPa.s), and viscosity increase control agent (with a molecular formula of HO-Si (CH) 2 )-O-[Si(CH 3 ) 2 ] n OH, n=60 to 100), 0.1 part, 2.5 parts of platinum catalyst (chelate of chloroplatinic acid and 1, 3-divinyl tetramethyl disiloxane, platinum content of 2000 ppm), 3 parts of inhibitor (divinyl tetramethyl disiloxane);
and the component B comprises the following components: 100 parts of base polymer (linear vinyl-terminated polysiloxane with a vinyl content of 0.25%) and reinforcing fillerMaterial (specific surface area 250 m) 2 20 parts of per gram of fumed silica), 6 parts of a silane treatment agent (hexamethyldisilazane), 20 parts of hydrogen-containing silicone oil (hydrogen content is 0.9 wt%) and 40 parts of a diluent (ethyl silicone oil, viscosity 8000 mPas), 3 parts of an inhibitor (tetramethyl divinyl disiloxane), and a viscosity increase control agent (molecular formula is HO-Si (CH) 2 )-O-[Si(CH 3 ) 2 ] n OH, n=60 to 100) 0.1 part.
Example 8
The embodiment relates to a double-component addition type room temperature vulcanizing mold silicon rubber, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 1:1 to prepare the mold silicon rubber VIII, wherein the specific preparation method is the same as that of the embodiment 1.
A component: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area of 200m 2 30 parts per g of fumed silica), 30 parts of heavy filler (calcium silicate with an average particle size of 4 μm), 5 parts of silane treatment agent (hexamethyldisilazane), 5 parts of diluent (methyl silicone oil, viscosity of 200 mPa.s), and viscosity increase control agent (molecular formula of HO-Si (CH) 2 )-O-[Si(CH 3 ) 2 ] n OH, n=1 to 15) 0.1 part, 1 part of a platinum catalyst (chloroplatinic acid isopropyl alcohol solution, platinum content 2000 ppm), an inhibitor (molecular formula (CH) 3 ) 3 SiO-[Si(CH 3 ) 2 O] m -[Si(CH 3 )（CH 2 =CH-）O] n -Si-(CH 3 ) 3 M=10 to 20, n=10 to 50, a viscosity of 20mpa·s) 0.5 part;
and the component B comprises the following components: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 100m 2 15 parts per g of fumed silica), 30 parts of heavy filler (calcium silicate with an average particle size of 4 μm), 20 parts of silane treating agent (hydroxy silicone oil), 10 parts of hydrogen-containing silicone oil (hydrogen content of 0.6 wt%) and a viscosity increase controlling agent (molecular formula is HO-Si (CH) 2 )-O-[Si(CH 3 ) 2 ] n OH, n=1 to 15) 0.2 parts.
Comparative example 1
In order to verify that the viscosity increase control agent introduced in the invention has the effect of prolonging the operation time of the die silicone rubber and simultaneously curing for 6-12 hours, the comparative example provides a double-component addition type room temperature vulcanized silicone rubber without viscosity increase control, the silicone rubber is prepared into a component A and a component B by the following raw materials in parts by mass, and the component A and the component B are mixed according to the mass ratio of 10:1 to prepare the silicone rubber A, and the specific preparation method is as shown in the example 1.
A component: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 200m 2 30 parts of a heavy filler (crystalline silica fine powder with an average particle diameter of 4 μm), 5 parts of a silane treatment agent (hexamethyldisilazane), 5 parts of a diluent (methyl silicone oil with a viscosity of 30 mPa.s), 0.2 part of a platinum catalyst (chelate of chloroplatinic acid and 1, 3-divinyl tetramethyl disiloxane), and 0.2 part of an inhibitor (tetramethyl divinyl disiloxane);
and the component B comprises the following components: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 200m 2 30 parts of per gram of fumed silica), 5 parts of a silane treatment agent (hexamethyldisilazane), 50 parts of hydrogen-containing silicone oil (hydrogen content of 0.6 wt%) and 1 part of an inhibitor (tetramethyl divinyl disiloxane).
Comparative example 2
In order to verify that the heavy filler introduced by the invention has the effect of prolonging the service life of the die silicon rubber, the comparative example provides a double-component addition type room temperature vulcanized silicon rubber without the heavy filler, the silicon rubber is prepared into a component A and a component B by the following raw materials in parts by mass, and the component A and the component B are mixed according to the mass ratio of 10:1 to prepare silicon rubber B;
a component: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 200m 2 Per gram of fumed silica) 30 parts,5 parts of silane treating agent (hexamethyldisilazane), 5 parts of diluent (methyl silicone oil with the viscosity of 30 mpa.s), 0.2 part of platinum catalyst (chelate of chloroplatinic acid and 1, 3-divinyl tetramethyl disiloxane), 0.2 part of inhibitor (tetramethyl divinyl disiloxane), and a viscosity increase control agent (molecular formula is HO (CH) 3 ) 2 Si-O-[Si(CH 3 ) 2 O] m H, m=15 to 30) 0.1 part;
and the component B comprises the following components: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 200m 2 15 parts of per gram of fumed silica), 10 parts of silane treating agent (hexamethyldisilazane), 50 parts of hydrogen-containing silicone oil (hydrogen content of 0.6 wt%) 1 part of inhibitor (tetramethyl divinyl disiloxane), and a viscosity increase control agent (molecular formula is HO (CH) 3 ) 2 Si-O-[Si(CH 3 ) 2 O] m H, m=15 to 30) 0.1 part.
The reinforcing filler and the base polymer are prepared into reinforcing filler base rubber, then the reinforcing filler base rubber is stirred and mixed with other raw materials to prepare a component A and a component B, and finally the component A and the component B are mixed according to the mass ratio of 10:1 to obtain the silicone rubber B.
Comparative example 3
The comparative example provides a double-component addition type room temperature vulcanized silicone rubber without adding heavy filler and viscosity increase control, wherein the silicone rubber is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and then mixing the component A and the component B according to the mass ratio of 10:1 to obtain silicone rubber C;
a component: 100 parts of a base polymer (linear vinyl-terminated polysiloxane having a vinyl content of 0.25%) and a reinforcing filler (specific surface area 200m 2 30 parts of per gram of fumed silica), 5 parts of a silane treatment agent (hexamethyldisilazane), 5 parts of a diluent (methyl silicone oil with the viscosity of 30 mpa.s), 0.2 part of a platinum catalyst (chelate of chloroplatinic acid and 1, 3-divinyl tetramethyl disiloxane) and 0.2 part of an inhibitor (tetramethyl divinyl disiloxane);
and the component B comprises the following components: base Polymer (Linear ethylene with 0.25% vinyl content)100 parts of a base-terminated polysiloxane, a reinforcing filler (specific surface area 200 m) 2 15 parts of per gram of fumed silica), 10 parts of a silane treatment agent (hexamethyldisilazane), 50 parts of hydrogen-containing silicone oil (hydrogen content of 0.6 wt%) and 1 part of an inhibitor (tetramethyl divinyl disiloxane).
The reinforcing filler and the base polymer are prepared into reinforcing filler base rubber, then the reinforcing filler base rubber is stirred and mixed with other raw materials to prepare a component A and a component B, and finally the component A and the component B are mixed according to the mass ratio of 10:1 to obtain the silicone rubber C.
The silicone rubbers prepared in examples 1 to 8 and comparative examples 1 to 3 were cured at room temperature (23 ℃) for 10 hours to obtain silicone rubber elastomers. The elastomers were subjected to related property (pot life, cure time, mechanical properties, hardness, etc.) tests, the test results being shown in table 1:
as can be seen from the performance test data in the table 1, the silicone rubbers I to VIII prepared according to the raw material proportion of the invention have the operation time of 1.5 to 2 hours, the use times (the replication times) of the mold are all over 120 times, the operability and the use times are obviously better than those of the silicone rubbers A to C of the comparative examples 1 to 3 (the operation time is 0.8 hour, the mold use times are 84 times), and meanwhile, the viscosity increase control agent can effectively increase the operation time of the silicone rubber without affecting the demolding time; the introduction of heavy fillers can increase the service life of the mold. In the invention, by using the viscosity thickening control agent and the heavy filler in the existing double-component silicone rubber formula, the silicone rubber of the die has better fluidity in a certain operation time, can obtain ideal mechanical property and service life of the die, can be cured and molded at room temperature, is very suitable for preparing dies of unsaturated polyester, polyurethane and other turnover die materials, and particularly can prepare large-sized dies.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present invention fall within the scope of the present invention.
Claims (8)
1. A two-component addition type room temperature vulcanization mold silicone rubber is characterized in that: the preparation method comprises the steps of preparing a component A and a component B from the following raw materials in parts by mass, and mixing the component A and the component B according to the mass ratio of 10:1-1:1 to prepare the die silicone rubber;
a component: 100 parts of base polymer, 15-30 parts of reinforcing filler, 10-40 parts of heavy filler, 5-20 parts of silane treating agent, 1-50 parts of diluent, 0.1-3 parts of platinum catalyst, 0.02-3 parts of inhibitor and 0.01-1 part of viscosity increase control agent;
and the component B comprises the following components: 100 parts of base polymer, 15-30 parts of reinforcing filler, 0-40 parts of heavy filler, 5-20 parts of silane treating agent, 40-120 parts of hydrogen-containing silicone oil, 0-40 parts of diluent, 0-3 parts of inhibitor, 0-3 parts of color paste and 0.01-1 part of viscosity increase control agent;
the reinforcing filler is fumed silica with a specific surface area of 100-400 g/cm 3 ；
The heavy filler is selected from calcium silicate with the average particle size of 0.5-20 mu m;
the viscosity build-up control agent is selected from the group consisting of compounds of the formula (CH) 3 ) 3 Si-O-[Si(CH 3 ) 2 O] m A monohydroxy-terminated polysiloxane having the formula H, m=0 to 100, or ho—si (CH) 2 ) 2 -O-[Si(CH 3 ) 2 ] n OH, n=1 to 100.
2. The two-component addition type room temperature vulcanizing mold silicone rubber according to claim 1, wherein: the base polymer is selected from linear vinyl terminated polysiloxanes having a vinyl content of 0.25%.
3. The two-component addition type room temperature vulcanizing mold silicone rubber according to claim 1, wherein: the silane treating agent is at least one selected from methyltriethoxysilane, vinyltriethoxysilane, methyltrimethoxysilane, hexamethyldisilazane, hydroxy silicone oil and divinyl tetramethylsilazane.
4. The two-component addition type room temperature vulcanizing mold silicone rubber according to claim 1, wherein: the diluent is methyl silicone oil or vinyl terminated silicone oil or a mixture of the methyl silicone oil and the vinyl terminated silicone oil; the viscosity of the diluent is 30-8000 mPa.s.
5. The two-component addition type room temperature vulcanizing mold silicone rubber according to claim 1, wherein: the inhibitor is at least one selected from 2-methyl-3-butynyl-2 alcohol, 3-methyl-1-hexynyl-3-alcohol, tetramethyl divinyl disiloxane, tetramethyl vinyl cyclotetrasiloxane, vinyl methyl mixed ring and polyvinyl linear polysiloxane; the formula of the polyvinyl linear polysiloxane is R (CH) 3 ) 2 SiO-[Si(CH 3 ) 2 O] m -[Si(CH 3 )（CH 2 =CH-）O] n -Si-R (CH 3 ) 2 Wherein R is-CH 3 Or-ch=ch 2 ，m=0～50，n=10～50。
6. The two-component addition type room temperature vulcanizing mold silicone rubber according to claim 1, wherein: the platinum catalyst is at least one selected from alcohol modified chloroplatinic acid, chloroplatinic acid hexahydrate and chelate of three compounds, and the platinum content of the platinum catalyst is 500-15000 ppm.
7. The two-component addition type room temperature vulcanizing mold silicone rubber according to claim 1, wherein: the hydrogen content of the hydrogen-containing silicone oil is 0.2-0.9 wt%.
8. A method for preparing the two-component addition type room temperature vulcanizing mold silicone rubber according to any one of claims 1 to 7, characterized by comprising the following steps:
(1) Preparation of reinforcing filler base adhesive
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, adding a reinforcing filler in batches after uniformly mixing, slowly heating to 60-120 ℃ after uniformly mixing, heating to 120-160 ℃ after kneading for 1-2 hours, vacuumizing to the vacuum degree of minus 0.06-minus 0.09MPa, continuously kneading for 2-4 hours, and cooling to obtain the reinforcing filler base adhesive;
(2) Preparation of heavy filler base gum
Adding a base polymer and a silane treating agent into a kneader according to the formula amount, adding a heavy filler after uniformly mixing, kneading for 1-2 hours, heating to 80-150 ℃, vacuumizing to the vacuum degree of-0.06-0.009 MPa, continuously kneading for 2-4 hours, and cooling to obtain the heavy filler base rubber;
(3) Preparation of component A
Weighing reinforcing filler base glue, heavy filler base glue, a diluent, an inhibitor, a platinum catalyst and a viscosity increase control agent according to a formula, and stirring in a planetary stirrer for 20-30 minutes at normal temperature to obtain a component A;
(4) Preparation of component B
Weighing reinforcing filler base glue, heavy filler base glue, diluent, inhibitor, hydrogen-containing silicone oil, viscosity increase control agent and color paste according to the formula, and stirring in a planetary stirrer for 20-30 minutes at normal temperature to obtain a component B;
(5) Mixing of the Components
Mixing the component A and the component B according to the mass ratio of 10:1-1:1, and vacuumizing and defoaming to obtain the die silicone rubber.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005307081A (en) * | 2004-04-23 | 2005-11-04 | Dow Corning Toray Co Ltd | Silicone rubber composition for use in forming mold |
| CN103467993A (en) * | 2013-08-30 | 2013-12-25 | 东莞兆舜有机硅新材料科技有限公司 | Condensed type die silicone rubber and preparation method thereof |
| CN104130581A (en) * | 2014-06-29 | 2014-11-05 | 惠州市永卓科技有限公司 | Addition type culture stone mold glue and preparation method thereof |
| CN111995871A (en) * | 2019-05-27 | 2020-11-27 | 信越化学工业株式会社 | Silicone rubber composition for mold production and silicone rubber mold |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005307081A (en) * | 2004-04-23 | 2005-11-04 | Dow Corning Toray Co Ltd | Silicone rubber composition for use in forming mold |
| CN103467993A (en) * | 2013-08-30 | 2013-12-25 | 东莞兆舜有机硅新材料科技有限公司 | Condensed type die silicone rubber and preparation method thereof |
| CN104130581A (en) * | 2014-06-29 | 2014-11-05 | 惠州市永卓科技有限公司 | Addition type culture stone mold glue and preparation method thereof |
| CN111995871A (en) * | 2019-05-27 | 2020-11-27 | 信越化学工业株式会社 | Silicone rubber composition for mold production and silicone rubber mold |
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| "填料对精密铸造模具硅橡胶使用寿命的影响";张叶琴等;《有机硅材料》;第31卷;第91-95页 * |
| 黄文润编.《热硫化硅橡胶》.四川科学技术出版社,2009,(第1版),第76页. * |
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