CN113248927A - Condensed type mold silicon rubber and preparation method thereof - Google Patents
Condensed type mold silicon rubber and preparation method thereof Download PDFInfo
- Publication number
- CN113248927A CN113248927A CN202110645354.1A CN202110645354A CN113248927A CN 113248927 A CN113248927 A CN 113248927A CN 202110645354 A CN202110645354 A CN 202110645354A CN 113248927 A CN113248927 A CN 113248927A
- Authority
- CN
- China
- Prior art keywords
- parts
- component
- carbon black
- white carbon
- silicone rubber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000006229 carbon black Substances 0.000 claims abstract description 45
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 36
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004945 silicone rubber Substances 0.000 claims abstract description 27
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000000741 silica gel Substances 0.000 claims abstract description 16
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 16
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000839 emulsion Substances 0.000 claims abstract description 14
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000010453 quartz Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920001971 elastomer Polymers 0.000 claims abstract description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 21
- 238000010992 reflux Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 20
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 20
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical group C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000004898 kneading Methods 0.000 claims description 16
- -1 diethoxymethyl Chemical group 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 229910000077 silane Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 238000004513 sizing Methods 0.000 claims description 2
- 230000007306 turnover Effects 0.000 abstract description 7
- 229920005989 resin Polymers 0.000 description 11
- 239000011347 resin Substances 0.000 description 11
- 239000003292 glue Substances 0.000 description 10
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 7
- 239000012975 dibutyltin dilaurate Substances 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- DCERHCFNWRGHLK-UHFFFAOYSA-N C[Si](C)C Chemical compound C[Si](C)C DCERHCFNWRGHLK-UHFFFAOYSA-N 0.000 description 6
- GSPGDJGLXPJZSV-UHFFFAOYSA-N diethoxymethylsilicon Chemical compound CCOC([Si])OCC GSPGDJGLXPJZSV-UHFFFAOYSA-N 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- 240000005020 Acaciella glauca Species 0.000 description 1
- 241000208966 Polygala Species 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004049 embossing Methods 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000005495 investment casting Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920003217 poly(methylsilsesquioxane) Polymers 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000003499 redwood Nutrition 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
Landscapes
- 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 condensed type die silicon rubber which comprises a component A and a component B, wherein the component A comprises 25-35 parts of basic silica gel, 25-40 parts of methyl silicone oil, 20-30 parts of modified white carbon black, 2-10 parts of quartz powder, 1-10 parts of calcium carbonate, 0.1-1 part of titanium dioxide, 1.5-3 parts of a burning resistant agent and 1-5 parts of methyl silicone oil water-based emulsion; the component B comprises 40-80 parts of ethyl orthosilicate, 0-20 parts of alcohol and 15-25 parts of organic tin. The invention also discloses a preparation method of the condensed type die silicone rubber. The condensed type mold silicon rubber provided by the invention has the advantages of good tensile property, moderate hardness and good tear resistance, and the mold rubber turnover frequency can be greatly improved.
Description
Technical Field
The invention relates to a silicon rubber product, in particular to a condensed type die silicon rubber and a preparation method thereof.
Background
The silicon rubber is organosilicon room temperature double-component mold rubber, called RTV for short, is a double-component compound, can be solidified at room temperature, has good fluidity, has no deformation, only has tiny linear shrinkage, and can form flexible and elastic colloid, so that the silicon rubber is suitable for the molding materials in industries such as glass resin (POLYSTER), EPOXY resin (EPOXY), PU foaming resin, gypsum, cement, candle, electronics and the like, toy factories, electronic factories, lamp factories, silk-screen factories, candle factories, production of decorative artware and duplicated products, manufacturing molds, building decoration materials, artware, imitation redwood furniture, precision casting, high-frequency embossing, cultural relic duplication, gypsum board manufacturing and the like.
The silicon rubber for the die belongs to condensed silicon rubber, has good performance, low cost, strong tearing resistance and tensile resistance, no oil, small shrinkage, no deformation and die turning. In practical application, the number of times of mold turning of the existing condensed type silicone rubber is generally less than hundred, the production requirements of downstream manufacturers cannot be met, and the problems of high cost, easiness in expansion of a silicone rubber mold and the like exist. The condensed silicone rubber with the mold turnover frequency of more than 200 times is high in price, and causes cost burden to downstream manufacturers.
Disclosure of Invention
In view of the above problems, it is an object of the present invention to provide a condensation type mold silicone rubber.
Specifically, the condensed type die silicone rubber comprises a component A and a component B, wherein the component A comprises the following components in parts by mass:
25-35 parts of basic silica gel
25-40 parts of methyl silicone oil
20-30 parts of modified white carbon black
2-10 parts of quartz powder
1-10 parts of calcium carbonate
0.1-1 part of titanium dioxide
1.5-3 parts of burning resistant agent and 1-5 parts of methyl silicone oil water-based emulsion;
the component B comprises:
40-80 parts of ethyl orthosilicate and 0-20 parts of alcohol
15-25 parts of organic tin.
In the invention, the mass ratio of the component A to the component B is 100: 2. Preferably, the a component comprises:
25-35 parts of basic silica gel
25-40 parts of methyl silicone oil
20-30 parts of modified white carbon black
2-10 parts of quartz powder
1-10 parts of calcium carbonate
0.1-1 part of titanium dioxide
2-2.5 parts of burning resistant agent
1-5 parts of methyl silicone oil water-based emulsion;
the component B comprises:
40-80 parts of ethyl orthosilicate
0-20 parts of alcohol
15-25 parts of organic tin.
The base silicone gum may be 107 room temperature vulcanized silicone rubber (107 gum).
The white carbon black is modified by silazane. Silazane has high activity, is easy to react with hydroxyl on the surface of white carbon black, but the cost of singly using silazane is higher. In order to reduce the using amount of silazane, the invention adopts the following method to modify the silazane-modified white carbon black: white carbon black, silazane and silane, wherein the weight ratio of the white carbon black to the silazane is 100:10: 5-100: 10: 15. Modification conditions are as follows: at normal temperature and normal pressure, in a reaction kettle equipped with a condensing reflux device, stirring at medium speed, and adding the treating agent in a spraying form. And a condensation reflux device is arranged, so that volatilization of hexamethyldisiloxane and silazane is reduced, and the utilization rate of the treating agent is improved.
In the invention, the burning resistant agent is bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide or [ gamma- (diethoxymethyl) propyl-gamma- (trimethyl silicon) propyl ] tetrasulfide. The two burning-resistant agents are both obtained by modifying bis- (gamma-triethoxysilylpropyl) tetrasulfide, namely a silane coupling agent Si-69, and can effectively avoid the surface reaction of a mold and a product (such as Poli resin and the like), so that the mold turnover frequency of the silicon rubber of the mold can reach more than 200 times, and the obtained resin product has smooth surface and uniform size due to the inhibiting effect of the burning-resistant agent.
The structural formula of bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide is as follows:
the structural formula of [ gamma- (diethoxymethyl) propyl-gamma- (trimethylsilyl) propyl ] tetrasulfide is as follows:
the invention also aims to provide a preparation method of the condensed type die silicone rubber, which comprises the following steps:
(1) modification of white carbon black: adding white carbon black into a reaction kettle provided with a condensation reflux device at normal temperature and normal pressure, and adding silazane and silane in a spraying mode under the stirring condition, wherein the white carbon black is silazane and the silane is 100:10: 5-100: 10: 15;
(2) preparing a condensed type die silicone rubber base sizing material: adding the basic silica gel, part of the methyl silicone oil, the modified white carbon black, the quartz powder and the calcium carbonate into a kneader, kneading for 1.5-2 hours at normal temperature, heating to 145-155 ℃, continuing kneading for 1.5-2 hours, then heating to 175-185 ℃, decompressing for 2.5-4 hours, cooling, and grinding by a three-roll machine to obtain a mixture.
(3) Preparing a component A: and adding the mixture, the rest of the methyl silicone oil, the titanium dioxide, the methyl silicone oil water-based emulsion and the burning-resistant auxiliary agent into a dispersion machine, and dispersing to obtain the component A.
(4) Preparing a component B: putting ethyl orthosilicate, alcohol and organic tin into a reactor, heating to 45-55 ℃, and reacting under the stirring condition to obtain a component B.
(5) And mixing the component A and the component B, uniformly stirring, and vulcanizing to obtain the rubber composition.
The invention has the following beneficial effects:
1. the condensed type mold silicon rubber provided by the invention has the advantages of good tensile property, moderate hardness and good tear resistance, and the mold rubber turnover frequency can be greatly improved.
2. The condensed type die silicon rubber provided by the invention can avoid the phenomenon of no die-firing, and the resin product has smooth surface and uniform size.
The unsaturated resin contains styrene, and the styrene is easy to permeate into the surface of the silica gel mold in the pouring process to cause the mold burning phenomenon. The condensed type mold silicon rubber provided by the invention is added with the burning resistant agent, so that the surface reaction of the mold and unsaturated resin (such as Polygala resin and the like) is effectively avoided, the mold turnover frequency of the mold rubber is ensured to be up to 200 and 400 times, and the prepared resin product has smooth surface and uniform size due to the suppression effect of the burning resistant agent.
3. The invention adopts bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide or [ gamma- (diethoxymethyl) propyl-gamma- (trimethyl silicon) propyl ] tetrasulfide as a burning resistant agent, because the ethoxy part is shielded, the storage period of colloid is prolonged, and after a curing agent is added, the cross-linking agent ethyl orthosilicate can better perform condensation reaction with hydroxyl on the base silica gel.
3. Low cost
The reinforcing material white carbon black used in the invention is modified by silazane, and the modification method provided by the invention is adopted, so that the usage amount of silazane treating agent is greatly reduced, and the cost of silicon rubber of the die is reduced to a certain extent.
Detailed Description
The present invention is described in further detail below with reference to examples, which are intended to facilitate the understanding of the present invention and are not intended to limit the present invention in any way. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
Example 1
Condensed type die silicon rubber:
the component A comprises: adding 30 parts of 107 glue, 34 parts of 350CS methyl silicone oil, 27 parts of modified white carbon black, 3 parts of quartz powder and 1 part of calcium carbonate into a kneader, kneading for 2 hours at normal temperature, heating to 150 ℃, continuing kneading for 2 hours, then heating to 180 ℃, decompressing for 3 hours, cooling, and grinding by a three-roll machine to obtain a mixture. Adding the mixture, 5 parts of 350CS methyl silicone oil, 0.5 part of titanium dioxide, 3 parts of methyl silicone oil water-based emulsion and 1.5 parts of bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide into a dispersion machine, and then dispersing for 1 hour to obtain the component A.
Modified white carbon black: adding white carbon black into a reaction kettle provided with a reflux device at normal temperature and normal pressure, stirring at medium speed, and adding hexamethyldisiloxane and silazane in a spraying mode. Wherein, the white carbon black is 100 parts, the hexamethyldisiloxane is 10 parts, and the silazane is 10 parts. The reaction kettle provided with the reflux device is characterized in that a condensing reflux device is arranged on an air outlet of the reaction kettle and is used for condensing the vaporized hexamethyldisiloxane and silazane to enable the hexamethyldisiloxane and silazane to flow back into the reaction kettle to participate in the reaction, so that the volatilization of the hexamethyldisiloxane and silazane is reduced, and the utilization rate of the treating agent is improved
And B component: 42 parts of ethyl orthosilicate, 6 parts of alcohol and 15 parts of dibutyltin dilaurate were added to a 1L glass bottle, stirred at room temperature for 30 minutes, and then heated to 70 ℃ for reflux for 1 hour to obtain a component B.
A burning resistant agent: the structural formula of bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide is as follows:
the reaction principle is as follows:
the preparation method of the bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide comprises the following steps: heating Si-69539 g and 108 g of sodium methoxide to 60 ℃ under the catalysis of sodium methoxide, carrying out reflux reaction for 4 hours, then carrying out decompression at 100 ℃ for 30 minutes, and filtering to obtain the product.
The preparation method of the condensed type die silicone rubber comprises the following steps: and adding 100 parts of the component A and 2 parts of the component B, uniformly stirring, then placing the mixture into a vacuum box for defoaming for 2 minutes, pouring the mould rubber with bubbles removed into a mould for curing, and standing at room temperature for 24 hours to obtain the mould silicon rubber with good strength.
Comparative example 1
The difference from example 1 is:
1.0 part of bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide.
Example 2
The difference from example 1 is:
the component A comprises: adding 32 parts of 107 glue, 32 parts of 350CS methyl silicone oil, 27 parts of modified white carbon black, 3 parts of quartz powder and 2 parts of calcium carbonate into a kneader, kneading for 2 hours at normal temperature, heating to 150 ℃, continuing kneading for 2 hours, then heating to 180 ℃, decompressing for 3 hours, cooling, and grinding by a three-roll machine to obtain a mixture. Adding the mixture, 8 parts of 350CS methyl silicone oil, 0.5 part of titanium dioxide, 3 parts of methyl silicone oil aqueous emulsion and 1.5 parts of bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide into a dispersion machine, and then rapidly dispersing for 1 hour to obtain the component A.
Modified white carbon black: adding white carbon black into a reaction kettle provided with a reflux device at normal temperature and normal pressure, stirring at medium speed, and adding hexamethyldisiloxane and silazane in a spraying mode. Wherein, the white carbon black is 100 parts, the hexamethyldisiloxane is 10 parts, and the silazane is 10 parts.
And B component: 42 parts of ethyl orthosilicate, 6 parts of alcohol and 12 parts of dibutyltin dilaurate were added to a 1L glass bottle, stirred at room temperature for 30 minutes, and then heated to 70 ℃ for reflux for 1 hour to obtain a component B.
Example 3
The difference from example 1 is:
the component A comprises: adding 32 parts of 107 glue, 32 parts of 350CS methyl silicone oil, 27 parts of modified white carbon black, 4 parts of quartz powder and 1 part of calcium carbonate into a kneader, kneading for 2 hours at normal temperature, heating to 150 ℃, continuing kneading for 2 hours, then heating to 180 ℃, decompressing for 3 hours, cooling, and grinding by a three-roll machine to obtain a mixture. Adding the mixture, 8 parts of methyl silicone oil, 0.5 part of titanium dioxide, 3 parts of methyl silicone oil aqueous emulsion and 2.5 parts of bis- [ gamma- (diethoxymethyl) propyl ] tetrasulfide into a dispersion machine, and then rapidly dispersing for 1 hour to obtain the component A.
Modified white carbon black: adding white carbon black into a reaction kettle provided with a reflux device at normal temperature and normal pressure, stirring at medium speed, and adding hexamethyldisiloxane and silazane in a spraying mode. Wherein, the white carbon black is 100 parts, the hexamethyldisiloxane is 10 parts, and the silazane is 10 parts.
And B component: 42 parts of ethyl orthosilicate, 6 parts of alcohol and 12 parts of dibutyltin dilaurate were added to a 1L glass bottle, stirred at room temperature for 30 minutes, and then heated to 70 ℃ for reflux for 1 hour to obtain a component B.
Example 4
Condensed type die silicon rubber:
the component A comprises: adding 30 parts of 107 glue, 32 parts of 350CS methyl silicone oil, 29 parts of modified white carbon black, 4 parts of quartz powder and 1 part of calcium carbonate into a kneader, kneading for 2 hours at normal temperature, heating to 150 ℃, continuing kneading for 2 hours, then heating to 180 ℃, decompressing for 3 hours, cooling, and grinding by a three-roll machine to obtain a mixture. Adding the mixture, 5 parts of 350CS methyl silicone oil, 0.5 part of titanium dioxide, 3 parts of methyl silicone oil water-based emulsion and 1.5 parts of [ gamma- (diethoxymethyl silicon) propyl-gamma- (trimethyl silicon) propyl ] tetrasulfide into a dispersion machine, and then rapidly dispersing for 1 hour to obtain a component A.
Modified white carbon black: adding white carbon black into a reaction kettle provided with a reflux device at normal temperature and normal pressure, stirring at medium speed, and adding hexamethyldisiloxane and silazane in a spraying mode. Wherein, the white carbon black is 100 parts, the hexamethyldisiloxane is 10 parts, and the silazane is 10 parts.
And B component: 42 parts of ethyl orthosilicate, 6 parts of alcohol and 12 parts of dibutyltin dilaurate were added to a 1L glass bottle, stirred at room temperature for 30 minutes, and then heated to 70 ℃ for reflux for 1 hour to obtain a component B.
A burning resistant agent: [ gamma- (diethoxymethyl) propyl-gamma- (trimethylsilyl) propyl ] tetrasulfide, having the following structural formula:
the preparation method of [ gamma- (diethoxymethyl silicon) propyl-gamma- (trimethyl silicon) propyl ] tetrasulfide comprises the following steps: : adding Si-69500 g and 400 g of sodium methoxide into a three-neck flask, heating to 60 ℃ under the catalysis of the sodium methoxide, carrying out reflux reaction for 5 hours, then carrying out decompression at 100 ℃ for 30 minutes, and filtering to obtain a reaction product.
The preparation method of the condensed type die silicone rubber comprises the following steps: and adding 100 parts by mass of the component A into 2 parts by mass of the component B, uniformly stirring, then placing the mixture into a vacuum box for defoaming for 2 minutes, pouring the mould rubber with bubbles removed into a mould for curing, and standing at room temperature for 24 hours to obtain the mould silicon rubber with good strength.
Comparative example 2
The difference from example 4 is: 1 part of [ gamma- (diethoxymethylsilicon) propyl-gamma- (trimethylsilyl) propyl ] tetrasulfide.
Example 5
The difference from example 4 is:
the component A comprises: adding 30 parts of 107 glue, 32 parts of 350CS methyl silicone oil, 29 parts of modified white carbon black, 4 parts of quartz powder and 1 part of calcium carbonate into a kneader, kneading for 2 hours at normal temperature, heating to 150 ℃, continuing kneading for 2 hours, then heating to 180 ℃, decompressing for 3 hours, cooling, and grinding by a three-roll machine to obtain a mixture. Adding the mixture, 8 parts of 350CS methyl silicone oil, 0.5 part of titanium dioxide, 3 parts of methyl silicone oil water-based emulsion and 2 parts of [ gamma- (diethoxymethyl silicon) propyl-gamma- (trimethyl silicon) propyl ] tetrasulfide into a dispersion machine, and then rapidly dispersing for 1 hour to obtain a component A.
Modified white carbon black: adding white carbon black into a reaction kettle provided with a reflux device at normal temperature and normal pressure, stirring at medium speed, and adding hexamethyldisiloxane and silazane in a spraying mode. Wherein, the white carbon black is 100 parts, the hexamethyldisiloxane is 10 parts, and the silazane is 10 parts.
And B component: 42 parts of ethyl orthosilicate, 6 parts of alcohol and 12 parts of dibutyltin dilaurate were added to a 1L glass bottle, stirred at room temperature for 30 minutes, and then heated to 70 ℃ for reflux for 1 hour to obtain a component B.
Example 6
The difference from example 4 is:
the component A comprises: adding 30 parts of 107 glue, 32 parts of 350CS methyl silicone oil, 29 parts of modified white carbon black, 4 parts of quartz powder and 1 part of calcium carbonate into a kneader, kneading for 2 hours at normal temperature, heating to 150 ℃, continuing kneading for 2 hours, then heating to 180 ℃, decompressing for 3 hours, cooling, and grinding by a three-roll machine to obtain a mixture. Adding the mixture, 8 parts of 350CS methyl silicone oil, 0.5 part of titanium dioxide, 3 parts of methyl silicone oil water-based emulsion and 2.5 parts of [ gamma- (diethoxymethyl silicon) propyl-gamma- (trimethyl silicon) propyl ] tetrasulfide into a dispersion machine, and then rapidly dispersing for 1 hour to obtain a component A.
Modified white carbon black: adding white carbon black into a reaction kettle provided with a reflux device at normal temperature and normal pressure, stirring at medium speed, and adding hexamethyldisiloxane and silazane in a spraying mode. Wherein, the white carbon black is 100 parts, the hexamethyldisiloxane is 10 parts, and the silazane is 10 parts.
And B component: 4 parts of ethyl orthosilicate, 6 parts of alcohol and 12 parts of dibutyltin dilaurate are added into a 1L glass bottle, stirred for 30 minutes at room temperature and then heated to 70 ℃ for reflux for 1 hour to obtain a component B.
Comparative example 3
The difference from example 4 is:
the component A comprises: adding the mixture, 5 parts of 350CS methyl silicone oil, 0.5 part of titanium dioxide, 3 parts of methyl silicone oil water-based emulsion and Si-691.5 parts into a dispersion machine, and then rapidly dispersing for 1 hour to obtain the component A.
And B component: 42 parts of ethyl orthosilicate, 6 parts of alcohol and 12 parts of dibutyltin dilaurate were added to a 1L glass bottle, stirred at room temperature for 30 minutes, and then heated to 70 ℃ for reflux for 1 hour to obtain a component B.
The product performance test methods in table 1 are as follows:
1. the tensile strength and elongation at break of the silicone rubber were determined in accordance with GB/T528-2009.
2. The tear strength of the silicone rubber was determined according to GB/T528-.
3. The hardness of the silicone rubber was measured according to GB/T531.1-2008.
4. The viscosity of the silicone rubber was determined according to GB/T2794-.
TABLE 1
As shown in the results of Table 1, the mold glue can be well protected from being corroded by unsaturated resin by adding the burning-resistant auxiliary agent, although the burning-resistant effect can be achieved by conventional Si69, Si69 thickens the glue, the storage period of the mold glue is influenced, the mixing viscosity is high, the foam discharging performance of the mold glue is also influenced, the strength of silicone rubber is influenced by more bubbles, the process surface of the turnover mold is subjected to 'needling', and the service life of a silicone mold is influenced. The two burning-resistant auxiliary agents used in the invention have little application difference, can reduce the viscosity of the silica gel, and when the addition amount is 2% of the base material, the burning-resistant effect is the best, and can reach 280 times.
When the burning-resistant additive reaches 2.5%, the number of times of mold turnover is not increased or decreased, and the burning-resistant additive is increased, so that firstly, the surface curing of unsaturated resin is inhibited, and the contact surface of the unsaturated resin and a silica gel mold is not dry and comfortable after curing, thereby affecting the quality of the handicraft article; and secondly, the excessive burning-resistant agent plays a role of a diluent, and after the silica gel mold is used for a period of time, the burning-resistant agent migrates to the surface of the silica gel to influence the structure of the silica gel, so that the strength of the silica gel is slowly reduced, and even the silica gel loses strength due to brittleness. Therefore, the amount of the burning preventive is preferably 2 to 2.5%.
Claims (8)
1. The condensed type die silicone rubber comprises a component A and a component B, and is characterized in that the component A comprises the following components in parts by mass:
25-35 parts of basic silica gel
25-40 parts of methyl silicone oil
20-30 parts of modified white carbon black
2-10 parts of quartz powder
1-10 parts of calcium carbonate
0.1-1 part of titanium dioxide
1.5-3 parts of burning resistant agent
1-5 parts of methyl silicone oil water-based emulsion;
the component B comprises:
40-80 parts of ethyl orthosilicate
0-20 parts of alcohol
15-25 parts of organic tin.
2. The condensation type mold silicone rubber according to claim 1, wherein said a component comprises, in parts by mass:
25-35 parts of basic silica gel
25-40 parts of methyl silicone oil
20-30 parts of modified white carbon black
2-10 parts of quartz powder
1-10 parts of calcium carbonate
0.1-1 part of titanium dioxide
2-2.5 parts of burning resistant agent
1-5 parts of methyl silicone oil water-based emulsion.
3. The condensation type mold silicone rubber according to claim 1 or 2, wherein the base silicone rubber is 107 room temperature vulcanizing silicone rubber.
4. The condensed-type mold silicone rubber according to claim 1, wherein said white carbon black is modified with silazane and silane.
5. The condensed type mold silicone rubber as claimed in claim 4, wherein the mass ratio of white carbon black to silazane to silane is 100:10:5 to 100:10: 15.
6. The condensation type mold silicone rubber according to claim 4 or 5, wherein the silane is hexamethyldisiloxane.
7. The condensation type silicone rubber for mold according to claim 1, wherein the burning-resistant agent is bis- [ γ - (diethoxymethyl) propyl ] tetrasulfide or [ γ - (diethoxymethyl) propyl- γ - (trimethylsilyl) propyl ] tetrasulfide.
8. The method for preparing the condensation type mold silicone rubber according to any one of claims 1 to 7, comprising the steps of:
(1) modification of white carbon black: adding white carbon black into a reaction kettle provided with a condensation reflux device at normal temperature and normal pressure, and adding silazane and silane in a spraying mode under the stirring condition, wherein the white carbon black is silazane and the silane is 100:10: 5-100: 10: 15;
(2) preparing a condensed type die silicone rubber base sizing material: adding the basic silica gel, part of the methyl silicone oil, the modified white carbon black, the quartz powder and the calcium carbonate into a kneader, kneading for 1.5-2 hours at normal temperature, heating to 145-155 ℃, continuing kneading for 1.5-2 hours, then heating to 175-185 ℃, decompressing for 2.5-4 hours, cooling, and grinding by a three-roll machine to obtain a mixture;
(3) preparing a component A: adding the mixture, the rest of the methyl silicone oil, the titanium dioxide, the methyl silicone oil water-based emulsion and the burning-resistant auxiliary agent into a dispersion machine, and dispersing to obtain a component A;
(4) preparing a component B: putting ethyl orthosilicate, alcohol and organic tin into a reactor, heating to 45-55 ℃, and reacting under the stirring condition to obtain a component B;
(5) and mixing the component A and the component B, uniformly stirring, and vulcanizing to obtain the rubber composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110645354.1A CN113248927A (en) | 2021-06-10 | 2021-06-10 | Condensed type mold silicon rubber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110645354.1A CN113248927A (en) | 2021-06-10 | 2021-06-10 | Condensed type mold silicon rubber and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113248927A true CN113248927A (en) | 2021-08-13 |
Family
ID=77187280
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110645354.1A Pending CN113248927A (en) | 2021-06-10 | 2021-06-10 | Condensed type mold silicon rubber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113248927A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020040086A1 (en) * | 2000-07-28 | 2002-04-04 | Noriko Yagi | Rubber composition for tyre treads and pneumatic tyre having tread thereof |
| 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 |
| CN104059473A (en) * | 2013-05-03 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Coating composition, preparation method and application thereof, and hot-dipped metal material |
| CN104406880A (en) * | 2014-11-17 | 2015-03-11 | 东莞兆舜有机硅新材料科技有限公司 | Method for testing burning resisting effect of burning resisting agent of room temperature vulcanization mold rubber |
-
2021
- 2021-06-10 CN CN202110645354.1A patent/CN113248927A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020040086A1 (en) * | 2000-07-28 | 2002-04-04 | Noriko Yagi | Rubber composition for tyre treads and pneumatic tyre having tread thereof |
| CN104059473A (en) * | 2013-05-03 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Coating composition, preparation method and application thereof, and hot-dipped metal material |
| 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 |
| CN104406880A (en) * | 2014-11-17 | 2015-03-11 | 东莞兆舜有机硅新材料科技有限公司 | Method for testing burning resisting effect of burning resisting agent of room temperature vulcanization mold rubber |
Non-Patent Citations (1)
| Title |
|---|
| 孙幼红: "硅橡胶模具胶生产工艺及加工设备的选择", 《有机硅材料》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8907001B2 (en) | Use of a pretreated precipitated silica as a reinforcing filler for silicon elastomer and the curable silicone elastomer compositions thus obtained by cold mixing | |
| CN113999531A (en) | Mold glue and preparation method thereof | |
| US3451833A (en) | Organosilicon binders | |
| CN113248927A (en) | Condensed type mold silicon rubber and preparation method thereof | |
| CN110128657A (en) | The synthesis of the more vinyl polysiloxanes of isotactic structure and the method for preparing High tear resistance silicon rubber | |
| US3112538A (en) | Processes for binding particulate solid materials | |
| US8044121B2 (en) | Cement mold-making silicone rubber composition | |
| CN103834179A (en) | Artificial cultured stone mould rubber and preparation method thereof | |
| CN109825187A (en) | A kind of insulating moulding coating and preparation method | |
| JPH02175759A (en) | Production of fluorosilione-treated silica | |
| CN1126738A (en) | Superfine hydrophobic silica powder and hydrophobic wollastonite powder and their prodn process | |
| CN115246990B (en) | Double-component addition type room temperature vulcanization mold silicon rubber and preparation method thereof | |
| EP0556955B1 (en) | Alkaline resol phenol-aldehyde resin binder compositions | |
| CN111454528A (en) | Preparation method of 3D printed acrylic reinforced bathtub material | |
| KR102645800B1 (en) | Flame retardant light stone having multi-color pattern, Manufacturing method of the same and interior and exterior materials for construction | |
| CN111807746A (en) | Curing agent for composite material | |
| CN115926524B (en) | Multifunctional auxiliary agent, glove finishing agent and protective glove | |
| CN113214649A (en) | Simulated bark mold silica gel and preparation method thereof | |
| CN108249821B (en) | Composition for improving artificial stone patterns and glossiness and application thereof | |
| CN107793920B (en) | Glass, ceramic container and preparation method thereof | |
| CN101143933A (en) | Solid epoxy plastic plate and producing method thereof | |
| CN117401932A (en) | Silane coupling agent mixture, preparation method thereof and artificial marble | |
| CN113512198A (en) | Method for preparing high-hardness single-component oxime type room temperature vulcanized silicone rubber by using hydrolysis material | |
| JP2001192541A (en) | Thixotropy imparting agent and unsaturated polyester resin | |
| JPS60124436A (en) | Production of molding sand composition for cold box |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210813 |
|
| RJ01 | Rejection of invention patent application after publication |