CN107312496B - Adhesive addition type liquid silicone rubber - Google Patents
Adhesive addition type liquid silicone rubber Download PDFInfo
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- CN107312496B CN107312496B CN201710340967.8A CN201710340967A CN107312496B CN 107312496 B CN107312496 B CN 107312496B CN 201710340967 A CN201710340967 A CN 201710340967A CN 107312496 B CN107312496 B CN 107312496B
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- silicone rubber
- addition type
- type liquid
- liquid silicone
- polysiloxane
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 31
- 239000000853 adhesive Substances 0.000 title claims abstract description 23
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 23
- 239000004944 Liquid Silicone Rubber Substances 0.000 title claims abstract description 18
- -1 polysiloxane Polymers 0.000 claims abstract description 55
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 43
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052796 boron Inorganic materials 0.000 claims abstract description 19
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 44
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 36
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 26
- 229920002554 vinyl polymer Polymers 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 13
- 229910052697 platinum Inorganic materials 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910021485 fumed silica Inorganic materials 0.000 claims description 8
- 230000002209 hydrophobic effect Effects 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- GBYPTTGTFMAEJL-UHFFFAOYSA-N B.Fc1cc(F)c(F)c(F)c1F.Fc1cc(F)c(F)c(F)c1F.Fc1cc(F)c(F)c(F)c1F Chemical compound B.Fc1cc(F)c(F)c(F)c1F.Fc1cc(F)c(F)c(F)c1F.Fc1cc(F)c(F)c(F)c1F GBYPTTGTFMAEJL-UHFFFAOYSA-N 0.000 claims description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910007161 Si(CH3)3 Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 6
- 239000010935 stainless steel Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 239000004945 silicone rubber Substances 0.000 description 10
- 229920002545 silicone oil Polymers 0.000 description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound 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 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- YLJJAVFOBDSYAN-UHFFFAOYSA-N dichloro-ethenyl-methylsilane Chemical compound C[Si](Cl)(Cl)C=C YLJJAVFOBDSYAN-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000012676 equilibrium polymerization Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052990 silicon hydride Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/56—Boron-containing linkages
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the field of chemistry and chemical engineering, and aims to solve the problem of a boron-containing polysiloxane tackifier. The adhesive addition type liquid silicone rubber is efficient and mild, and has good adhesion to base materials such as aluminum, stainless steel and the like.
Description
Technical Field
The invention relates to the field of chemistry and chemical engineering, in particular to adhesive addition type liquid silicone rubber.
Background
The addition type silicone rubber is an elastomer with a three-dimensional net structure formed by hydrosilylation reaction of vinyl-containing polysiloxane and hydrogen-containing polysiloxane under the action of a platinum catalyst. Compared with condensed silicone rubber, the addition type silicone rubber has many excellent properties, such as deep curing, small linear shrinkage, no corrosivity and the like, and is widely applied to industries such as electronics, machinery, industry and the like.
However, addition type silicone rubbers are highly saturated nonpolar rubbers, have low molecular surface energy and low adhesion to other substrates, and are usually undercoated or added with an adhesion promoter. With the continuous improvement of the requirement on the bonding performance, the development of corresponding bonding addition type silicone rubber varieties is a hot spot in the field.
Boron-containing polysiloxane tackifiers are one of the most commonly used tackifiers for adhesive addition silicone rubbers. The synthesis method mainly uses boric acid, chlorosilane, alkoxy silane, hydroxyl polysiloxane and the like to prepare the polyborosiloxane through a hydrolysis or non-hydrolysis method. This process either generates environmentally harmful substances such as hydrogen chloride or requires more severe conditions, such as higher temperatures and longer times. Therefore, an efficient preparation method of the boron-containing polysiloxane tackifier is sought, and the method has important significance for the research of the adhesive silicone rubber.
Disclosure of Invention
The invention provides an adhesive addition type liquid silicone rubber for solving the problems of boron-containing polysiloxane tackifier, and the adhesive addition type liquid silicone rubber is efficient and mild and has good adhesion to base materials such as aluminum, stainless steel and the like.
The invention is realized by the following technical scheme: the adhesive addition type liquid silicone rubber is prepared by mixing polysiloxane containing terminal vinyl and side vinyl, trimethylsiloxy terminated methyl hydrogen polysiloxane, boron-containing polysiloxane, hydrophobic fumed silica and platinum catalyst.
The structural formula of the polysiloxane containing terminal vinyl and side vinyl is as follows: (CH)2＝CH)(CH3)2SiO[Si(CH3)2O]n[Si(CH3)(CH＝CH2)O]mSi(CH3)2(CH＝CHa) Wherein n and m are positive integers, and the viscosity is 20000 to 50000 mPa.S at 25 ℃. Among them, the preferable vinyl content is 0.1 to 0.3% by mass. The n and m values can be obtained by nuclear magnetic resonance hydrogen spectrogram calculation. By calculation, n is 1000-1500, and m is 1-10. By changing the values of m and n, a series of polysiloxanes with different molecular weights, different viscosities and different vinyl contents can be obtained.
The structural formula of the trimethylsiloxy terminated methylhydrogenpolysiloxane is as follows: (CH)3)3SiO[Si(CH3)2O]n[Si(CH3)HO]mSi(CH3)3Wherein n and m are positive integers. Among them, the hydrogen content is preferably 0.1 to 0.5% by mass, and the viscosity is preferably 40 to 100 mPaS at 25 ℃. The n and m values can be obtained by nuclear magnetic resonance hydrogen spectrogram calculation. By calculation, n is 10-50, and m is 3-25. By changing the values of m and n, a series of polysiloxanes with different molecular weights, different viscosities and different hydrogen contents can be obtained.
Preferably, the mass ratio of the trimethylsiloxy terminated methylhydrogenpolysiloxane to the terminal vinyl group-containing and side vinyl group-containing polysiloxane is 2-7: 100, and more preferably, the ratio of the molar amount of the hydrosilyl groups in the trimethylsiloxy terminated methylhydrogenpolysiloxane to the molar amount of the vinyl groups in the terminal vinyl group-containing and side vinyl group-containing polysiloxane is 1.2-1.5: 1.
The boron-containing polysiloxane is prepared by the following steps: 71.7 parts by weight of H (CH) is weighed3)2SiO[Si(CH3)(CH＝CH2)O]4Si(CH3)2H. Placing 0.2 part of tris (pentafluorobenzene) borane and 10 parts of toluene in a reaction bottle equipped with a stirring and constant-pressure dropping funnel, weighing 6.2 parts of boric acid and 5 parts of toluene in the dropping funnel, dropping the boric acid and the toluene into the reaction bottle within 30min at room temperature, continuing stirring for reaction for 2h after the dropping is finished, adding 1 part of neutral alumina, stirring for 30min, filtering, and evaporating toluene and low-boiling-point substances in the filtrate to obtain the boron-containing polysiloxane.
The tris (pentafluorobenzene) borane can efficiently catalyze the condensation reaction of silicon hydride and boric acid for removing hydrogen, has high selectivity, and can play a very effective role in catalysis only by a trace amount of catalyst. H (CH)3)2SiO[Si(CH3)(CH＝CH2)O]4Si(CH3)2The H can be prepared by the joint hydrolysis condensation reaction of dimethyl hydrogen chlorosilane and methyl vinyl dichlorosilane, and can also be prepared by the joint equilibrium polymerization of tetramethyl disiloxane and tetramethyl tetravinylcyclotetrasiloxane under the acid catalyst. The prepared boron-containing polysiloxane contains vinyl and can participate in the vulcanization of addition type silicone rubber.
Preferably, the amount of the boron-containing polysiloxane is 2 to 5% by mass of the polysiloxane containing terminal vinyl groups and side vinyl groups.
Preferably, the amount of the hydrophobic fumed silica is 20-30% of the mass of the polysiloxane containing terminal vinyl groups and side vinyl groups.
The platinum catalyst is selected from divinyl tetramethyl disiloxane and chloroplatinic acid complex, and the dosage of the platinum catalyst is calculated by platinum, preferably 60-100 ppm of the total mass sum of the vinyl-terminated and side vinyl polysiloxane and the trimethylsiloxy-terminated methylhydrogenpolysiloxane.
The adhesive addition type liquid silicone rubber of the invention generates excellent adhesion to base materials such as aluminum, stainless steel and the like by heating at 120 ℃ for 10 min.
Compared with the prior art, the invention has the beneficial effects that:
(1) the boron-containing polysiloxane tackifier has high synthesis efficiency and mild preparation conditions;
(2) the adhesive addition type liquid silicone rubber has good adhesion to base materials such as aluminum, stainless steel and the like.
Detailed Description
The present invention will be described in further detail by way of examples.
In the embodiment, the hydrophobic fumed silica is commercially available American cabot TS-530, TS-720 and Germany Degussa R974, and a platinum catalyst divinyl tetramethyl disiloxane and a chloroplatinic acid complex are Karsted catalysts produced by Heley;
the vinyl-terminated and side vinyl-terminated polysiloxane is DY-V421 series vinyl silicone oil of Shandong Dayihua chemical industry Co., Ltd, and can also be products of other manufacturers in the market, such as DX-1203 vinyl silicone oil of Guangzhou Daxiong chemical raw material Co., Ltd, LV-206 polyvinyl silicone oil produced by Jiuden Yingying organosilicon material Co., Ltd.
The trimethylsiloxy terminated methylhydrogenpolysiloxane is DX-1202 hydrogen-containing silicone oil from chemical raw material Co., Ltd, Guangzhou Daxi chemical industry, or other products in the market, such as DY-H212 hydrogen-containing silicone oil from Shandong Dayi chemical industry Co., Ltd, or XHG-202 hydrogen-containing silicone oil from Zhejiang Xinan chemical industry group Co., Ltd.
Example 1: preparation of boron-containing polysiloxanes
71.7 parts of H (CH) are weighed out3)2SiO[Si(CH3)(CH＝CH2)O]4Si(CH3)2H. 0.2 part of tris (pentafluorobenzene) borane and 10 parts of toluene are placed in a reaction vessel equipped with a stirred, constant-pressure dropping funnel. 6.2 parts of boric acid and 5 parts of toluene are weighed and placed in a dropping funnel, and are dropped into a reaction bottle within 30min at room temperature, and after dropping, the stirring reaction is continued for 2 h. 1 part of neutral alumina is added, stirred for 30 minutes and filtered. And (3) evaporating and removing toluene and low-boiling-point substances in the filtrate to obtain the boron-containing polysiloxane.
(1H NMR(CDCl3): 0.03, 4.46, 5.76 ppm; GPC (toluene as mobile phase versus polystyrene): mn — 17600).
Example 2
100 parts of polysiloxane containing terminal vinyl groups and side vinyl groups (DY-V421-20000) (viscosity is 20000mPa & S, vinyl content is 0.1%), 5 parts of trimethylsiloxy-terminated methylhydrogenpolysiloxane (DY-H212-40) (viscosity is 40mPa & S, hydrogen content is 0.1%), 2 parts of boron-containing polysiloxane prepared in example 1, 20 parts of hydrophobic fumed silica (Kabert TS-530) and 1.0 part of Karsted catalyst (platinum concentration is 8000ppm), which were mixed and stirred for 20min to obtain adhesive addition type silicone rubber 1.
Example 3
100 parts of polysiloxane containing terminal vinyl groups and side vinyl groups (DX-1203-30000) (viscosity is 30000mPa & S, vinyl content is 0.2%), 2.6 parts of trimethylsiloxy-terminated methylhydrogenpolysiloxane (DX-1202-60) (viscosity is 60mPa & S, hydrogen content is 0.4%), 3 parts of boron-containing polysiloxane prepared in example 1, 25 parts of hydrophobic fumed silica (Kabert TS-720) and 0.8 part of Karsted catalyst (platinum concentration is 8000ppm) were mixed and stirred for 20min to obtain adhesive addition type silicone rubber 2.
Example 4
100 parts of a polysiloxane containing terminal vinyl groups and side vinyl groups (LV-206-50000) (viscosity: 50000 mPaS, vinyl content: 0.3%), 6.8 parts of trimethylsiloxy-terminated methylhydrogenpolysiloxane (XHG-202-100) (viscosity: 100 mPaS, hydrogen content: 0.2%), 5 parts of the boron-containing polysiloxane prepared in example 1, 30 parts of hydrophobic fumed silica (Degussa R974), and 1.3 parts of Karsted catalyst (platinum concentration: 8000ppm) were mixed and stirred for 20 minutes to obtain an adhesive addition type silicone rubber 3.
Test example
The silicone rubbers 1-3 prepared in examples 2-4 were coated on an aluminum sheet or stainless steel substrate, and cured by heating at 120 ℃ for 10 min. Then, the shear strength of the cured silicone rubber is tested according to GB/T13936-92 "determination method of tensile shear strength of vulcanized rubber and metal bonding" shown in Table 1:
table 1:
| example 2 | Example 3 | Example 4 | |
| Shear strength (MPa) | 2.5 (aluminum sheet substrate) | 3.2 (stainless steel substrate) | 3.8 (aluminum sheet substrate) |
Claims (9)
1. The adhesive addition type liquid silicone rubber is characterized by being prepared by mixing terminated vinyl and side vinyl polysiloxane, trimethylsiloxy terminated methylhydrogenpolysiloxane, boron-containing polysiloxane, hydrophobic fumed silica and a platinum catalyst;
the boron-containing polysiloxane is prepared by the following steps: 71.7 parts by weight of H (CH) is weighed3)2SiO[Si(CH3)(CH＝CH2)O]4Si (CH3)2H. Placing 0.2 part of tris (pentafluorobenzene) borane and 10 parts of toluene in a reaction bottle equipped with a stirring and constant-pressure dropping funnel, weighing 6.2 parts of boric acid and 5 parts of toluene in the dropping funnel, dropping the boric acid and the toluene into the reaction bottle within 30min at room temperature, continuing stirring for reaction for 2h after the dropping is finished, adding 1 part of neutral alumina, stirring for 30min, filtering, and evaporating toluene and low-boiling-point substances in the filtrate to obtain the boron-containing polysiloxane.
2. The adhesive addition type liquid silicone rubber according to claim 1, wherein the polysiloxane containing terminal vinyl groups and side vinyl groups has the structural formula: (CH)2＝CH)(CH3)2SiO[Si(CH3)2O]n[Si(CH3)(CH＝CH2)O]mSi(CH3)2(CH＝CH2) Wherein n and m are positive integers, and the viscosity is 20000 to 50000 mPas at 25 ℃.
3. The adhesive addition type liquid silicone rubber according to claim 1 or 2, wherein the mass content of vinyl groups in the terminal vinyl group-containing and side vinyl group-containing polysiloxane is 0.1 to 0.3%.
4. The adhesive addition type liquid silicone rubber according to claim 1, wherein the trimethylsiloxy terminated methylhydrogenpolysiloxane has the structural formula: (CH)3)3SiO[Si(CH3)2O]n[Si(CH3)HO]mSi(CH3)3Wherein n and m are positive integers, and the viscosity is 40 to 100 mPas at 25 ℃.
5. The adhesive addition type liquid silicone rubber according to claim 1 or 4, wherein the trimethylsiloxy terminated methylhydrogenpolysiloxane contains 0.1 to 0.5% by mass of hydrogen.
6. The adhesive addition type liquid silicone rubber according to claim 1, 2 or 4, wherein the mass ratio of the trimethylsiloxy terminated methylhydrogenpolysiloxane to the polysiloxane containing terminal vinyl groups and side vinyl groups is 2-7: 100.
7. The adhesive addition type liquid silicone rubber according to claim 1, wherein the amount of the boron-containing polysiloxane is 2 to 5% by mass based on the mass of the polysiloxane containing terminal vinyl groups and side vinyl groups.
8. The adhesive addition type liquid silicone rubber according to claim 1, wherein the amount of the hydrophobic fumed silica is 20 to 30% by mass of the polysiloxane containing terminal vinyl groups and side vinyl groups.
9. The adhesive addition type liquid silicone rubber according to claim 1, wherein the platinum catalyst is selected from the group consisting of divinyltetramethyldisiloxane and chloroplatinic acid complex, and the amount of the platinum catalyst is 60 to 100ppm in terms of platinum, based on the total mass of the terminal vinyl and side vinyl polysiloxanes combined with trimethylsiloxy terminated methylhydrogenpolysiloxanes.
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| CN108300408B (en) * | 2017-12-21 | 2020-09-04 | 宁波凯耀电器制造有限公司 | Organic silicon material for packaging LED with high luminous flux maintenance rate |
| CN111712767A (en) * | 2018-04-20 | 2020-09-25 | 惠普发展公司，有限责任合伙企业 | Intermediate transfer blanket |
| CN111394054A (en) * | 2020-03-24 | 2020-07-10 | 新安天玉有机硅有限公司 | Silicone rubber for self-adhesive tape and preparation method thereof |
| CN113667310B (en) * | 2021-08-18 | 2023-02-28 | 佛山市天宝利硅工程科技有限公司 | Liquid silicone rubber and preparation method and application thereof |
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| CN101935455B (en) * | 2010-07-28 | 2012-10-24 | 杭州师范大学 | Organosilicon material for packaging LED and preparation method thereof |
| US9246173B2 (en) * | 2012-11-16 | 2016-01-26 | Mitsubishi Chemical Corporation | Process for synthesis of hybrid siloxy derived resins and crosslinked networks therefrom |
| CN104449439A (en) * | 2013-09-17 | 2015-03-25 | 河北联合大学 | High self-adhesive silicone rubber belt as well as preparation and application of high self-adhesive silicone rubber belt |
| CN103739848B (en) * | 2013-12-25 | 2016-06-01 | 北京化工大学 | Additional organosilicon packaging plastic tackifier and its preparation method |
| CN104497906B (en) * | 2014-12-03 | 2016-08-17 | 中国科学院化学研究所 | A kind of boracic viscosifier for addition-type silicon rubber and preparation method thereof |
| CN104910829B (en) * | 2015-05-05 | 2017-05-17 | 深圳新宙邦科技股份有限公司 | Tackifying agent for LED sealed packaging adhesive and preparation method thereof |
| CN105524282B (en) * | 2016-02-04 | 2018-06-22 | 华南理工大学 | Organic borosilicate adhesion promoters of high refractive index and its preparation method and application |
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