CN116676057A - Silica gel tackifier and preparation method and application thereof - Google Patents
Silica gel tackifier and preparation method and application thereof Download PDFInfo
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- CN116676057A CN116676057A CN202310670052.9A CN202310670052A CN116676057A CN 116676057 A CN116676057 A CN 116676057A CN 202310670052 A CN202310670052 A CN 202310670052A CN 116676057 A CN116676057 A CN 116676057A
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- silica gel
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- tackifier
- vinyl
- catalyst
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000000741 silica gel Substances 0.000 title claims abstract description 44
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 100
- 239000003054 catalyst Substances 0.000 claims abstract description 59
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000003112 inhibitor Substances 0.000 claims abstract description 34
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 27
- 239000001257 hydrogen Substances 0.000 claims abstract description 27
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 27
- -1 vinyl siloxane Chemical class 0.000 claims abstract description 22
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 19
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 125000005375 organosiloxane group Chemical group 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 28
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000008098 formaldehyde solution Substances 0.000 claims description 14
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 14
- 229920002379 silicone rubber Polymers 0.000 claims description 13
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-UHFFFAOYSA-N 0.000 claims description 12
- 239000004945 silicone rubber Substances 0.000 claims description 11
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002318 adhesion promoter Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 6
- MBGQQKKTDDNCSG-UHFFFAOYSA-N ethenyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(C=C)OCC MBGQQKKTDDNCSG-UHFFFAOYSA-N 0.000 claims description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 9
- 239000000853 adhesive Substances 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- SSDZYLQUYMOSAK-UHFFFAOYSA-N ethynylcyclohexane Chemical compound C#CC1CCCCC1 SSDZYLQUYMOSAK-UHFFFAOYSA-N 0.000 description 12
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 9
- 239000000243 solution Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- OWRXWSVBJIIORE-UHFFFAOYSA-N 3,7,11-trimethyldodec-1-yn-3-ol Chemical compound CC(C)CCCC(C)CCCC(C)(O)C#C OWRXWSVBJIIORE-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 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
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- 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
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a silica gel tackifier, a preparation method and application thereof, comprising the following components: vinyl siloxane, hydrogen-containing organosiloxane, inhibitor and platinum catalyst, wherein the platinum catalyst is a platinum-palladium catalyst prepared by an activated carbon supported impregnation method; compared with the existing silica gel tackifier, the invention adopts the platinum-palladium catalyst, reduces the dosage of platinum, the platinum and palladium exist in an elemental state on the surface of the active carbon, the crystal grain is smaller, and simultaneously the combination energy of extra-nuclear electrons of the platinum and the palladium deviates to generate interaction, the activity is better than that of the platinum catalyst independently loaded, the curing reaction of vinyl and silicon hydrogen bonds in vinyl siloxane and hydrogen-containing organosiloxane is better catalyzed, and the adhesive strength of the tackifier is improved.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a silica gel tackifier, a preparation method and application thereof.
Background
The addition type organic silicon rubber has excellent performances of low curing shrinkage, aging resistance, weather resistance, corrosion resistance and the like, and can be well applied to the fields of construction, transportation, aerospace, medical treatment, electronic components and the like. However, in the above-mentioned fields of application, there is often a problem that the lack of reactive groups, weak forces with the substrate molecules, result in poor adhesion properties. Aiming at the problem of poor adhesiveness, the prior art mainly has three solving approaches: 1, carrying out surface modification on a polyoxy silane molecule; 2, carrying out primary coating treatment on the base material; 3, selecting and adding proper tackifier. The former two approaches have obvious defects, the surface modification cost is high, and the actual production is complex; solvents introduced by the priming process can pollute the environment and cause harm to the human body.
The patent with publication number CN104497906A discloses a preparation method of a boron-containing addition type silicone rubber tackifier, which can improve the adhesive property of the addition type silicone rubber and stainless steel, aluminum metal, PET, PC and other materials, but ether reagents are used in the preparation process, and the ether reagents are distilled and removed under reduced pressure after the reaction is finished, so that the preparation cost is increased, and the environmental protection is not facilitated;
the patent with publication number CN107629211A discloses a preparation method and application of a tackifier in silica gel, however, the preparation cost of hydrogen-containing silicone oil is higher, which is not beneficial to the industrialized wide application;
the adhesion promoter prepared in the patent with publication number of CN111363103A uses a platinum catalyst, so that the preparation cost is low, and the platinum catalyst is likely to fail when a phosphorus-containing substance is encountered in the application of a silicon rubber model, and the platinum catalyst is also poisoned when the platinum catalyst is caused by substances containing nitrogen, antimony and other elements.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a silica gel tackifier, a preparation method and application thereof, and solves the problems of low adhesion of the tackifier and easy failure of a platinum catalyst.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
in a first aspect, the invention provides a silicone tackifier comprising the following components: vinyl siloxane, hydrogen-containing organosiloxane, inhibitor and platinum catalyst.
Further preferably, the vinyl siloxane comprises at least one of vinyl methyl dimethoxy silane, vinyl methyl diethoxy silane, vinyl trimethoxy silane, or vinyl triethoxy silane.
Further preferably, the hydrogen-containing organosiloxane comprises a dimethylsilyl or trimethylhydrosilyl-terminated polymethylhydrosilyl.
For molding, injection molding requirements in tackifier applications, it is further preferred that the inhibitor is a combination of 1-ethynyl cyclohexane and 3,7, 11-trimethyl-1-dodecyn-3-ol.
Further preferably, the mass percentage of the 1-ethynyl cyclohexane in the combined inhibitor is 40-50%.
In order to promote the reaction of vinyl siloxane with hydrogen-containing organosiloxane, further preferably, the platinum catalyst is an activated carbon-supported platinum palladium catalyst.
Further preferably, the preparation process of the platinum-palladium catalyst comprises the following steps:
s1, weighing active carbon, drying, adding distilled water for dispersion, adding chloroplatinic acid, stirring for 2-4 hours at 40-45 ℃, adding palladium chloride, and stirring for 2-4 hours;
s2, adding excessive formaldehyde solution, and stirring for 2-4 hours at 60-65 ℃;
s3, filtering and drying the filter cake to obtain the platinum-palladium catalyst.
In order to obtain a better adsorption effect, it is further preferred that the particle size of the activated carbon in step S1 is < 0.08mm.
Further preferably, the mass concentration of the activated carbon after being dispersed in water in the step S1 is 10-15%.
Further preferably, the molar ratio of chloroplatinic acid, palladium chloride and formaldehyde solution in steps S1, S2 is 1: (2.2-3.5): (3.2-4).
In a second aspect, the present invention provides a method for preparing the silica gel tackifier according to the first aspect, comprising the following steps:
a1, under the protection of gas, adding vinyl siloxane and hydrogen-containing organosiloxane in proportion, uniformly mixing, and stirring at 50-60 ℃ for 0.5-1h;
and A2, dropwise adding a platinum catalyst, continuing to react for 4-6 hours, adding an inhibitor, and obtaining the silica gel tackifier after the reaction is completed.
Further preferably, the molar ratio of vinyl siloxane, hydrogen-containing organosiloxane, platinum catalyst and inhibitor in steps A1, A2 is 1: (4.2-5.1): (1.2-1.3): (12-16).
In a third aspect, the invention also provides an application of the silica gel tackifier, wherein the silicone rubber is added into the tackifier obtained by the preparation method of the silica gel tackifier in the second aspect, and the addition proportion is 2-3% of the mass of the silicone rubber.
Compared with the prior art, the silica gel tackifier and the preparation method and application thereof have the following beneficial effects:
(1) The existing silica gel tackifier is added with a platinum catalyst to promote the reaction, so that the preparation cost is increased, and the poisoning of the platinum catalyst can be caused; the invention adopts the platinum-palladium catalyst loaded by the active carbon, the cost of palladium is low, the dosage of platinum is reduced, platinum and palladium exist in an elemental state on the surface of the active carbon, the crystal grain is smaller, and simultaneously the combination energy of electrons outside the core of the platinum and the palladium is offset to generate interaction, so that the activity is better than that of the platinum catalyst loaded independently, and the curing reaction of vinyl and silicon-hydrogen bonds is better catalyzed;
(2) The vinyl of vinyl siloxane in the silica gel tackifier is added with the silicon hydrogen bond of hydrogen-containing organosiloxane to form active groups for enhancing the adhesive force, so that the adhesive strength is improved, and the curing effect is not affected;
(3) The silica gel tackifier provided by the invention has the advantages that the adhesive effect of organic silica gel and aluminum sheets, PPA, PC, PET and other base materials is well promoted, primer and titanate catalyst are not required to be introduced, the tackifier has good transparency, and the adhesive is suitable for various addition type adhesive products and has good application prospects.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Example 1
A silica gel tackifier, which comprises the following components: vinyl methyl dimethoxy silane, dimethyl hydrosilyl end-capped polymethyl hydrogen dimethyl siloxane, an inhibitor and a platinum catalyst, wherein the inhibitor is a combination of 1-ethynyl cyclohexane and 3,7, 11-trimethyl-1-dodecyn-3-alcohol, and the mass percentage of the 1-ethynyl cyclohexane in the combination inhibitor is 40%;
the specific preparation process of the platinum catalyst comprises the following steps:
s1, weighing activated carbon with the thickness of 0.07mm, drying, adding distilled water to prepare an activated carbon solution with the mass concentration of 10%, dispersing, adding chloroplatinic acid, stirring for 4 hours at the temperature of 40 ℃, adding palladium chloride, and stirring for 4 hours;
s2, adding excessive formaldehyde solution, and stirring for 4 hours at 60 ℃; wherein the molar ratio of the chloroplatinic acid, the palladium chloride and the formaldehyde solution in the steps S1 and S2 is 1:2:3.2;
s3, filtering and drying the filter cake to obtain the platinum-palladium catalyst.
The preparation method of the silica gel tackifier comprises the following steps:
a1, under the protection of gas, adding vinyl methyl dimethoxy silane and dimethyl hydrosilyl end-capped polymethyl hydrogen dimethyl siloxane in proportion, uniformly mixing, and stirring for 1h at 50 ℃;
and A2, dropwise adding a platinum catalyst, continuously reacting for 6 hours, adding an inhibitor, and obtaining the silica gel tackifier after the reaction is completed, wherein the molar ratio of the vinyl methyl dimethoxy silane to the dimethyl hydrogen silicon-based end-capped polymethyl hydrogen dimethyl siloxane to the platinum catalyst to the inhibitor in the steps A1 and A2 is 1:4.2:1.2:12.
example 2
A silica gel tackifier, which comprises the following components: vinyl methyl dimethoxy silane, vinyl methyl diethoxy silane, dimethyl hydrosilyl end-capped polymethyl hydrosilyl siloxane, an inhibitor and a platinum catalyst, wherein the mass ratio of the vinyl methyl dimethoxy silane to the vinyl methyl diethoxy silane is 1:1, the inhibitor is a combination of 1-ethynyl cyclohexane and 3,7, 11-trimethyl-1-dodecyn-3-ol, and the mass percentage of the 1-ethynyl cyclohexane in the combination inhibitor is 50%;
the specific preparation process of the platinum catalyst comprises the following steps:
s1, weighing activated carbon with the thickness of 0.07mm, drying, adding distilled water to prepare an activated carbon solution with the mass concentration of 10%, dispersing, adding chloroplatinic acid, stirring for 2 hours at 45 ℃, adding palladium chloride, and stirring for 2 hours;
s2, adding excessive formaldehyde solution, and stirring for 2 hours at 65 ℃, wherein the molar ratio of chloroplatinic acid to palladium chloride to formaldehyde solution in the steps S1 and S2 is 1:3.5:4, a step of;
s3, filtering and drying the filter cake to obtain the platinum-palladium catalyst.
The preparation method of the silica gel tackifier comprises the following steps:
a1, under the protection of gas, adding vinyl methyl dimethoxy silane, vinyl methyl diethoxy silane and dimethyl hydrosilyl end-capped polymethyl hydrosilyl siloxane in proportion, uniformly mixing, and stirring at 60 ℃ for 0.5h;
and A2, dropwise adding a platinum catalyst, continuously reacting for 4 hours, adding an inhibitor, and obtaining the silica gel tackifier after the reaction is completed, wherein the mole ratio of the vinyl methyl dimethoxy silane, the vinyl methyl diethoxy silane, the dimethyl hydrogen silicon-based terminated polymethyl hydrogen dimethyl siloxane, the platinum catalyst and the inhibitor in the steps A1 and A2 is 1:4.2:1.2:12.
example 3
A silica gel tackifier, which comprises the following components: vinyl trimethoxy silane, trimethylhydrosilyl-terminated polymethylhydrosiloxane, an inhibitor and a platinum catalyst, wherein the inhibitor is a combination of 1-ethynyl cyclohexane and 3,7, 11-trimethyl-1-dodecyn-3-ol, and the mass percentage of the 1-ethynyl cyclohexane in the combination inhibitor is 50%;
the specific preparation process of the platinum catalyst comprises the following steps:
s1, weighing activated carbon with the thickness of 0.07mm, drying, adding distilled water to prepare an activated carbon solution with the mass concentration of 15%, dispersing, adding chloroplatinic acid, stirring for 3 hours at the temperature of 42 ℃, adding palladium chloride, and stirring for 3 hours;
s2, adding excessive formaldehyde solution, and stirring for 3 hours at 63 ℃, wherein the molar ratio of chloroplatinic acid to palladium chloride to formaldehyde solution in the steps S1 and S2 is 1:3:3.5;
s3, filtering and drying the filter cake to obtain the platinum-palladium catalyst.
The preparation method of the silica gel tackifier comprises the following steps:
a1, under the protection of gas, adding vinyl trimethoxy silane and trimethylhydrosilyl-terminated polymethylhydrosiloxane in proportion, uniformly mixing, and stirring at 55 ℃ for 0.8h;
and A2, dropwise adding a platinum catalyst, continuously reacting for 5 hours, adding an inhibitor, and obtaining the silica gel tackifier after the reaction is completed, wherein the molar ratio of the vinyl trimethoxy silane to the trimethylhydrosilyl-terminated polymethylhydrosiloxane to the platinum catalyst to the inhibitor in the steps A1 and A2 is 1:5.1:1.3:16.
example 4
A silica gel tackifier, which comprises the following components: vinyl trimethoxy silane, vinyl triethoxy silane, trimethylhydrosilyl-terminated polymethylhydrosilyl siloxane, an inhibitor and a platinum catalyst, wherein the mass ratio of the vinyl trimethoxy silane to the vinyl triethoxy silane is 1:1, wherein the inhibitor is a combination of 1-ethynyl cyclohexane and 3,7, 11-trimethyl-1-dodecyn-3-ol, and the mass percentage of the 1-ethynyl cyclohexane in the combination inhibitor is 50%;
the specific preparation process of the platinum catalyst comprises the following steps:
s1, weighing activated carbon with the thickness of 0.07mm, drying, adding distilled water to prepare an activated carbon solution with the mass concentration of 15%, dispersing, adding chloroplatinic acid, stirring for 2 hours at 45 ℃, adding palladium chloride, and stirring for 2 hours;
s2, adding excessive formaldehyde solution, and stirring for 2 hours at 65 ℃, wherein the molar ratio of chloroplatinic acid to palladium chloride to formaldehyde solution in the steps S1 and S2 is 1:3:3.5;
s3, filtering and drying the filter cake to obtain the platinum-palladium catalyst.
The preparation method of the silica gel tackifier comprises the following steps:
a1, under the protection of gas, adding vinyl trimethoxy silane, vinyl triethoxy silane and trimethylhydrosilyl-terminated polymethylhydrosiloxane in proportion, uniformly mixing, and stirring at 60 ℃ for 0.5h;
and A2, dropwise adding a platinum catalyst, continuously reacting for 4 hours, adding an inhibitor, and obtaining the silica gel tackifier after the reaction is completed, wherein the mole ratio of the vinyl trimethoxy silane, the vinyl triethoxy silane, the trimethylhydrosilyl-terminated polymethylhydrosilyl siloxane, the platinum catalyst and the inhibitor in the steps A1 and A2 is 1:4.5:1.2:15.
example 5
A silica gel tackifier, which comprises the following components: vinyl methyl dimethoxy silane, dimethyl hydrosilyl end-capped polymethyl hydrogen dimethyl siloxane, an inhibitor and a platinum catalyst, wherein the inhibitor is a combination of 1-ethynyl cyclohexane and 3,7, 11-trimethyl-1-dodecyn-3-alcohol, and the mass percentage of the 1-ethynyl cyclohexane in the combination inhibitor is 50%;
the specific preparation process of the platinum catalyst comprises the following steps:
s1, weighing activated carbon with the thickness of 0.07mm, drying, adding distilled water to prepare an activated carbon solution with the mass concentration of 12%, dispersing, adding chloroplatinic acid, stirring for 2 hours at 45 ℃, adding palladium chloride, and stirring for 2 hours;
s2, adding excessive formaldehyde solution, and stirring for 2 hours at 65 ℃, wherein the molar ratio of chloroplatinic acid to palladium chloride to formaldehyde solution in the steps S1 and S2 is 1:3:3.5;
s3, filtering and drying the filter cake to obtain the platinum-palladium catalyst.
The preparation method of the silica gel tackifier comprises the following steps:
a1, under the protection of gas, adding vinyl methyl dimethoxy silane and dimethyl hydrosilyl end-capped polymethyl hydrogen dimethyl siloxane in proportion, uniformly mixing, and stirring at 60 ℃ for 0.5h;
and A2, dropwise adding a platinum catalyst, continuously reacting for 4 hours, adding an inhibitor, and obtaining the silica gel tackifier after the reaction is completed, wherein the molar ratio of the vinyl methyl dimethoxy silane to the dimethyl hydrogen silicon-based end-capped polymethyl hydrogen dimethyl siloxane to the platinum catalyst to the inhibitor in the steps A1 and A2 is 1:4.2:1.2:12.
comparative example 1
A silica gel tackifier is prepared from the components of vinyl-free siloxane and hydrogen-containing organosiloxane (CN 104059590) and epoxy resin as main components.
Comparative example 2
A silicone tackifier is distinguished from example 2 in that a titanate catalyst is used.
Comparative example 3
A silica gel tackifier differs from example 3 in that a platinum catalyst is used.
Comparative example 4
A silica gel tackifier differs from example 4 in that a platinum catalyst which is not supported on activated carbon is used.
Comparative example 5
A silica gel tackifier is different from example 5 in that the addition ratio is 5% of the mass of the silicone rubber.
The tackifiers obtained in examples 1 to 5 and comparative examples 1 to 5 were added to silicone rubber, the amounts of addition of examples 1 to 4 and comparative examples 1 to 4 were 2% by mass of the silicone rubber, the amount of addition of example 5 was 3% by mass of the silicone rubber, the amount of addition of comparative example 5 was 5% by mass of the silicone rubber, and viscosity measurements were carried out on examples by referring to the related method of GB/T2794-2013, a substrate of 50 mm. Times.50 mm. Times.2.5 mm was selected as a bonding sample, the surface was cleaned with acetone before application, the surface of the substrate was lightly pressed after application, and cured for 24 hours, and the adhesive strength was tested.
TABLE 1 adhesion promoter Performance test obtained in examples 1-5 and comparative examples 1-5
TABLE 2 adhesion Strength test results (MPa) for different substrates
| Examples | Aluminum sheet | PPA | PC | PET |
| Example 1 | 2.30 | 1.94 | 1.82 | 2.34 |
| Example 2 | 2.43 | 2.08 | 1.95 | 2.50 |
| Example 3 | 2.25 | 1.85 | 1.61 | 2.30 |
| Example 4 | 2.18 | 1.74 | 1.50 | 2.26 |
| Example 5 | 2.06 | 1.66 | 1.44 | 2.15 |
| Comparative example 1 | 1.42 | 1.12 | 0.95 | 1.23 |
| Comparative example 2 | 1.66 | 1.30 | 1.08 | 1.42 |
| Comparative example 3 | 1.87 | 1.41 | 0.80 | 1.56 |
| Comparative example 4 | 1.73 | 1.23 | 0.63 | 1.32 |
| Comparative example 5 | 1.55 | 1.05 | 0.54 | 1.20 |
As can be seen from tables 1-2, example 1 and comparative example 1 demonstrate that the cured adhesion promoters of the present invention have adhesion superior to that of epoxy resins; examples 2-4 and comparative examples 2-4 illustrate the different effects of adhesion strength of the adhesion promoters of the present invention after the addition of different catalysts and without the addition of catalysts; example 5 and comparative example 5 illustrate that when the amount of the cured tackifier is excessively added, the adhesive strength to the substrate may be lowered.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. The silica gel tackifier is characterized by comprising the following components: vinyl siloxane, hydrogen-containing organosiloxane, inhibitor and platinum catalyst.
2. A silicone gum adhesion promoter of claim 1, wherein said vinyl siloxane comprises at least one of vinyl methyl dimethoxy silane, vinyl methyl diethoxy silane, vinyl trimethoxy silane, or vinyl triethoxy silane.
3. A silicone gum adhesion promoter according to claim 1, wherein said hydrogen-containing organosiloxane comprises a dimethylsilyl or trimethylhydrosilyl-terminated polymethylhydrosilyl siloxane.
4. A silica gel adhesion promoter as set forth in claim 1, wherein said platinum catalyst is an activated carbon supported platinum palladium catalyst.
5. The silica gel tackifier according to claim 4, wherein the platinum palladium catalyst is prepared by a process comprising the steps of:
s1, weighing active carbon, drying, adding distilled water for dispersion, adding chloroplatinic acid, stirring for 2-4 hours at 40-45 ℃, adding palladium chloride, and stirring for 2-4 hours;
s2, adding excessive formaldehyde solution, and stirring for 2-4 hours at 60-65 ℃;
s3, filtering and drying the filter cake to obtain the platinum-palladium catalyst.
6. A silica gel tackifier according to claim 5 wherein the activated carbon in step S1 has a particle size of < 0.08mm.
7. The silica gel tackifier according to claim 5, wherein the molar ratio of chloroplatinic acid, palladium chloride and formaldehyde solution in steps S1 and S2 is 1: (2.2-3.5): (3.2-4).
8. A method for preparing a silicone tackifier according to any one of claims 1 to 7, comprising the steps of:
a1, under the protection of gas, adding vinyl siloxane and hydrogen-containing organosiloxane in proportion, uniformly mixing, and stirring at 50-60 ℃ for 0.5-1h;
and A2, dropwise adding a platinum catalyst, continuing to react for 4-6 hours, adding an inhibitor, and obtaining the silica gel tackifier after the reaction is completed.
9. The method for preparing a silica gel tackifier according to claim 8, wherein the molar ratio of vinyl siloxane, hydrogen-containing organosiloxane, platinum catalyst and inhibitor in steps A1 and A2 is 1: (4.2-5.1): (1.2-1.3): (12-16).
10. The application of the silica gel tackifier is characterized in that the silicone rubber is added into the tackifier obtained by the preparation method of the silica gel tackifier according to any one of claims 8-9, and the addition proportion is 2-3% of the mass of the silicone rubber.
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