CN114958293A - Low-odor coated dealcoholized transparent flowing sealant for electronic and electric appliances - Google Patents
Low-odor coated dealcoholized transparent flowing sealant for electronic and electric appliances Download PDFInfo
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- CN114958293A CN114958293A CN202210781139.9A CN202210781139A CN114958293A CN 114958293 A CN114958293 A CN 114958293A CN 202210781139 A CN202210781139 A CN 202210781139A CN 114958293 A CN114958293 A CN 114958293A
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- 239000000565 sealant Substances 0.000 title claims abstract description 29
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 66
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 57
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 55
- 239000003381 stabilizer Substances 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 18
- 239000007822 coupling agent Substances 0.000 claims abstract description 18
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 16
- 239000004014 plasticizer Substances 0.000 claims abstract description 16
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 52
- 238000002360 preparation method Methods 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 229920002554 vinyl polymer Polymers 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 9
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- 229940126062 Compound A Drugs 0.000 claims description 6
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- LVTJOONKWUXEFR-FZRMHRINSA-N protoneodioscin Natural products O(C[C@@H](CC[C@]1(O)[C@H](C)[C@@H]2[C@]3(C)[C@H]([C@H]4[C@@H]([C@]5(C)C(=CC4)C[C@@H](O[C@@H]4[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@@H](O)[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@H](CO)O4)CC5)CC3)C[C@@H]2O1)C)[C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1 LVTJOONKWUXEFR-FZRMHRINSA-N 0.000 claims description 6
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229910002011 hydrophilic fumed silica Inorganic materials 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 4
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 claims description 3
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 claims description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 3
- OHYZAXNDAOHLDC-UHFFFAOYSA-N C(=C)(C)C(CC)O[Si](C=C)(OC(CC)C(=C)C)OC(CC)C(=C)C Chemical compound C(=C)(C)C(CC)O[Si](C=C)(OC(CC)C(=C)C)OC(CC)C(=C)C OHYZAXNDAOHLDC-UHFFFAOYSA-N 0.000 claims description 3
- GJWAPAVRQYYSTK-UHFFFAOYSA-N [(dimethyl-$l^{3}-silanyl)amino]-dimethylsilicon Chemical compound C[Si](C)N[Si](C)C GJWAPAVRQYYSTK-UHFFFAOYSA-N 0.000 claims description 3
- XQBCVRSTVUHIGH-UHFFFAOYSA-L [dodecanoyloxy(dioctyl)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCCCCCC)(CCCCCCCC)OC(=O)CCCCCCCCCCC XQBCVRSTVUHIGH-UHFFFAOYSA-L 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- 238000004383 yellowing Methods 0.000 abstract description 6
- 238000003860 storage Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 13
- FKRCODPIKNYEAC-UHFFFAOYSA-N propionic acid ethyl ester Natural products CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 9
- 238000010276 construction Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- RCNRJBWHLARWRP-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane;platinum Chemical compound [Pt].C=C[Si](C)(C)O[Si](C)(C)C=C RCNRJBWHLARWRP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 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
- 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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of electrical sealants, in particular to a low-odor batch-type dealcoholized transparent flowing sealant for electronic and electric appliances, which aims to solve the problems of poor yellowing resistance, insufficient transparency and insufficient storage stability of the traditional product and comprises the following raw materials in parts by weight: 80-120 parts of alkoxy modified polydimethylsiloxane, 10-20 parts of reinforcing filler, 5-30 parts of plasticizer, 3-10 parts of cross-linking agent, 0.5-4 parts of stabilizer, 0.1-0.5 part of catalyst and 0.5-2.5 parts of coupling agent. The invention is matched with a stabilizer, a coupling agent and a catalyst, has the advantages of excellent transparency, lower smell and good yellowing resistance, has the storage stability of more than half a year, almost has no corrosivity on most base materials, has wide base material adaptability and can meet most of related application requirements on the market.
Description
Technical Field
The invention relates to the technical field of electric sealants, in particular to a low-odor batch-type dealcoholized transparent flowing sealant for electronic and electric appliances.
Background
The prior organic silicon transparent flowing sealant for the traditional electronic and electric appliances on the market mainly comprises a dealcoholized ethanol type and a dealcoholized ketoxime type. The two traditional transparent flowing organosilicon sealants have some common advantages, such as simple production process, controllable economic cost and capability of being produced by common organosilicon manufacturers, and the used raw materials are common organosilicon raw materials on the market. However, both clear, running sealants also suffer from some significant performance deficiencies.
Among them, the ethanol-removed single-component flowing transparent sealant usually has the defects of poor yellowing resistance, large smell, poor high temperature and high humidity resistance, insufficient storage stability and the like, while the ketoxime-removed single-component flowing sealant also has the defects of poor yellowing resistance, large smell, insufficient transparency, corrosivity to some substrates such as copper, PC and the like. Therefore, the low-odor coated dealcoholized transparent flowing sealant for electronic and electric appliances is provided by the technical personnel in the field to solve the problems in the background art.
Disclosure of Invention
The invention aims to provide a low-odor coated dealcoholized transparent flowing sealant for electronic and electric appliances, which solves the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a low-odor coated dealcoholized transparent flowing sealant for electronic appliances comprises the following raw materials in parts by weight: 80-120 parts of alkoxy modified polydimethylsiloxane, 10-20 parts of reinforcing filler, 5-30 parts of plasticizer, 3-10 parts of cross-linking agent, 0.5-4 parts of stabilizer, 0.1-0.5 part of catalyst and 0.5-2.5 parts of coupling agent;
the preparation method comprises the following steps:
s1: putting alkoxy modified polydimethylsiloxane and plasticizer into a planetary stirrer, adding reinforcing filler, heating to 120 ℃, and carrying out reduced pressure reduction stirring for 2 hours under the vacuum environment of-0.09 Mpa, wherein the stirring speed is 1000-1200 rpm;
s2: after cooling, the cross-linking agent, the stabilizing agent, the catalyst and the coupling agent are sequentially added, and the mixture is stirred for 50min at the rotating speed of 300-600rpm under the environment of vacuum-0.09 to-0.1 Mpa, and the finished product is obtained after discharging.
As a further aspect of the invention: the alkoxy modified polydimethylsiloxane adopts triethoxysilyethylene end-blocked polydimethylsiloxane A, trimethoxy end-blocked modified polydimethylsiloxane and triethoxysilyethylene end-blocked polydimethylsiloxane B;
the preparation method of triethoxysilyethylene-terminated polydimethylsiloxane A comprises the following steps: putting 1000 parts by weight of hydrogen-terminated polydimethylsiloxane with the viscosity of 2 ten thousand mPas, 20 parts by weight of vinyl triethoxysilane and 0.5 part by weight of platinum-vinyl siloxane complex with the mass fraction of 0.3% into a stirrer, and reacting for 1 hour at the temperature of 60-70 ℃;
the preparation method of the trimethoxy end-capped modified polydimethylsiloxane comprises the following steps: putting 1000 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 1 ten thousand mPas and 25 parts by weight of alpha-trimethoxysilylethyl propionate into a stirrer, reacting for 8 hours at 80-100 ℃ under the protection of nitrogen, and then reducing the pressure for 1 hour at 130 ℃ and under the vacuum degree of-0.09 MPa to obtain trimethoxy terminated polydimethylsiloxane;
the preparation method of triethoxysilyethylene end-blocked polydimethylsiloxane B is as follows: putting 1000 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 3 ten thousand mPas and 3-5 parts by weight of tetramethyldisilazane into a stirrer, heating to 50-70 ℃ under the protection of nitrogen, adding 0.5-1 part by weight of acetic acid, stirring for 1-2 hours under the protection of nitrogen, adding 15-20 parts by weight of vinyltriethoxysilane and 2 parts by weight of platinum-vinyl siloxane complex with the platinum mass fraction of 0.5%, and finally reacting for 3 hours at 60-80 ℃ to obtain triethoxysilylethylene-terminated polydimethylsiloxane.
As a further aspect of the invention: the reinforcing filler has a specific surface area of 150 or 200m 2 The/g of hydrophilic fumed silica.
As a further aspect of the invention: the plasticizer is any one of dimethyl terminated polydimethylsiloxane, single-ended alkoxy polydimethylsiloxane, MDT silicone oil and paraffin mixture.
As a further aspect of the invention: the cross-linking agent is any one of dimethyl dimethoxy silane, dimethyl diethoxy silane, methyl trimethoxy silane, methyl triethoxy silane, vinyl trimethoxy silane, vinyl triethoxy silane or hydrolyzed oligomer thereof, polymethyl triethoxy silane, tetraethoxy silane or oligomer thereof, n-propyl silicate or oligomer thereof, and tetramethoxy silane or oligomer thereof.
As a further aspect of the invention: the stabilizer adopts any one of alpha-trimethoxysilyl ethyl propionate and high-activity polyalkoxysilane;
the preparation method of the alpha-trimethoxysilylethyl propionate comprises the following steps: adding 122 parts by weight of trimethoxy silane, 100 parts of ethyl acrylate and 1 part by weight of platinum-vinyl siloxane complex with platinum mass fraction of 0.3% into a reaction kettle, reacting for 4-12 hours at 50-60 ℃ under the protection of nitrogen, then heating to 80 ℃, and reducing pressure and removing for 1 hour under the vacuum degree of-0.01 Mpa to obtain a stabilizer of alpha-trimethoxy silicon-based ethyl propionate;
the preparation method of the high-activity polyalkoxysilane is as follows: 122 parts by weight of triethoxy hydrosilane, 226 parts by weight of vinyl tri (isopropenylpropoxy) silane and 0.5 part by weight of platinum-vinyl siloxane complex with the mass fraction of 0.3 percent are put into a reaction kettle and react for 2 to 4 hours at the temperature of 40 to 60 ℃ under the protection of nitrogen, thus obtaining the high-activity polyalkoxysilane of the stabilizer B.
As a further scheme of the invention: the coupling agent adopts any one of a compound A, a compound B and a compound C;
the preparation method of the compound A comprises the following steps: adding 150 parts by weight of gamma-aminopropyltrimethoxysilane, 200 parts by weight of 3-glycidoxypropyltrimethoxysilane and 100 parts by weight of 3- (methacryloyloxy) propyltrimethoxysilane into a reaction kettle, reacting for 12-48 hours at 80-100 ℃ under the protection of nitrogen, and then heating to 120-130 ℃ for removing the low temperature for 4-8 hours to obtain the product;
the preparation method of the compound B comprises the following steps: adding 108 parts by weight of gamma-aminopropyltrimethoxysilane, 69 parts by weight of allyl glycidyl ether and 137 parts by weight of methyl orthosilicate into a reaction kettle, reacting for 2-4 hours at 80-110 ℃ under the protection of nitrogen, and then heating to 150-180 ℃ for removing the silane for 2-4 hours;
the preparation method of the compound C comprises the following steps: putting 555 parts by weight of gamma-aminopropyltriethoxysilane, 205 parts by weight of 3-isocyanatopropyltrimethoxysilane and 237 parts by weight of 3-glycidoxypropyltrimethoxysilane into a reaction kettle, stirring for 2-4 hours under the protection of nitrogen, heating to 100-120 ℃, and reducing the temperature for 1-3 hours under the vacuum degree of-0.09 Mpa.
As a further aspect of the invention: the catalyst adopts any one of a composition A and a composition B;
the preparation method of the composition A comprises the following steps: adding 41 parts by weight of dibutyltin oxide and 130 parts by weight of acetylacetone into a reaction kettle, heating to a reflux state, stirring for 8-10 hours, and then reducing the pressure at 140-150 ℃ for 2 hours.
The preparation method of the composition B comprises the following steps: adding 100 parts by weight of dioctyltin dilaurate and 200-600 parts by weight of tetraethoxysilane into a reaction kettle, heating to a reflux state, stirring for 3-6 hours, and then reducing the pressure at 160-180 ℃ for 2 hours.
Compared with the prior art, the invention has the beneficial effects that: the invention is matched with a stabilizer, a coupling agent and a catalyst, has the advantages of excellent transparency, lower smell and good yellowing resistance, has storage stability of more than half a year, almost has no corrosivity on most base materials, has wide base material adaptability, and can meet most of related application requirements on the market.
Detailed Description
Example 1
In the embodiment of the invention, the low-odor coated dealcoholized transparent flowing sealant for the electronic and electric appliances comprises the following raw materials in parts by weight: 85-105 parts of alkoxy modified polydimethylsiloxane, 10-20 parts of reinforcing filler, 10-20 parts of plasticizer, 3-10 parts of cross-linking agent, 0.5-3 parts of stabilizer, 0.1-0.5 part of catalyst and 0.5-3 parts of coupling agent;
the preparation method comprises the following steps:
s1: putting alkoxy modified polydimethylsiloxane and plasticizer into a planetary stirrer, adding reinforcing filler, heating to 120 ℃, and carrying out reduced pressure reduction stirring for 2 hours under the vacuum environment of-0.09 Mpa, wherein the stirring speed is 1000-1200 rpm;
s2: after cooling, the cross-linking agent, the stabilizing agent, the catalyst and the coupling agent are sequentially added, and the mixture is stirred for 50min at the rotating speed of 600rpm of 300-.
Further, the alkoxy modified polydimethylsiloxane adopts triethoxysilylethylene-terminated polydimethylsiloxane A;
the preparation method of triethoxysilyethylene-terminated polydimethylsiloxane A comprises the following steps: 1000 parts by weight of hydrogen-terminated polydimethylsiloxane having a viscosity of 2 ten thousand mPas, 20 parts by weight of vinyltriethoxysilane and 0.5 part by weight of platinum-vinylsiloxane complex having a platinum mass fraction of 0.3% were put into a stirrer and reacted at 60 to 70 ℃ for 1 hour.
Furthermore, the reinforcing filler adopts the specific surface area of 150m 2 The hydrophilic fumed silica/g can meet the requirements on transparency and mechanical properties of the product.
Furthermore, the plasticizer adopts single-end alkoxy polydimethylsiloxane, mainly reduces the viscosity of rubber materials, improves the construction performance, improves the usability of the sealant, and improves the fluidity and the construction performance of products.
Further, the cross-linking agent adopts vinyl trimethoxy silane.
Further, the stabilizer adopts alpha-trimethoxysilyl ethyl propionate;
the preparation method of the alpha-trimethoxysilylethyl propionate comprises the following steps: adding 122 parts by weight of trimethoxy silane, 100 parts of ethyl acrylate and 1 part by weight of platinum-vinyl siloxane complex with platinum mass fraction of 0.3% into a reaction kettle, reacting for 4-12 hours at 50-60 ℃ under the protection of nitrogen, then heating to 80 ℃, and reducing pressure for 1 hour under the vacuum degree of-0.01 Mpa to obtain the stabilizer of the alpha-trimethoxy silicon-based ethyl propionate.
Further, the coupling agent adopts a compound A;
the preparation method of the compound A comprises the following steps: adding 150 parts by weight of gamma-aminopropyltrimethoxysilane, 200 parts by weight of 3-glycidoxypropyltrimethoxysilane and 100 parts by weight of 3- (methacryloyloxy) propyltrimethoxysilane into a reaction kettle, reacting for 12-48 hours at 80-100 ℃ under the protection of nitrogen, and then heating to 120-130 ℃ for removing the low temperature for 4-8 hours to obtain the product;
further, the catalyst adopts a composition A;
the preparation method of the composition A comprises the following steps: adding 41 parts by weight of dibutyltin oxide and 130 parts by weight of acetylacetone into a reaction kettle, heating to a reflux state, stirring for 8-10 hours, and then reducing the pressure at 140-150 ℃ for 2 hours.
The preparation method of the single-end methyl polydimethylsiloxane comprises the following steps: 1000 parts of single-end vinyl single-end methyl silicone oil with the viscosity of 450 mPas (purchased from Shanghai Jing New materials science and technology Co., Ltd.), 15 parts of trimethoxyhydrosilane and 0.5 part of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (0) with the mass fraction of 0.3 percent are put into a stirrer, stirred and reacted for 1 hour at the temperature of 60-70 ℃ under the protection of nitrogen at the speed of 600r/min, then heated to the temperature of 85-95 ℃, and stirred for 1 hour at the vacuum degree of-0.09-0.1 MPa at the speed of 600 plus 800rpm, and then the single-end vinyl single-end methyl silicone oil with the viscosity of 500 mPas can be obtained.
Example 2
A low-odor coated dealcoholized transparent flowing sealant for electronic appliances comprises the following raw materials in parts by weight: 80-110 parts of alkoxy modified polydimethylsiloxane, 10-20 parts of reinforcing filler, 5-25 parts of plasticizer, 3-8 parts of cross-linking agent, 1-4 parts of stabilizer, 0.1-0.5 part of catalyst and 0.8-2.5 parts of coupling agent;
the preparation method comprises the following steps:
s1: putting alkoxy modified polydimethylsiloxane and plasticizer into a planetary stirrer, adding reinforcing filler, heating to 120 ℃, and carrying out reduced pressure reduction stirring for 2 hours under the vacuum environment of-0.09 Mpa, wherein the stirring speed is 1000-1200 rpm;
s2: after cooling, the cross-linking agent, the stabilizing agent, the catalyst and the coupling agent are sequentially added, and the mixture is stirred for 50min at the rotating speed of 600rpm of 300-.
Further, the alkoxy modified polydimethylsiloxane adopts trimethoxy end-capped modified polydimethylsiloxane;
the preparation method of the trimethoxy end-capped modified polydimethylsiloxane comprises the following steps: 1000 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 1 ten thousand mPas and 25 parts by weight of alpha-trimethoxysilylethyl propionate are put into a stirrer to react for 8 hours at 80-100 ℃ under the protection of nitrogen, and then the reaction product is reduced by 1 hour under the environment of 130 ℃ and the vacuum degree of-0.09 MPa to obtain the trimethoxy terminated polydimethylsiloxane.
Furthermore, the reinforcing filler has a specific surface area of 200m 2 The hydrophilic fumed silica/g can not only ensure the transparency and mechanical property requirements of the product, but also better control the product cost.
Furthermore, the plasticizer adopts dimethyl-terminated polydimethylsiloxane, so that the viscosity of the rubber material is mainly reduced, the construction performance is improved, the usability of the sealant is improved, and the flowability and the construction performance of the product are improved.
Further, the cross-linking agent adopts methyl trimethoxy silane.
Further, the stabilizing agent adopts high-activity polyalkoxysilane;
the preparation method of the high-activity polyalkoxysilane is as follows: 122 parts by weight of triethoxy hydrosilane, 226 parts by weight of vinyl tri (isopropenylpropoxy) silane and 0.5 part by weight of platinum-vinyl siloxane complex with the mass fraction of 0.3 percent are put into a reaction kettle and react for 2 to 4 hours at the temperature of 40 to 60 ℃ under the protection of nitrogen, thus obtaining the high-activity polyalkoxysilane of the stabilizer B.
Further, the coupling agent adopts a compound B;
the preparation method of the compound B comprises the following steps: 108 parts by weight of gamma-aminopropyltrimethoxysilane, 69 parts by weight of allyl glycidyl ether and 137 parts by weight of methyl orthosilicate are added into a reaction kettle, the mixture reacts for 2 to 4 hours at 80 to 110 ℃ under the protection of nitrogen, and then the temperature is raised to 150 to 180 ℃ for 2 to 4 hours to remove the impurities.
Further, the catalyst adopts a composition A;
the preparation method of the composition A comprises the following steps: adding 41 parts by weight of dibutyltin oxide and 130 parts by weight of acetylacetone into a reaction kettle, heating to a reflux state, stirring for 8-10 hours, and then reducing the pressure at 140-150 ℃ for 2 hours.
Example 3
A low-odor coated dealcoholized transparent flowing sealant for electronic and electric appliances comprises the following raw materials in parts by weight: 90-100 parts of alkoxy modified polydimethylsiloxane, 10-20 parts of reinforcing filler, 10-20 parts of plasticizer, 4-9 parts of cross-linking agent, 0.5-2 parts of stabilizer, 0.1-0.5 part of catalyst and 1-3 parts of coupling agent;
the preparation method comprises the following steps:
s1: putting alkoxy modified polydimethylsiloxane and plasticizer into a planetary stirrer, adding reinforcing filler, heating to 120 ℃, and carrying out reduced pressure reduction stirring for 2 hours under the vacuum environment of-0.09 Mpa, wherein the stirring speed is 1000-1200 rpm;
s2: after cooling, the cross-linking agent, the stabilizing agent, the catalyst and the coupling agent are sequentially added, and the mixture is stirred for 50min at the rotating speed of 600rpm of 300-.
Further, the alkoxy modified polydimethylsiloxane adopts triethoxysilylethylene-terminated polydimethylsiloxane B;
the preparation method of triethoxysilyethylene end-blocked polydimethylsiloxane B is as follows: putting 1000 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 3 ten thousand mPas and 3-5 parts by weight of tetramethyldisilazane into a stirrer, heating to 50-70 ℃ under the protection of nitrogen, adding 0.5-1 part by weight of acetic acid, stirring for 1-2 hours under the protection of nitrogen, adding 15-20 parts by weight of vinyltriethoxysilane and 2 parts by weight of platinum-vinyl siloxane complex with the platinum mass fraction of 0.5%, and finally reacting for 3 hours at 60-80 ℃ to obtain triethoxysilylethylene-terminated polydimethylsiloxane.
Furthermore, the reinforcing filler adopts hydrophilic fumed silica with the specific surface area of 150m2/g, so that the requirements on the transparency and the mechanical property of the product can be met, and the product cost can be well controlled.
Furthermore, the plasticizer adopts dimethyl-terminated polydimethylsiloxane, mainly reduces the viscosity of the rubber material, improves the construction performance, improves the usability of the used sealant, has good compatibility with the base rubber, and improves the fluidity and the construction performance of the product.
Furthermore, the cross-linking agent is vinyl triethoxysilane.
Further, the stabilizer adopts alpha-trimethoxysilyl ethyl propionate;
the preparation method of the alpha-trimethoxysilylethyl propionate comprises the following steps: adding 122 parts by weight of trimethoxy silane, 100 parts of ethyl acrylate and 1 part by weight of platinum-vinyl siloxane complex with platinum mass fraction of 0.3% into a reaction kettle, reacting for 4-12 hours at 50-60 ℃ under the protection of nitrogen, then heating to 80 ℃, and reducing pressure for 1 hour under the vacuum degree of-0.01 Mpa to obtain the stabilizer of the alpha-trimethoxy silicon-based ethyl propionate.
Further, the coupling agent adopts a compound C;
the preparation method of the compound C comprises the following steps: putting 555 parts by weight of gamma-aminopropyltriethoxysilane, 205 parts by weight of 3-isocyanatopropyltrimethoxysilane and 237 parts by weight of 3-glycidoxypropyltrimethoxysilane into a reaction kettle, stirring for 2-4 hours under the protection of nitrogen, heating to 100-120 ℃, and reducing the temperature for 1-3 hours under the vacuum degree of-0.09 Mpa.
Further, the catalyst adopts a composition B;
the preparation method of the composition B comprises the following steps: adding 100 parts by weight of dioctyltin dilaurate and 200-600 parts by weight of tetraethoxysilane into a reaction kettle, heating to a reflux state, stirring for 3-6 hours, and then reducing the pressure at 160-180 ℃ for 2 hours.
Test example
And (3) testing groups: example 1, example 2, example 3, comparative example (same type of product common on the market);
the test contents are as follows: the 4 products were tested for curing time, heat resistance, bond strength, and light transmission attenuation (mild degree of 30 mW/cm) 2 Irradiating for 3 hours by using ultraviolet light, and measuring the light transmission attenuation rate);
and (3) testing results:
according to the test result, the data of the invention are superior to those of a comparison document, the invention has the advantages of excellent transparency, lower smell and good yellowing resistance, the storage stability of the invention reaches more than half a year, meanwhile, the invention hardly has corrosivity to most base materials, the adaptability of the base materials is wide, and most related application requirements on the market can be met.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.
Claims (8)
1. The low-odor coated dealcoholized transparent flowing sealant for the electronic and electric appliances is characterized by comprising the following raw materials in parts by weight: 80-120 parts of alkoxy modified polydimethylsiloxane, 10-20 parts of reinforcing filler, 5-30 parts of plasticizer, 3-10 parts of cross-linking agent, 0.5-4 parts of stabilizer, 0.1-0.5 part of catalyst and 0.5-2.5 parts of coupling agent;
the preparation method comprises the following steps:
s1: putting alkoxy modified polydimethylsiloxane and plasticizer into a planetary stirrer, adding reinforcing filler, heating to 120 ℃, and carrying out reduced pressure reduction stirring for 2 hours under the vacuum environment of-0.09 Mpa, wherein the stirring speed is 1000-1200 rpm;
s2: after cooling, the cross-linking agent, the stabilizing agent, the catalyst and the coupling agent are sequentially added, and the mixture is stirred for 50min at the rotating speed of 600rpm of 300-.
2. The low-odor batch-type dealcoholized transparent trickling sealant for electronic and electric appliances according to claim 1, wherein the alkoxy-modified polydimethylsiloxane is any one of triethoxysilyethylene-terminated polydimethylsiloxane A, trimethoxy-terminated modified polydimethylsiloxane and triethoxysilyethylene-terminated polydimethylsiloxane B;
the preparation method of triethoxysilyethylene end-blocked polydimethylsiloxane A is as follows: putting 1000 parts by weight of hydrogen-terminated polydimethylsiloxane with the viscosity of 2 ten thousand mPas, 20 parts by weight of vinyl triethoxysilane and 0.5 part by weight of platinum-vinyl siloxane complex with the mass fraction of 0.3% into a stirrer, and reacting for 1 hour at the temperature of 60-70 ℃;
the preparation method of the trimethoxy end-capped modified polydimethylsiloxane comprises the following steps: putting 1000 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 1 ten thousand mPas and 25 parts by weight of alpha-trimethoxysilylethyl propionate into a stirrer, reacting for 8 hours at 80-100 ℃ under the protection of nitrogen, and then reducing the pressure for 1 hour under the environment of 130 ℃ and the vacuum degree of-0.09 MPa to obtain the product;
the preparation method of triethoxysilyethylene end-blocked polydimethylsiloxane B is as follows: putting 1000 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 3 ten thousand mPas and 3-5 parts by weight of tetramethyldisilazane into a stirrer, heating to 50-70 ℃ under the protection of nitrogen, then adding 0.5-1 part by weight of acetic acid, stirring for 1-2 hours under the protection of nitrogen, then adding 15-20 parts by weight of vinyltriethoxysilane and 2 parts by weight of platinum-vinylsiloxane complex with the mass fraction of 0.5%, and finally reacting for 3 hours at 60-80 ℃ to obtain the catalyst.
3. The low gas for electronic and electric appliances according to claim 1The odor batch dealcoholization transparent flowing sealant is characterized in that the reinforcing filler adopts the sealant with the specific surface area of 150-200 m 2 The hydrophilic fumed silica/g.
4. The low odor batch-type dealcoholized clear flow sealant for electronic and electrical appliances according to claim 1, wherein the plasticizer is any one of dimethyl terminated polydimethylsiloxane, single end alkoxy polydimethylsiloxane, MDT silicone oil and paraffin mixture.
5. The low-odor batch-type dealcoholized transparent trickling sealant for electronic and electric appliances according to claim 1, wherein the cross-linking agent is any one of dimethyldimethoxysilane, dimethyldiethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane or hydrolyzed oligomer thereof, polymethyltriethoxysilane, tetraethoxysilane or oligomer thereof, n-propyl silicate or oligomer thereof, and tetramethoxysilane or oligomer thereof.
6. The low-odor batch-type dealcoholized transparent flowing sealant for the electronic and electric appliances as claimed in claim 1, wherein the stabilizer is any one of alpha-trimethoxysilylethyl propionate and high-activity polyalkoxysilane;
the preparation method of the alpha-trimethoxysilylethyl propionate comprises the following steps: adding 122 parts by weight of trimethoxy silane, 100 parts of ethyl acrylate and 1 part by weight of platinum-vinyl siloxane complex with platinum mass fraction of 0.3% into a reaction kettle, reacting for 4-12 hours at 50-60 ℃ under the protection of nitrogen, then heating to 80 ℃, and reducing pressure and removing for 1 hour under the vacuum degree of-0.01 Mpa;
the preparation method of the high-activity polyalkoxysilane is as follows: adding 122 parts by weight of triethoxy hydrosilane, 226 parts by weight of vinyl tri (isopropenylpropoxy) silane and 0.5 part by weight of platinum-vinyl siloxane complex with the platinum mass fraction of 0.3% into a reaction kettle, and reacting for 2-4 hours at 40-60 ℃ under the protection of nitrogen.
7. The low-odor batch-type dealcoholized transparent flowing sealant for the electronic and electric appliances as claimed in claim 1, wherein the coupling agent is any one of a compound A, a compound B and a compound C;
the preparation method of the compound A comprises the following steps: adding 150 parts by weight of gamma-aminopropyltrimethoxysilane, 200 parts by weight of 3-glycidoxypropyltrimethoxysilane and 100 parts by weight of 3- (methacryloyloxy) propyltrimethoxysilane into a reaction kettle, reacting for 12-48 hours at 80-100 ℃ under the protection of nitrogen, and then heating to 120-130 ℃ for removing the low temperature for 4-8 hours to obtain the product;
the preparation method of the compound B comprises the following steps: putting 108 parts by weight of gamma-aminopropyltrimethoxysilane, 69 parts by weight of allyl glycidyl ether and 137 parts by weight of methyl orthosilicate into a reaction kettle, reacting for 2-4 hours at 80-110 ℃ under the protection of nitrogen, and then heating to 150-180 ℃ for removing the aluminum hydroxide for 2-4 hours;
the preparation method of the compound C comprises the following steps: putting 555 parts by weight of gamma-aminopropyltriethoxysilane, 205 parts by weight of 3-isocyanatopropyltrimethoxysilane and 237 parts by weight of 3-glycidoxypropyltrimethoxysilane into a reaction kettle, stirring for 2-4 hours under the protection of nitrogen, heating to 100-120 ℃, and reducing the temperature for 1-3 hours under the vacuum degree of-0.09 Mpa.
8. The low odor batch-type dealcoholized clear flow sealant for electronic and electrical appliances according to claim 1, wherein the catalyst is any one of composition a and composition B;
the preparation method of the composition A comprises the following steps: adding 41 parts by weight of dibutyltin oxide and 130 parts by weight of acetylacetone into a reaction kettle, heating to a reflux state, stirring for 8-10 hours, and then reducing the pressure at 140-150 ℃ for 2 hours.
The preparation method of the composition B comprises the following steps: adding 100 parts by weight of dioctyltin dilaurate and 200-600 parts by weight of tetraethoxysilane into a reaction kettle, heating to a reflux state, stirring for 3-6 hours, and then decompressing and reducing at 160-180 ℃ for 2 hours.
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