CN115895587A - Alcohol-type silicone sealant capable of quickly eliminating thin layer adhesion and preparation method thereof - Google Patents
Alcohol-type silicone sealant capable of quickly eliminating thin layer adhesion and preparation method thereof Download PDFInfo
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- CN115895587A CN115895587A CN202211716622.5A CN202211716622A CN115895587A CN 115895587 A CN115895587 A CN 115895587A CN 202211716622 A CN202211716622 A CN 202211716622A CN 115895587 A CN115895587 A CN 115895587A
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- type silicone
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- 239000004590 silicone sealant Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 14
- -1 polysiloxane Polymers 0.000 claims abstract description 27
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000077 silane Inorganic materials 0.000 claims abstract description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 5
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 5
- 239000011256 inorganic filler Substances 0.000 claims abstract description 5
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 5
- 239000013464 silicone adhesive Substances 0.000 claims abstract description 4
- 239000012974 tin catalyst Substances 0.000 claims abstract description 4
- UMUXBDSQTCDPJZ-UHFFFAOYSA-N chromium titanium Chemical compound [Ti].[Cr] UMUXBDSQTCDPJZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 20
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- KXJLGCBCRCSXQF-UHFFFAOYSA-N [diacetyloxy(ethyl)silyl] acetate Chemical compound CC(=O)O[Si](CC)(OC(C)=O)OC(C)=O KXJLGCBCRCSXQF-UHFFFAOYSA-N 0.000 claims description 11
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims description 5
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 5
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 5
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 4
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical group CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000013522 chelant Substances 0.000 claims description 4
- WIEGKKSLPGLWRN-UHFFFAOYSA-N ethyl 3-oxobutanoate;titanium Chemical compound [Ti].CCOC(=O)CC(C)=O WIEGKKSLPGLWRN-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 3
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 3
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 3
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004898 kneading Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 claims description 2
- 229960003493 octyltriethoxysilane Drugs 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 2
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 claims description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 claims 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims 1
- 125000005474 octanoate group Chemical group 0.000 claims 1
- 229910021487 silica fume Inorganic materials 0.000 claims 1
- 239000000454 talc Substances 0.000 claims 1
- 229910052623 talc Inorganic materials 0.000 claims 1
- 239000000565 sealant Substances 0.000 abstract description 12
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 23
- 238000012360 testing method Methods 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 238000010998 test method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 239000003566 sealing material Substances 0.000 description 4
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 3
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 description 2
- 239000004636 vulcanized rubber Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- NVJMGQMXNBBZIU-UHFFFAOYSA-N dibutyltin;1-dodecylsulfanyldodecane Chemical compound CCCC[Sn]CCCC.CCCCCCCCCCCCSCCCCCCCCCCCC NVJMGQMXNBBZIU-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Sealing Material Composition (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to an alcohol-type silicone sealant capable of quickly eliminating viscosity of a thin layer and a preparation method thereof, wherein the sealant comprises the following raw materials: 100 portions of dihydroxy polysiloxane, 80 to 150 portions of inorganic filler, 2 to 8 portions of silane cross-linking agent, 2 to 8 portions of titanium chromium compound, 0.5 to 2 portions of silane coupling agent, 0.5 to 2 portions of viscosity-breaking accelerant and 0.1 to 0.5 portion of organic tin catalyst. The dealcoholized silicone adhesive for quickly eliminating the adhesive of the thin layer not only accelerates the thin layer curing and eliminating speed of the sealant, but also keeps good mechanical properties such as elongation and the like, and has particularly remarkable effect of improving the processing efficiency of a door and window processing factory.
Description
Technical Field
The invention belongs to the technical field of sealants, and particularly relates to an alcohol-type silicone sealant capable of quickly eliminating viscosity of a thin layer and a preparation method thereof.
Background
The existing alcohol-type silicone sealant basically has slower tack-eliminating, most of the sealant needs more than 6 hours, some of the sealant can reach 4 hours, and particularly when the relative humidity is more than 85 percent, the tack-eliminating of the sealant is slow, thereby seriously affecting the construction performance.
In the field of door and window processing and decoration and finishing application, the sealant at the edge part of a glue seam is very thin, a certain amount of sealant is remained and hung at the edge part of a metal material, the part of the sealant is thinner, when the relative humidity is more than 85 percent RH (relative humidity), the part of the sealant is difficult to completely eliminate the adhesive within 12 to 24 hours, and a small amount of adhesive marks are left when the part of the sealant is touched by hands or even pressed by hands to have marks. Certain influences are caused to the use efficiency and the user experience.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an alcohol-type silicone sealant capable of realizing quick tack-free.
The invention also provides a preparation method of the alcohol-type silicone sealant.
The technical scheme adopted for realizing the aim of the invention is as follows:
the alcohol-type silicone sealant capable of quickly eliminating the viscosity of the thin layer is characterized by comprising the following raw materials in parts by weight:
the viscosity of the dihydroxy polysiloxane at 25 ℃ is 8-200Pa.s.
The inorganic filler is at least one of nano active calcium carbonate, heavy calcium carbonate, silicon micropowder, diatomite, kaolin and talcum powder.
The silane cross-linking agent is one of methyltrimethoxysilane, methyltriethoxysilane, polymethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, octyltrimethoxysilane and octyltriethoxysilane.
The titanium complex is at least one of ethyl acetoacetate titanium chelate, tetraisopropyl di (dioctyl phosphite acyloxy) titanate, di (acetylacetone) diisopropyl titanate, tetra (ethyl) titanate, butyl titanate and isopropyl titanate.
The silane coupling agent is at least two of chloropropyl trimethoxy silane, chloropropyl triethoxy silane, gamma-aminopropyl trimethoxy silane, gamma-aminopropyl triethoxy silane, gamma-glycidoxypropyl trimethoxy silane, gamma-glycidoxypropyl triethoxy silane, epoxypropyltrimethoxy silane and epoxypropyltriethoxy silane.
The viscosity-breaking accelerant is a product obtained by mutually polymerizing N-beta aminoethyl gamma-aminopropyltriethoxysilane, beta- (3, 4 epoxy cyclohexyl) -ethyltriethoxysilane and ethyltriacetoxysilane at the temperature of 80-100 ℃, and the mass ratio of the N-beta aminoethyl gamma-aminopropyltriethoxysilane, the beta- (3, 4 epoxy cyclohexyl) -ethyltriethoxysilane to the ethyltriacetoxysilane is 1.5: 1.
The organic tin catalyst is at least one of dibutyltin dilaurate, dibutyltin diacetate, dioctyltin dilaurate, dibutyltin didodecyl sulfide and stannous octoate.
The preparation method of the rapid-debonding thin-layer debonding dealcoholization type silicone adhesive comprises the following steps:
1) And (3) synthesis of the viscosity-reducing accelerant: putting N-beta aminoethyl gamma-aminopropyltriethoxysilane, beta- (3, 4 epoxy cyclohexyl) -ethyltriethoxysilane and ethyltriacetoxysilane into a reaction container, mixing, and performing reflux reaction for 8 hours in a water bath at the reaction temperature of 80-100 ℃;
2) Adding dihydroxy polysiloxane and inorganic filler into a kneading machine, dehydrating and blending for 120-300min at the temperature of 100-150 ℃ and the vacuum degree of-0.08-0.10 MPa to prepare a base material;
3) Adding the prepared base material and silane cross-linking agent into a planetary machine or a high-speed dispersion stirrer at room temperature, and reacting for 20-60 min at the vacuum degree of-0.08-0.10 MPa and the rotating speed of 100-300 rpm; adding the titanium-chromium compound, the silane coupling agent, the adhesion-eliminating accelerant and the organic tin catalyst into the mixture, and reacting for 40-80 min at the vacuum degree of-0.08-0.10 MPa and the rotating speed of 100-300 rpm to obtain the rapid thin-layer adhesion-eliminating alcohol type silicone sealant.
The dealcoholized silicone adhesive for quickly eliminating the adhesive of the thin layer not only accelerates the thin layer curing and eliminating speed of the sealant, but also keeps good mechanical properties such as elongation and the like, and has particularly remarkable effect of improving the processing efficiency of a door and window processing factory.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples, but the scope of the present invention is not limited thereto. The embodiments described below are only a part of the embodiments of the present invention, and not all embodiments, and all other similar embodiments performed by those skilled in the art without inventive work are within the scope of the present invention.
The viscosity in the invention refers to the viscosity under the test condition of 25 ℃.
In the following examples, "parts" means parts by weight unless otherwise specified.
Example 1
The embodiment provides a quick thin-layer adhesive-removal dealcoholized silicone sealant, and the preparation method comprises the following steps:
(1) And (3) synthesis of the viscosity-reducing accelerant: beta-aminoethyl gamma-aminopropyltriethoxysilane, beta- (3, 4-epoxycyclohexyl) -ethyltriethoxysilane, and ethyltriacetoxysilane (in a mass ratio of 1.5: 1) are added into a reaction vessel, the reaction vessel is placed in a water bath, and a reflux device is installed, and the reaction is carried out for 8 hours under the condition of heating to 90 ℃.
(2) 100 parts of dihydroxy polysiloxane, 80 parts of nano calcium carbonate and 50 parts of ground calcium carbonate are added into a kneader, and are dehydrated and blended for 120min at the temperature of 120 ℃ and the vacuum degree of-0.085 MPa to prepare the base material.
(3) At room temperature, adding the prepared base material and 6 parts of methyltrimethoxysilane into a planetary machine or a high-speed dispersion stirrer, and stirring for 40min at the vacuum degree of-0.095 MPa and the rotating speed of 200 rpm; 5 parts of ethyl acetoacetate titanium chelate, 1 part of gamma-aminopropyltriethoxysilane, 0.5 part of gamma-glycidyl ether oxypropyltriethoxysilane, 1 part of viscosity-breaking accelerator and 0.2 part of dibutyltin dilaurate are added, and stirred for 60min at the rotating speed of 200rpm and the vacuum degree of-0.095 MPa to prepare the rapid thin-layer viscosity-breaking alcohol type silicone sealant, wherein the performance indexes of the product are shown in Table 1.
Example 2
The embodiment provides a rapid thin-layer anti-sticking dealcoholization type silicone sealant, and the preparation method comprises the following steps:
(1) Synthesis of the adhesion-removing accelerant: the beta aminoethyl gamma-aminopropyl triethoxysilane, beta- (3, 4 epoxycyclohexyl) -ethyl triethoxysilane and ethyl triacetoxysilane (in a mass ratio of 1.5: 1) are put into a reaction vessel, the reaction vessel is placed in a water bath kettle and is provided with a reflux device, the temperature is heated to 90 ℃, and the reaction is carried out for 8 hours.
(2) 100 parts of dihydroxy polysiloxane, 80 parts of nano calcium carbonate and 50 parts of diatomite are added into a kneader, and are dehydrated and blended for 200min at the temperature of 120 ℃ and the vacuum degree of-0.085 MPa to prepare the base material.
(3) At room temperature, adding the prepared base material and 6 parts of methyltrimethoxysilane into a planetary machine or a high-speed dispersion stirrer, and stirring for 40min at the vacuum degree of-0.095 MPa and the rotating speed of 200 rpm; 5 parts of ethyl acetoacetate titanium chelate, 1 part of gamma-aminopropyltriethoxysilane, 0.5 part of gamma-glycidyl ether oxypropyltriethoxysilane, 1.5 parts of adhesion promoter and 0.2 part of dibutyltin dilaurate are added, and stirred for 60min at the rotating speed of 200rpm and the vacuum degree of-0.095 MPa to prepare the rapid thin-layer adhesion-removing alcohol type silicone sealant, wherein the performance index of the product is shown in Table 1.
Example 3
The embodiment provides a fast thin-layer anti-tack alcohol type silicone sealant, and the preparation method comprises the following steps:
(1) And (3) synthesis of the viscosity-reducing accelerant: the beta aminoethyl gamma-aminopropyl triethoxysilane, beta- (3, 4 epoxycyclohexyl) -ethyl triethoxysilane and ethyl triacetoxysilane (in a mass ratio of 1.5: 1) are put into a reaction vessel, the reaction vessel is placed in a water bath kettle and is provided with a reflux device, the temperature is heated to 90 ℃, and the reaction is carried out for 8 hours.
(2) 100 parts of dihydroxy polysiloxane, 80 parts of nano calcium carbonate and 30 parts of talcum powder are added into a kneader, and the mixture is dehydrated and blended for 300min at the temperature of 120 ℃ and the vacuum degree of-0.085 MPa to prepare the base material.
(3) At room temperature, adding the prepared base material and 5 parts of methyltrimethoxysilane into a planetary machine or a high-speed dispersion stirrer, and stirring for 40min at the vacuum degree of-0.095 MPa and the rotating speed of 200 rpm; 4 parts of diisopropyl di (acetylacetonate) titanate, 1 part of chloropropyl trimethoxyl silane, 0.5 part of gamma-glycidyl ether oxypropyl triethoxysilane, 1 part of a viscosity-breaking accelerant and 0.2 part of dibutyltin diacetate are added and stirred for 60min at the vacuum degree of-0.095 MPa and the rotating speed of 200rpm to prepare the rapid thin-layer viscosity-breaking alcohol type silicone sealant, and the performance index of the product is shown in table 1.
Example 4
The embodiment provides a rapid thin-layer anti-sticking dealcoholization type silicone sealant, and the preparation method comprises the following steps:
(1) And (3) synthesis of the viscosity-reducing accelerant: the beta aminoethyl gamma-aminopropyl triethoxysilane, beta- (3, 4 epoxycyclohexyl) -ethyl triethoxysilane and ethyl triacetoxysilane (in a mass ratio of 1.5: 1) are put into a reaction vessel, the reaction vessel is placed in a water bath kettle and is provided with a reflux device, the temperature is heated to 90 ℃, and the reaction is carried out for 8 hours.
(2) 100 parts of dihydroxy polysiloxane, 80 parts of nano calcium carbonate and 30 parts of talcum powder are added into a kneader, and dehydrated and blended for 250min at the temperature of 120 ℃ and the vacuum degree of-0.085 MPa to prepare the base material.
(3) At room temperature, adding the prepared base material and 5 parts of methyltrimethoxysilane into a planetary machine or a high-speed dispersion stirrer, and stirring for 40min at the vacuum degree of-0.095 MPa and the rotating speed of 200 rpm; 4 parts of diisopropyl di (acetylacetonate) titanate, 1 part of chloropropyl trimethoxyl silane, 0.5 part of gamma-glycidyl ether oxypropyl triethoxysilane, 1.5 parts of a viscosity-breaking accelerator and 0.2 part of dibutyltin diacetate are added, and stirred for 60min at the vacuum degree of-0.095 MPa and the rotating speed of 200rpm to prepare the rapid thin-layer viscosity-breaking alcohol type silicone seal, wherein the performance index of the product is shown in Table 1.
Example 5
The embodiment provides a fast thin-layer anti-tack alcohol type silicone sealant, and the preparation method comprises the following steps:
(1) And (3) synthesis of the viscosity-reducing accelerant: the beta aminoethyl gamma-aminopropyl triethoxysilane, beta- (3, 4 epoxycyclohexyl) -ethyl triethoxysilane and ethyl triacetoxysilane (in a mass ratio of 1.5: 1) are put into a reaction vessel, the reaction vessel is placed in a water bath kettle and is provided with a reflux device, the temperature is heated to 90 ℃, and the reaction is carried out for 8 hours.
(2) 100 parts of dihydroxy polysiloxane and 90 parts of nano calcium carbonate are added into a kneader, and are dehydrated and blended for 150min at the temperature of 120 ℃ and the vacuum degree of-0.085 MPa to prepare the base material.
(3) At room temperature, adding the prepared base material and 4 parts of methyltriethoxysilane into a planetary machine or a high-speed dispersion stirrer, and stirring for 40min at the vacuum degree of-0.095 MPa and the rotating speed of 200 rpm; 3 parts of butyl titanate, 1 part of gamma-aminopropyltriethoxysilane, 0.5 part of gamma-glycidyl ether oxypropyltrimethoxysilane, 1 part of a viscosity-breaking accelerator and 0.2 part of dioctyltin dilaurate are added, and stirred for 60min at the rotating speed of 200rpm and the vacuum degree of-0.095 MPa to prepare the rapid thin-layer viscosity-breaking alcohol type silicone sealant, wherein the performance index of the product is shown in Table 1.
Example 6
The embodiment provides a rapid thin-layer anti-sticking dealcoholization type silicone sealant, and the preparation method comprises the following steps:
(1) Synthesis of the adhesion-removing accelerant: the beta aminoethyl gamma-aminopropyl triethoxysilane, beta- (3, 4 epoxy cyclohexyl) -ethyl triethoxysilane and ethyl triacetoxysilane (in the mass ratio of 1.5: 1) are put into a reaction vessel, the reaction vessel is placed in a water bath, a reflux device is installed, the temperature is heated to 90 ℃, and the reaction is carried out for 8 hours.
(2) 100 parts of dihydroxy polysiloxane and 90 parts of nano calcium carbonate are added into a kneader, and are dehydrated and blended for 120-300min at the temperature of 120 ℃ and the vacuum degree of-0.085 MPa to prepare the base material.
(3) Adding the prepared base material and 4 parts of methyltriethoxysilane into a planetary machine or a high-speed dispersion stirrer at room temperature, and stirring for 40min at the vacuum degree of-0.095 MPa and the rotating speed of 200 rpm; 3 parts of butyl titanate, 1 part of gamma-aminopropyltriethoxysilane, 0.5 part of gamma-glycidyl ether oxypropyltrimethoxysilane, 1.5 parts of a viscosity-breaking accelerator and 0.2 part of dioctyltin dilaurate are added, and stirred for 60min at the rotating speed of 200rpm and the vacuum degree of-0.095 MPa to prepare the rapid thin-layer viscosity-breaking alcohol type silicone sealant, wherein the performance index of the product is shown in Table 1.
Comparative example 1
The comparative example provides an alcohol-type silicone sealant, the preparation method of which comprises the following steps:
(1) 100 parts of dihydroxy polysiloxane, 80 parts of nano calcium carbonate and 30 parts of talcum powder are added into a kneader, and the mixture is dehydrated and blended for 300min at the temperature of 120 ℃ and the vacuum degree of-0.085 MPa to prepare the base material.
(2) At room temperature, adding the prepared base material and 5 parts of methyltrimethoxysilane into a planetary machine or a high-speed dispersion stirrer, and stirring for 40min at the vacuum degree of-0.095 MPa and the rotating speed of 200 rpm; 4 parts of diisopropyl di (acetylacetonate) titanate, 1 part of chloropropyltrimethoxysilane, 0.5 part of gamma-glycidyl ether oxypropyltriethoxysilane and 0.2 part of dibutyltin diacetate are added, and the mixture is stirred for 60min at the rotating speed of 200rpm and the vacuum degree of-0.095 MPa, and the product performance index is shown in table 1.
Comparative example 2
The preparation method of the alcohol-type silicone sealant comprises the following steps:
(1) 100 parts of dihydroxy polysiloxane, 80 parts of nano calcium carbonate and 30 parts of ground calcium carbonate are added into a kneader, and are dehydrated and blended for 120-300min at the temperature of 120 ℃ and the vacuum degree of-0.085 MPa to prepare the base material.
(2) At room temperature, adding the prepared base material and 5 parts of methyltrimethoxysilane into a planetary machine or a high-speed dispersion stirrer, and stirring for 40min at the vacuum degree of-0.095 MPa and the rotating speed of 200 rpm; 4 parts of isopropyl titanate, 1 part of gamma-aminopropyl triethoxysilane, 0.5 part of gamma-glycidyl ether oxypropyl triethoxysilane and 0.4 part of dibutyltin dilaurate are added, and the mixture is stirred for 60min at the rotation speed of 200rpm and the vacuum degree of-0.095 MPa to prepare the alcohol-type silicone sealant, wherein the performance index of the product is shown in table 1.
The instant thin-layer tack-free alcohol-type silicone sealants prepared in examples 1 to 6 and the silicone sealants prepared in comparative examples 1 to 2 were subjected to the following thin-layer tack-free and mechanical property tests:
and (3) testing conditions are as follows: 15 ℃,85% RH humidity.
The thin layer anti-sticking test method comprises the following steps:
1. extruding the glue to be tested on a polyethylene film to form a glue strip, and scraping the glue strip into a thin sheet (the thickness is within 0.3 mm); .
2. After surface drying (surface drying is tested by adopting a 13477.5-2002 building sealing material test method), testing and viscosity breaking are carried out by adopting a 13477.5-2002 building sealing material test method A; in the process of removing the polyethylene film, the test piece is not taken away from the surface of the object on which the test piece is placed, the thin adhesive layer is determined to be tack-free, and the time is recorded as tack-free time test results shown in table 1.
Tensile strength: the test is carried out according to GB/T13477 & lt test method for building sealing materials & gt and GB/T528 & lt determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber & gt.
Maximum strength elongation: the test is carried out according to GB/T13477 'test method for building sealing materials' and GB/T528 'determination for tensile stress strain performance of vulcanized rubber or thermoplastic rubber'.
TABLE 1
It can be seen from table 1 that the tensile strength and the elongation at maximum strength are both significantly improved after the adhesion-breaking promoter is added, and especially the thin layer adhesion-breaking is significantly improved.
Claims (9)
1. The alcohol-type silicone sealant capable of quickly eliminating the viscosity of the thin layer is characterized by comprising the following raw materials in parts by weight:
2. the rapid thin layer detackifying alcohol silicone sealant according to claim 1 wherein the dihydroxy polysiloxane has a viscosity of 8 to 200pa.s at 25 ℃.
3. The fast thin-layer detackifying alcohol-type silicone sealant according to claim 1 wherein the inorganic filler is at least one of nano-calcium carbonate, ground calcium carbonate, silica fume, diatomaceous earth, kaolin, talc.
4. The fast thin-layer detackifying alcohol-type silicone sealant according to claim 1 wherein the silane crosslinking agent is one of methyltrimethoxysilane, methyltriethoxysilane, polymethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, octyltrimethoxysilane, octyltriethoxysilane.
5. The fast thin-layer detackifying alcohol-type silicone sealant according to claim 1 wherein the titanium complex is at least one of titanium ethyl acetoacetate chelate, tetraisopropyl bis (dioctylphosphite-yloxy) titanate, diisopropyl bis (acetylacetonate) titanate, ethyl (tetra) titanate, butyl titanate, and isopropyl titanate.
6. The fast thin-layer detackifying alcohol-type silicone sealant according to claim 1 wherein the silane coupling agent is at least two of chloropropyltrimethoxysilane, chloropropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, glycidoxypropyltrimethoxysilane, glycidoxypropyltriethoxysilane.
7. The rapid thin layer detackifying alcohol-based silicone sealant as claimed in claim 1 in which said detackifying promoter is N- β aminoethyl γ -aminopropyltriethoxysilane, β - (3, 4 epoxycyclohexyl) -ethyltriethoxysilane and ethyltriacetoxysilane which are polymerized with one another at 80-100 ℃ in a mass ratio of 1.5: 1.
8. The rapid thin-layer detackifying alcohol-type silicone sealant according to claim 1 wherein the organotin catalyst is at least one of dibutyltin dilaurate, dibutyltin diacetate, dioctyltin dilaurate, dibutyltin bis (dodecylthio) octoate.
9. A method for preparing the fast-detackifying thin-layer detackifying dealcoholizing type silicone adhesive as claimed in any one of claims 1 to 8, comprising the steps of:
1) And (3) synthesis of the viscosity-reducing accelerant: putting N-beta aminoethyl gamma-aminopropyltriethoxysilane, beta- (3, 4 epoxy cyclohexyl) -ethyltriethoxysilane and ethyltriacetoxysilane into a reaction container, mixing, and performing reflux reaction for 8 hours in a water bath at the reaction temperature of 80-100 ℃;
2) Adding dihydroxy polysiloxane and inorganic filler into a kneading machine, dehydrating and blending for 120-300min at the temperature of 100-150 ℃ and the vacuum degree of-0.08-0.10 MPa to prepare a base material;
3) At room temperature, adding the prepared base material and the silane crosslinking agent into a planetary machine or a high-speed dispersion stirrer, and reacting for 20-60 min at the vacuum degree of-0.08 to-0.10 MPa and the rotating speed of 100-300 rpm; adding the titanium-chromium compound, the silane coupling agent, the adhesion-eliminating accelerant and the organic tin catalyst into the mixture, and reacting for 40-80 min at the vacuum degree of-0.08-0.10 MPa and the rotating speed of 100-300 rpm to obtain the rapid thin-layer adhesion-eliminating alcohol type silicone sealant.
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| US4395526A (en) * | 1981-06-26 | 1983-07-26 | General Electric Company | One package, stable, moisture curable, polyalkoxy-terminated organopolysiloxane compositions and method for making |
| US4489199A (en) * | 1983-08-08 | 1984-12-18 | General Electric Company | Room temperature vulcanizable organopolysiloxane compositions |
| US4680364A (en) * | 1985-06-18 | 1987-07-14 | General Electric Company | Room temperature vulcanizable silicone compositions having improved adhesion |
| WO2016030185A1 (en) * | 2014-08-25 | 2016-03-03 | Wacker Chemie Ag | Fast curing condensation rtv silicone rubber in bonding application |
| US20190194508A1 (en) * | 2017-12-26 | 2019-06-27 | Nano And Advanced Materials Institute Limited | Room temperature curable polyoranopolysloxane silicone sealant composition, the silicone sealant and method for preparing thereof |
| CN111253907A (en) * | 2020-04-08 | 2020-06-09 | 山东飞度胶业科技股份有限公司 | Environment-friendly alcohol-type adhesive for silicone and modified silicone sealant and preparation method thereof |
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| US4395526A (en) * | 1981-06-26 | 1983-07-26 | General Electric Company | One package, stable, moisture curable, polyalkoxy-terminated organopolysiloxane compositions and method for making |
| US4489199A (en) * | 1983-08-08 | 1984-12-18 | General Electric Company | Room temperature vulcanizable organopolysiloxane compositions |
| US4680364A (en) * | 1985-06-18 | 1987-07-14 | General Electric Company | Room temperature vulcanizable silicone compositions having improved adhesion |
| WO2016030185A1 (en) * | 2014-08-25 | 2016-03-03 | Wacker Chemie Ag | Fast curing condensation rtv silicone rubber in bonding application |
| US20190194508A1 (en) * | 2017-12-26 | 2019-06-27 | Nano And Advanced Materials Institute Limited | Room temperature curable polyoranopolysloxane silicone sealant composition, the silicone sealant and method for preparing thereof |
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