CN108753198B - Adhesion promoter for silicone sealant, preparation method of adhesion promoter, silicone sealant applied to ballastless track and preparation method of silicone sealant - Google Patents

Adhesion promoter for silicone sealant, preparation method of adhesion promoter, silicone sealant applied to ballastless track and preparation method of silicone sealant Download PDF

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CN108753198B
CN108753198B CN201810516791.1A CN201810516791A CN108753198B CN 108753198 B CN108753198 B CN 108753198B CN 201810516791 A CN201810516791 A CN 201810516791A CN 108753198 B CN108753198 B CN 108753198B
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silicone sealant
adhesion promoter
parts
stirring
diisocyanate
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CN108753198A (en
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艾九红
毛先安
柳培
宋文柱
谢静英
黄海康
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Zhuzhou Feilu High Tech Materials Co ltd
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Zhuzhou Feilu High Tech Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • C08G18/4825Polyethers containing two hydroxy groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/83Chemically modified polymers
    • C08G18/833Chemically modified polymers by nitrogen containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/83Chemically modified polymers
    • C08G18/837Chemically modified polymers by silicon containing compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate

Abstract

The invention discloses an adhesion promoter for silicone sealant, which comprises the following components in part by weight: r [ OCO-NH-R1‑NHCO‑NH‑R2‑Si‑(O‑N=CR3R4)3]n, wherein R is a group having [ CH ]2‑CH(CH3)‑O]An organic of repeating units; r1Represents a divalent alkyl or phenyl radical, R2Represents a divalent alkyl radical having at least 2 carbon atoms, R3And R4Respectively represent a straight chain or branched chain alkyl of 1 to 7 carbon atoms, and n is 2 or 3; also discloses a preparation method of the adhesion promoter and application of the adhesion promoter in silicone sealant. The adhesion promoter disclosed by the invention is applied to a silicone sealant of a ballastless track, so that the silicone sealant has good flexibility, elongation and viscosity, is good in adhesion with a concrete base material, and meets the requirement of waterproof sealing of a CRTS III ballastless track bridge deck caulking joint.

Description

Adhesion promoter for silicone sealant, preparation method of adhesion promoter, silicone sealant applied to ballastless track and preparation method of silicone sealant
Technical Field
The invention belongs to the field of sealants, and particularly relates to a silicone sealant applied to CRTS III type ballastless track bridge deck caulking, an adhesion promoter applied to the silicone sealant and a preparation method of the adhesion promoter.
Background
With the rapid development of the construction of a high-speed railway network, a ballastless track structure becomes a main track structure type adopted by the construction of high-speed railways in China. The CRTS III type ballastless track bridge deck system completely possessing independent intellectual property rights becomes a main technical standard system for construction of high-speed railways in China, and telescopic separation seams are required to be arranged at intervals of 6m on the base plate in the CRTS III type ballastless track bridge deck structure, so that the base plate structure can be normally stretched and deformed without cracking under the change of external temperature, and the sealing and the water prevention of the separation seams are one of protection methods for most effectively protecting the durability of a main prefabricated box girder.
At present, the main sealing materials on the market comprise asphalt, polyurethane and silicone, and the asphalt and polyurethane sealing materials have the defects of poor weather resistance, aging resistance, low temperature resistance and the like. The silicone sealant on the market has poor adhesion to a concrete material with a porous interface, and in order to reduce the viscosity of the silicone adhesive, a filler is additionally added to reduce the cost, a plasticizer silicone oil or white oil is added in the preparation of the silicone adhesive, and the addition of the plasticizer causes oil leakage to pollute a base material, so that the adhesion is reduced, particularly the white oil. Therefore, the sealing material cannot meet the sealing requirement of the ballastless track bridge deck caulking. Therefore, the development of the high-cohesiveness silicone sealant for the bridge deck caulking waterproofing of the CRTS III type ballastless track has very important practical significance.
Disclosure of Invention
The invention aims to solve the technical problems, overcome the defects and defects in the background technology and provide a bonding accelerator for a silicone sealant, a preparation method of the bonding accelerator, a high-cohesiveness silicone sealant meeting the requirement of CRTS III ballastless track bridge deck caulking waterproof sealing and a preparation method of the high-cohesiveness silicone sealant.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
an adhesion promoter for silicone sealants, the adhesion promoter having the structure:
R[OCO-NH-R1-NHCO-NH-R2-Si-(O-N=CR3R4)3]n,
wherein R is a group having [ CH ]2-CH(CH3)-O]An organic of repeating units;
R1represents a divalent alkyl or phenyl radical, R2Represents a divalent alkyl radical having at least 2 carbon atoms, R3And R4Respectively represent a straight chain or branched chain alkyl of 1 to 7 carbon atoms, and n is 2 or 3.
As a general inventive concept, the present invention also provides a preparation method of the above adhesion promoter for silicone sealant, comprising the steps of:
(1) selecting a compound having [ CH2-CH(CH3)-O]The polyoxypropylene polyol with a repeating unit structure is used as a raw material, the molecular weight is 2000-7000, and the functionality is 2 or 3;
(2) adding isocyanate into the polyoxypropylene polyol, and reacting for 2 hours at the temperature of 60-80 ℃, wherein the adding amount of the isocyanate is 2 times of that of-OH substances in the polyoxypropylene polyol to obtain a product A, and the product A is R- (OCO-NH-R1-NCO) n; the isocyanate structure is NCO-R1-NCO, specifically any one of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), Hexamethylene Diisocyanate (HDI), methylcyclohexyl diisocyanate (HTDI), dicyclohexyl methane diisocyanate (HMDI) and isophorone diisocyanate (IPDI), and further preferably TDI and MDI;
(3) adding amino alkoxy silane with the same mass as isocyanate into the product A to react at the temperature of not higher than 50 ℃ to obtain a product B, wherein the structure of the product B is R- (OCO-NH-R)1-NHCONHR2-Si-(OCH3)3) n or R- (OCO-NH-R)1-NHCONHR2-Si-(OCH2CH3)3) N, finally adding 3 times of the mass of HO-N ═ CR of amino alkoxy silane3R4Reacting at 120 ℃ for 2-3h, and distilling out low-boiling-point substances under reduced pressure after the reaction is finished to obtain the adhesion promoter; said HO-N ═ CR3R4Preferably one or more of methyl isobutyl ketoxime, dimethyl ketoxime, methyl ethyl ketoxime and methyl amyl ketoxime.
The other technical scheme of the invention is as follows: the silicone sealant applied to the ballastless track is mainly prepared from the following raw materials in parts by weight:
Figure BDA0001673501520000021
the silicone sealant is preferably characterized in that the adhesion promoter has the following structure:
R[OCO-NH-R1-NHCO-NH-R2-Si-(O-N=CR3R4)3]n,
wherein R is a group having [ C ]H2-CH(CH3)-O]Organic matter of repeating unit, R1Represents a divalent alkyl or phenyl radical, R2Represents a divalent alkyl radical having at least 2 carbon atoms, R3And R4Respectively represent a straight chain or branched chain alkyl of 1 to 7 carbon atoms, and n is 2 or 3.
In the above preparation method, preferably, the preparation method of the adhesion promoter is as follows:
(1) selecting a compound having [ CH2-CH(CH3)-O]The polyoxypropylene polyol with a repeating unit structure is used as a raw material, the molecular weight is 2000-7000, and the functionality is 2 or 3;
(2) adding isocyanate into the polyoxypropylene polyol, and reacting for 2 hours at the temperature of 60-80 ℃, wherein the adding amount of the isocyanate is 2 times of that of-OH substances in the polyoxypropylene polyol to obtain a product A, and the product A is R- (OCO-NH-R1-NCO) n; the isocyanate structure is NCO-R1-NCO, specifically any one of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), Hexamethylene Diisocyanate (HDI), methylcyclohexyl diisocyanate (HTDI), dicyclohexyl methane diisocyanate (HMDI) and isophorone diisocyanate (IPDI), and further preferably TDI and MDI;
(3) adding amino alkoxy silane with the same mass as isocyanate into the product A to react at the temperature of not higher than 50 ℃ to obtain a product B, wherein the structure of the product B is R- (OCO-NH-R)1-NHCONHR2-Si-(OCH3)3) n or R- (OCO-NH-R)1-NHCONHR2-Si-(OCH2CH3)3) N, finally adding 3 times of the mass of HO-N ═ CR of amino alkoxy silane3R4Reacting at 120 ℃ for 2-3h, and distilling out low-boiling-point substances under reduced pressure after the reaction is finished to obtain the adhesion promoter; said HO-N ═ CR3R4Preferably one or more of methyl isobutyl ketoxime, dimethyl ketoxime, methyl ethyl ketoxime and methyl amyl ketoxime.
The silicone sealant applied to the ballastless track adopts the low-viscosity ketoxime end-capped polymer containing polyether or polyether polyurethane main chain as the adhesion promoter, and the adhesion promoter contains ether bond, so that the adhesion promoter has good flexibility and elongation; the silicone sealant has good adhesion with a base material, and the adhesion promoter has low viscosity, can remarkably reduce the viscosity of the hydroxyl-terminated polydimethylsiloxane, plays a role of a plasticizer, but can be hydrolyzed and condensed to form a part of the silicone sealant elastomer, so that poor oil leakage caused by adopting silicone oil and white oil as the plasticizer is avoided, and the adhesion of the silicone sealant and a concrete base material is improved.
In the silicone sealant, isocyanate group siloxane oligomer is used as a water removal agent, one end of the isocyanate group siloxane oligomer contains high-activity isocyanate group, one end of the isocyanate group siloxane oligomer contains organic silicon functional group capable of being hydrolyzed, the isocyanate group can react with trace water in the rubber material, so that the trace water in the rubber material is eliminated, the organic silicon functional group at the other end can be formed into one part of the silicone sealant elastomer through hydrolysis and condensation, and the final product can not be separated out and the cohesiveness of the silicone sealant and a base material can not be influenced; while excess isocyanate groups will react away the amino groups in the coupling agent. Therefore, the water removal agent is selected, so that the removal of trace water in the sizing material can be ensured, the storage stability of the silicone sealant product is improved, and the moisture in the use of the silicone sealant product can not be prevented from entering, so that the curing efficiency is influenced.
The silicone sealant preferably further comprises 0.005-0.01 part by weight of pigment.
The viscosity of the silicone sealant is preferably 1000-6000 mPa.s; the viscosity of the hydroxyl-terminated polydimethylsiloxane is 10000 mPas-80000 mPas.
Preferably, the water scavenger is an isocyanate propyl siloxane oligomer; the coupling agent is an amino silane oligomer; the catalyst is an organic tin catalyst.
Preferably, the water removing agent is isocyanatopropyl triethoxysilane or/and isocyanatopropyl trimethoxysilane;
the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldiethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, Y-aminopropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropylmethyldimethoxysilane.
Preferably, the chain extender is one or more of vinyl dibutyloxime, methyl vinyl diacetamidosilane and dimethyl dibutyloxime silane, and more preferably vinyl dibutyloxime;
the cross-linking agent is one or more of phenyl tributyrine oxime silane and methyl tributyrine oxime silane, and is more preferably phenyl tributyrine oxime.
Preferably, the filler is surface modified nano calcium carbonate with the average particle size of less than 80nm and surface modified activated calcium carbonate with the average particle size of less than 13 mu m, wherein the dosage of the surface modified activated calcium carbonate is 20-50% of that of the surface modified nano calcium carbonate. The modifier of the calcium carbonate in the surface modification process is stearic acid or organic amine modifier.
Based on the same inventive concept, the invention also provides a preparation method of the silicone sealant, which comprises the following steps:
(1) carrying out vacuum dehydration and stirring on hydroxyl-terminated polydimethylsiloxane, 50-125 parts of filler and pigment, and cooling to room temperature to obtain a base material A;
(2) adding an adhesion promoter and the rest of the filler into the material A, and performing vacuum dehydration and stirring to obtain a material B;
(3) adding a water removing agent into the material B, and performing vacuum dehydration and stirring to obtain a material C;
(4) adding a cross-linking agent and a chain extender into the material C, and performing vacuum dehydration and stirring to obtain a material D;
(5) and adding a coupling agent and a catalyst into the material D, performing vacuum dehydration and stirring, discharging, filling and sealing to complete the preparation of the silicone sealant.
In the preparation method, preferably, in the step (1), the temperature of vacuum dehydration and stirring is 110-;
in the step (2) and the step (3), in the vacuum dehydration and stirring process, the vacuum degree is 0.09-0.1MPa, the stirring time is 10-40 minutes, and the material temperature is controlled below 60 ℃;
in the steps (4) and (5), in the vacuum dehydration and stirring process, the vacuum degree is 0.09-0.1MPa, the stirring time is 20-40 minutes, and the material temperature is controlled below 60 ℃.
Compared with the prior art, the invention has the advantages that:
(1) the adhesion promoter disclosed by the invention is applied to a silicone sealant of a ballastless track, so that the silicone sealant has good flexibility, elongation and viscosity, is good in adhesion with a concrete base material, and meets the requirement of waterproof sealing of a CRTS III ballastless track bridge deck caulking joint.
(2) The silicone sealant disclosed by the invention is added with isocyanate propyl siloxane oligomer, so that trace moisture and hydroxyl compounds in a system are reduced, and the storage time can be obviously prolonged.
(3) The silicone sealant does not need to adopt a micromolecular polymer as a plasticizer, does not have the phenomena of oil leakage and the like, and has difficult surface pollution.
(4) The silicone sealant disclosed by the invention adopts calcium carbonate with different particle sizes and types as a reinforcing material and a thixotropic agent, and does not need to adopt a white carbon black material as the thixotropic agent, so that the cost can be obviously reduced.
(5) The silicone sealant disclosed by the invention adopts a segmented production process, can provide production efficiency under the condition of the same equipment, and is beneficial to reducing the production cost.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a silicone sealant applied to a ballastless track, which is mainly prepared from the following raw materials in parts by weight:
Figure BDA0001673501520000051
wherein the viscosity of the hydroxyl-terminated polydimethylsiloxane is 20000mPa & s, the viscosity of the adhesion promoter is 4000mPa & s, the filler is surface modified nano calcium carbonate with the particle size of less than 80nm and surface modified active calcium carbonate with the particle size of less than 13 mu m, and the amount of the surface modified active calcium is 20 percent of the mass of the surface modified nano calcium carbonate; the structural formula of the adhesion promoter is R [ OCO-NH-Ph-CH2-Ph-NHCO-NH-CH2-CH2-CH2-Si-(O-N=CCH3CH2-CH(CH3)2)3]2The adhesion promoter is prepared by the following preparation method:
(1) selecting 100 portions of a catalyst having [ CH ]2-CH(CH3)-O]Polyoxypropylene polyol (Jinxiong chemical N-220) with a repeating unit structure is used as a raw material, the molecular weight is 2000, and the functionality is 2;
(2) adding 25 parts of diphenylmethane diisocyanate into the polyoxypropylene polyol obtained in the step (1), and reacting at the temperature of 70 ℃ for 2h to obtain a product A, wherein the product A is R- (OCO-NH-Ph-CH)2-Ph-NCO)2
(3) Adding 22 parts of R-aminopropyltriethoxysilane into the product A for reaction to obtain a product B, wherein the structure of the product B is R- (OCO-NH-R)1-NHCONHCH2-CH2-CH2-Si-(OCH2CH3)3)2And finally, adding 34 parts of methyl isobutyl ketoxime, reacting at 120 ℃, and distilling a low-boiling-point substance under reduced pressure after the reaction is finished to obtain the adhesion promoter.
The preparation method of the silicone sealant applied to the ballastless track of the embodiment comprises the following specific steps:
(1) dehydrating and stirring 100 parts of hydroxyl-terminated polydimethylsiloxane, 125 parts of filler and 0.01 part of pigment for 3 hours at the temperature of 120 ℃ and the vacuum degree of 0.09MPa, and cooling to room temperature to obtain a material A;
(2) adding 20 parts of adhesion promoter and the rest 125 parts of filler into the material A, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material B, and controlling the material temperature to be below 60 ℃;
(3) adding 0.5 part of water removing agent (isocyanate propyl triethoxysilane) into the material B, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material C, and controlling the material temperature to be below 60 ℃;
(4) adding 10 parts of a cross-linking agent (phenyl tributyl ketoxime silane) and 5 parts of a chain extender (vinyl dibutyloxime) into the material C, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material D, and controlling the material temperature to be below 60 ℃;
(5) and adding 2 parts of coupling agent (gamma-aminopropyltriethoxysilane) and 0.001 part of dibutyltin dilaurate into the material D, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa, controlling the material temperature to be below 60 ℃, discharging, filling and sealing, and thus completing the preparation of the silicone sealant.
Example 2:
the invention relates to a silicone sealant applied to a ballastless track, which is mainly prepared from the following raw materials in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane,
50 parts of an adhesion promoter, namely,
10 parts of phenyl tributyl ketoxime silane,
5 parts of vinyl-dibutyl ketoxime,
2 parts of gamma-aminopropyl triethoxysilane,
250 parts of a filler, namely a filler,
0.5 part of isocyanatopropyl trimethoxy silane,
0.01 part of a pigment, and
0.001 part of dibutyltin dilaurate;
wherein the viscosity of the hydroxyl-terminated polydimethylsiloxane is 20000mPa & s, the viscosity of the adhesion promoter is 4000mPa & s, the filler is surface modified nano calcium carbonate with the particle size of less than 80nm and surface modified active calcium carbonate with the particle size of less than 13 mu m, and the amount of the surface modified active calcium is 40 percent of the mass of the surface modified nano calcium carbonate; the structural formula of the adhesion promoter is R [ OCO-NH-Ph-CH2-Ph-NHCO-NH-CH2-CH2-CH2-Si-(O-N=CCH3CH2-CH(CH3)2)3]2The adhesion promoter is prepared by the following preparation method:
(1) selecting a mixture having 100 parts of [ CH ]2-CH(CH3)-O]Polyoxypropylene polyol (Jinxiong chemical N-220) with a repeating unit structure is used as a raw material, the molecular weight is 2000, and the functionality is 2;
(2) adding 25 parts of diphenylmethane diisocyanate into the polyoxypropylene polyol obtained in the step (1), and reacting at the temperature of 70 ℃ for 2h to obtain a product A, wherein the product A is R- (OCO-NH-Ph-CH)2-Ph-NCO)2
(3) Adding 22 parts of R-aminopropyltriethoxysilane into the product A for reaction to obtain a product B, wherein the structure of the product B is R- (OCO-NH-R)1-NHCONHCH2-CH2-CH2-Si-(OCH2CH3)3)2And finally, adding 34 parts of methyl isobutyl ketoxime, reacting at 120 ℃, and distilling a low-boiling-point substance under reduced pressure after the reaction is finished to obtain the adhesion promoter.
The preparation method of the silicone sealant applied to the ballastless track of the embodiment comprises the following specific steps:
(1) dehydrating and stirring 100 parts of hydroxyl-terminated polydimethylsiloxane, 125 parts of filler and 0.01 part of pigment for 3 hours at the temperature of 120 ℃ and the vacuum degree of 0.09MPa, and cooling to room temperature to obtain a material A;
(2) adding 50 parts of adhesion promoter and the rest 125 parts of filler into the material A, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material B, and controlling the material temperature to be below 60 ℃;
(3) adding 0.5 part of water removing agent (isocyanate propyl trimethoxy silane) into the material B, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material C, and controlling the material temperature to be below 60 ℃;
(4) adding 10 parts of a cross-linking agent (phenyl tributyl ketoxime silane) and 5 parts of a chain extender (vinyl dibutyloxime) into the material C, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material D, and controlling the material temperature to be below 60 ℃;
(5) and adding 2 parts of coupling agent (gamma-aminopropyltriethoxysilane) and 0.001 part of catalyst dibutyltin dilaurate into the material D, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa, controlling the material temperature to be below 60 ℃, discharging, filling and sealing, and thus completing the preparation of the silicone sealant.
Example 3:
the invention relates to a silicone sealant applied to a ballastless track, which is mainly prepared from the following raw materials in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane,
20 parts of an adhesion promoter, namely 20 parts of,
10 parts of phenyl tributyl ketoxime silane,
5 parts of vinyl-dibutyl ketoxime,
2 parts of gamma-aminopropyl triethoxysilane,
200 parts of a filler, namely 200 parts of a filler,
0.5 part of isocyanatopropyl trimethoxy silane,
0.01 part of a pigment, and
0.001 part of dibutyltin dilaurate;
wherein the viscosity of the hydroxyl-terminated polydimethylsiloxane is 80000 mPas, the viscosity of the adhesion promoter is 2000 mPas, the filler is surface modified nano calcium carbonate with the particle size of less than 80nm and surface modified activated calcium carbonate with the particle size of less than 13 mu m, and the amount of the surface modified activated calcium is surface modified nano calcium carbonate30% of the mass of calcium; the structural formula of the adhesion promoter is R [ OCO-NH-Ph (CH)3)-NHCO-NH-CH2-CH2-CH2-Si-(O-N=CCH3CH2-CH(CH3)2)3]2The adhesion promoter is prepared by the following preparation method:
(1) selecting a compound having [ CH2-CH(CH3)-O]Polyoxypropylene polyol (Jinxiong chemical D-240) with a repeating unit structure is used as a raw material, the molecular weight is 4000, and the functionality is 2;
(2) to 200 parts of polyoxypropylene polyol of step (1) was added 17.5 parts of toluene diisocyanate, and reacted at 70 ℃ for 2 hours to give product A, which was R- (OCO-NH-Ph (CH)3)-NCO)2
(3) Adding 22 parts of R-aminopropyltriethoxysilane into the product A for reaction to obtain a product B, wherein the structure of the product B is R- (OCO-NH-R)1-NHCONHCH2-CH2-CH2-Si-(OCH2CH3)3)2And finally, adding 34 parts of methyl isobutyl ketoxime, reacting at 120 ℃, and distilling a low-boiling-point substance under reduced pressure after the reaction is finished to obtain the adhesion promoter.
The preparation method of the silicone sealant applied to the ballastless track of the embodiment comprises the following specific steps:
(1) dehydrating and stirring 100 parts of hydroxyl-terminated polydimethylsiloxane, 100 parts of filler and 0.01 part of pigment for 3 hours at the temperature of 120 ℃ and the vacuum degree of 0.09MPa, and cooling to room temperature to obtain a material A;
(2) adding 20 parts of adhesion promoter and the rest 100 parts of filler into the material A, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material B, and controlling the material temperature to be below 60 ℃;
(3) adding 0.5 part of water removing agent (isocyanate propyl trimethoxy silane) into the material B, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material C, and controlling the material temperature to be below 60 ℃;
(4) adding 10 parts of a cross-linking agent (phenyl tributyl ketoxime silane) and 5 parts of a chain extender (vinyl dibutyloxime) into the material C, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material D, and controlling the material temperature to be below 60 ℃;
(5) and adding 2 parts of coupling agent (gamma-aminopropyltriethoxysilane) and 0.001 part of catalyst into the material D, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa, controlling the material temperature to be below 60 ℃, discharging, filling and sealing to complete the preparation of the silicone sealant.
Example 4:
the invention relates to a silicone sealant applied to a ballastless track, which is mainly prepared from the following raw materials in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane,
50 parts of an adhesion promoter, namely,
10 parts of methyl-tributyl ketoxime silane,
5 parts of methyl vinyl diacetamido silane,
2 parts of gamma-aminopropyl triethoxysilane,
250 parts of a filler, namely a filler,
0.5 part of isocyanatopropyl trimethoxy silane,
0.01 part of a pigment, and
0.001 part of dibutyltin dilaurate;
wherein, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 80000 mPas, the viscosity of the adhesion promoter is 2000 mPas, the filler is surface modified nano calcium carbonate with the particle size of less than 80nm and surface modified activated calcium carbonate with the particle size of less than 13 mu m, and the amount of the surface modified activated calcium is 20 percent of the mass of the surface modified nano calcium carbonate; the structural formula of the adhesion promoter is R [ OCO-NH-Ph (CH)3)-NHCO-NH-CH2-CH2-CH2-Si-(O-N=CCH3CH2-CH(CH3)2)3]2The adhesion promoter is prepared by the following preparation method:
(1) selecting a compound having [ CH2-CH(CH3)-O]Polyoxypropylene polyol (Jinxiong chemical D-240) with repeating unit structure as raw material and with molecular weight of 4000, functionality of 2;
(2) to 200 parts of polyoxypropylene polyol of step (1) was added 17.5 parts of toluene diisocyanate, and reacted at 70 ℃ for 2 hours to give product A, which was R- (OCO-NH-Ph (CH)3)-NCO)2
(3) Adding 22 parts of R-aminopropyltriethoxysilane into the product A for reaction to obtain a product B, wherein the structure of the product B is R- (OCO-NH-R)1-NHCONHCH2-CH2-CH2-Si-(OCH2CH3)3)2And finally, adding 34 parts of methyl isobutyl ketoxime, reacting at 120 ℃, and distilling a low-boiling-point substance under reduced pressure after the reaction is finished to obtain the adhesion promoter.
The preparation method of the silicone sealant applied to the ballastless track of the embodiment comprises the following specific steps:
(1) dehydrating and stirring 100 parts of hydroxyl-terminated polydimethylsiloxane, 125 parts of filler and 0.01 part of pigment for 3 hours at the temperature of 120 ℃ and the vacuum degree of 0.09MPa, and cooling to room temperature to obtain a material A;
(2) adding 50 parts of adhesion promoter and the rest 125 parts of filler into the material A, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material B, and controlling the material temperature to be below 60 ℃;
(3) adding 0.5 part of water removing agent (isocyanate propyl trimethoxy silane) into the material B, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material C, and controlling the material temperature to be below 60 ℃;
(4) adding 10 parts of cross-linking agent (methyl tributyl ketoxime silane) and 5 parts of chain extender (methyl vinyl diacetamidosilane) into the material C, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09-MPa to obtain a material D, and controlling the material temperature to be below 60 ℃;
(5) and adding 2 parts of coupling agent (gamma-aminopropyltriethoxysilane) and 0.001 part of catalyst dibutyltin dilaurate into the material D, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa, controlling the material temperature to be below 60 ℃, discharging, filling and sealing, and thus completing the preparation of the silicone sealant.
Example 5:
the invention relates to a silicone sealant applied to a ballastless track, which is mainly prepared from the following raw materials in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane,
20 parts of an adhesion promoter, namely 20 parts of,
10 parts of methyl-tributyl ketoxime silane,
5 parts of dimethyl-dibutylketoximino silane,
2 parts of gamma-aminopropyl triethoxysilane,
200 parts of a filler, namely 200 parts of a filler,
0.5 part of isocyanatopropyl trimethoxy silane,
0.01 part of a pigment, and
0.001 part of dibutyltin dilaurate;
wherein, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 80000 mPas, the viscosity of the adhesion promoter is 6000 mPas, the filler is surface modified nano calcium carbonate with the particle size of less than 80nm and surface modified activated calcium carbonate with the particle size of less than 13 mu m, and the amount of the surface modified activated calcium is 40 percent of the mass of the surface modified nano calcium carbonate; the structural formula of the adhesion promoter is R [ OCO-NH-Ph (CH)3)-NHCO-NH-CH2-CH2-CH2-Si-(O-N=CCH3CH2-CH(CH3)2)3]3The adhesion promoter is prepared by the following preparation method:
(1) selecting a compound having [ CH2-CH(CH3)-O]Polyoxypropylene polyol (Jinxiong chemical N-330N) with a repeating unit structure is used as a raw material, the molecular weight is 5000, and the functionality is 3;
(2) adding 10.5 parts of toluene diisocyanate to 100 parts of polyoxypropylene polyol in step (1), and reacting at 70 ℃ for 2h to obtain product A, wherein the product A is R- (OCO-NH-Ph (CH)3)-NCO)3
(3) Adding 13.3 parts of R-aminopropyltriethoxysilane into the product A for reaction to obtain a product B, wherein the structure of the product B is R- (OCO-NH-R)1-NHCONHCH2-CH2-CH2-Si-(OCH2CH3)3)3And finally, adding 13 parts of dimethyl ketoxime, reacting at 120 ℃, and distilling the low-boiling-point substances under reduced pressure after the reaction is finished to obtain the adhesion promoter.
The preparation method of the silicone sealant applied to the ballastless track of the embodiment comprises the following specific steps:
(1) dehydrating and stirring 100 parts of hydroxyl-terminated polydimethylsiloxane, 100 parts of filler and 0.01 part of pigment for 3 hours at the temperature of 120 ℃ and the vacuum degree of 0.09MPa, and cooling to room temperature to obtain a material A;
(2) adding 20 parts of adhesion promoter and the rest 100 parts of filler into the material A, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material B, and controlling the material temperature to be below 60 ℃;
(3) adding 0.5 part of water removing agent (isocyanate propyl trimethoxy silane) into the material B, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material C, and controlling the material temperature to be below 60 ℃;
(4) adding 10 parts of cross-linking agent (methyl tributyl ketoxime silane) and 5 parts of chain extender (dimethyl dibutylketoxime silane) into the material C, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material D, wherein the material temperature is controlled below 60 ℃;
(5) and adding 2 parts of coupling agent (gamma-aminopropyltriethoxysilane) and 0.001 part of catalyst dibutyltin dilaurate into the material D, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa, controlling the material temperature to be below 60 ℃, discharging, filling and sealing, and thus completing the preparation of the silicone sealant.
Example 6:
the invention relates to a silicone sealant applied to a ballastless track, which is mainly prepared from the following raw materials in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane,
50 parts of an adhesion promoter, namely,
10 parts of methyl-tributyl ketoxime silane,
5 parts of dimethyl-dibutylketoximino silane,
2 parts of gamma-aminopropyl triethoxysilane,
150 parts of a filler, namely a filler,
0.5 part of isocyanatopropyl trimethoxy silane,
0.01 part of a pigment, and
0.001 part of dibutyltin dilaurate;
wherein, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 80000 mPas, the viscosity of the adhesion promoter is 6000 mPas, the filler is surface modified nano calcium carbonate with the particle size of less than 80nm and surface modified activated calcium carbonate with the particle size of less than 13 mu m, and the amount of the surface modified activated calcium is 20 percent of the mass of the surface modified nano calcium carbonate; the structural formula of the adhesion promoter is R [ OCO-NH-Ph (CH)3)-NHCO-NH-CH2-CH2-CH2-Si-(O-N=CCH3CH2-CH(CH3)2)3]3The adhesion promoter is prepared by the following preparation method:
(1) selecting a compound having [ CH2-CH(CH3)-O]Polyoxypropylene polyol (Jinxiong chemical N-330N) with a repeating unit structure is used as a raw material, the molecular weight is 5000, and the functionality is 3;
(2) adding 10.5 parts of toluene diisocyanate to 100 parts of polyoxypropylene polyol in step (1), and reacting at 70 ℃ for 2h to obtain product A, wherein the product A is R- (OCO-NH-Ph (CH)3)-NCO)3
(3) Adding 13.3 parts of R-aminopropyltriethoxysilane into the product A for reaction to obtain a product B, wherein the structure of the product B is R- (OCO-NH-R)1-NHCONHCH2-CH2-CH2-Si-(OCH2CH3)3)3And finally, adding 13 parts of dimethyl ketoxime, reacting at 120 ℃, and distilling the low-boiling-point substances under reduced pressure after the reaction is finished to obtain the adhesion promoter.
The preparation method of the silicone sealant applied to the ballastless track of the embodiment comprises the following specific steps:
(1) dehydrating and stirring 100 parts of hydroxyl-terminated polydimethylsiloxane, 75 parts of filler and 0.01 part of pigment for 3 hours at the temperature of 120 ℃ and the vacuum degree of 0.09MPa, and cooling to room temperature to obtain a material A;
(2) adding 20 parts of adhesion promoter and the rest 75 parts of filler into the material A, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material B, wherein the material temperature is controlled below 60 ℃;
(3) adding 0.5 part of water removing agent (isocyanate propyl trimethoxy silane) into the material B, dehydrating and stirring for 20 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material C, and controlling the material temperature to be below 60 ℃;
(4) adding 10 parts of cross-linking agent (methyl tributyl ketoxime silane) and 5 parts of chain extender (dimethyl dibutylketoxime silane) into the material C, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material D, wherein the material temperature is controlled below 60 ℃;
(5) and adding 2 parts of coupling agent (gamma-aminopropyltriethoxysilane) and 0.001 part of catalyst dibutyltin dilaurate into the material D, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa, controlling the material temperature to be below 60 ℃, discharging, filling and sealing, and thus completing the preparation of the silicone sealant.
Comparative example:
the silicone sealant of the comparative example is mainly prepared from the following raw materials in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane,
15 parts of silicone oil, namely 15 parts of,
10 parts of methyl-tributyl ketoxime silane,
5 parts of dimethyl-dibutylketoximino silane,
2 parts of gamma-aminopropyl triethoxysilane,
250 parts of a filler, namely a filler,
0.01 part of pigment, namely,
0.001 part of dibutyltin dilaurate;
wherein, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 80000 mPas, the fillers are surface modified nano calcium carbonate with the particle size of less than 80nm and surface modified activated calcium carbonate with the particle size of less than 13 mu m, and the amount of the surface modified activated calcium is 20 percent of the mass of the surface modified nano calcium carbonate.
The preparation method of the silicone sealant in the comparative example comprises the following specific steps:
(1) dehydrating and stirring 100 parts of hydroxyl-terminated polydimethylsiloxane, 15 parts of silicone oil, 250 parts of filler and 0.01 part of pigment for 3 hours at the temperature of 120 ℃ and the vacuum degree of 0.09MPa, and cooling to room temperature to obtain a material A;
(2) adding 10 parts of methyl tributyl ketoxime silane and 5 parts of dimethyl diacetyl ketoxime silane into the material B, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa to obtain a material C, wherein the material temperature is controlled below 60 ℃;
(3) and adding 2 parts of gamma-aminopropyltriethoxysilane and 0.001 part of dibutyltin dilaurate into the material C, dehydrating and stirring for 30 minutes under the condition that the vacuum degree is 0.09MPa, controlling the material temperature to be below 60 ℃, discharging, filling and sealing, and thus completing the preparation of the silicone sealant.
The silicone sealants obtained in examples 1 to 6 and the comparative example were tested for tensile modulus, sag, definite elongation adhesion, adhesion after cold drawing and hot pressing, and adhesion after stretch-compression cycle according to GB/T134777-2002, and for tensile strength and elongation at break according to GB/T16777-2008, and the obtained performance parameters are shown in Table 1. And (3) testing environment: temperature: 23 ℃, humidity: 50 percent.
TABLE 1 relevant Properties of the Silicone sealants of the examples and comparative examples
Figure BDA0001673501520000131
As can be seen from Table 1, the silicone sealant of the present invention has excellent flexibility and elongation, high viscosity, and long shelf life.

Claims (9)

1. The preparation method of the adhesion promoter for the silicone sealant is characterized by comprising the following steps:
(1) selecting a compound having [ CH2-CH(CH3)-O]Repeating unit junctionStructural polypropylene oxide polyhydric alcohol is used as a raw material, the molecular weight is 2000-7000, and the functionality is 2 or 3;
(2) adding isocyanate into the polyoxypropylene polyol for reaction, wherein the adding amount of the isocyanate is 2 times of that of-OH substances in the polyoxypropylene polyol, so as to obtain a product A; the isocyanate structure is NCO-R1-NCO, and the isocyanate structure is any one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, methylcyclohexyl diisocyanate, dicyclohexylmethane diisocyanate and isophorone diisocyanate;
(3) adding amino alkoxy silane into the product A for reaction, and finally adding HO-N ═ CR3R4Reacting, and distilling a low-boiling-point substance under reduced pressure after the reaction is finished to obtain the adhesion promoter; the structure of the adhesion promoter is as follows:
R[OCO-NH-R1-NHCO-NH-R2-Si-(O-N=CR3R4)3]n,
wherein R is a group having [ CH ]2-CH(CH3)-O]An organic of repeating units;
R1represents a divalent alkyl or phenyl radical, R2Represents a divalent alkyl radical having at least 2 carbon atoms, R3And R4Respectively represent a straight chain or branched chain alkyl of 1 to 7 carbon atoms, and n is 2 or 3.
2. The silicone sealant applied to the ballastless track is characterized by being mainly prepared from the following raw materials in parts by weight:
Figure FDA0002642345870000011
wherein the structure of the adhesion promoter is as follows:
R[OCO-NH-R1-NHCO-NH-R2-Si-(O-N=CR3R4)3]n,
wherein R is a group having [ CH ]2-CH(CH3)-O]An organic of repeating units;
R1represents a divalent alkyl or phenyl radical, R1The isocyanate is derived from isocyanate with a structural formula of NCO-R1-NCO, and the isocyanate structure is any one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, methylcyclohexyl diisocyanate, dicyclohexylmethane diisocyanate and isophorone diisocyanate; r2Represents a divalent alkyl radical having at least 2 carbon atoms, R3And R4Respectively represent a straight chain or branched chain alkyl of 1 to 7 carbon atoms, and n is 2 or 3; or the adhesion promoter is obtained by the following preparation method:
(1) selecting a compound having [ CH2-CH(CH3)-O]The polyoxypropylene polyol with a repeating unit structure is used as a raw material, the molecular weight is 2000-7000, and the functionality is 2 or 3;
(2) adding isocyanate into the polyoxypropylene polyol for reaction, wherein the adding amount of the isocyanate is 2 times of that of-OH substances in the polyoxypropylene polyol, so as to obtain a product A; the isocyanate is any one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, methylcyclohexyl diisocyanate, dicyclohexylmethane diisocyanate and isophorone diisocyanate; (3) adding amino alkoxy silane into the product A for reaction, and finally adding HO-N ═ CR3R4And (3) reacting, and distilling the low-boiling-point substances under reduced pressure after the reaction is finished to obtain the adhesion promoter.
3. The silicone sealant of claim 2 wherein said base stock further comprises 0.005 to 0.01 parts by weight of a pigment.
4. The silicone sealant according to any one of claims 2 to 3 wherein the adhesion promoter has a viscosity of 1000-; the viscosity of the hydroxyl-terminated polydimethylsiloxane is 10000 mPas-80000 mPas.
5. The silicone sealant according to any of claims 2-3 wherein the water scavenger is an isocyanatopropyl siloxane oligomer; the coupling agent is an amino silane oligomer; the catalyst is an organic tin catalyst.
6. The silicone sealant of claim 5 wherein said water scavenger is isocyanatopropyltriethoxysilane or/and isocyanatopropyltrimethoxysilane;
the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldiethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, Y-aminopropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropylmethyldimethoxysilane;
the chain extender is one or more of vinyl diacetylmonoxime, methyl vinyl diacetyl amide silane and dimethyl diacetylmonoxime silane;
the cross-linking agent is one or more of phenyl tributyl ketoxime silane and methyl tributyl ketoxime silane;
the catalyst is dibutyltin dilaurate.
7. The silicone sealant according to any of claims 2 to 3 wherein the filler is surface modified nano calcium carbonate having an average particle size of less than 80nm and surface modified activated calcium carbonate having an average particle size of less than 13 μm, wherein the surface modified activated calcium carbonate is present in an amount of 20% to 50% of the amount of surface modified nano calcium carbonate.
8. A method of preparing the silicone sealant according to any one of claims 2 to 7 comprising the steps of:
(1) carrying out vacuum dehydration and stirring on hydroxyl-terminated polydimethylsiloxane, 50-125 parts of filler and pigment, and cooling to room temperature to obtain a material A;
(2) adding an adhesion promoter and the rest of the filler into the material A, and performing vacuum dehydration and stirring to obtain a material B;
(3) adding a water removing agent into the material B, and performing vacuum dehydration and stirring to obtain a material C;
(4) adding a cross-linking agent and a chain extender into the material C, and performing vacuum dehydration and stirring to obtain a material D;
(5) and adding a coupling agent and a catalyst into the material D, performing vacuum dehydration and stirring, discharging, filling and sealing to complete the preparation of the silicone sealant.
9. The method according to claim 8, wherein in the step (1), the temperature of the vacuum dehydration stirring is 110-;
in the step (2) and the step (3), in the vacuum dehydration and stirring process, the vacuum degree is 0.09-0.1MPa, the stirring time is 10-40 minutes, and the material temperature is controlled below 60 ℃;
in the steps (4) and (5), in the vacuum dehydration and stirring process, the vacuum degree is 0.09-0.1MPa, the stirring time is 20-40 minutes, and the material temperature is controlled below 60 ℃.
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