CN116042173B - Alkali-resistant self-leveling silicone sealant and production process thereof - Google Patents
Alkali-resistant self-leveling silicone sealant and production process thereof Download PDFInfo
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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
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J11/06—Non-macromolecular additives organic
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- 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses an alkali-resistant self-leveling silicone sealant and a production process thereof, belonging to the technical field of silicone sealants, and comprising the following steps: firstly, adding a coupling agent pretreatment filler and methyl acrylate into methanol, and stirring for reaction to obtain an intermediate product; adding the intermediate product and the amino-terminated hyperbranched flame retardant component into methanol, and continuing to react to obtain a reinforcing filler; secondly, stirring, mixing, dehydrating and blending 107 silicon rubber, reinforcing filler and plasticizer, cooling, adding a cross-linking agent, and dispersing and stirring under vacuum to obtain a mixture; and thirdly, adding a coupling agent, a catalyst and a water scavenger into the mixture, and dispersing and stirring under vacuum. The reinforcing filler has better promotion effect on the improvement of the sealant performance. And the alkali-resistant self-leveling silicone sealant added with the treated reinforcing filler has better yellowing resistance.
Description
Technical Field
The invention belongs to the technical field of silicone sealants, and particularly relates to an alkali-resistant self-leveling silicone sealant and a production process thereof.
Background
The silicone sealant has the advantages of excellent weather resistance, excellent water resistance, good cohesiveness and the like, and can realize flexible adhesion between two rigid materials; the silicone sealant can be widely applied to industries such as construction, electronics, electrics, aerospace, automobile industry and the like due to excellent performances and the like.
Silicone sealants are of various types, among which self-leveling silicone sealants can be used for sealing concrete joints of tunnels, bridges, roads, airport runways, squares, etc. Can automatically flow into joints and irregular gaps without trimming, thereby reducing labor cost: little or no waste, and can save the material cost.
In practical application, the self-leveling silicone sealant also has the defects of poor low-temperature flexibility, poor yellowing resistance, poor adhesive property and the like. For example, the silicone sealant contains plasticizers with certain components, so that the leveling property of the sealant can be improved, and the plasticizers often have a certain influence on the ageing resistance of the silicone sealant and also influence the alkali corrosion resistance of the silicone sealant. For example, chinese patent CN103725009a discloses a method for preparing a fast curing dealcoholized transparent room temperature vulcanized silicone adhesive, and discloses the use of hexamethyldisilazane as a stabilizer, which releases ammonia gas with a pungent odor and causes severe yellowing of the adhesive.
Disclosure of Invention
The invention aims to provide an alkali-resistant self-leveling silicone sealant and a production process thereof, which are used for solving the problems in the background technology.
The aim of the invention can be achieved by the following technical scheme:
a production process of alkali-resistant self-leveling silicone sealant comprises the following steps:
firstly, adding a coupling agent pretreatment filler and methyl acrylate into methanol, setting the temperature to 50 ℃, stirring and reacting for 5 hours, and vacuum-filtering and vacuum-drying at 60 ℃ after the reaction is finished to obtain an intermediate product; adding the intermediate product and the amino-terminated hyperbranched flame retardant component into methanol, setting the temperature to be 50 ℃, continuing to react for 6-8h, and after the reaction is finished, performing vacuum filtration and vacuum drying at the temperature of 60 ℃ to obtain the reinforcing filler. The dosage ratio of the coupling agent pretreatment filler, methyl acrylate and methanol is 10g:3g:150mL; the dosage ratio of the intermediate product, the amino-terminated hyperbranched flame retardant component and the methanol is 10g:10g:300mL.
Secondly, adding 107 silicon rubber, reinforcing filler and plasticizer into a planetary mixer under the conditions of 110 ℃ and 0.09MPa of vacuum degree, stirring, mixing, dehydrating and blending for 3 hours, cooling, adding a cross-linking agent, and dispersing and stirring under vacuum to obtain a mixture;
and thirdly, adding a coupling agent, a catalyst and a water scavenger into the mixture at the temperature of 25 ℃, and dispersing and stirring under vacuum to prepare the alkali-resistant self-leveling silicone sealant.
Further, the coupling agent pretreatment filler is prepared by the steps of:
adding the filler into ethanol water solution, adding gamma-aminopropyl triethoxysilane, stirring for 24 hours at 20 ℃, washing and filtering with absolute ethanol after stirring, and vacuum drying for 24 hours at 60 ℃ to obtain the coupling agent pretreated filler. The dosage ratio of the filler, the ethanol water solution and the gamma-aminopropyl triethoxysilane is 10g:100mL:2g.
Further, the filler is white carbon black and calcium carbonate according to the mass ratio of 1:10, wherein the average particle size of the filler is 2-4 mu m; the volume fraction of the ethanol aqueous solution is 50%;
further, the amino-terminated hyperbranched flame retardant component is prepared by the following steps:
adding hexachlorocyclotriphosphazene and ethylenediamine into tetrahydrofuran under the protection of nitrogen, stirring, dispersing, adding triethylamine, heating, refluxing for reaction for 12h, cooling to room temperature after the reaction is finished, washing with ethanol, and vacuum drying at 45 ℃ to constant weight to obtain an amino-terminated hyperbranched flame-retardant component; and (3) carrying out nucleophilic substitution reaction on the chlorcyclotriphosphazene and ethylenediamine to obtain an amino-terminated hyperbranched flame-retardant component, wherein the amino-terminated hyperbranched flame-retardant component reacts with methyl ester groups on intermediate products, and the filler is grafted on the filler by taking the filler as a reaction core.
The mol ratio of the hexachlorocyclotriphosphazene to the ethylenediamine is 6:1, a step of; the dosage ratio of hexachlorocyclotriphosphazene, triethylamine and tetrahydrofuran is 2.5g:4.3g:100mL.
Further, the plasticizer is selected from acetylated butoxyethyl ricinoleate; the acetylated butoxyethyl ricinoleate is prepared by using ricinoleic acid as a raw material, performing esterification reaction with ethylene glycol butyryl to generate butoxyethyl ricinoleate, and acylating hydroxyl under the catalysis of p-toluenesulfonic acid to obtain the acetylated butoxyethyl ricinoleate. Compared with castor oil, the acetylated butoxyethyl ricinoleate has better water resistance, volatilization resistance and migration resistance, the plasticizer is used for improving the leveling property of the alkali-resistant self-leveling silicone sealant, the acetylated butoxyethyl ricinoleate has good environmental protection, and the ether bond of the acetylated butoxyethyl ricinoleate is more stable under alkaline conditions, has better migration resistance and is more beneficial to alkali corrosion resistance of the alkali-resistant self-leveling silicone sealant.
Further, the viscosity of the 107 silicone rubber was 80000 mPa.S.
Further, the coupling agent is one or two of gamma-aminopropyl triethoxysilane and 3-mercaptopropyl trimethoxysilane which are mixed according to any proportion.
Further, the cross-linking agent is methyl tributyl ketoxime group siloxane; the catalyst is dibutyl tin dilaurate, and the water scavenger is vinyl trimethoxy silane. The vinyl trimethoxy silane and water molecules have high reactivity, can react with water vapor in a sealant system, and consume the water vapor to improve the storage stability of the sealant.
Further, 100 parts of 107 silicone rubber, 1-4 parts of plasticizer, 10-17 parts of cross-linking agent, 3-7 parts of coupling agent, 18-21 parts of reinforcing filler, 0.5-1.5 parts of catalyst and 3-9 parts of water remover.
The alkali-resistant self-leveling silicone sealant is prepared through the steps.
The invention has the beneficial effects that:
aiming at the defects of the silicone sealant in the prior art, the invention provides an alkali-resistant self-leveling silicone sealant which is prepared by taking Si-O-Si as a main chain and adding a cross-linking agent, a coupling agent, a catalyst and various powder for mixing. Crosslinking and curing the polymer into a high-molecular polymer with excellent performance by absorbing moisture in air in a room temperature environment; the reinforcing filler is prepared by treating the filler in the process of preparing the silicone sealant; the reinforcing filler obtained after treatment has better promotion effect on the improvement of the sealant performance. And the alkali-resistant self-leveling silicone sealant added with the treated reinforcing filler has better yellowing resistance.
The amino-terminated hyperbranched flame-retardant component is introduced to the surface of the filler, and has good effect on improving the flame retardance of the silicone sealant. The amino-terminated hyperbranched flame retardant component has the structural characteristics of a large number of branched structures, a large number of cavities and the like, has better solubility compared with a linear polymer, and has the advantages that from the thermodynamic point of view, the surface energy of nano particles is inversely proportional to the particle size, the smaller the particle size is, the higher the surface energy is, the surface of the treated filler is rougher, the viscosity between the filler and the raw materials is better, the filler has better dispersibility due to the introduction of the hyperbranched structure, the phenomenon of agglomeration during filler blending can be improved, and the compatibility between the filler and a matrix can be enhanced.
More prominently, a large number of unique cavities in the amino-terminated hyperbranched flame retardant component can play a role in stabilizing and coating free radicals, so as to play a role in inhibiting the aging of the silicone sealant, and meanwhile, active hydrogen in the amino-terminated hyperbranched flame retardant component can be extracted by the free radicals, so as to play a role in chain transfer, namely, the occurrence of free radical chain reaction can be slowed down while the silicone sealant is aged, and the yellowing resistance of the silicone sealant is improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides an amino-terminated hyperbranched flame retardant component, which is prepared by the following steps:
adding hexachlorocyclotriphosphazene and ethylenediamine into tetrahydrofuran under the protection of nitrogen, stirring, dispersing, adding triethylamine, heating, refluxing for reaction for 12h, cooling to room temperature after the reaction is finished, washing with ethanol, and vacuum drying at 45 ℃ to constant weight to obtain an amino-terminated hyperbranched flame-retardant component; the mol ratio of the hexachlorocyclotriphosphazene to the ethylenediamine is 6:1, a step of; the dosage ratio of hexachlorocyclotriphosphazene, triethylamine and tetrahydrofuran is 2.5g:4.3g:100mL.
Example 2
The present example provides a coupling agent pretreated filler prepared by the steps of:
adding the filler into ethanol water solution, adding gamma-aminopropyl triethoxysilane, stirring for 24 hours at 20 ℃, washing and filtering with absolute ethanol after stirring, and vacuum drying for 24 hours at 60 ℃ to obtain the coupling agent pretreated filler. The dosage ratio of the filler, the ethanol water solution and the gamma-aminopropyl triethoxysilane is 10g:100mL:2g; the filler is white carbon black and calcium carbonate according to the mass ratio of 1:10, wherein the average particle size of the filler is 2-4 mu m; the volume fraction of the ethanol aqueous solution is 50%;
example 3
A production process of alkali-resistant self-leveling silicone sealant comprises the following steps:
firstly, adding the coupling agent pretreatment filler prepared in the embodiment 2 and methyl acrylate into methanol, setting the temperature to be 50 ℃, stirring and reacting for 5 hours, and vacuum-filtering after the reaction is finished, and vacuum-drying at 60 ℃ to obtain an intermediate product; adding the intermediate product and the amino-terminated hyperbranched flame-retardant component prepared in the example 1 into methanol, setting the temperature to 50 ℃, continuing to react for 6 hours, and after the reaction is finished, performing vacuum filtration and vacuum drying at 60 ℃ to obtain the reinforcing filler. The dosage ratio of the coupling agent pretreatment filler, methyl acrylate and methanol is 10g:3g:150mL; the dosage ratio of the intermediate product, the amino-terminated hyperbranched flame retardant component and the methanol is 10g:10g:300mL.
Secondly, adding 100 parts of 107 silicon rubber, 18 parts of reinforcing filler and 1 part of acetylated butoxyethyl ricinoleate into a planetary mixer according to parts by weight under the conditions of 110 ℃ and 0.09MPa of vacuum degree, stirring, mixing, dehydrating and blending for 3 hours, cooling, adding 10 parts of methyltributylketone oxime siloxane, and dispersing and stirring under vacuum to obtain a mixture; the viscosity of 107 silicone rubber was 80000 mPa.S.
Thirdly, adding 3 parts of gamma-aminopropyl triethoxysilane, 0.5 part of dibutyltin dilaurate and 3 parts of vinyl trimethoxysilane into the mixture at the temperature of 25 ℃, and dispersing and stirring under vacuum to prepare the alkali-resistant self-leveling silicone sealant.
Example 4
A production process of alkali-resistant self-leveling silicone sealant comprises the following steps:
firstly, adding the coupling agent pretreatment filler prepared in the embodiment 2 and methyl acrylate into methanol, setting the temperature to be 50 ℃, stirring and reacting for 5 hours, and vacuum-filtering after the reaction is finished, and vacuum-drying at 60 ℃ to obtain an intermediate product; adding the intermediate product and the amino-terminated hyperbranched flame-retardant component prepared in the example 1 into methanol, setting the temperature to 50 ℃, continuing to react for 7 hours, and after the reaction is finished, performing vacuum filtration and vacuum drying at 60 ℃ to obtain the reinforcing filler. The dosage ratio of the coupling agent pretreatment filler, methyl acrylate and methanol is 10g:3g:150mL; the dosage ratio of the intermediate product, the amino-terminated hyperbranched flame retardant component and the methanol is 10g:10g:300mL.
Secondly, adding 100 parts of 107 silicon rubber, 18 parts of reinforcing filler and 2 parts of acetylated butoxyethyl ricinoleate into a planetary mixer according to parts by weight under the conditions of 110 ℃ and 0.09MPa of vacuum degree, stirring, mixing, dehydrating and blending for 3 hours, cooling, adding 15 parts of methyltributylketone oxime siloxane, and dispersing and stirring under vacuum to obtain a mixture; the viscosity of 107 silicone rubber was 80000 mPa.S.
And thirdly, adding 5 parts of coupling agent, 1 part of dibutyltin dilaurate and 5 parts of vinyl trimethoxy silane into the mixture at the temperature of 25 ℃ and dispersing and stirring under vacuum to prepare the alkali-resistant self-leveling silicone sealant. The coupling agent is prepared by mixing gamma-aminopropyl triethoxysilane, 3-mercaptopropyl trimethoxysilane and the like by mass.
Example 5
A production process of alkali-resistant self-leveling silicone sealant comprises the following steps:
firstly, adding the coupling agent pretreatment filler prepared in the embodiment 2 and methyl acrylate into methanol, setting the temperature to be 50 ℃, stirring and reacting for 5 hours, and vacuum-filtering after the reaction is finished, and vacuum-drying at 60 ℃ to obtain an intermediate product; adding the intermediate product and the amino-terminated hyperbranched flame-retardant component prepared in the example 1 into methanol, setting the temperature to 50 ℃, continuing to react for 8 hours, and after the reaction is finished, performing vacuum filtration and vacuum drying at 60 ℃ to obtain the reinforcing filler. The dosage ratio of the coupling agent pretreatment filler, methyl acrylate and methanol is 10g:3g:150mL; the dosage ratio of the intermediate product, the amino-terminated hyperbranched flame retardant component and the methanol is 10g:10g:300mL.
Secondly, adding 100 parts of 107 silicon rubber, 21 parts of reinforcing filler and 4 parts of acetylated butoxyethyl ricinoleate into a planetary mixer according to parts by weight under the conditions of 110 ℃ and 0.09MPa of vacuum degree, stirring, mixing, dehydrating and blending for 3 hours, cooling, adding 17 parts of methyltributylketone oxime siloxane, and dispersing and stirring under vacuum to obtain a mixture; the viscosity of 107 silicone rubber was 80000 mPa.S.
And thirdly, adding 7 parts of gamma-aminopropyl triethoxysilane, 1.5 parts of dibutyltin dilaurate and 9 parts of vinyl trimethoxysilane into the mixture at the temperature of 25 ℃ and dispersing and stirring the mixture in vacuum to prepare the alkali-resistant self-leveling silicone sealant.
Comparative example 1
In this comparative example, as compared with example 5, the reinforcing filler was replaced with the coupling agent-pretreated filler prepared in example 2, and the remaining raw materials and preparation process were kept the same as in example 5.
Performance tests were performed on examples 3-5 and comparative example 1:
the specific test of yellowing resistance comprises: after the sealant is extruded from the rubber tube, the rubber tube is immediately put into a baking oven at 120 ℃ and yellowing time is recorded.
The tensile strength and the elongation at break were measured according to GB/T5282009 "measurement of tensile stress Strain Properties of vulcanized rubber or thermoplastic rubber". Placing the mould on foil paper, injecting sealant into polytetrafluoroethylene mould (mould depth is 2.0-2.1 mm) with a sealant gun, and scraping off excessive sealant with a scraper; vulcanizing at a temperature of 23+ -2deg.C and a relative humidity of 55+ -5% for 7d, taking out the film, cutting into dumbbell-shaped test pieces, and stretching at 500 mm/min.
The results are shown in Table 1:
TABLE 1
The prepared sample was immersed in a 5% sodium hydroxide solution at 45 ℃ for 15 days. The recorded part of the sample is softened and wrinkled, but has no dissolution and obvious performance change, the plasticizer in the invention selects acetylated butoxyethyl ricinoleate, and the addition amount is small, thus the invention has strong alkali corrosion resistance.
As can be seen from Table 1, comparative example 1 has a poor reinforcing effect relative to examples 4 to 5, i.e., the treated reinforcing filler has a better promoting effect on the improvement of properties. And the alkali-resistant self-leveling silicone sealant added with the treated reinforcing filler has better yellowing resistance.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The production process of the alkali-resistant self-leveling silicone sealant is characterized by comprising the following steps of:
firstly, adding a coupling agent pretreatment filler and methyl acrylate into methanol, setting the temperature to 50 ℃, stirring and reacting for 5 hours, and vacuum-filtering and vacuum-drying at 60 ℃ after the reaction is finished to obtain an intermediate product; adding the intermediate product and the amino-terminated hyperbranched flame retardant component into methanol, setting the temperature to 50 ℃, continuing to react for 6-8 hours, and vacuum-filtering after the reaction is finished, and vacuum-drying at 60 ℃ to obtain a reinforcing filler;
secondly, adding 107 silicon rubber, reinforcing filler and plasticizer into a planetary mixer under the conditions of 110 ℃ and 0.09MPa of vacuum degree, stirring, mixing, dehydrating and blending for 3 hours, cooling, adding a cross-linking agent, and dispersing and stirring under vacuum to obtain a mixture;
thirdly, adding a coupling agent, a catalyst and a water scavenger into the mixture at the temperature of 25 ℃, and dispersing and stirring under vacuum to prepare the alkali-resistant self-leveling silicone sealant;
the amino-terminated hyperbranched flame retardant component is prepared by the following steps:
under the protection of nitrogen, adding hexachlorocyclotriphosphazene and ethylenediamine into tetrahydrofuran, stirring, dispersing, adding triethylamine, heating, refluxing for reaction for 12h, cooling to room temperature after the reaction is finished, washing with ethanol, and vacuum drying at 45 ℃ to constant weight to obtain the amino-terminated hyperbranched flame-retardant component.
2. The process for producing an alkali-resistant self-leveling silicone sealant according to claim 1, wherein the coupling agent pretreatment filler is prepared by the steps of:
adding the filler into ethanol water solution, adding gamma-aminopropyl triethoxysilane, stirring for 24 hours at 20 ℃, washing and filtering with absolute ethanol after stirring, and vacuum drying for 24 hours at 60 ℃ to obtain the coupling agent pretreated filler.
3. The production process of the alkali-resistant self-leveling silicone sealant according to claim 2, wherein the filler is white carbon black and calcium carbonate according to a mass ratio of 1:10, wherein the average particle size of the filler is 2-4 mu m; the volume fraction of the aqueous ethanol solution was 50%.
4. The process for producing an alkali-resistant self-leveling silicone sealant according to claim 1, wherein the plasticizer is acetylated butoxyethyl ricinoleate.
5. The process for producing an alkali-resistant self-leveling silicone sealant according to claim 1, wherein the viscosity of the 107 silicone rubber is 80000 mPa-S.
6. The production process of the alkali-resistant self-leveling silicone sealant according to claim 1, wherein the coupling agent is one or two of gamma-aminopropyl triethoxysilane and 3-mercaptopropyl trimethoxysilane which are mixed according to any proportion.
7. The process for producing an alkali-resistant self-leveling silicone sealant according to claim 1, wherein the cross-linking agent is methyltributylketon oxime siloxane; the catalyst is dibutyl tin dilaurate.
8. The production process of the alkali-resistant self-leveling silicone sealant according to claim 1, wherein the alkali-resistant self-leveling silicone sealant comprises, by weight, 100 parts of 107 silicone rubber, 1-4 parts of a plasticizer, 10-17 parts of a cross-linking agent, 3-7 parts of a coupling agent, 18-21 parts of a reinforcing filler, 0.5-1.5 parts of a catalyst and 3-9 parts of a water scavenger.
9. An alkali-resistant self-leveling silicone sealant, characterized in that it is prepared according to the production process of any one of claims 1-8.
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| CN112831174A (en) * | 2021-02-20 | 2021-05-25 | 青岛理工大学 | Preparation and application of ZnO @ MOF @ polyphosphazene flame retardant |
| CN114560983A (en) * | 2022-02-21 | 2022-05-31 | 陕西科技大学 | Flame-retardant self-repairing waterborne polyurethane composite coating agent and preparation method and application thereof |
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