CN109762511B - Single-component dealcoholized room temperature vulcanized silicone sealant and preparation method thereof - Google Patents
Single-component dealcoholized room temperature vulcanized silicone sealant and preparation method thereof Download PDFInfo
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Abstract
The invention provides a single-component dealcoholized room temperature vulcanized silicone sealant, a preparation method and application thereof, and relates to the technical field of silicone sealants. The sealant comprises the following raw materials in parts by weight: 100 parts of poly alkoxy end-capped polydimethylsiloxane, 0-10 parts of dimethyl silicone oil, 2-6 parts of cross-linking agent, 5-15 parts of filler, 0.8-2.5 parts of tackifier and 0.1-0.6 part of tin catalyst. The single-component dealcoholized room temperature vulcanized silicone sealant has the characteristics of good storage stability, good adhesion and good yellowing resistance.
Description
Technical Field
The invention relates to the technical field of organosilicon sealants, in particular to a single-component dealcoholized room temperature vulcanized silicone sealant and a preparation method and application thereof.
Background
The dealcoholized silicone sealant has the characteristics of methanol removal by reaction, no color and no smell, and no corrosion to a base material, so the dealcoholized silicone sealant has better environmental protection performance than acid glue and oxime glue. Modern industries, particularly the processing and manufacturing industries of electronic components, develop rapidly, the demand for pure adhesives is also rapidly expanded, and although the de-acetone silicone rubber can also be used as a pure grade adhesive for the electronic components, the cost is high, and the development is limited. The dealcoholized silicone rubber has no corrosivity to metal and low price, can be widely used in electronic products, and becomes a research hotspot.
However, the existing dealcoholization type room temperature vulcanized silicone sealant has the problems of insufficient storage stability, adhesion and yellowing resistance, is easy to pollute when being used for adhesion of electronic and electric appliances, and limits the popularization and the application of the dealcoholization type room temperature vulcanized silicone sealant.
Disclosure of Invention
Therefore, the single-component dealcoholized room temperature vulcanized silicone sealant and the preparation method thereof are needed to solve the problems of insufficient storage stability, adhesion and yellowing resistance of the existing dealcoholized room temperature vulcanized silicone sealant.
The single-component dealcoholized room temperature vulcanized silicone sealant comprises the following raw materials in parts by weight:
the single-component dealcoholized room temperature vulcanized silicone sealant is prepared by end-capping the poly dimethyl siloxane end-capped by the polyalkoxy by using an end-capping agent in the presence of an acid catalyst; because the end-capping system is adopted, the generation of the monoalkoxy end group without crosslinking capacity is reduced, and therefore, the sealant has excellent storage stability; different cross-linking agents are adopted for composite use, so that excellent adhesion is obtained; the tin catalytic system is adopted to replace a titanium catalytic system, so that excellent yellowing resistance is obtained.
In one embodiment, the part of the dimethyl silicone oil is 2 to 10 parts.
In one embodiment, the dimethicone has a viscosity of 50 to 500mPa · s at 25 ℃.
In one embodiment, the cross-linking agent is selected from: at least one of methyltrimethoxysilane, vinyltrimethoxysilane, tetramethoxysilane and tetraethoxysilane.
In one embodiment, the filler is selected from: the specific surface area is more than or equal to 150m2Per g fumed silica; the specific surface area is measured by a BET method, and the fumed silica can be hydrophilic fumed silica and hydrophobic fumed silica.
In one embodiment, the tackifier is selected from: gamma-aminopropyltriethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane, and beta- (3, 4-epoxycyclohexane) ethyltrimethoxysilane.
In one embodiment, the tin catalyst is selected from: at least one of dibutyltin dilaurate, dibutyltin bis (ethyl acetoacetate), dibutyltin bis (acetylacetone), dibutyltin bis (acetoxy) and ethyl orthosilicate. Under the same condition, the dosage of the titanium catalyst is 30 times of that of the tin catalyst, and the tin catalyst system is more economical.
In one embodiment, the poly-alkoxy-terminated polydimethylsiloxane is prepared from the following raw materials in parts by weight:
in one embodiment, the α, ω -dihydroxypolydimethylsiloxane has a viscosity of 10000-.
In one embodiment, the capping agent is selected from: at least one of methyltrimethoxysilane, vinyltrimethoxysilane, tetramethoxysilane and tetraethoxysilane.
In one embodiment, the acidic catalyst is selected from the group consisting of: at least one of dibutyl phosphate, monobutyl phosphate and di (2-ethylhexyl) phosphate.
In one embodiment, the basic neutralizing agent is selected from: at least one of dibutylamine, triethylamine, sodium hydroxide and potassium hydroxide.
The invention also comprises a preparation method of the poly-alkoxy-terminated polydimethylsiloxane, which comprises the following steps:
step one, end capping reaction: uniformly mixing alpha, omega-dihydroxy polydimethylsiloxane and an end-capping reagent at 20-30 ℃, adding an acid catalyst, mixing, and carrying out end-capping reaction;
step two, neutralization reaction: and after the end-capping reaction is finished, adding an alkaline neutralizing agent for neutralization to obtain the poly-alkoxy end-capped polydimethylsiloxane.
In the preparation method, the temperature is controlled to be 20-30 ℃, the viscosity deviation range of the alpha, omega-dihydroxy polydimethylsiloxane is +/-5000 mPa & s, the quality of the prepared poly-alkoxy-terminated polydimethylsiloxane is ensured, and the quality of the single-component dealcoholized room temperature vulcanized silicone sealant is further ensured.
In one embodiment, in the first step: the end-capping reaction is carried out in a reaction kettle, the temperature is 25 ℃, the viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is 10000-100000 mPa.s, the vacuum degree in the reaction kettle is less than or equal to-0.08 MPa, the stirring speed is 600-1000 rpm, the alpha, omega-dihydroxy polydimethylsiloxane and the end-capping agent are stirred and mixed for 5-20 min, an acid catalyst is added, and the stirring is carried out for 20-60 min. If the amount of the acidic catalyst is too small, the viscosity of the α, ω -dihydroxypolydimethylsiloxane will vary to more than ± 5000mPa · s, and the viscosity will increase significantly. During the capping reaction, whether the capping reaction is completed can be tested by the following method: and (3) taking a small amount of sample, dropwise adding a proper amount of tetraisopropyl titanate, quickly stirring, and finishing end capping if no viscosity peak exists.
In one embodiment, in the second step: and adding an alkaline neutralizing agent, controlling the pH to be 6-8, and stirring for 30-70 min at the same temperature and stirring speed to obtain the poly-alkoxy-terminated polydimethylsiloxane. pH values below or outside this range can lead to poor sealant performance.
The invention also discloses a preparation method of the single-component dealcoholized room temperature vulcanized silicone sealant, which comprises the following steps: mixing poly dimethyl siloxane with a plurality of alkoxy end capping, dimethyl silicone oil and a cross-linking agent for reaction; then adding the filler and mixing uniformly; and then adding a tackifier and a tin catalyst, and mixing and reacting to obtain the single-component dealcoholized room temperature vulcanized silicone sealant.
In one embodiment, at the temperature of 10-40 ℃, the vacuum degree of-0.08-0.1 MPa, adding poly-alkoxy-terminated polydimethylsiloxane, dimethyl silicone oil and a cross-linking agent into a planetary mixer, stirring for 10-30min, adding a filler, continuing stirring for 30-50min, adding a tackifier and a tin catalyst, and stirring for 20-50min to obtain the single-component dealcoholized room-temperature vulcanized silicone sealant.
The invention also comprises the application of the single-component dealcoholized room temperature vulcanized silicone sealant in the sealing and bonding of electronic appliances, circuit boards, mirrors, artware and LED lamps.
Compared with the prior art, the invention has the following beneficial effects:
the single-component dealcoholized room temperature vulcanized silicone sealant has the characteristics of good room temperature vulcanization property, convenient use and good storage stability; the adhesive also has the advantages of good connectivity, yellowing resistance, no corrosion to a base material and no pollution, and can be widely applied to sealing and bonding of electronic appliances, circuit boards, mirrors, artware and LED lamps.
The preparation method of the single-component dealcoholized room temperature vulcanized silicone sealant has simple and feasible process, and the end-capping system and the tin catalytic system ensure lower production cost and have better economic benefit and social benefit.
Detailed Description
In order that the invention may be more fully understood, preferred embodiments will now be given. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The starting materials used in the following examples are commercially available, unless otherwise specified.
All the following examples and comparative examples were carried out at 10 to 40 ℃.
Example 1
The single-component dealcoholized room temperature vulcanized silicone sealant is prepared by the following method:
(1) putting 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000 mPas and 3 parts of tetramethoxysilane into a stirring kettle, uniformly stirring at 25 ℃ and vacuum degree of-0.08 MPa, wherein the stirring speed is 1000rpm, then adding 1.2 parts of dibutyl phosphate, adding 0.96 part of dibutylamine after stirring in vacuum for 30min, and continuing stirring in vacuum for 70min to obtain the poly-alkoxy-terminated polydimethylsiloxane;
(2) adding 100 parts of the poly-alkoxy-terminated polydimethylsiloxane, 10 parts of simethicone and 4 parts of methyltrimethoxysilane into a stirring kettle, vacuumizing and stirring for 20min, adding the BET specific surface area of 150m210 parts of hydrophilic fumed silica per gram, vacuumizing and stirring at a high speed for 40min at the rotating speed of 1200rpm, then sequentially adding 1 part of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, 0.5 part of gamma-glycidoxypropyltrimethoxysilane and 0.3 part of a compound of dibutyltin bis (acetoxyl) and ethyl orthosilicate, and stirring for 20-50min under a vacuum condition to obtain the hydrophilic fumed silica.
Example 2
The single-component dealcoholized room temperature vulcanized silicone sealant is prepared by the following method:
(1) putting 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 80000 mPas and 2 parts of tetramethoxysilane into a stirring kettle, uniformly stirring at 25 ℃ and the vacuum degree of-0.08 MPa, wherein the stirring speed is 1000rpm, adding 1 part of dibutyl phosphate, adding 0.8 part of dibutylamine after stirring in vacuum for 30min, and continuously stirring in vacuum for 70min to obtain the poly-alkoxy-terminated polydimethylsiloxane;
(2) adding 100 parts of the poly dimethyl siloxane blocked by the alkoxy groups and 4 parts of vinyl trimethoxy silane into a planetary mixer, vacuumizing and stirring for 20min, adding the mixture with the BET specific surface area of 150m210 parts of hydrophobic fumed silica per gram, vacuumizing and stirring at high speed for 40min, sequentially adding 1 part of gamma-aminopropyl trimethoxy silane, 0.5 part of beta- (3, 4-epoxy cyclohexane) ethyl trimethoxy silane and 0.3 part of dibutyltin bis (ethyl acetoacetate), and stirring for 20-50min under vacuum conditions to obtain the hydrophobic fumed silica.
Example 3
The single-component dealcoholized room temperature vulcanized silicone sealant is prepared by the following method:
(1) putting 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000 mPas and 2 parts of tetramethoxysilane into a stirring kettle, uniformly stirring at 25 ℃ and vacuum degree of-0.08 MPa, wherein the stirring speed is 1000rpm, adding 1 part of di (2-ethylhexyl) phosphate, stirring for 30min in vacuum, adding 0.8 part of triethylamine, and continuing to stir for 70min in vacuum to obtain the poly-alkoxy-terminated polydimethylsiloxane;
(2) adding 100 parts of the poly dimethyl siloxane blocked by the poly alkoxy and 3 parts of tetraethoxysilane into a planetary stirrer, vacuumizing and stirring for 20min, and adding 150m BET specific surface area210 parts of hydrophilic fumed silica per gram, vacuumizing, stirring at a high speed for 40min, sequentially adding 1 part of gamma-aminopropyltriethoxysilane, 0.5 part of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane and 0.3 part of dibutyltin dilaurate, and stirring for 20-50min under a vacuum condition to obtain the hydrophilic fumed silica.
Example 4
The single-component dealcoholized room temperature vulcanized silicone sealant is prepared by the following method:
(1) 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 20000 mPas, 10 parts of dimethyl silicone oil and 3 parts of tetramethoxysilane are put into a stirring kettle and are uniformly stirred at the temperature of 25 ℃ and the vacuum degree of-0.08 MPa, the stirring speed is 1000rpm, 1.2 parts of dibutyl phosphate is added, after 30min of vacuum stirring, 0.96 part of dibutylamine is added, and the vacuum stirring is continued for 70min, so that the poly-alkoxy-terminated polydimethylsiloxane is obtained;
(2) adding 100 parts of the poly dimethyl siloxane blocked by the alkoxy groups and 4 parts of methyltrimethoxysilane into a planetary mixer, vacuumizing and stirring for 20min, adding the mixture with the BET specific surface area of 150m210 parts of hydrophilic fumed silica per gram, vacuumizing and stirring at high speed for 40min, sequentially adding 1 part of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, 0.5 part of gamma-glycidoxypropyltrimethoxysilane and 0.3 part of dibutyltin diacetate, and stirring under vacuum condition for 20-50min to obtain the finished product.
For comparison with the above examples, the following comparative examples were set.
Comparative example 1
The single-component dealcoholized room temperature vulcanized silicone sealant is prepared by the following method:
adding 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000 mPas and 7 parts of methyltrimethoxysilane into a stirring kettle, vacuumizing and stirring for 20min, adding BET specific surface area of 150m210 parts of hydrophilic fumed silica per gram, vacuumizing and stirring at high speed for 40min, sequentially adding 1 part of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, 0.5 part of gamma-glycidoxypropyltrimethoxysilane and 4 parts of tetraisopropyl titanate bis (ethyl acetoacetate), and stirring under vacuum condition for 20-50min to obtain the finished product.
Comparative example 2
The single-component dealcoholized room temperature vulcanized silicone sealant is prepared by the following method:
(1) 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 80000 mPas and 3 parts of tetramethoxysilane are put into a stirring kettle and are uniformly stirred under a vacuum state, 1 part of dibutyl phosphate is added, after 30min of vacuum stirring, 0.8 part of dibutylamine is added, and vacuum stirring is continued for 70min, so that the poly-alkoxy-terminated polydimethylsiloxane is obtained;
(2) adding 100 parts of the poly dimethyl siloxane blocked by the alkoxy groups and 4 parts of methyltrimethoxysilane into a planetary mixer, vacuumizing and stirring for 20min, adding the mixture with the BET specific surface area of 150m210 parts of hydrophilic fumed silica per gram, vacuumizing and stirring at high speed for 40min, sequentially adding 1 part of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, 0.5 part of gamma-glycidoxypropyltrimethoxysilane and 4 parts of tetraisopropyl titanate bis (ethyl acetoacetate), and stirring under vacuum condition for 20-50min to obtain the finished product.
Comparative example 3
A single-component dealcoholized room temperature vulcanized silicone sealant is prepared by the method which is basically the same as that in example 1, except that: the amount of the alkaline neutralizing agent in the end capping reaction is changed to 2 parts.
Examples of the experiments
The sealants prepared in the above examples and comparative examples were subjected to performance tests including a tack free time test, an adhesion test, a test for tensile adhesive strength and elongation at 23 ℃, a test for storage stability, and the like. The test methods or standards are as follows:
(1) surface drying time: according to GB/T13477.5-2003 (test method for building sealants part 5: determination of open time).
(2) And (3) testing the adhesion: the adhesion strength was tested according to GB/T7124-2008 and the adhesion to various substrates was visually observed.
(3) Tensile bond strength and elongation at 23 ℃: tested according to GB/T528-2009.
(4) Yellowing resistance test: and (3) beating the glue material on a glass sheet to form a glue strip with the diameter of 4-10mm and the length of 10-15cm, after the glue material is completely cured, placing the glue strip in an oven at 100 ℃ for 300 hours, and observing the yellowing degree of the glue strip.
(5) Testing of storage stability: and placing the prepared sealant in an oven at 100 ℃ for 1 day, 3 days and 5 days, and beating the sealant to test the surface drying time and the curing condition.
The results of the above tests are shown in the following table.
TABLE 1 Performance test results for the single-component dealcoholized room temperature vulcanized Silicone sealants
From the above results, it can be proved that the dealcoholization type room temperature vulcanized silicone sealant prepared in the embodiment of the invention adopts a capped 107 glue tin catalytic system, the production process has no viscosity peak, the prepared sealant has good storage stability, high curing speed, no yellowing, good adhesion to a base material and low production cost, and small molecular alcohol substances released in the curing process have no corrosion to the base material, and can be widely applied to sealing adhesion of electronic components and other non-structural sealing adhesion.
The sealant prepared in the comparative example has poor effect because the alpha, omega-dihydroxy polydimethylsiloxane blocked by the polyalkoxy is not selected (comparative example 1) or the catalyst is not selected (comparative example 2). In comparative example 3, the amount of the alkali neutralizing agent in the preparation of the polyalkoxy-terminated polydimethylsiloxane exceeded the amount of the present invention, and the effect was also poor.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. The single-component dealcoholized room temperature vulcanized silicone sealant is characterized by comprising the following raw materials in parts by weight:
the poly dimethyl siloxane terminated by the polyalkoxy group is prepared by the following raw materials in parts by weight:
the viscosity of the alpha, omega-dihydroxy polydimethylsiloxane at 25 ℃ is 10000-100000 mPas;
the end-capping agent is selected from: at least one of methyltrimethoxysilane, vinyltrimethoxysilane, tetramethoxysilane and tetraethoxysilane;
the acidic catalyst is selected from: at least one of dibutyl phosphate, monobutyl phosphate and di (2-ethylhexyl) phosphate;
the alkaline neutralizing agent is selected from: at least one of dibutylamine, triethylamine, sodium hydroxide and potassium hydroxide;
the polyalkoxy-terminated polydimethylsiloxane is prepared by the following method:
step one, end capping reaction: uniformly mixing alpha, omega-dihydroxy polydimethylsiloxane and an end-capping reagent at 20-30 ℃, adding an acid catalyst, mixing, and carrying out end-capping reaction;
step two, neutralization reaction: and after the end-capping reaction is finished, adding an alkaline neutralizing agent for neutralization to obtain the poly-alkoxy end-capped polydimethylsiloxane.
2. The one-component dealcoholized room temperature vulcanized silicone sealant according to claim 1, wherein,
the viscosity of the dimethyl silicone oil at 25 ℃ is 50-500mPa & s;
the cross-linking agent is selected from: at least one of methyltrimethoxysilane, vinyltrimethoxysilane, tetramethoxysilane and tetraethoxysilane;
the filler is selected from: the specific surface area is more than or equal to 150m2Per g fumed silica;
the tackifier is selected from: at least one of gamma-aminopropyltriethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane, and beta- (3, 4-epoxycyclohexane) ethyltrimethoxysilane;
the tin catalyst is selected from: at least one of dibutyltin dilaurate, dibutyltin bis (ethyl acetoacetate), dibutyltin bis (acetylacetone), dibutyltin bis (acetoxy) and ethyl orthosilicate.
3. The one-component dealcoholized room temperature vulcanized silicone sealant according to claim 1, wherein,
in the first step: the end-capping reaction is carried out in a reaction kettle, the temperature is 24-26 ℃, the viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is 10000-plus 100000mPa & s, the vacuum degree in the reaction kettle is less than or equal to-0.08 MPa, the stirring speed is 600-1000 rpm, the alpha, omega-dihydroxy polydimethylsiloxane and the end-capping agent are stirred and mixed for 5-20 min, an acid catalyst is added, and the stirring is carried out for 20-60 min;
in the second step: and adding an alkaline neutralizing agent, controlling the pH to be 6-8, and stirring for 30-70 min at the same temperature to obtain the poly-alkoxy-terminated polydimethylsiloxane.
4. A method for preparing the one-component dealcoholized room temperature vulcanized silicone sealant according to any one of claims 1 to 3, which comprises the steps of: mixing poly dimethyl siloxane with a plurality of alkoxy end capping, dimethyl silicone oil and a cross-linking agent for reaction; then adding the filler and mixing uniformly; and then adding a tackifier and a tin catalyst, and mixing and reacting to obtain the single-component dealcoholized room temperature vulcanized silicone sealant.
5. The preparation method of the one-component dealcoholization type room temperature vulcanized silicone sealant as claimed in claim 4, wherein the one-component dealcoholization type room temperature vulcanized silicone sealant is prepared by adding the polyalkoxy-terminated polydimethylsiloxane, the dimethicone and the cross-linking agent into a planetary mixer at the temperature of 10-40 ℃ and the vacuum degree of-0.08-0.1 MPa, stirring for 10-30min, adding the filler, continuing stirring for 30-50min, adding the tackifier and the tin catalyst, and stirring for 20-50 min.
6. Use of the one-component dealcoholized room temperature vulcanized silicone sealant according to any one of claims 1 to 3 for the sealing and bonding of electronic appliances, circuit boards, mirrors, artware and LED lamps.
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| CN110577747B (en) * | 2019-10-12 | 2022-04-12 | 广州福泽新材料有限公司 | Room temperature vulcanized fluorosilicone rubber and preparation method thereof |
| CN112143451A (en) * | 2020-10-13 | 2020-12-29 | 广州市高士实业有限公司 | Single-component dealcoholized room temperature vulcanized silicone sealant and preparation method thereof |
| CN112898947A (en) * | 2021-02-08 | 2021-06-04 | 佛山市元通胶粘实业有限公司 | Dealcoholized organosilicon sealant by gas phase method and preparation method thereof |
| CN115449338B (en) * | 2022-10-20 | 2023-11-07 | 浙江新安化工集团股份有限公司 | Dealcoholized silicone sealant and preparation method thereof |
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