CN108314990B - High-strength high-temperature-resistant silicone sealant and preparation method thereof - Google Patents
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Abstract
The invention discloses a high-strength high-temperature-resistant silicone sealant which comprises the following components: organopolysiloxane, modified nano kaolin, modified silicone oil, a silane composite cross-linking agent, a compound silane coupling agent and a catalyst. The invention has the following advantages: 1. the surface modification is carried out on the nano kaolin by using the azido silane, so that the silicone sealant has better reinforcement effect, can replace calcium carbonate and partial white carbon black, reduce the production cost, improve the mechanical properties of the product such as tensile strength and the like, and endow the material with special physicochemical properties such as corrosion resistance, flame retardance, insulation and the like; 2. compared with common long-chain alkyl silicone oil, the phenyl hydrogen-containing silicone oil modified by the long-chain alkyl has better high temperature resistance, and the introduction of the long-chain alkyl can enhance the hydrophobicity of the silicone oil and improve the surface performance of the silicone oil, so that the silicone oil has better compatibility with organic polymers; 3. the compound silane coupling agent is adopted to improve the adhesive property of the silicone sealant to base materials such as metal, plastic, stainless steel and the like.
Description
Technical Field
The invention relates to a silicone sealant, in particular to a high-strength high-temperature-resistant silicone sealant.
Background
The silicone sealant has good electrical insulation performance, chemical stability, weather aging resistance, displacement resistance, elastic recovery capability and small shrinkage after curing, has good bonding force on materials such as metal, aluminum doors and windows, plastics and the like, is widely applied to the fields of electronic and electrical products, buildings, aviation, automobiles, medical and health materials and the like, and becomes an indispensable material in the industry at present. With the increasing demand for silicone sealants, the requirements for high temperature resistance and high strength of silicone sealants are also increasing.
The common silicone sealant in the market has generally poor high-temperature resistance and low strength, and the application of novel high-temperature resistant materials and the like can improve the high-temperature resistance and tensile property of products, but the cost of the products is improved, so that the industrialization of the products is influenced to a certain degree.
There are many published studies on silicone sealants. CN201710077333.8 provides a formula of a high-temperature-resistant silicone sealant, although the high-temperature resistance can reach 300 ℃, in the formula, in order to improve the high-temperature resistance of the product, excessive high-temperature-resistant filler metal oxide is added, and the tensile property of the silicone sealant is seriously influenced. Patent CN201310002398.8 also provides a silicone sealant formula with high temperature resistance, which improves the high temperature resistance of the product by adding zirconium-based ceramic powder, but the zirconium-based ceramic powder has high cost and is not beneficial to the industrialization of the product.
The above patent provides different solutions for the research of different silicone sealant product systems and for the performances of high temperature resistance and the like, but no solution is provided for improving the high temperature resistance, the tensile property and the like of the silicone sealant while reducing the production cost.
Therefore, the high-strength high-temperature-resistant silicone sealant is developed, the production cost of enterprises is reduced, the high-temperature-resistant performance and the tensile property of the silicone sealant are improved, and certain economic benefits are achieved.
Disclosure of Invention
The invention aims to provide a high-strength high-temperature-resistant silicone sealant, which is used for solving the defects of the prior art and reducing the production cost.
The invention provides a high-strength high-temperature-resistant silicone sealant which comprises the following components in parts by weight:
40-70 parts of organopolysiloxane
30-60 parts of modified nano kaolin
0.2-5 parts of modified silicone oil
3-10 parts of silane composite cross-linking agent
0.5-3 parts of compound silane coupling agent
0-0.5 part of catalyst;
the organopolysiloxane comprises one or more linear polymers having the following structural formula:
wherein R is1、R2、R3、R6、R7、R8Is C2-C4Hydrocarbyloxy groups formed from unsaturated hydrocarbon radicals of (2), R4、R5Is C1-C3M is 5500-8000.
The viscosity of the organopolysiloxane at 25 ℃ ranges from 60000-900000 mPa.s.
The modified nano kaolin is nano kaolin subjected to surface treatment by azido silane, and the azido silane is [ YR' SiRaX3-aR is alkyl, aryl, cycloalkyl, alkaryl, aralkyl; r' is divalent alkyl, haloalkyl, carbonylalkyl, thioalkyl, etc.; y is N3COO-、N3CONH-、N3SO2-、N3-; and a =0 ~ 3. The nano kaolin has the characteristics of high surface energy, hydrophilic and oleophobic surface and extremely easy agglomeration, is difficult to be uniformly dispersed when being added into the silicone sealant and influences the product performance, therefore, the azido silane is adopted to carry out surface modification on the nano kaolin, so that the surface of nano kaolin particles is coated with a layer of organic matter, the nano kaolin particles are changed from oleophobic and hydrophilic to hydrophobic and oleophilic, thus not only enhancing the compatibility and the bonding force of the nano kaolin and the organic polysiloxane matrix, but also improving the dispersibility of the nano kaolin and increasing the filling amount thereof, thereby achieving the purpose of improving the physical performance of the silicone sealant, the nano kaolin after surface modification has better reinforcing effect on the silicone sealant, can replace calcium carbonate and white carbon black partially, so as to reduce production cost, improve mechanical properties such as tensile strength and the like of the material, and endow the material with special physical and chemical properties such as corrosion resistance, flame retardance, insulation and the like.
The modified silicone oil is phenyl hydrogen-containing silicone oil modified by long-chain alkyl, and the long-chain alkane is at least one of long-chain alkane such as 1-dodecene, 3-pentadecene and the like. The phenyl silicone oil is obtained by substituting part of methyl groups in the methyl silicone oil by phenyl groups, and has the advantages of high temperature resistance and low temperature resistance compared with other silicone oils. Compared with common long-chain alkyl silicone oil, the phenyl hydrogen-containing silicone oil modified by long-chain alkyl has better high temperature resistance and higher refractive index, and the introduction of the long-chain alkyl can enhance the hydrophobicity of the silicone oil and improve the surface performance of the silicone oil, so that the silicone oil has better compatibility with organic polymers.
The silane composite cross-linking agent is at least two of methyl tributyl ketoxime silane, vinyl tributyroxime silane, phenyl tributyroxime silane, methyl triacetoneoxime silane, methyl vinyl dibutyroxime silane, methyl phenyl dibutyroxime silane and diphenyl dibutyroxime silane, and is added according to a certain weight ratio. The silane composite cross-linking agent belongs to a specific additive, and can optimize a cross-linked three-dimensional network structure of the cured silicone sealant by using a proper addition amount, improve the mechanical properties of the cured silicone sealant, such as elasticity, elongation and the like, and further realize high displacement capacity of the cured silicone sealant.
The compound silane coupling agent is prepared from a mixture of an aminosilane coupling agent and an isocyanate silane coupling agent in parts by weight: isocyanate silane coupling agent = 2-3: 1-2. Wherein the aminosilane coupling agent is at least one of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, N-beta-aminoethyl gamma-aminopropyltrimethoxysilane, N-beta-aminoethyl gamma-aminopropyltriethoxysilane, N-beta-aminoethyl gamma-aminopropylmethyldimethoxysilane, N-beta-aminoethyl gamma-aminopropylmethyldiethoxysilane and the like; the isocyanate silane coupling agent is at least one of isocyanate propyl trimethoxy silane, isocyanate propyl triethoxy silane and the like.
The catalyst is any one of dibutyltin diacetate, dibutyltin dilaurate, dioctyltin dilaurate, stannous octoate, dimethyltin dineodecanoate and dibutyltin bis (beta-diketone ester).
The preparation method of the high-strength high-temperature-resistant silicone sealant comprises the following steps:
a. adding the organopolysiloxane, the modified nano kaolin and the modified silicone oil into a kneading machine according to the weight part ratio, dehydrating and blending for 60-120min at the temperature of 130-150 ℃ and the vacuum degree of 0.06-0.099MPa, and cooling to obtain a base adhesive;
b. adding the silane composite cross-linking agent, the compound silane coupling agent and the catalyst into a stirrer, and stirring for 10-20min at room temperature to obtain a mixture;
c. adding the base glue into a stirrer at room temperature, stirring for 10-20min, adding the mixture, and reacting at the vacuum degree of 0.08-0.099MPa and the rotation speed of 10-800rpm for 30-60min to obtain the high-strength high-temperature-resistant silicone sealant.
And the steps b and c are carried out under the protection of nitrogen.
The test result of the silicone sealant prepared by the invention shows that compared with the prior art, the silicone sealant has the following advantages: 1, performing surface modification on nano kaolin by using azido silane, adding the azido silane into silicone sealant, having a better reinforcing effect, being capable of replacing calcium carbonate and partial white carbon black, reducing the production cost, improving the mechanical properties of the material such as tensile strength and the like, and endowing the material with special physicochemical properties such as corrosion resistance, flame retardance, insulation and the like;
2. compared with common long-chain alkyl silicone oil, the phenyl hydrosilicon oil modified by the long-chain alkyl has better high temperature resistance, and the introduction of the long-chain alkyl can not only enhance the hydrophobicity of the silicone oil, but also improve the surface performance of the silicone oil, so that the silicone oil has better compatibility with organic polymers, and the high temperature resistance can be improved to 300 ℃;
3. the compound silane coupling agent is adopted, so that the adhesive property of the silicone sealant to base materials such as metal, plastic, stainless steel and the like is improved, and a certain adhesive strength is achieved to special base materials which are difficult to adhere.
Detailed Description
The present invention is illustrated by the following examples, but the present invention is not limited to these examples. Modifications to the embodiments of the invention or equivalent substitutions of parts of technical features without departing from the spirit of the invention are intended to be covered by the scope of the claims of the invention.
Example 1
a. Adding 60 parts of alpha, omega-dipropenyloxy polydimethylsiloxane with the viscosity of 6000mPa.s, 30 parts of azido formyl oxygen hydrocarbon silane modified nano kaolin and 3 parts of 1-dodecene modified phenyl hydrogen-containing silicone oil into a kneading machine, dehydrating and blending for 15-25min at 140 ℃ and the vacuum degree of 0.06-0.099MPa, and cooling to obtain base adhesive;
b. methyl-tributyrinoxime silane: diphenyldibutyloximosilane = 2: 1, 5 parts of a mixture of diphenyldibutyloxime silanaminopropyltriethoxysilane: isocyanatopropyltrimethoxysilane = 2: 1, adding 1.9 parts of the mixture of 1 and 0.1 part of dibutyltin dilaurate into a stirrer, and stirring for 10-20min at room temperature to obtain a mixture;
c. adding the base glue into a stirrer at room temperature, stirring for 15min, adding the mixture, and reacting for 50min at the vacuum degree of 0.08-0.099MPa and the rotating speed of 10-800rpm to obtain the high-strength high-temperature-resistant silicone sealant. And the steps b and c are carried out under the protection of nitrogen.
Example 2
a. Adding 35 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 90000mPa.s, 7 parts of single-end hydroxyl polydimethylsiloxane with the viscosity of 1000mPa.s, 50 parts of azido sulfonyl hydrocarbon silane modified nano kaolin and 2 parts of 3-pentadecene modified phenyl hydrogen-containing silicone oil into a kneading machine, dehydrating and blending for 60min at 135 ℃ and the vacuum degree of 0.06-0.099MPa, and cooling to obtain base adhesive;
b. phenyl tributyrinoxime silane: methyl vinyl dibutyloximosilane = 3: 1, 4 parts of a mixture of gamma-aminopropyltrimethoxysilane: isocyanatopropyltriethoxysilane = 2: 2 and 0.1 part of dineodecanoic acid dimethyl tin, adding the mixture into a stirrer, and stirring for 20min at room temperature to obtain a mixture;
c. adding the base glue into a stirrer at room temperature, stirring for 15min, adding the mixture, and reacting for 40min at the vacuum degree of 0.08-0.099MPa and the rotating speed of 10-800rpm to obtain the high-strength high-temperature-resistant silicone sealant. And the steps b and c are carried out under the protection of nitrogen.
Example 3
a. Adding 40 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 80000mPa.s, 13 parts of single-end hydroxyl polydimethylsiloxane with the viscosity of 500mPa.s, 40 parts of azido formamide hydrocarbon silane modified nano kaolin and 2 parts of 2-tridecene modified phenyl hydrogen-containing silicone oil into a kneader, dehydrating and blending for 60min at 145 ℃ and under the vacuum degree of 0.06-0.099MPa, and cooling to obtain base adhesive;
b. vinyl tributyrinoxime silane: methyl phenyl dibutyloximosilane = 2: 1, N- β aminoethyl γ aminopropyltrimethoxysilane: isocyanatopropyltriethoxysilane = 3: 1, 1.95 parts of the mixture and 0.05 part of dimethyltin dineodecanoate are added into a stirrer and stirred for 20min at room temperature to obtain a mixture;
c. adding the base glue into a stirrer at room temperature, stirring for 20min, adding the mixture, and reacting for 45min at the vacuum degree of 0.08-0.099MPa and the rotating speed of 10-800rpm to obtain the high-strength high-temperature-resistant silicone sealant. And the steps b and c are carried out under the protection of nitrogen.
Comparative example 4
a. Adding 45 parts of alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000mPa.s, 25 parts of nano calcium carbonate, 20 parts of ferric oxide and 2 parts of fumed silica into a kneading machine according to the weight parts, dehydrating and blending for 60min at 135 ℃ under the vacuum degree of 0.06-0.099MPa, and cooling to obtain a base adhesive;
b. adding 1 part of vinyl tributyrinoxime silane, 5 parts of methyl tributyrinoxime silane, 1.8 parts of gamma-aminopropyltriethoxysilane and 0.2 part of dibutyltin diacetate into a stirrer, and stirring at room temperature for 20min to obtain a mixture;
c. adding the base glue into a stirrer at room temperature, stirring for 10min, adding the mixture, and reacting for 45min at the vacuum degree of 0.08-0.099MPa and the rotating speed of 10-800rpm to obtain the high-strength high-temperature-resistant silicone sealant. And the steps b and c are carried out under the protection of nitrogen.
Comparative example 5
a. Adding 40 parts of alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 30000mPa.s, 30 parts of active nano calcium carbonate, 20 parts of bismaleimide and 2 parts of fumed silica into a kneading machine, dehydrating and blending for 60min at 135 ℃ under the vacuum degree of 0.06-0.099MPa, and cooling to obtain base rubber;
b. adding 2 parts of vinyl tributyrinoxime silane, 4 parts of propyl tributyrinoxime silane, 1.9 parts of gamma-aminopropyl triethoxysilane and 0.1 part of dibutyltin diacetate into a stirrer, and stirring at room temperature for 20min to obtain a mixture;
c. adding the base glue into a stirrer at room temperature, stirring for 10min, adding the mixture, and reacting for 45min at the vacuum degree of 0.08-0.099MPa and the rotating speed of 10-800rpm to obtain the high-strength high-temperature-resistant silicone sealant. And the steps b and c are carried out under the protection of nitrogen.
The related performances of the high-strength high-temperature-resistant silicone sealants of examples 1 to 3 and comparative examples 4 to 5 were tested by the following methods:
1. determination of tensile Strength: the assay was performed as specified in GB/T528-.
2. Determination of elongation: the assay was performed as specified in GB/T528-.
3. Measurement of adhesive Properties: the assay was performed as specified in GB/T16776-2005.
The results of the performance test on the high-strength and high-temperature resistant silicone sealants obtained in the embodiments 1 to 3 and the comparative examples 4 to 5 are shown in tables 1 and 2.
TABLE 1
TABLE 2
Note: -complete interfacial debonding; o partial interface peeling or residual glue layer on the surface of the base material is less than 10 percent; the V is completely cohesive failure and the residual glue layer on the surface of the substrate is more than 10 percent.
As can be seen from the above tables 1 and 2, compared with the prior art (comparative examples 4 and 5), the sealant of the present invention has the following advantages: on the basis of reducing the cost, the product not only has good high temperature resistance (300 ℃) and tensile property, but also can keep better strength in a high temperature state, and has better adhesive property to the difficult-to-stick base material.
Claims (5)
1. The high-strength high-temperature-resistant silicone sealant is characterized by comprising the following components in parts by weight:
40-70 parts of organopolysiloxane
30-60 parts of modified nano kaolin
0.2-5 parts of modified silicone oil
3-10 parts of silane composite cross-linking agent
0.5-3 parts of compound silane coupling agent
0-0.5 part of catalyst;
the organopolysiloxane comprises one or more linear polymers with the following structural formula,
wherein R is1、R2、R3、R6、R7、R8Hydrocarbyloxy radicals formed from unsaturated hydrocarbon radicals having from C2 to C4, R4、R5Is a C1-C3 hydrocarbyl group, m is 5500-8000;
the viscosity of the organopolysiloxane at 25 ℃ is in the range of 60000-900000 mPa.s;
the modified nano kaolin is nano kaolin subjected to surface treatment by using azido silane, wherein the azido silane is one of azido formyloxy hydrocarbon silane, azido sulfonyl hydrocarbon silane and azido formamide hydrocarbon silane;
the modified silicone oil is phenyl hydrogen-containing silicone oil modified by 1-dodecene or 3-pentadecene;
the compound silane coupling agent is a mixture of an aminosilane coupling agent and an isocyanate silane coupling agent, and the aminosilane coupling agent is prepared from the following components in parts by weight: isocyanate silane coupling agent = 2-3: 1-2;
the preparation method of the high-strength high-temperature-resistant silicone sealant comprises the following steps:
a. adding the organopolysiloxane, the modified nano kaolin and the modified silicone oil into a kneading machine according to the weight part ratio, dehydrating and blending for 60-120min at the temperature of 130-150 ℃ and the vacuum degree of 0.06-0.099MPa, and cooling to obtain a base adhesive;
b. adding the silane composite cross-linking agent, the compound silane coupling agent and the catalyst into a stirrer, and stirring for 10-20min at room temperature to obtain a mixture;
c. adding the base glue into a stirrer at room temperature, stirring for 10-20min, adding the mixture, and reacting at the vacuum degree of 0.08-0.099MPa and the rotation speed of 10-800rpm for 30-60min to obtain the high-strength high-temperature-resistant silicone sealant.
2. The high strength, high temperature resistant silicone sealant according to claim 1 wherein said silane complex crosslinker is at least two of methyltributanone oxime silane, vinyltributone oxime silane, phenyltributone oxime silane, methyltripropontoximino silane, methylvinyldibutyloximino silane, methylphenyldiketoximino silane, diphenyldibutyloximino silane.
3. The high strength, high temperature resistant silicone sealant according to claim 1, wherein said aminosilane coupling agent is at least one of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, N-beta-aminoethyl-gamma-aminopropyltrimethoxysilane, N-beta-aminoethyl-gamma-aminopropyltriethoxysilane, N-beta-aminoethyl-gamma-aminopropylmethyldimethoxysilane, N-beta-aminoethyl-gamma-aminopropylmethyldiethoxysilane; the isocyanate silane coupling agent is at least one of isocyanate propyl trimethoxy silane and isocyanate propyl triethoxy silane.
4. The high strength, high temperature resistant silicone sealant according to claim 1 wherein said catalyst is any one of dibutyltin diacetate, dibutyltin dilaurate, dioctyltin dilaurate, stannous octoate, dimethyltin dineodecanoate, dibutyltin bis (β -diketonate).
5. The high strength, high temperature resistant silicone sealant of claim 1 wherein said steps b and c are performed under nitrogen.
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| CN118085805A (en) * | 2024-03-19 | 2024-05-28 | 山东元腾新材料科技有限公司 | Organic silica gel for windshield and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101768420B (en) * | 2008-12-30 | 2012-07-04 | 上海回天化工新材料有限公司 | Dealcoholized organosilicon sealant with damp-heat resistance and stable storage |
| JP2012131898A (en) * | 2010-12-21 | 2012-07-12 | Shin-Etsu Chemical Co Ltd | Room temperature curable organopolysiloxane composition, production method thereof, and article coated by cured organopolysiloxane composition |
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