Preparation method of high-temperature-resistant high-strength dealcoholized single-component room-temperature vulcanized silicone rubber

Abstract

The invention discloses a preparation method of high-temperature-resistant high-strength dealcoholized single-component room-temperature vulcanized silicone rubber. The high-temperature-resistant high-strength dealcoholized single-component room-temperature vulcanized silicone rubber is prepared from 30-90 parts of self-made masterbatch; 2-10 parts of a cross-linking agent; 30-60 parts of a filler; 1-10 parts of a catalyst; the self-made rubber master batch is prepared by treating 10 to 200 parts of fumed silica with 1 to 20 parts of silazane in 10 to 100 parts of dimethyl silicone oil and then adding 10 to 1000 parts of dihydroxy polydimethylsiloxane. According to the preparation method of the high-temperature-resistant high-strength dealcoholized single-component room-temperature vulcanized silicone rubber, the self-made masterbatch is used as a basic polymer, so that the rubber body can obtain very high mechanical property.

Description

Technical Field

[0001] The invention relates to the technical field of sealant preparation, in particular to a method for preparing high-temperature resistant and high-strength dealcoholized single-component room temperature vulcanized silicone rubber. Background Art

[0002] Room temperature vulcanized silicone rubber is a new type of silicone elastomer that came out in the 1960s. It uses low-viscosity polysiloxane as a polymer and can be vulcanized into an elastomer by mixing with moisture and a crosslinking agent at room temperature. It can be cured in situ at room temperature without heating or molding, and is extremely convenient to use. As a result, it quickly became an important component and research and application area of ​​the entire silicone field as soon as it came out. It has been widely used in aerospace, aviation, automobiles, electronics, electrical appliances, medical and health, construction, light industry, petrochemicals, transportation machinery and other industries.

[0003] One-component room temperature vulcanized silicone rubber generally consists of the following ingredients: reactive base polymer - hydroxyl-terminated diorganosilane; crosslinking agent - multifunctional silane compound containing hydrolyzable groups; catalyst - organotin; filler - white carbon black, calcium carbonate; thickener - non-reactive dimethyl silicone oil, etc. When one-component room temperature vulcanized silicone rubber is used as an adhesive, the performance requirements after vulcanization are mainly good adhesion to the contacted substrate, no corrosion, and good physical and mechanical properties, electrical properties and flame retardancy.

[0004] The current colloid has poor high temperature resistance and insufficient strength. To address the above problems, existing equipment needs to be improved. Summary of the invention

[0005] The object of the present invention is to provide a method for preparing a high-temperature resistant and high-strength dealcoholized one-component room temperature vulcanized silicone rubber to solve the problems raised in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solution: a method for preparing a high-temperature resistant and high-strength dealcoholized one-component room temperature vulcanized silicone rubber,

[0007] A method for preparing a high-temperature resistant and high-strength dealcoholized single-component room temperature vulcanized silicone rubber, the formula of which is as follows: 30 to 90 parts of homemade masterbatch; 2 to 10 parts of a cross-linking agent; 30 to 60 parts of a filler; 1 to 10 parts of a catalyst; and 1 to 10 parts of an adhesion promoter.

[0008] Preferably, the homemade masterbatch is prepared by treating 10 to 200 parts of fumed silica with 1 to 20 parts of silazane in 10 to 100 parts of dimethyl silicone oil, and then adding 10 to 1000 parts of dihydroxy polydimethylsiloxane.

[0009] Preferably, the crosslinking agent is one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, ethyl orthosilicate, and methyl orthosilicate.

[0010] Preferably, the filler is one or more of titanium oxide, cerium oxide, cerium hydroxide, iron oxide, calcium carbonate, and silicon powder.

[0011] Preferably, the catalyst is a titanate.

[0012] Preferably, the adhesion promoter is one or more of γ-aminopropyltriethoxysilane, γ-aminopropyltrimethoxysilane, and 3-(2,3-epoxypropyloxy)propyltrimethoxysilane.

[0013] Preferably, the preparation method is as follows: add dimethyl silicone oil and fumed silica into a stirrer, add silazane, heat-treat the fumed silica, add dihydroxy polydimethylsiloxane after treatment to mix and prepare a masterbatch, add homemade masterbatch, filler, cross-linking agent, catalyst, and adhesion promoter into the stirrer, stir and mix evenly under vacuum to prepare a high-temperature resistant and high-strength dealcoholized one-component room temperature vulcanized silicone rubber.

[0014] Compared with the prior art, the invention has the following beneficial effects: the preparation method of the high-temperature resistant and high-strength dealcoholized one-component room temperature vulcanized silicone rubber is a high-temperature resistant and high-strength dealcoholized one-component room temperature vulcanized silicone rubber made with a homemade masterbatch as the base polymer, wherein the homemade masterbatch is the base polymer, which can make the colloid obtain very high mechanical properties; in addition, one or more of titanium oxide, cerium oxide, cerium hydroxide, iron oxide, calcium carbonate, and silicon micropowder are used as fillers, which can greatly improve the high temperature resistance of the colloid. Through the combination of the two, the rubber has the advantages of high temperature resistance and high strength. DETAILED DESCRIPTION

[0015] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0016] The present invention provides a technical solution: a method for preparing a high-temperature resistant and high-strength dealcoholized single-component room temperature vulcanized silicone rubber.

[0017] Example 1

[0018] Add 50 parts of dimethyl silicone oil and 100 parts of fumed silica into a kneader, add 10 parts of silazane to heat treat the fumed silica, and after treatment, add 250 parts of dihydroxy polydimethylsiloxane to make a masterbatch. Add 60 parts of self-made masterbatch, 7 parts of titanium oxide, 7 parts of cerium oxide, 7 parts of cerium hydroxide, 7 parts of iron oxide, 7 parts of calcium carbonate, 7 parts of silicon powder, 1 part of methyl trimethoxy silane, 1 part of methyl triethoxy silane, 1 part of vinyl trimethoxy silane, 1 part of vinyl triethoxy silane, 1 part of ethyl orthosilicate, 1 part of methyl orthosilicate, 2 parts of γ-aminopropyl triethoxy silane, 2 parts of γ-aminopropyl trimethoxy silane, 2 parts of 3-(2,3-epoxypropoxy)propyl trimethoxy silane, and 5 parts of titanate into a planetary agitator with vacuum, stir and mix evenly under vacuum to obtain a high temperature resistant and high strength dealcoholization type one-component room temperature vulcanized silicone rubber. The rubber was made into a sample, and the tensile strength was tested to be 4 MPa. The sample was aged at 200°C for 600 hours, and the tensile strength was tested to be 3.4 MPa.

[0019] Example 2

[0020] Add 10 parts of dimethyl silicone oil and 50 parts of fumed silica to the kneader, add 1 part of silazane to heat the fumed silica, and after treatment, add 500 parts of dihydroxy polydimethylsiloxane to make a masterbatch. Add 30 parts of homemade masterbatch, 5 parts of titanium oxide, 5 parts of cerium oxide, 5 parts of cerium hydroxide, 5 parts of iron oxide, 5 parts of calcium carbonate, 5 parts of silicon powder, 1 part of methyl trimethoxy silane, 1 part of ethyl orthosilicate, 1 part of γ-aminopropyl triethoxy silane, and 1 part of titanate to a planetary mixer with vacuum. Stir and mix evenly under vacuum to obtain a high-temperature resistant and high-strength dealcoholized single-component room temperature vulcanized silicone rubber. The rubber is made into a sample, and the tensile strength is tested to be 3.7MPa. The sample is aged at 200℃ for 600h, and the tensile strength is tested to be 3MPa.

[0021] Example 3

[0022] 100 parts of dimethyl silicone oil and 200 parts of fumed silica were added to a kneader, and 20 parts of silazane were added to heat treat the fumed silica. After treatment, 100 parts of dihydroxy polydimethylsiloxane were added to prepare a masterbatch. 90 parts of self-made masterbatch, 9 parts of titanium oxide, 9 parts of cerium oxide, 9 parts of cerium hydroxide, 9 parts of iron oxide, 9 parts of calcium carbonate, 15 parts of silicon powder, 2 parts of methyltrimethoxysilane, 2 parts of methyltriethoxysilane, 2 parts of vinyltrimethoxysilane, 2 parts of vinyltriethoxysilane, 1 part of ethyl orthosilicate, 1 part of methyl orthosilicate, 6 parts of γ-aminopropyltriethoxysilane, 3 parts of γ-aminopropyltrimethoxysilane, 3 parts of 3-(2,3-epoxypropoxy)propyltrimethoxysilane, and 10 parts of titanate were added to a planetary agitator with vacuum, and the mixture was stirred and mixed evenly under vacuum to prepare a high-temperature resistant and high-strength dealcoholization type single-component room temperature vulcanized silicone rubber. The rubber was made into a sample, and the tensile strength was tested to be 4.2MPa. The sample was aged at 200℃ for 600h, and the tensile strength was tested to be 3.6MPa.

[0023] Through the experimental process of Examples 1-3, a high-temperature resistant and high-strength dealcoholized one-component room temperature vulcanized silicone rubber was successfully prepared. In each example, according to a specific raw material ratio and preparation process, a masterbatch was first prepared in a kneader, and then the homemade masterbatch and a variety of additives were added to a planetary agitator with vacuum, and the silicone rubber product was obtained after vacuum stirring and mixing, which proved the feasibility of the preparation method;

[0024] The changes in the raw material ratios in different embodiments affect the tensile strength of silicone rubber. In Example 1, the initial tensile strength of the silicone rubber sample prepared under a specific ratio is 4MPa; in Example 2, after the raw material ratio is changed, the initial tensile strength is 3.7MPa; in Example 3, under another different ratio, the initial tensile strength reaches 4.2MPa. This shows that changes in the content of dimethyl silicone oil, fumed silica, dihydroxy polydimethylsiloxane, etc. in the raw materials will make the initial mechanical properties of silicone rubber different. Reasonable adjustment of the ratio can regulate the tensile strength of silicone rubber to a certain extent.

[0025] After the samples were aged at 200°C for 600h, the tensile strength of Example 1 was 3.4MPa, that of Example 2 was 3MPa, and that of Example 3 was 3.6MPa. It can be seen that although the tensile strength decreased after aging, it still maintained a certain level, indicating that the silicone rubber prepared by the present invention has good high temperature aging resistance, and can still maintain certain structural integrity and mechanical properties under the action of high temperature environment for a long time, and can be suitable for relevant application scenarios under high temperature conditions;

[0026] By comparing the results of different embodiments, it can be seen that as the content of fumed silica increases (such as Example 3 compared to Example 2), the tensile strength of silicone rubber is improved within a certain range, but at the same time, more silazane may be needed to treat fumed silica to ensure dispersibility and other properties; and the change in the content of dihydroxy polydimethylsiloxane (such as Example 1 and Example 3) also affects the tensile strength and high temperature aging resistance. These results provide a reference direction for further optimizing the formula. In the future, more experiments can be conducted to study the interaction between the raw materials and find a better ratio combination to obtain a high temperature resistant and high strength dealcoholized single-component room temperature vulcanized silicone rubber with better comprehensive performance.

[0027] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a high temperature resistant and high strength dealcoholization type one-component room temperature vulcanized silicone rubber, characterized in that: The formula is as follows: 30-90 parts of homemade masterbatch; 2-10 parts of cross-linking agent; 30-60 parts of filler; 1-10 parts of catalyst; and 1-10 parts of adhesion promoter.

2. The method for preparing a high temperature resistant and high strength dealcoholization type one-component room temperature vulcanized silicone rubber according to claim 1, characterized in that: The homemade masterbatch is prepared by treating 10 to 200 parts of fumed silica with 1 to 20 parts of silazane in 10 to 100 parts of dimethyl silicone oil, and then adding 10 to 1000 parts of dihydroxy polydimethylsiloxane.

3. The method for preparing a high temperature resistant and high strength dealcoholization type one-component room temperature vulcanized silicone rubber according to claim 1, characterized in that: The crosslinking agent is one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, ethyl orthosilicate, and methyl orthosilicate.

4. The method for preparing a high temperature resistant and high strength dealcoholization type one-component room temperature vulcanized silicone rubber according to claim 1, characterized in that: The filler is one or more of titanium oxide, cerium oxide, cerium hydroxide, iron oxide, calcium carbonate and silicon micropowder.

5. The method for preparing a high temperature resistant and high strength dealcoholization type one-component room temperature vulcanized silicone rubber according to claim 1, characterized in that: The catalyst is titanate.

6. The method for preparing a high temperature resistant and high strength dealcoholization type one-component room temperature vulcanized silicone rubber according to claim 1, characterized in that: The adhesion promoter is one or more of γ-aminopropyltriethoxysilane, γ-aminopropyltrimethoxysilane, and 3-(2,3-epoxypropyloxy)propyltrimethoxysilane.

7. The method for preparing a high temperature resistant and high strength dealcoholization type one-component room temperature vulcanized silicone rubber according to claim 1, characterized in that: The preparation method is as follows: add dimethyl silicone oil and fumed silica into a blender, add silazane, heat-treat the fumed silica, add dihydroxy polydimethylsiloxane after treatment to mix and prepare a masterbatch, add homemade masterbatch, filler, cross-linking agent, catalyst, and adhesion promoter into the blender, stir and mix evenly under vacuum to prepare a high-temperature resistant and high-strength dealcoholized one-component room temperature vulcanized silicone rubber.