CN107936562B - Non-corrosive ketoxime type room temperature curing silicone rubber and preparation method thereof - Google Patents
Non-corrosive ketoxime type room temperature curing silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of room temperature curing silicone rubber, in particular to non-corrosive ketoxime type room temperature curing silicone rubber and a preparation method thereof. The formula of the ketoxime type room temperature curing silicone rubber is obtained by mixing 40-60 parts by weight of hydroxyl-terminated polysiloxane, 3-6 parts by weight of methyl isobutyl ketoximino silane, 1-5 parts by weight of silane coupling agent, 5-15 parts by weight of plasticizer, 0.1-1 part by weight of catalyst, 10-30 parts by weight of filler and 1-10 parts by weight of pigment, mixing and stirring the hydroxyl-terminated polysiloxane, the plasticizer, the filler and the pigment in vacuum, then sequentially adding the methyl isobutyl ketoximino silane, the silane coupling agent and the catalyst, and stirring in vacuum to obtain the rubber material of the room temperature curing silicone rubber. Methyl isobutanone oxime generated in the vulcanization process of the ketoxime type room temperature curing silicone rubber has no corrosivity on polyurethane materials, the requirements of automobiles, electronic industries and the like on the ketoxime type room temperature curing silicone rubber are met, the tensile strength of a colloid is high, the adhesive property of the rubber material is strong, and the preparation method is simple.
Description
Technical Field
The invention relates to the technical field of room temperature curing silicone rubber, in particular to non-corrosive ketoxime type room temperature curing silicone rubber and a preparation method thereof.
Background
The room temperature curing silicone rubber, also called room temperature vulcanized silicone rubber, takes hydroxyl-terminated polysiloxane as a basic polymer, adds filler, a cross-linking agent, a coupling agent, a plasticizer, a catalyst, pigment and the like, mixes the mixture into a rubber material under a dry condition, and then subpackages, seals and stores the rubber material, and when the rubber material is used, the rubber material can generate a cross-linking reaction to generate an elastomer by contacting with moisture at room temperature. Room temperature curing silicone rubbers are classified into acetic acid type, ketoxime type, alcohol type, amine type, amide type, and acetone type according to the by-products released upon vulcanization. Wherein the ketoxime type room temperature curing silicone rubber has good comprehensive performance and good storage property. The commonly used cross-linking agent of the ketoxime type silicone rubber is methyl tributyl ketoxime silane, vinyl tributyloxime silane and the like, and the by-product generated by vulcanization is butanone oxime. Butanone oxime is corrosive to polycarbonate materials, and can cause cracking of the polycarbonate materials. In the industries of automobiles, electronics and the like, the LED display screen module shell, the electronic device box and the like are made of polycarbonate materials, so that the application of ketoxime type silicone rubber in the fields is limited. Moreover, butanone oxime has a carcinogenic risk and has been classified as a hazardous substance in the european union and is limited.
Chinese patent 200810028077, application date 2008.05.14, discloses a deeply cured corrosion-free single-component ketoxime removing type pouring sealant, wherein one or more of TDI, MDI, HMDI or IPDI is/are added into the formula of the ketoxime type pouring sealant to be used as a ketoxime scavenger, so that the influence of the ketoxime on the LED display screen module shell is eliminated, but the ketoxime scavenger is easy to react with water to lose efficacy, and the ketoxime scavenger is not thoroughly removed.
Disclosure of Invention
Aiming at the problem that the application is affected by the corrosion of a butanone oxime byproduct generated by vulcanizing the existing ketoxime type room temperature curing silicone rubber, the invention aims to provide the ketoxime type room temperature curing silicone rubber without corrosion, the production of butanone oxime as a byproduct during vulcanization is avoided, the produced vulcanization byproduct is non-corrosive, the cracking of a polyurethane material is avoided, the application of the ketoxime type room temperature curing silicone rubber in the fields of automobiles, electronic industry and the like is met, the carcinogenic risk caused by the production of butanone oxime during vulcanization of the silicone rubber is avoided, and the ketoxime type room temperature curing silicone rubber has good comprehensive performance.
The invention also aims to provide a preparation method of the non-corrosive ketoxime type room-temperature-curing silicone rubber.
The invention provides the following technical scheme:
the ketoxime type room temperature curing silicone rubber is non-corrosive, and the formulation of the ketoxime type room temperature curing silicone rubber is obtained by mixing the following components in parts by weight: 40-60 parts of hydroxyl-terminated polysiloxane, 3-6 parts of methyl isobutyl ketoximino silane, 1-5 parts of silane coupling agent, 5-15 parts of plasticizer, 0.1-1 part of catalyst, 10-30 parts of filler and 1-10 parts of pigment.
As an improvement of the invention, the methyl isobutyl ketoximino silane is one or more of methyl tri (methyl isobutyl ketoximino) silane, vinyl tri (methyl isobutyl ketoximino) silane, tetra (methyl isobutyl ketoximino) silane and phenyl tri (methyl isobutyl ketoximino) silane.
As an improvement of the invention, the silane coupling agent is one of an aminosilane coupling agent, an epoxy silane coupling agent and an isocyanato silane coupling agent.
As an improvement of the invention, the plasticizer is silicone oil or white oil.
As an improvement of the invention, the catalyst is an organic tin catalyst.
As an improvement of the invention, the filler is a mixture of calcium carbonate and white carbon black.
The ketoxime type room temperature curing silicone rubber adopts methyl isobutyl ketoximyl silane as a cross-linking agent, and comprises one or more of methyl tri (methyl isobutyl ketoximyl) silane, vinyl tri (methyl isobutyl ketoximyl) silane, tetra (methyl isobutyl ketoximyl) silane and phenyl tri (methyl isobutyl ketoximyl) silane, wherein the by-products generated during vulcanization of the formed room temperature curing silicone rubber are methyl isobutyl ketoxime, and the methyl isobutyl ketoxime is non-corrosive to polyurethane materials and does not have carcinogenic risk compared with the butyl ketoxime, so that the generation of the butyl ketoxime by-products is avoided. The methyl isobutyl ketoximyl silane cross-linking agent selected by the invention has strong cross-linking effect on hydroxyl-terminated polysiloxane, and the obtained ketoxime type room temperature curing silicone rubber has stable indexes such as tensile strength, tensile elongation and elasticity, and has excellent comprehensive performance.
The preparation method of the non-corrosive ketoxime type room temperature curing silicone rubber comprises the following steps:
(1) respectively weighing hydroxyl-terminated polysiloxane, plasticizer, filler and pigment, adding into a planetary stirrer or a kneader, and stirring for 30-60 minutes in vacuum;
(2) weighing methyl isobutyl ketoximyl silane, adding the methyl isobutyl ketoximyl silane, and continuously stirring the mixture in vacuum for 30 to 60 minutes;
(3) and weighing the silane coupling agent and the catalyst, adding the silane coupling agent and the catalyst, stirring for 30-60 minutes in vacuum, and packaging under the protection of nitrogen to obtain the rubber material of the room-temperature curing silicone rubber.
The preparation process of the ketoxime type room temperature curing silicone rubber is simple and easy to operate, the hydroxyl-terminated polysiloxane, the plasticizer, the filler and the pigment are fully mixed and then added with the methyl isobutyl ketoxime group silane for stirring, the formation of a cross-linked network in the hydroxyl-terminated polysiloxane is promoted, and the silane coupling agent and the catalyst are added for fully stirring and then packaged to obtain the ketoxime type room temperature curing silicone rubber sizing material.
The invention has the following beneficial effects:
methyl isobutanone oxime produced in the vulcanization process of the ketoxime type room temperature curing silicone rubber disclosed by the invention has no corrosivity on polyurethane materials, can meet the application requirements of industries such as automobiles and electronics on the ketoxime type room temperature curing silicone rubber, avoids the carcinogenic risk caused by the production of the butanone oxime during the vulcanization of the silicone rubber, and has the advantages of good comprehensive performance, simple preparation method and easiness in operation.
Detailed Description
The following further describes the embodiments of the present invention.
The starting materials used in the present invention are commercially available or commonly used in the art, unless otherwise specified, and the methods in the following examples are conventional in the art, unless otherwise specified.
The formula of the non-corrosive ketoxime type room-temperature curing silicone rubber is obtained by mixing 40-60 parts by weight of hydroxyl-terminated polysiloxane, 3-6 parts by weight of methyl isobutyl ketoximyl silane, 1-5 parts by weight of a silane coupling agent, 5-15 parts by weight of a plasticizer, 0.1-1 part by weight of a catalyst, 10-30 parts by weight of a filler and 1-10 parts by weight of a pigment, wherein the methyl isobutyl ketoximyl silane is one or more of methyl tris (methyl isobutyl ketoximyl) silane, vinyl tris (methyl isobutyl ketoximyl) silane, tetra (methyl isobutyl ketoximyl) silane and phenyl tris (methyl isobutyl ketoximyl) silane, the silane coupling agent is one of an aminosilane coupling agent, an epoxy silane coupling agent and an isocyanic silane coupling agent, the plasticizer is silicone oil or white oil, the catalyst is an organic tin catalyst, and the filler is a mixture of calcium carbonate and white carbon black.
The preparation method of the ketoxime type room temperature curing silicone rubber comprises the following steps:
(1) respectively weighing hydroxyl-terminated polysiloxane, plasticizer, filler and pigment, adding into a planetary stirrer or a kneader, and stirring for 30-60 minutes in vacuum;
(2) weighing methyl isobutyl ketoximyl silane, adding the methyl isobutyl ketoximyl silane, and continuously stirring the mixture in vacuum for 30 to 60 minutes;
(3) weighing silane coupling agent and catalyst, adding, stirring in vacuum for 30-60 min, and packaging under nitrogen protection to obtain the rubber material of the room temperature cured silicone rubber.
Example 1
The formula of the non-corrosive ketoxime type room-temperature curing silicone rubber is obtained by mixing 40g of hydroxyl-terminated polysiloxane, 3g of methyl isobutyl ketoximino silane, 1g of silane coupling agent, 5g of plasticizer, 0.1g of catalyst, 10g of filler and 1g of pigment, wherein the methyl isobutyl ketoximino silane is methyl tri (methyl isobutyl ketoximino) silane, the silane coupling agent is amino silane coupling agent, the plasticizer is silicone oil, the catalyst is organic tin catalyst, and the filler is a mixture of calcium carbonate and white carbon black. The preparation method comprises the following steps:
(1) respectively weighing hydroxyl-terminated polysiloxane, plasticizer, filler and pigment, adding into a planetary stirrer or a kneader, and stirring for 30 minutes in vacuum;
(2) weighing methyl tri (methyl isobutyl ketoximyl) silane, adding, and continuing to stir in vacuum for 30 minutes;
(3) weighing and adding the silane coupling agent and the catalyst, stirring for 30 minutes in vacuum, and packaging under the protection of nitrogen to obtain the rubber material of the room-temperature curing silicone rubber.
Example 2
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the silicone rubber of example 1 in that the methyl isobutyl ketoximino silane is selected to be vinyl tri (methyl isobutyl ketoximino) silane.
Example 3
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the silicone rubber of example 1 in that the methyl isobutyl ketoximino silane is selected to be phenyl tri (methyl isobutyl ketoximino) silane.
Example 4
The formula of the non-corrosive ketoxime type room-temperature curing silicone rubber is obtained by mixing 45g of hydroxyl-terminated polysiloxane, 4g of methyl isobutyl ketoximino silane, 2.3g of silane coupling agent, 8.3g of plasticizer, 0.4g of catalyst, 16.3g of filler and 4g of pigment, wherein the methyl isobutyl ketoximino silane is a mixture of methyl tri (methyl isobutyl ketoximino) silane and vinyl tri (methyl isobutyl ketoximino) silane, the silane coupling agent is epoxy silane coupling agent, the plasticizer is white oil, the catalyst is organic tin catalyst, and the filler is a mixture of calcium carbonate and white carbon black. The preparation method comprises the following steps:
(1) respectively weighing hydroxyl-terminated polysiloxane, plasticizer, filler and pigment, adding into a planetary stirrer or a kneader, and stirring for 40 minutes in vacuum;
(2) weighing a mixture of methyl tri (methyl isobutyl ketoximyl) silane and vinyl tri (methyl isobutyl ketoximyl) silane, adding the mixture, and continuing to stir in vacuum for 40 minutes;
(3) weighing a silane coupling agent and a catalyst, adding the silane coupling agent and the catalyst, stirring for 40 minutes in vacuum, and packaging under the protection of nitrogen to obtain the rubber material of the room-temperature curing silicone rubber.
Example 5
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the one in example 4 in that the methyl isobutyl ketoximino silane is a mixture of methyl tri (methyl isobutyl ketoximino) silane and tetra (methyl isobutyl ketoximino) silane.
Example 6
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the one in example 4 in that the methyl isobutyl ketoximino silane is a mixture of methyl tris (methyl isobutyl ketoximino) silane and phenyl tris (methyl isobutyl ketoximino) silane.
Example 7
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the one in example 4 in that the methyl isobutyl ketoximino silane is a mixture of vinyl tri (methyl isobutyl ketoximino) silane and tetra (methyl isobutyl ketoximino) silane.
Example 8
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the one in example 4 in that the methyl isobutyl ketoximino silane is a mixture of vinyl tris (methyl isobutyl ketoximino) silane and phenyl tris (methyl isobutyl ketoximino) silane.
Example 9
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the one in example 4 in that the methyl isobutyl ketoximino silane is a mixture of tetra (methyl isobutyl ketoximino) silane and phenyltri (methyl isobutyl ketoximino) silane.
Example 10
The formula of the non-corrosive ketoxime type room-temperature curing silicone rubber is obtained by mixing 50g of hydroxyl-terminated polysiloxane, 5g of methyl isobutyl ketoximino silane, 3.6g of silane coupling agent, 11.6g of plasticizer, 0.7g of catalyst, 22.6g of filler and 7g of pigment, wherein the methyl isobutyl ketoximino silane is a mixture of methyl tri (methyl isobutyl ketoximino) silane, vinyl tri (methyl isobutyl ketoximino) silane and tetra (methyl isobutyl ketoximino) silane, the silane coupling agent is an isocyanatosilane coupling agent, the plasticizer is silicone oil, the catalyst is an organic tin catalyst, and the filler is a mixture of calcium carbonate and white carbon black. The preparation method comprises the following steps:
(1) respectively weighing hydroxyl-terminated polysiloxane, plasticizer, filler and pigment, adding into a planetary stirrer or a kneader, and stirring for 50 minutes in vacuum;
(2) weighing a mixture of methyl tri (methyl isobutyl ketoximyl) silane, vinyl tri (methyl isobutyl ketoximyl) silane and tetra (methyl isobutyl ketoximyl) silane, adding, and continuing to stir in vacuum for 50 minutes;
(3) weighing and adding the silane coupling agent and the catalyst, stirring for 50 minutes in vacuum, and packaging under the protection of nitrogen to obtain the rubber material of the room-temperature curing silicone rubber.
Example 11
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the silicone rubber of example 10 in that the methyl isobutyl ketoximino silane is a mixture of methyl tris (methyl isobutyl ketoximino) silane, vinyl tris (methyl isobutyl ketoximino) silane and benzene tris (methyl isobutyl ketoximino) silane.
Example 12
The non-corrosive ketoxime type room temperature curing silicone rubber is different from the silicone rubber of example 10 in that the methyl isobutyl ketoximino silane is a mixture of vinyl tris (methyl isobutyl ketoximino) silane, tetrakis (methyl isobutyl ketoximino) silane and benzene tris (methyl isobutyl ketoximino) silane.
Example 13
The formula of the non-corrosive ketoxime type room-temperature curing silicone rubber is obtained by mixing 60g of hydroxyl-terminated polysiloxane, 6g of methyl isobutyl ketoximino silane, 5g of silane coupling agent, 15g of plasticizer, 1g of catalyst, 30g of filler and 10g of pigment, wherein the methyl isobutyl ketoximino silane is a mixture of methyl tri (methyl isobutyl ketoximino) silane, vinyl tri (methyl isobutyl ketoximino) silane, tetra (methyl isobutyl ketoximino) silane and phenyl tri (methyl isobutyl ketoximino) silane, the silane coupling agent is amino silane coupling agent, the plasticizer is white oil, the catalyst is an organic tin catalyst, and the filler is a mixture of calcium carbonate and white carbon black. The preparation method comprises the following steps:
(1) respectively weighing hydroxyl-terminated polysiloxane, plasticizer, filler and pigment, adding into a planetary stirrer or a kneader, and stirring for 60 minutes in vacuum;
(2) weighing methyl isobutyl ketoximino silane which is a mixture of methyl tri (methyl isobutyl ketoximino) silane, vinyl tri (methyl isobutyl ketoximino) silane, tetra (methyl isobutyl ketoximino) silane and phenyl tri (methyl isobutyl ketoximino) silane, adding, and continuing to stir in vacuum for 60 minutes;
(3) weighing and adding the silane coupling agent and the catalyst, stirring for 60 minutes in vacuum, and packaging under the protection of nitrogen to obtain the rubber material of the room-temperature curing silicone rubber.
Comparative example
Methyl tributyl ketoxime silane is used as a cross-linking agent, the other components and the addition quality are the same as those in the example 1, and the rubber material of the room-temperature curing silicone rubber of the comparative example is obtained by the same preparation method.
Performance testing
1. Test of comprehensive Properties
The compounds obtained in examples 1 to 13 and comparative examples were tested according to GT/T13477-2002, wherein J1, J2, J3 and J4 respectively represent methyltris (methylisobutylketonoximino) silane, vinyltris (methylisobutylketonoximino) silane, tetrakis (methylisobutylketonoximino) silane and phenyltris (methylisobutylketonoximino) silane. The results are shown in Table 1.
2. Corrosion testing of polycarbonate
The corrosiveness of the sizing materials obtained in examples 1-13 and comparative examples to polyurethane was tested by the following method: 2 polycarbonate plates with the thickness of 50mm x 100mm are taken, sealing glue with the thickness of 5mm is coated on the middle of the 2 polycarbonate plates, the two polycarbonate plates are placed for 7 days under the environment with the temperature of 25 ℃ and the humidity of 50 percent, and whether the two polycarbonate plates crack or not is observed, and the result is shown in table 1.
TABLE 1 test results
Claims (6)
1. The non-corrosive ketoxime type room temperature curing silicone rubber is characterized in that the formulation of the ketoxime type room temperature curing silicone rubber is prepared by mixing the following components in parts by weight: 40-60 parts of hydroxyl-terminated polysiloxane, 3-6 parts of methyl isobutyl ketoximino silane, 1-5 parts of silane coupling agent, 5-15 parts of plasticizer, 0.1-1 part of catalyst, 10-30 parts of filler and 1-10 parts of pigment; the methyl isobutyl ketoximino silane is a mixture of vinyl tri (methyl isobutyl ketoximino) silane and methyl tri (methyl isobutyl ketoximino) silane;
or the methyl isobutyl ketoximino silane is a mixture of vinyl tri (methyl isobutyl ketoximino) silane and phenyl tri (methyl isobutyl ketoximino) silane;
or the methyl isobutyl ketoximino silane is a mixture of tetra (methyl isobutyl ketoximino) silane and methyl tri (methyl isobutyl ketoximino) silane;
or the methyl isobutyl ketoximino silane is a mixture of tetra (methyl isobutyl ketoximino) silane and phenyl tri (methyl isobutyl ketoximino) silane;
or the methyl isobutyl ketoximino silane is a mixture of vinyl tri (methyl isobutyl ketoximino) silane and tetra (methyl isobutyl ketoximino) silane;
or the methyl isobutyl ketoximino silane is a mixture of vinyl tri (methyl isobutyl ketoximino) silane, tetra (methyl isobutyl ketoximino) silane and methyl tri (methyl isobutyl ketoximino) silane;
or the methyl isobutyl ketoximino silane is a mixture of vinyl tri (methyl isobutyl ketoximino) silane, tetra (methyl isobutyl ketoximino) silane and phenyl tri (methyl isobutyl ketoximino) silane;
or the methyl isobutyl ketoximino silane is a mixture of vinyl tri (methyl isobutyl ketoximino) silane, tetra (methyl isobutyl ketoximino) silane, methyl tri (methyl isobutyl ketoximino) silane and phenyl tri (methyl isobutyl ketoximino) silane.
2. The ketoxime type room-temperature-curing silicone rubber according to claim 1, wherein the silane coupling agent is one of an aminosilane coupling agent, an epoxy silane coupling agent, and an isocyanatosilane coupling agent.
3. The ketoxime type room-temperature-curing silicone rubber according to claim 1, wherein the plasticizer is a silicone oil or a white oil.
4. The ketoxime type room-temperature-curing silicone rubber according to claim 1, wherein the catalyst is an organotin catalyst.
5. The ketoxime type room-temperature-curing silicone rubber according to claim 1, wherein the filler is a mixture of calcium carbonate and white carbon black.
6. The method for producing ketoxime type room temperature-curing silicone rubber according to any one of claims 1 to 5, comprising the steps of:
(1) respectively weighing hydroxyl-terminated polysiloxane, plasticizer, filler and pigment, adding into a planetary stirrer or a kneader, and stirring for 30-60 minutes in vacuum;
(2) weighing methyl isobutyl ketoximyl silane, adding the methyl isobutyl ketoximyl silane, and continuously stirring the mixture in vacuum for 30 to 60 minutes;
(3) and weighing the silane coupling agent and the catalyst, adding the silane coupling agent and the catalyst, stirring for 30-60 minutes in vacuum, and packaging under the protection of nitrogen to obtain the rubber material of the room-temperature curing silicone rubber.
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| CN103571197B (en) * | 2013-11-07 | 2015-10-28 | 湖北新蓝天新材料股份有限公司 | A kind of Alkoxyl ketoxime type room temperature vulcanized silicone rubber and preparation method thereof |
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