CN112300396A - PA tackifier for addition type liquid silicone rubber and preparation method thereof - Google Patents
PA tackifier for addition type liquid silicone rubber and preparation method thereof Download PDFInfo
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- CN112300396A CN112300396A CN201910705477.2A CN201910705477A CN112300396A CN 112300396 A CN112300396 A CN 112300396A CN 201910705477 A CN201910705477 A CN 201910705477A CN 112300396 A CN112300396 A CN 112300396A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/10—Block- or graft-copolymers containing polysiloxane sequences
Abstract
The invention discloses a PA tackifier for addition type liquid silicone rubber and a preparation method thereof, and aims to provide a tackifier with excellent bonding performance and high refractive index; the technical scheme comprises the following components: 20-40 parts of hydrogen-containing silicone oil, 10-20 parts of methyl triallyl silane, 0.001-0.1 part of platinum complex catalyst, 10-20 parts of gamma-glycidyl ether oxypropyl trimethoxy silane and 30-40 parts of toluene; belongs to the technical field of adhesives.
Description
Technical Field
The invention discloses a tackifier, particularly a PA tackifier for addition type liquid silicone rubber, and also discloses a preparation method of the PA tackifier for addition type liquid silicone rubber, belonging to the technical field of adhesives.
Background
PA plastic was the resin developed for fibers by one company in the united states first, and was commercialized in 1939. In the 50 th of the 20 th century, injection molded products are developed and produced to replace metals to meet the requirements of light weight and cost reduction of downstream industrial products. The PA has good comprehensive properties including mechanical property, heat resistance, abrasion resistance, chemical resistance and self-lubricity, has low friction coefficient and certain flame retardance, is easy to process, is suitable for being filled with glass fiber and other fillers for reinforcing modification, improves the performance and expands the application range.
The liquid silicone rubber is also called double-component addition silicone rubber, has good fluidity and fast vulcanization, can be cast and molded, and can be injection molded. The addition type liquid silicone rubber is non-polar, the main chain is composed of silicon-oxygen bonds, and a layer of non-polar alkyl is arranged outside the main chain, so that the surface energy of the material is low, the adhesion to the material is low, and great trouble is brought to actual production, so that the PA tackifier for the addition type liquid silicone rubber becomes a research hotspot of people.
CN201810004570.6 discloses a preparation process of an environment-friendly tackifier, which comprises the following steps: taking dimer acid, oleic acid and dioctyl ester according to a certain proportion; step 2: adding the mixture into a reaction kettle, starting a heating device to heat the mixture, observing the temperature display value of the temperature sensor, and starting a stirrer to stir the dimer acid, the oleic acid and the dioctyl ester added into the reaction kettle when the temperature reaches 120 ℃; and step 3: stirring for 3 hours to enable dimer acid, oleic acid and dioctyl ester to react to generate an environment-friendly tackifier, and then stopping the reaction of the reaction kettle for cooling; and 4, step 4: when the temperature of the environment-friendly tackifier is reduced to normal temperature, the environment-friendly tackifier is discharged out of the reaction kettle, and the bonding performance of the adhesive on PA plastic is also poor.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a viscosity increasing agent with excellent bonding performance and high refractive index.
The second technical scheme provided by the invention is to provide a preparation method of the adhesive.
Therefore, the first technical scheme provided by the invention is as follows:
the PA tackifier for the addition type liquid silicone rubber is synthesized from the following components in parts by weight:
20-40 parts of hydrogen-containing silicone oil, 10-20 parts of methyl triallyl silane, 0.001-0.1 part of platinum complex catalyst, 10-20 parts of gamma-glycidyl ether oxypropyl trimethoxy silane and 30-40 parts of toluene.
Further, the PA tackifier for the addition type liquid silicone rubber is synthesized from the following components in parts by weight: 25-35 parts of hydrogen-containing silicone oil, 12-18 parts of methyl triallyl silane, 0.01-0.08 part of platinum complex catalyst, 12-18 parts of gamma-glycidyl ether oxypropyl trimethoxy silane and 32-38 parts of toluene.
Further, the PA tackifier for the addition type liquid silicone rubber has the hydrogen content of 0.35-1.5.
Further, the PA tackifier for the addition type liquid silicone rubber has a platinum content of 2000ppm in the platinum complex catalyst.
Further, the viscosity of the PA tackifier for the addition type liquid silicone rubber is 1500-3000cps, the refractive index is 1.43-1.47, and the shear strength is 1.5-2.2 MPa.
The invention provides another technical scheme which is a preparation method of the PA tackifier for the addition type liquid silicone rubber, and the method sequentially comprises the following steps:
(1) adding 30-40 parts by weight of toluene into a reaction kettle, adding 10-20 parts by weight of methyl triallyl silane, adding 0.001-0.1 part by weight of platinum complex catalyst, and uniformly stirring at normal temperature;
(2) heating to 80-90 ℃ under the protection of nitrogen, dripping 20-40 parts by weight of hydrogen-containing silicone oil, and reacting for 3-6h at 90-105 ℃;
(3) cooling to 70-80 deg.C, adding 10-20 weight parts of gamma-glycidyl ether oxypropyl trimethoxysilane dropwise, reacting at 70-80 deg.C for 2-3 hr, and turning off nitrogen;
(4) after the reaction is finished, the low-boiling-point substances and the toluene are removed under reduced pressure at the temperature of 60-80 ℃, and the platinum complex catalyst is adsorbed by an adsorption layer under the vacuum condition, so that the tackifier is obtained.
Further, in the preparation method of the PA tackifier for the addition type liquid silicone rubber, the adsorption layer is a mixture of diatomite and activated carbon.
Compared with the prior art, the technical scheme provided by the invention has the following technical advantages:
1. according to the technical scheme provided by the invention, the tackifier has higher refractive index and better tackifying effect by using hydrogen-containing silicone oil, methyl triallyl silane, a platinum complex catalyst and gamma-glycidyl ether oxypropyl trimethoxy silane, and has better compatibility with PA plastic, so that the tackifying property is increased, and the viscosity is 1500-3000cps, the refractive index is 1.45-1.55 and the shear strength is 1.5-2.2MPa through detection.
2. The preparation method provided by the invention has the advantages of simple process, easily obtained raw materials, easy amplification and suitability for large-scale production.
Detailed Description
The claims of the present invention will be further described in detail with reference to specific embodiments.
Example 1
The invention provides a PA tackifier for addition type liquid silicone rubber, which is prepared by the following method:
(1) adding 30 parts by weight of toluene into a reaction kettle, adding 20 parts by weight of methyl triallyl silane, adding 0.001 part by weight of platinum complex catalyst (the content of platinum in the platinum complex catalyst is 2000ppm), and uniformly stirring at normal temperature;
(2) heating to 90 ℃ under the protection of nitrogen, dropwise adding 20 parts by weight of hydrogen-containing silicone oil, and reacting for 3 hours at 105 ℃;
(3) cooling to 80 ℃, dropwise adding 10 parts by weight of gamma-glycidyl ether oxypropyl trimethoxy silane, reacting for 2 hours at 80 ℃, and turning off nitrogen;
(4) after the reaction is finished, the low-boiling-point substances and the toluene are removed under the reduced pressure of 80 ℃, and the platinum complex catalyst is adsorbed by using diatomite and an active carbon adsorption layer under the vacuum condition, so that the tackifier is obtained.
Example 2
The invention provides a PA tackifier for addition type liquid silicone rubber, which is prepared by the following method:
(1) adding 40 parts by weight of toluene into a reaction kettle, adding 10 parts by weight of methyl triallyl silane, adding 0.1 part by weight of platinum complex catalyst (the content of platinum in the platinum complex catalyst is 2000ppm), and uniformly stirring at normal temperature;
(2) heating to 80 ℃ under the protection of nitrogen, dripping 40 parts by weight of hydrogen-containing silicone oil, and reacting for 6 hours at 90 ℃;
(3) cooling to 70 ℃, dropwise adding 20 parts by weight of gamma-glycidoxypropyltrimethoxysilane, reacting for 3 hours at 70 ℃, and turning off nitrogen;
(4) after the reaction is finished, removing low-boiling-point substances and toluene at 60 ℃ under reduced pressure, and adsorbing a platinum complex catalyst by using diatomite and an active carbon adsorption layer under the vacuum condition of 0.1MPa to obtain the tackifier.
Example 3
The invention provides a PA tackifier for addition type liquid silicone rubber, which is prepared by the following method:
(1) adding 35 parts by weight of toluene into a reaction kettle, adding 15 parts by weight of methyl triallyl silane, adding 0.08 part by weight of platinum complex catalyst (the content of platinum in the platinum complex catalyst is 2000ppm), and uniformly stirring at normal temperature;
(2) heating to 88 ℃ under the protection of nitrogen, dripping 38 parts by weight of hydrogen-containing silicone oil, and reacting for 6 hours at 100 ℃;
(3) cooling to 75 ℃, dropwise adding 10 parts by weight of gamma-glycidoxypropyltrimethoxysilane, reacting for 2 hours at 80 ℃, and turning off nitrogen;
(4) after the reaction is finished, removing low-boiling-point substances and toluene at 75 ℃ under reduced pressure, and adsorbing a platinum complex catalyst by using diatomite and an active carbon adsorption layer under the vacuum condition of 0.1MPa to obtain the tackifier.
Example 4
The invention provides a PA tackifier for addition type liquid silicone rubber, which is prepared by the following method:
(1) adding 25 parts by weight of toluene into a reaction kettle, adding 18 parts by weight of methyl triallyl silane, adding 0.08 part by weight of platinum complex catalyst (the content of platinum in the platinum complex catalyst is 2000ppm), and uniformly stirring at normal temperature;
(2) heating to 85 ℃ under the protection of nitrogen, dripping 35 parts by weight of hydrogen-containing silicone oil, and reacting for 4 hours at 100 ℃;
(3) cooling to 78 ℃, dropwise adding 18 parts by weight of gamma-glycidoxypropyltrimethoxysilane, reacting for 2.7h at 78 ℃, and turning off nitrogen;
(4) after the reaction is finished, removing low-boiling-point substances and toluene at 76 ℃ under reduced pressure, and adsorbing a platinum complex catalyst by using diatomite and an active carbon adsorption layer under the vacuum condition of 0.1MPa to obtain the tackifier.
Example 5
The invention provides a PA tackifier for addition type liquid silicone rubber, which is prepared by the following method:
(1) adding 32 parts by weight of toluene into a reaction kettle, adding 22 parts by weight of methyl triallyl silane, adding 0.05 part by weight of platinum complex catalyst (the content of platinum in the platinum complex catalyst is 2000ppm), and uniformly stirring at normal temperature;
(2) heating to 88 ℃ under the protection of nitrogen, dripping 20 parts by weight of hydrogen-containing silicone oil, and reacting for 5 hours at 98 ℃;
(3) cooling to 72 ℃, dropwise adding 14 parts by weight of gamma-glycidoxypropyltrimethoxysilane, reacting for 2.5h at 80 ℃, and turning off nitrogen;
(4) after the reaction is finished, removing low-boiling-point substances and toluene at 77 ℃ under reduced pressure, and adsorbing a platinum complex catalyst by using diatomite and an active carbon adsorption layer under the vacuum condition of 0.1MPa to obtain the tackifier.
The following data for the performance tests of the PA tackifier for addition type liquid silicone rubber prepared in examples 1 to 5 are as follows:
TABLE 1
| Item | Viscosity (cps) | Refractive index | Shear strength (MPa) |
| Example 1 | 1900 | 1.45 | 1.8 |
| Example 2 | 1800 | 1.43 | 2.2 |
| Example 3 | 2200 | 1.44 | 2.1 |
| Example 4 | 3000 | 1.44 | 2.0 |
| Example 5 | 2700 | 1.46 | 1.9 |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The PA tackifier for the addition type liquid silicone rubber is characterized by being synthesized from the following components in parts by weight: 20-40 parts of hydrogen-containing silicone oil, 10-20 parts of methyl triallyl silane, 0.001-0.1 part of platinum complex catalyst, 10-20 parts of gamma-glycidyl ether oxypropyl trimethoxy silane and 30-40 parts of toluene.
2. The PA tackifier for the addition type liquid silicone rubber according to claim 1, which is characterized by being synthesized from the following components in parts by weight: 25-35 parts of hydrogen-containing silicone oil, 12-18 parts of methyl triallyl silane, 0.01-0.08 part of platinum complex catalyst, 12-18 parts of gamma-glycidyl ether oxypropyl trimethoxy silane and 32-38 parts of toluene.
3. The PA tackifier for addition type liquid silicone rubber according to claim 1, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.35 to 1.5.
4. The PA tackifier for addition type liquid silicone rubber according to claim 1, wherein the platinum content in the platinum complex catalyst is 2000 ppm.
5. The PA tackifier for addition type liquid silicone rubber according to claim 1, wherein the PA tackifier for addition type liquid silicone rubber has a viscosity of 1500-3000cps, a refractive index of 1.43-1.47 and a shear strength of 1.5-2.2 MPa.
6. The method for preparing the PA tackifier for addition type liquid silicone rubber according to claim 1, characterized by comprising the following steps in order:
(1) adding 30-40 parts by weight of toluene into a reaction kettle, adding 10-20 parts by weight of methyl triallyl silane, adding 0.001-0.1 part by weight of platinum complex catalyst, and uniformly stirring at normal temperature;
(2) heating to 80-90 ℃ under the protection of nitrogen, dripping 20-40 parts by weight of hydrogen-containing silicone oil, and reacting for 3-6h at 90-105 ℃;
(3) cooling to 70-80 deg.C, adding 10-20 weight parts of gamma-glycidyl ether oxypropyl trimethoxysilane dropwise, reacting at 70-80 deg.C for 2-3 hr, and turning off nitrogen;
(4) after the reaction is finished, the low-boiling-point substances and the toluene are removed under reduced pressure at the temperature of 60-80 ℃, and the platinum complex catalyst is adsorbed by an adsorption layer under the vacuum condition, so that the tackifier is obtained.
7. The method for preparing the PA tackifier for the addition type liquid silicone rubber according to claim 6, wherein the adsorption layer is a mixture of diatomite and activated carbon.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910705477.2A CN112300396A (en) | 2019-08-01 | 2019-08-01 | PA tackifier for addition type liquid silicone rubber and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910705477.2A CN112300396A (en) | 2019-08-01 | 2019-08-01 | PA tackifier for addition type liquid silicone rubber and preparation method thereof |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060127347A (en) * | 2005-06-07 | 2006-12-12 | 주식회사 엘지화학 | Acrylic pressure sensitive adhesive compositions |
| CN102775611A (en) * | 2012-07-24 | 2012-11-14 | 东莞兆舜有机硅新材料科技有限公司 | Tackifier and production method thereof |
| CN104892945A (en) * | 2015-06-06 | 2015-09-09 | 深圳市富达瑞有机硅材料有限公司 | Organic silicon rubber composite tackifier and preparation method thereof |
| CN104892942A (en) * | 2015-06-04 | 2015-09-09 | 成都拓利化工实业有限公司 | Tackifier for addition-type organic silicon rubber and preparation method thereof |
| CN105131291A (en) * | 2015-09-29 | 2015-12-09 | 肇庆皓明有机硅材料有限公司 | Tackifier and preparation thereof as well as adhesion addition type liquid silicone rubber and preparation thereof |
| CN105482120A (en) * | 2015-12-18 | 2016-04-13 | 杭州福斯特光伏材料股份有限公司 | Preparation method of tackifier for addition type liquid silicone rubber |
| CN106279700A (en) * | 2016-08-08 | 2017-01-04 | 岳胜武 | Add-on type liquid silicon rubber viscosifier, preparation method and applications |
-
2019
- 2019-08-01 CN CN201910705477.2A patent/CN112300396A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060127347A (en) * | 2005-06-07 | 2006-12-12 | 주식회사 엘지화학 | Acrylic pressure sensitive adhesive compositions |
| CN102775611A (en) * | 2012-07-24 | 2012-11-14 | 东莞兆舜有机硅新材料科技有限公司 | Tackifier and production method thereof |
| CN104892942A (en) * | 2015-06-04 | 2015-09-09 | 成都拓利化工实业有限公司 | Tackifier for addition-type organic silicon rubber and preparation method thereof |
| CN104892945A (en) * | 2015-06-06 | 2015-09-09 | 深圳市富达瑞有机硅材料有限公司 | Organic silicon rubber composite tackifier and preparation method thereof |
| CN105131291A (en) * | 2015-09-29 | 2015-12-09 | 肇庆皓明有机硅材料有限公司 | Tackifier and preparation thereof as well as adhesion addition type liquid silicone rubber and preparation thereof |
| CN105482120A (en) * | 2015-12-18 | 2016-04-13 | 杭州福斯特光伏材料股份有限公司 | Preparation method of tackifier for addition type liquid silicone rubber |
| CN106279700A (en) * | 2016-08-08 | 2017-01-04 | 岳胜武 | Add-on type liquid silicon rubber viscosifier, preparation method and applications |
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