CN113429931A - Addition type silk-screen silica gel and preparation method thereof - Google Patents
Addition type silk-screen silica gel and preparation method thereof Download PDFInfo
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- CN113429931A CN113429931A CN202110798044.3A CN202110798044A CN113429931A CN 113429931 A CN113429931 A CN 113429931A CN 202110798044 A CN202110798044 A CN 202110798044A CN 113429931 A CN113429931 A CN 113429931A
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- silicone oil
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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
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a silicon rubber product, in particular to an addition type silk-screen silica gel and a preparation method thereof, wherein the addition type silk-screen silica gel comprises a component A and a component B, and the component A comprises the following components in parts by weight: the component B comprises a first vinyl silicone oil, a reinforcing filler, hexamethyldisilazane, water, a second vinyl silicone oil, a hydrogen-containing silicone oil, a tackifier and an alkynol, wherein the component B comprises: a kast catalyst and a third vinyl silicone oil. The tackifier greatly increases the cohesiveness of the silica gel system, so that the silica gel system has good cohesiveness to the smooth and compact surface fabrics of nylon, terylene and the like, the reinforcing filler enables the silica gel system to have good fluidity, the thixotropy of the silica gel system is prevented from being reduced due to the addition of the tackifier, and the construction operation is convenient.
Description
Technical Field
The invention relates to a silicon rubber product, in particular to addition type silk-screen silicon rubber and a preparation method thereof.
Background
The addition liquid silicone rubber is widely applied to the aspects of clothing labels, printing, anti-skid coatings and the like, has the characteristics of no toxicity, no odor, green environmental protection and the like, can be mixed with various pigments to prepare colorful patterns, can be applied to color register silk screen to prepare beautiful landscape flowers with texture similar to oil paintings, and has the excellent characteristics which are more and more widely advocated and pursued by people.
However, silicone rubbers are known to have natural release characteristics and to have poor adhesion to substrate surfaces, especially for smooth surfaces. For cotton fabrics, the surface is rough, the fiber gaps are large, and the silicon rubber has good permeability, so the adhesive property with the cotton fabrics is good, but for fabrics with smooth and compact surfaces, such as polyester (polyester fiber) woven fabrics, nylon (polyamide fibers) and the like, the adhesive property is very difficult.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the addition type silk-screen silica gel, and the adhesion of a silica gel system is greatly improved by mixing a plurality of coupling agents as the tackifier of the invention, so that the silica gel system has good adhesion to smooth and compact fabrics of nylon, terylene and the like, and the silica gel system has good fluidity by mixing precipitated white carbon black and vinyl MQ resin as the reinforcing filler of the invention, thereby avoiding the reduction of the thixotropy of the silica gel system due to the addition of the tackifier and facilitating the construction operation.
The technical purpose of the invention is realized by the following technical scheme that the addition type silk-screen silica gel comprises a component A and a component B, wherein the components comprise the following components in parts by weight:
component A
90-110 parts of first vinyl silicone oil
10-15 parts of reinforcing filler
0.5-3 parts of hexamethyldisilazane
8-12 parts of water
90-110 parts of second vinyl silicone oil
130-140 parts of hydrogen-containing silicone oil
20-25 parts of tackifier
10-20 parts of alkynol
B component
5-15 parts of Kaster catalyst
And 90-110 parts of third vinyl silicone oil.
In the invention, the viscosity of the tackifier is 2000-3000 mPa.s, and the hydroxyl content in the tackifier is 6-10%.
In the invention, the tackifier comprises the following synthetic formula in parts by weight: 8-10 parts of gamma-glycidyl ether oxypropyltrimethoxysilane, 8-10 parts of hydroxyl-terminated vinyl silicone oil and 1-5 parts of butyl titanate.
In the invention, the viscosity of the first vinyl silicone oil is 38000-45000 mPa.s, and the content of vinyl in the first vinyl silicone oil is 0.30-0.40%.
In the invention, the reinforcing filler comprises precipitated silica and vinyl MQ resin, and the mass ratio of the precipitated silica to the vinyl MQ resin is 4-6: 1.
In the invention, the specific surface area of the precipitated silica white is 150-220m2(iv)/g, the ratio of M/Q in the vinyl MQ resin is 0.9.
In the invention, the viscosity of the hydrogen-containing silicone oil is 50-100mPa & s, and the hydrogen content in the hydrogen-containing silicone oil is 0.10-0.20%.
In the invention, the hydrogen-containing silicone oil comprises the following formula in parts by weight: 90-100 parts of octamethylcyclotetrasiloxane, 28-32 parts of tetramethylcyclotetrasiloxane, 6-10 parts of hexamethyldisiloxane and 1-2 parts of concentrated sulfuric acid.
The invention also aims to provide a preparation method of the addition type silk-screen silica gel, which is characterized by comprising the following steps of:
(1) preparing a basic sizing material: adding the first vinyl silicone oil, the reinforcing filler, hexamethyldisilazane and water into a modification kneader and mixing to prepare a base rubber material;
(2) preparation of hydrogen-containing silicone oil: putting octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, hexamethyldisiloxane and concentrated sulfuric acid into a reaction kettle, heating and stirring, standing and cooling, filtering, and removing low-boiling-point substances in vacuum to prepare hydrogen-containing silicone oil;
(3) preparing a tackifier: adding gamma-glycidoxypropyltrimethoxysilane, hydroxyl-terminated vinyl silicone oil and butyl titanate into a reaction kettle, heating, stirring and refluxing to remove low-boiling-point substances, and preparing to obtain the tackifier;
(4) preparing a component A and a component B: uniformly mixing a basic rubber material, second vinyl silicone oil, hydrogen-containing silicone oil, a tackifier and alkynol to prepare a component A; uniformly mixing the kast catalyst and the third vinyl silicone oil to prepare a component B;
(5) preparation of silica gel: and uniformly mixing the component A and the component B, and heating and curing to prepare the silk-screen silica gel.
In the invention, in the step (1), the mixing temperature is 140-; in the step (2), heating to 50-70 ℃, and stirring for 8-10 h; in the step (3), the ambient temperature of the reaction kettle is 200-220 ℃, and stirring and refluxing are carried out for 4-6 hours; in the step (5), heating and curing are carried out at the temperature of 100-120 ℃.
The invention has the following beneficial effects:
(1) the precipitation-method white carbon black and the vinyl MQ resin are mixed to be used as reinforcing filler, so that the thixotropy of a silica gel system can be increased, the operability is improved, and the silica gel system has better fluidity even when the using amount of the tackifier is larger, so that the construction operation is facilitated;
(2) the coupling agent is used as the adhesion promoter of the silica gel system, so that the adhesive strength of the silica gel system can be increased, and the silica gel has good adhesion to the fabric fabrics with smooth surfaces, such as nylon, terylene and the like.
Detailed Description
Example 1
The component A comprises: 123.5 parts of basic rubber, 100 parts of second vinyl silicone oil, 137 parts of hydrogen-containing silicone oil, 21 parts of tackifier and 15 parts of alkynol; and B component: 10 parts of a Kaster catalyst and 100 parts of third vinyl silicone oil.
Wherein the mass ratio of the component A to the component B is 10: 1.
wherein the viscosity of the tackifier is 2000 mPas, and the hydroxyl content of the tackifier is 6%.
Wherein the tackifier comprises gamma-glycidoxypropyltrimethoxysilane (KH560), hydroxyl-terminated vinyl silicone oil and butyl titanate. The coupling agent is used as the adhesion promoter of the silica gel system, so that the adhesive strength of the silica gel system can be increased, and the silica gel has good adhesion to the fabric fabrics with smooth surfaces, such as nylon, terylene and the like.
Further, in the tackifier, the content of the components is as follows according to parts by weight: 10 parts of gamma-glycidyl ether oxypropyl trimethoxy silane, 10 parts of hydroxyl-terminated vinyl silicone oil and 1 part of butyl titanate.
Wherein the base sizing material comprises a first vinyl silicone oil, a reinforcing filler, hexamethyldisilazane, and water.
Further, in the base rubber material, the contents of the components are as follows according to parts by weight: 100 parts of first vinyl silicone oil, 12 parts of reinforcing filler, 1.5 parts of hexamethyldisilazane and 10 parts of water.
Wherein the viscosity of the first vinyl silicone oil is 41000 mPas, and the content of vinyl in the first vinyl silicone oil is 0.30-0.40%.
Wherein the reinforcing filler comprises precipitated silica and vinyl MQ resin, and the mass ratio of the precipitated silica to the vinyl MQ resin is 5: 1.
Further, the specific surface area of the precipitated silica is 180m2The ratio of M/Q in the vinyl MQ resin was 0.9. The precipitation-method white carbon black and the vinyl MQ resin are mixed to be used as reinforcing filler, so that the thixotropy of a silica gel system can be increased, the operability is increased, and the silica gel system has better fluidity even when the using amount of the tackifier is larger.
Wherein, the hydrogen-containing silicone oil is used as the cross-linking agent of the invention, the viscosity of the hydrogen-containing silicone oil is 80 mPas, and the hydrogen content in the hydrogen-containing silicone oil is 0.10-0.20%.
Further, the hydrogen-containing silicone oil comprises the following formula in parts by weight: 100 parts of octamethylcyclotetrasiloxane, 30 parts of tetramethylcyclotetrasiloxane, 6 parts of hexamethyldisiloxane and 1 part of concentrated sulfuric acid.
Wherein the concentration of the concentrated sulfuric acid is 98 percent.
Wherein the alkynol is methylbutynol, and can inhibit hydrosilylation in a silica gel system.
Wherein, the content of platinum element in the Kaster catalyst is 1000 ppm.
The preparation method of the embodiment comprises the following steps:
(1) preparing a basic sizing material: adding vinyl silicone oil, precipitated white carbon black, vinyl MQ resin, hexamethyldisilazane and water into a modification kneader, and mixing for 5 hours at 150 ℃ to prepare a basic rubber material;
(2) preparation of hydrogen-containing silicone oil: putting octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, hexamethyldisiloxane and concentrated sulfuric acid into a reaction kettle, heating to 60 ℃, stirring and balancing for 8 hours, standing, cooling, filtering, and removing low-boiling-point substances in vacuum to prepare hydrogen-containing silicone oil;
(3) preparing a tackifier: adding KH560, hydroxyl-terminated vinyl silicone oil and butyl titanate into a reaction kettle environment with a thermometer, a condenser pipe and a nitrogen interface, heating, stirring and refluxing for 4h at the reaction kettle environment temperature of 200 ℃, and removing low-boiling-point substances to prepare the tackifier;
(4) preparing a component A and a component B: uniformly mixing a basic rubber material, second vinyl silicone oil, hydrogen-containing silicone oil, a tackifier and alkynol to prepare a component A; uniformly mixing the kast catalyst and the third vinyl silicone oil to prepare a component B;
(5) preparation of silica gel: and uniformly mixing the component A and the component B, and curing at 110 ℃ to prepare the silk-screen silica gel.
Example 2
The component A comprises: 108.5 parts of basic rubber material, 90 parts of second vinyl silicone oil, 130 parts of hydrogen-containing silicone oil, 20 parts of tackifier and 10 parts of alkynol; and B component: 5 parts of a Kaster catalyst and 90 parts of third vinyl silicone oil.
Wherein the mass ratio of the component A to the component B is 50: 1.
wherein the viscosity of the tackifier is 2500 mPas, and the hydroxyl content of the tackifier is 8%.
Wherein, in the tackifier, the contents of the components are as follows according to parts by weight: 8 parts of gamma-glycidyl ether oxypropyltrimethoxysilane, 8 parts of hydroxyl-terminated vinyl silicone oil and 4 parts of butyl titanate.
Wherein, in the basic rubber material, the contents of the components are as follows according to the parts by weight: 90 parts of first vinyl silicone oil, 10 parts of reinforcing filler, 0.5 part of hexamethyldisilazane and 8 parts of water.
Wherein the viscosity of the first vinyl silicone oil is 38000mPa · s.
Wherein the mass ratio of the precipitated white carbon black to the vinyl MQ resin is 4: 1, the specific surface area of the precipitated silica is 150m2/g。
The hydrogen-containing silicone oil is used as the cross-linking agent of the invention, the viscosity of the hydrogen-containing silicone oil is 50mPa & s, and the hydrogen-containing silicone oil comprises the following components in parts by weight: 90 parts of octamethylcyclotetrasiloxane, 28 parts of tetramethylcyclotetrasiloxane, 10 parts of hexamethyldisiloxane and 2 parts of concentrated sulfuric acid.
The difference between the preparation method of this example and example 1 is that: in the step (1), the heating temperature is 140 ℃, and the mixing time is 7 h; in the step (2), the heating temperature is 50 ℃, and the stirring time is 10 hours; in the step (3), the ambient temperature of the reaction kettle is 210 ℃, and the reflux time is 6 hours; in the step (5), the heating temperature is 100 ℃.
Example 3
The component A comprises: 140 parts of base rubber, 110 parts of second vinyl silicone oil, 140 parts of hydrogen-containing silicone oil, 25 parts of tackifier and 20 parts of alkynol; and B component: 15 parts of a Kaster catalyst and 110 parts of third vinyl silicone oil.
Wherein the mass ratio of the component A to the component B is 100: 1.
wherein the viscosity of the tackifier is 3000 mPas, and the hydroxyl content of the tackifier is 10%.
Wherein, in the tackifier, the contents of the components are as follows according to parts by weight: 10 parts of gamma-glycidyl ether oxypropyl trimethoxy silane, 10 parts of hydroxyl-terminated vinyl silicone oil and 5 parts of butyl titanate.
Wherein, in the basic rubber material, the contents of the components are as follows according to the parts by weight: 110 parts of first vinyl silicone oil, 15 parts of reinforcing filler, 3 parts of hexamethyldisilazane and 12 parts of water.
Wherein the viscosity of the first vinyl silicone oil is 45000 mPas.
Wherein the mass ratio of the precipitated white carbon black to the vinyl MQ resin is 6:1, the specific surface area of the precipitated silica is 220m2/g。
The hydrogen-containing silicone oil is used as the cross-linking agent of the invention, the viscosity of the hydrogen-containing silicone oil is 100mPa & s, and the hydrogen-containing silicone oil comprises the following components in parts by weight: 100 parts of octamethylcyclotetrasiloxane, 32 parts of tetramethylcyclotetrasiloxane, 6 parts of hexamethyldisiloxane and 2 parts of concentrated sulfuric acid.
The difference between the preparation method of this example and example 1 is that: in the step (1), the heating temperature is 170 ℃, and the mixing time is 6 h; in the step (2), the heating temperature is 70 ℃, and the stirring time is 9 hours; in the step (3), the ambient temperature of the reaction kettle is 220 ℃, and the reflux time is 5 hours; in the step (5), the heating temperature is 120 ℃.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is conceivable, and the examples presented herein demonstrate the results of applicants' actual experiments. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The addition type silk-screen silica gel is characterized by comprising a component A and a component B, wherein the components comprise the following components in parts by weight:
component A
90-110 parts of first vinyl silicone oil
10-15 parts of reinforcing filler
0.5-3 parts of hexamethyldisilazane
8-12 parts of water
90-110 parts of second vinyl silicone oil
130-140 parts of hydrogen-containing silicone oil
20-25 parts of tackifier
10-20 parts of alkynol
B component
5-15 parts of Kaster catalyst
And 90-110 parts of third vinyl silicone oil.
2. The addition type silk-screen silica gel as claimed in claim 1, wherein the viscosity of the tackifier is 2000 to 3000 mPa-s, and the content of hydroxyl in the tackifier is 6 to 10%.
3. The addition type silk-screen silica gel of claim 1, wherein the tackifier comprises the following synthetic formula in parts by weight: 8-10 parts of gamma-glycidyl ether oxypropyltrimethoxysilane, 8-10 parts of hydroxyl-terminated vinyl silicone oil and 1-5 parts of butyl titanate.
4. The addition type silk-screen silica gel of claim 1, wherein the viscosity of the first vinyl silicone oil is 38000-45000mPa · s, and the content of vinyl in the first vinyl silicone oil is 0.30-0.40%.
5. The addition type silk-screen printing silica gel of claim 1, wherein the reinforcing filler comprises precipitated silica and vinyl MQ resin, and the mass ratio of the precipitated silica to the vinyl MQ resin is 4-6: 1.
6. The addition type silk-screen silica gel as claimed in claim 5, wherein the specific surface area of the precipitated silica white is 150-220m2(iv)/g, the ratio of M/Q in the vinyl MQ resin is 0.9.
7. The addition type silk-screen silica gel as claimed in claim 1, wherein the viscosity of the hydrogen-containing silicone oil is 50-100 mPa-s, and the hydrogen content in the hydrogen-containing silicone oil is 0.10-0.20%.
8. The addition type silk-screen silica gel of claim 7, wherein the hydrogen-containing silicone oil comprises the following components in parts by weight: 90-100 parts of octamethylcyclotetrasiloxane, 28-32 parts of tetramethylcyclotetrasiloxane, 6-10 parts of hexamethyldisiloxane and 1-2 parts of concentrated sulfuric acid.
9. The method for preparing the addition type silk-screen silica gel as claimed in claim 1, which is characterized by comprising the following steps:
(1) preparing a basic sizing material: adding the first vinyl silicone oil, the reinforcing filler, hexamethyldisilazane and water into a modification kneader and mixing to prepare a base rubber material;
(2) preparation of hydrogen-containing silicone oil: putting octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, hexamethyldisiloxane and concentrated sulfuric acid into a reaction kettle, heating and stirring, standing and cooling, filtering, and removing low-boiling-point substances in vacuum to prepare hydrogen-containing silicone oil;
(3) preparing a tackifier: adding gamma-glycidoxypropyltrimethoxysilane, hydroxyl-terminated vinyl silicone oil and butyl titanate into a reaction kettle, heating, stirring and refluxing to remove low-boiling-point substances, and preparing to obtain the tackifier;
(4) preparing a component A and a component B: uniformly mixing a basic rubber material, second vinyl silicone oil, hydrogen-containing silicone oil, a tackifier and alkynol to prepare a component A; uniformly mixing the kast catalyst and the third vinyl silicone oil to prepare a component B;
(5) preparation of silica gel: and uniformly mixing the component A and the component B, and heating and curing to prepare the silk-screen silica gel.
10. The method for preparing addition type silk-screen silica gel according to claim 9, wherein in the step (1), the mixing temperature is 140-170 ℃, and the mixing time is 5-7 h; in the step (2), heating to 50-70 ℃, and stirring for 8-10 h; in the step (3), the ambient temperature of the reaction kettle is 200-220 ℃, and stirring and refluxing are carried out for 4-6 hours; in the step (5), the curing is carried out by heating at the temperature of 100-120 ℃.
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| CN202110798044.3A CN113429931A (en) | 2021-07-15 | 2021-07-15 | Addition type silk-screen silica gel and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386333A (en) * | 2022-09-13 | 2022-11-25 | 硅宝(深圳)研发中心有限公司 | Low-compression permanent-deformation single-component heat-cured organosilicon sealant and preparation method thereof |
| CN115418192A (en) * | 2022-10-15 | 2022-12-02 | 江苏矽时代材料科技有限公司 | Addition type room temperature curing high-bonding-strength pouring sealant and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104774333A (en) * | 2015-04-30 | 2015-07-15 | 绵阳惠利电子材料有限公司 | Addition type organic silicon rubber tackifier, preparation method and application thereof |
| CN106868891A (en) * | 2017-04-20 | 2017-06-20 | 东莞市科多有机硅材料有限公司 | Silk-screen printing spends silica gel and preparation method thereof with nature xerography |
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2021
- 2021-07-15 CN CN202110798044.3A patent/CN113429931A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104774333A (en) * | 2015-04-30 | 2015-07-15 | 绵阳惠利电子材料有限公司 | Addition type organic silicon rubber tackifier, preparation method and application thereof |
| CN106868891A (en) * | 2017-04-20 | 2017-06-20 | 东莞市科多有机硅材料有限公司 | Silk-screen printing spends silica gel and preparation method thereof with nature xerography |
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| 黄文润: "《硅油及其应用》", 31 July 2018, 四川科学技术出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386333A (en) * | 2022-09-13 | 2022-11-25 | 硅宝(深圳)研发中心有限公司 | Low-compression permanent-deformation single-component heat-cured organosilicon sealant and preparation method thereof |
| CN115386333B (en) * | 2022-09-13 | 2023-09-08 | 硅宝(深圳)研发中心有限公司 | Low-compression permanent deformation single-component thermosetting organosilicon sealant and preparation method thereof |
| CN115418192A (en) * | 2022-10-15 | 2022-12-02 | 江苏矽时代材料科技有限公司 | Addition type room temperature curing high-bonding-strength pouring sealant and preparation method and application thereof |
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Application publication date: 20210924 |