CN112795367A - Preparation of high-refractivity silica gel capable of being quickly defoamed - Google Patents
Preparation of high-refractivity silica gel capable of being quickly defoamed Download PDFInfo
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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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- 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
- C08L83/04—Polysiloxanes
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- 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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- 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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- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention relates to the technical field of optical silica gel, in particular to preparation of high-refractivity silica gel capable of being defoamed quickly. The quick defoaming high-refractivity silicon gel comprises a component A and a component B, wherein the component A consists of base glue, a cross-linking agent, an additive and an inhibitor, the component B consists of base glue, a catalyst and an additive, the base glue is vinyl phenyl silicone oil, the cross-linking agent is phenyl hydrogen-containing silicone oil, the inhibitor is at least one selected from alkynol, vinyl cyclic bodies and methyl butynol, the catalyst is selected from platinum catalysts, in the preparation of the quick defoaming high-refractivity silicon gel, the added additive is nano solid powder selected from modified nano white carbon black and nano vinyl MQ silicone resin, on one hand, the light transmittance and the refractive index are not influenced by adding the nano powder, and meanwhile, the solid substance plays a role in foaming and can be quickly self-defoamed or defoam.
Description
Technical Field
The invention relates to the technical field of optical silica gel, in particular to preparation of high-refractivity silica gel capable of being defoamed quickly.
Background
The silicon gel material is widely applied to the field of optical full-lamination due to the characteristics of excellent optical performance, low shrinkage rate, good temperature resistance and the like, the conventional silicon gel material generally uses a polydimethylsiloxane main body material to perform a bonding effect after cross-linking and curing, the refractive index of the polydimethylsiloxane is about 1.4 generally, and the refractive index of the polydimethylsiloxane is different from that of glass to a certain extent, so that certain loss is caused when light passes through the interface between the glass and the gel, and the display effect of a picture is influenced.
The high-refractive-index silicone gel material can reduce optical loss, has good heat resistance, and has good shielding effect on ultraviolet rays to protect a screen well, so that the high-refractive-index silicone gel material has good application prospect, but the high-refractive-index silicone gel system is difficult to remove once bubbles are generated in application due to excessive system viscosity and excessive surface tension of base glue, and the application of the high-refractive-index silicone gel material is greatly limited.
Disclosure of Invention
The invention aims to provide a preparation method of a high-refractivity silica gel capable of being defoamed rapidly, so as to solve the problems in the background technology.
In order to achieve the above object, in one aspect, the present invention provides a high refractive index silica gel that is rapidly defoamed, which comprises a formulation, wherein the formulation comprises a component a and a component B in a weight ratio;
the component A consists of the following raw materials: 80-97 parts of base adhesive, 0.01-15 parts of cross-linking agent, 0.01-2 parts of additive and 0.001-1 part of inhibitor;
the component B consists of the following raw materials: 70-99 parts of base rubber, 0.001-1 part of catalyst and 0.01-2 parts of additive.
As a further improvement of the technical scheme, the base rubber is vinyl phenyl silicone oil, the silicone oil product has stable quality, low volatile matter, no yellowing and no crosslinking, and is a main raw material of addition type liquid silicone rubber, an organic silicon potting material, silicone gel and the like.
As a further improvement of the technical scheme, the cross-linking agent is phenyl hydrogen-containing silicone oil which at least contains three Si-H bonds and has better compatibility with vinyl phenyl silicone oil, and the strength, the wear resistance, the heat resistance and the like of the silicone rubber can be improved.
As a further improvement of the technical scheme, the inhibitor is selected from at least one of alkynol, vinyl ring body and methylbutynol and is used as an addition type silicone rubber storage stabilizer.
As a further improvement of the technical scheme, the additive is nano solid powder, the nano solid powder is selected from modified nano white carbon black and nano vinyl MQ silicon resin, the modified nano white carbon black is specifically silanization modified gas phase method nano white carbon black, and the specific surface area of the modified nano white carbon black is 100-500m2The nano powder does not influence the light transmission and the refractive index, and the solid matter plays a role in puncturing and foaming and can be quickly self-defoamed or easily defoamed.
As a further improvement of the technical proposal, the catalyst is selected from platinum catalysts, and the platinum content of the platinum catalyst is 5000 x 10-6The catalyst has the advantages of high catalytic activity, strong selectivity, convenient preparation of the catalyst, small usage amount, optimized catalytic performance by compounding with other metals or promoter active components through the change and improvement of the preparation method, wide application field, repeated regeneration and activation, long service life, capability of recycling the metal palladium of the waste catalyst and the like.
On the other hand, the invention provides a preparation method of the quickly-defoamed high-refractivity silica gel, which comprises the following operation steps:
s1, mixing the component A and the component B respectively according to a proportion;
s2, adding the component A and the component B into a double-helix conical mixer, and mixing to obtain silica gel;
s3, placing the silica gel in a vacuum drying oven for defoaming;
and S4, introducing the rubber material into a mold, vulcanizing, and preparing test pieces with different thicknesses as required for later use.
Preferably, in the S2, the weight ratio of the component A to the component B is 1: 1.
Preferably, in S3, the vacuum degassing time is 2-5 min.
Preferably, in the S4, the vulcanization temperature is 70-100 ℃, and the vulcanization time is 15-30 min.
Compared with the prior art, the invention has the beneficial effects that:
1. in the preparation of the high-refractivity silicon gel capable of being quickly defoamed, the added additive is nano solid powder selected from modified nano white carbon black and nano vinyl MQ silicon resin, on one hand, the light transmittance and the refractive index are not influenced by adding the nano powder, and meanwhile, the solid matter plays a role in foaming and can be quickly self-defoamed or be defoamed more easily.
Drawings
Fig. 1 is an overall flow chart of embodiment 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1 a preparation of a rapidly debubbled high refractive index silica gel comprising:
firstly, preparation of component A
97 parts of base rubber and 0.01 part of cross-linking agent are taken and added into a double-helix conical mixer, and then 0.01 part of additive and 1 part of inhibitor are added and mixed evenly to prepare the component A.
Preparation of two and B components
Taking 70 parts of base rubber, 0.001 part of catalyst and 2 parts of additive, adding into a double-helix conical mixer, and uniformly mixing to obtain the component B.
Preparation of optical silica gel
Adding the component A and the component B into a double-helix conical mixer according to the weight ratio of 1:1, mixing to obtain silica gel, placing the silica gel in a vacuum drying oven for defoaming for 2-5min, introducing the rubber material into a mold, vulcanizing at 70-100 ℃ for 15-30min, and preparing test pieces with different thicknesses as required for later use.
Example 2 a preparation of a rapidly debubbled high refractive index silica gel, comprising:
firstly, preparation of component A
And (3) adding 95 parts of base rubber and 3.5 parts of cross-linking agent into a double-helix conical mixer, then adding 0.5 part of additive and 0.75 part of inhibitor, and uniformly mixing to obtain the component A.
Preparation of two and B components
And (3) adding 77.5 parts of base rubber, 0.25 part of catalyst and 1.5 parts of additive into a double-helix conical mixer, and uniformly mixing to obtain the component B.
Preparation of optical silica gel
Adding the component A and the component B into a double-helix conical mixer according to the weight ratio of 1:1, mixing to obtain silica gel, placing the silica gel in a vacuum drying oven for defoaming for 2-5min, introducing the rubber material into a mold, vulcanizing at 70-100 ℃ for 15-30min, and preparing test pieces with different thicknesses as required for later use.
Example 3 a preparation of a rapidly debubbled high refractive index silica gel, comprising:
firstly, preparation of component A
And (3) adding 90 parts of base rubber and 7.5 parts of cross-linking agent into a double-helix conical mixer, then adding 1 part of additive and 0.5 part of inhibitor, and uniformly mixing to obtain the component A.
Preparation of two and B components
And adding 85 parts of base rubber, 0.5 part of catalyst and 1 part of additive into a double-helix conical mixer, and uniformly mixing to obtain the component B.
Preparation of optical silica gel
Adding the component A and the component B into a double-helix conical mixer according to the weight ratio of 1:1, mixing to obtain silica gel, placing the silica gel in a vacuum drying oven for defoaming for 2-5min, introducing the rubber material into a mold, vulcanizing at 70-100 ℃ for 15-30min, and preparing test pieces with different thicknesses as required for later use.
Example 4 a preparation of a rapidly debubbled high refractive index silica gel, comprising:
firstly, preparation of component A
Taking 85 parts of base rubber and 11 parts of cross-linking agent, adding into a double-helix conical mixer, then adding 1.5 parts of additive and 0.25 part of inhibitor, and uniformly mixing to obtain the component A.
Preparation of two and B components
And adding 92.5 parts of base rubber, 0.75 part of catalyst and 0.5 part of additive into a double-helix conical mixer, and uniformly mixing to obtain the component B.
Preparation of optical silica gel
Adding the component A and the component B into a double-helix conical mixer according to the weight ratio of 1:1, mixing to obtain silica gel, placing the silica gel in a vacuum drying oven for defoaming for 2-5min, introducing the rubber material into a mold, vulcanizing at 70-100 ℃ for 15-30min, and preparing test pieces with different thicknesses as required for later use.
Example 5 preparation of a rapidly debubbled high refractive index silica gel comprising:
firstly, preparation of component A
And (3) adding 80 parts of base rubber and 15 parts of cross-linking agent into a double-helix conical mixer, then adding 2 parts of additive and 0.001 part of inhibitor, and uniformly mixing to obtain the component A.
Preparation of two and B components
And (3) adding 99 parts of base rubber, 1 part of catalyst and 0.01 part of additive into a double-helix conical mixer, and uniformly mixing to obtain the component B.
Preparation of optical silica gel
Adding the component A and the component B into a double-helix conical mixer according to the weight ratio of 1:1, mixing to obtain silica gel, placing the silica gel in a vacuum drying oven for defoaming for 2-5min, introducing the rubber material into a mold, vulcanizing at 70-100 ℃ for 15-30min, and preparing test pieces with different thicknesses as required for later use.
The base rubber is vinyl phenyl silicone oil, the silicone oil product has stable quality, low volatile matter content, no yellowing and no crosslinking, and is the main raw material of addition type liquid silicone rubber, organic silicon potting material, silicone gel and the like;
the phenyl hydrogen-containing silicone oil at least contains three Si-H bonds, has better compatibility with vinyl phenyl silicone oil, and can improve the strength, the wear resistance, the heat resistance and the like of the silicone rubber;
the inhibitor is selected from at least one of alkynol, vinyl ring body and methylbutynol, and is used as an addition type silicone rubber storage stabilizer;
the additive is nano solid powder, the nano solid powder is selected from modified nano white carbon black and nano vinyl MQ silicon resin, the modified nano white carbon black is specifically silanization modified gas phase method nano white carbon black, the specific surface area of the modified nano white carbon black is 100-500m2The nano powder does not influence the light transmission and the refractive index, and meanwhile, the solid substance plays a role in pricking and can be quickly self-defoamed or easily defoamed;
the catalyst is selected from platinum catalysts with a platinum content of 5000 x 10-6The catalyst has the advantages of high catalytic activity, strong selectivity, convenient preparation of the catalyst, small usage amount, optimized catalytic performance by compounding with other metals or promoter active components through the change and improvement of the preparation method, wide application field, repeated regeneration and activation, long service life, capability of recycling the metal palladium of the waste catalyst and the like.
In the rapidly-defoamed high-refractivity silica gel prepared by the invention, the defoaming time is short, and the refractive index and the light transmittance are good, and the detection indexes of the rapidly-defoamed high-refractivity silica gel prepared by the invention are shown in table 1:
TABLE 1
According to table 1, in examples 1-5, the light transmittance of the prepared optical silica gel is above 90.0%, and the refractive index is higher than 13.5N, so that the optical silica gel prepared by the invention has better refractive index and light transmittance;
in examples 1-5, when 90 parts of the base rubber, 7.5 parts of the crosslinking agent, 1 part of the additive and 0.5 part of the inhibitor are contained in the component A, and 85 parts of the base rubber, 0.5 part of the catalyst and 1 part of the additive are contained in the component B, the defoaming time of the prepared optical silica gel is shortest, so that the defoaming effect of the high-refractive-index silica gel prepared in example 3 is the best.
Comparative example 1 a preparation of a rapidly debubbled high refractive index silica gel comprising:
firstly, preparation of component A
And (3) adding 90 parts of base rubber and 7.5 parts of cross-linking agent into a double-helix conical mixer, then adding 0.5 part of inhibitor, and uniformly mixing to obtain the component A.
Preparation of two and B components
And adding 85 parts of base rubber and 0.5 part of catalyst into a double-helix conical mixer, and uniformly mixing to obtain the component B.
Preparation of optical silica gel
Adding the component A and the component B into a double-helix conical mixer according to the weight ratio of 1:1, mixing to obtain silica gel, placing the silica gel in a vacuum drying oven for defoaming for 2-5min, introducing the rubber material into a mold, vulcanizing at 70-100 ℃ for 15-30min, and preparing test pieces with different thicknesses as required for later use.
In the rapidly-defoamed high-refractive-index silica gel prepared by the invention, the defoaming effect is good, the light transmittance and the refractive index of the silica gel are not influenced, and the defoaming effect has a large relationship with the added colorant, and in order to verify the related technical scheme, the applicant performs the following tests:
comparative example 1: by using the method of example 3, the relevant indexes of the prepared high refractive index silica gel were examined under the condition of removing the additives in the component a and the component B, and are specifically shown in table 2:
TABLE 2
According to table 2, in comparative example 1, when the additives in the a component and the B component are removed, the defoaming time in the prepared high refractive index silica gel is 10min, which is obviously increased, but the light transmittance and the refractive index are not changed, so it can be seen that the additives are important factors affecting the defoaming effect of the high refractive index silica gel.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A high-refractivity silica gel capable of being defoamed quickly comprises a formula, and is characterized in that: the formula consists of a component A and a component B in a weight ratio;
the component A consists of the following raw materials: 80-97 parts of base adhesive, 0.01-15 parts of cross-linking agent, 0.01-2 parts of additive and 0.001-1 part of inhibitor;
the component B consists of the following raw materials: 70-99 parts of base rubber, 0.001-1 part of catalyst and 0.01-2 parts of additive.
2. The rapidly debubbling high refractive index silica gel according to claim 1, wherein: the base adhesive is vinyl phenyl silicone oil.
3. The rapidly debubbling high refractive index silica gel according to claim 1, wherein: the cross-linking agent is phenyl hydrogen-containing silicone oil which at least contains three Si-H bonds.
4. The rapidly debubbling high refractive index silica gel according to claim 1, wherein: the inhibitor is selected from at least one of alkynol, vinyl ring body and methylbutynol.
5. The rapidly debubbling high refractive index silica gel according to claim 1, wherein: the additive is nano solid powder, the nano solid powder is selected from modified nano white carbon black and nano vinyl MQ silicon resin, and the modified nano white carbon black is specifically silanization modifiedThe specific surface area of the fumed silica is 100-500m2/g。
6. The rapidly debubbling high refractive index silica gel according to claim 1, wherein: the catalyst is selected from platinum catalysts with a platinum content of 5000 x 10-6。
7. The preparation method of the high-refractivity silica gel capable of being quickly defoamed is characterized by comprising the following steps of: the rapidly debubbling high refractive index silica gel according to any one of claims 1 to 6, which is carried out by the following steps:
s1, mixing the component A and the component B respectively according to a proportion;
s2, adding the component A and the component B into a double-helix conical mixer, and mixing to obtain silica gel;
s3, placing the silica gel in a vacuum drying oven for defoaming;
and S4, introducing the rubber material into a mold, vulcanizing, and preparing test pieces with different thicknesses as required for later use.
8. The preparation of the rapidly debubbled high refractive index silica gel according to claim 7, wherein: in the S2, the weight ratio of the component A to the component B is 1: 1.
9. The preparation of the rapidly debubbled high refractive index silica gel according to claim 7, wherein: and in the step S3, the vacuum defoaming time is 3-5 min.
10. The preparation of the rapidly debubbled high refractive index silica gel according to claim 7, wherein: in the S4, the vulcanizing temperature is 70-100 ℃, and the vulcanizing time is 15-30 min.
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Cited By (1)
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| CN116254002A (en) * | 2023-02-23 | 2023-06-13 | 深圳市森日有机硅材料股份有限公司 | Liquid silicone rubber composition for coating air bags and preparation method thereof |
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| CN116254002B (en) * | 2023-02-23 | 2023-12-19 | 深圳市森日有机硅材料股份有限公司 | Liquid silicone rubber composition for coating air bags and preparation method thereof |
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Application publication date: 20210514 |