CN112778966A - Ketoxime-removing type silicone sealant with high light transmittance and preparation method thereof - Google Patents
Ketoxime-removing type silicone sealant with high light transmittance and preparation method thereof Download PDFInfo
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- CN112778966A CN112778966A CN202010302237.0A CN202010302237A CN112778966A CN 112778966 A CN112778966 A CN 112778966A CN 202010302237 A CN202010302237 A CN 202010302237A CN 112778966 A CN112778966 A CN 112778966A
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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
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- 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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Abstract
The invention discloses a ketoxime removing type silicone sealant with high light transmittance, which consists of alpha, omega-dihydroxy polydimethylsiloxane (107 glue), MQ silicone resin, a crosslinking agent 1, a crosslinking agent 2, a coupling agent and a catalyst, and comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane (107 glue), 50-100 parts of MQ silicon resin, 115-30 parts of cross-linking agent, 25-10 parts of cross-linking agent, 1-5 parts of coupling agent and 0.1-1 part of catalyst; the invention also discloses a preparation method of the ketoxime removal type silicone sealant with high light transmittance; the invention has the beneficial effects that: the problem that the mutual solubility of the ketoxime type cross-linking agent and alpha, omega-dihydroxy polydimethylsiloxane (107 glue) is poor is solved; after ultraviolet accelerated aging, the light transmittance performance of the sealant meets the requirement that the T is more than or equal to 96% in GB/T2410-2008 test results, and the problem of poor light transmittance of the ketoxime-removing type silicone sealant can be well solved.
Description
Technical Field
The invention belongs to the technical field of silicone sealants, and particularly relates to a ketoxime removing type silicone sealant with high light transmittance and a preparation method of the silicone sealant.
Background
The silicone sealant is a paste prepared by mixing polydimethylsiloxane as a main raw material, a cross-linking agent, a filler, a plasticizer, a coupling agent and a catalyst in a vacuum state, and is cured to form the elastic silicone rubber by reacting with water in the air at room temperature.
The silicone sealant is a polymer material with wide application, common applications are building bonding sealing, lamp bonding sealing, household appliance bonding sealing, furniture home decoration bonding sealing, rail transit bonding sealing and the like, and the wide application inevitably puts a plurality of requirements on the performance of products. The ketoxime removal type silicone sealant has the advantages of stable production process, good product storage performance, large curing performance adjustment space and the like, but because the ketoxime type cross-linking agent used by the ketoxime removal type silicone sealant is poor in intersolubility with alpha, omega-dihydroxy polydimethylsiloxane (107 glue), the ketoxime removal type silicone sealant is not suitable for producing a product with high light transmittance and is generally used for producing a semitransparent product.
For the application requiring high light transmittance for bonding and sealing, a sealant prepared from methyl phenyl silicone resin is generally used, for example, the preparation method of methyl phenyl vinyl silicone resin for LED packaging, which is filed as application No. cn200810120378.x, discloses methyl phenyl vinyl silicone resin which has the characteristics of high refractive index, clarity, transparency, radiation resistance, high and low temperature resistance, weather resistance and the like, is particularly suitable for high-molecular base glue in LED packaging materials, but does not describe the actual effect thereof. For example, CN201410581833.1, a silicone sealant for a daylighting panel and a preparation method thereof, discloses a silicone sealant for a daylighting panel with high elongation, low modulus and high light transmittance, which uses excessive fillers, flame retardants and other substances to reduce the light transmittance of the product, and has no feasible technical scheme to solve the technical problem of poor light transmittance of a ketoxime type silicone sealant caused by poor intersolubility of a ketoxime type cross-linking agent and alpha, omega-dihydroxy polydimethylsiloxane (107 glue).
In recent years, along with the development of the silicone sealant industry and the refinement of product performance, no relevant literature report or product market exists for a deketoxime type silicone sealant product with high light transmittance.
In order to solve the problem of poor light transmittance of the ketoxime removing silicone sealant, the ketoxime removing silicone sealant with high light transmittance and the preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide a ketoxime removing type silicone sealant with high light transmittance and a preparation method thereof, and solves the problem of poor light transmittance of the ketoxime removing type silicone sealant.
In order to achieve the purpose, the invention provides the following technical scheme: a deketoxime type silicone sealant with high light transmittance is composed of alpha, omega-dihydroxy polydimethylsiloxane (107 glue), MQ silicone resin, a cross-linking agent 1, a cross-linking agent 2, a coupling agent and a catalyst, and comprises the following components in parts by mass:
100 portions of alpha, omega-dihydroxy polydimethylsiloxane (107 glue)
50-100 parts of MQ silicon resin
115-30 parts of cross-linking agent
25-10 parts of cross-linking agent
1-5 parts of coupling agent
0.1-1 part of catalyst.
As a preferred technical scheme of the invention, the viscosity range of the alpha, omega-dihydroxy polydimethylsiloxane (107 glue) is 50000-500000 cps.
As a preferred technical scheme of the invention, the viscosity range of the MQ silicon resin is 1000-15000 cps.
As a preferable technical scheme of the invention, the crosslinking agent 1 is one or two of methyl tributyl ketoximyl silane, vinyl tributyl ketoximyl silane, phenyl tributyl ketoximyl silane and tetrabutoximyl silane.
In a preferred embodiment of the present invention, the crosslinking agent 2 is one or two selected from propyltrimethoxysilane and its oligomer, propyltriethoxysilane and its oligomer, octyltrimethoxysilane and its oligomer, and octyltriethoxysilane and its oligomer.
In a preferred embodiment of the present invention, the coupling agent is one or two of (N-propyl) aminopropyltrimethoxysilane and (N-propyl) aminopropyltriethoxysilane.
As a preferable technical scheme of the invention, the catalyst is one or two of dibutyltin diacetate, dibutyltin dilaurate, dibutyltin diacetylacetonate and dibutyltin diacetylacetate.
The invention also discloses a preparation method of the high-light-transmittance deketoxime type silicone sealant, which comprises the following steps:
the method comprises the following steps: preparing raw materials: the adhesive comprises alpha, omega-dihydroxy polydimethylsiloxane (107 glue), MQ silicon resin, a crosslinking agent 1, a crosslinking agent 2, a coupling agent and a catalyst, and comprises the following components in parts by mass:
100 portions of alpha, omega-dihydroxy polydimethylsiloxane (107 glue)
50-100 parts of MQ silicon resin
115-30 parts of cross-linking agent
25-10 parts of cross-linking agent
1-5 parts of coupling agent
0.1-1 part of catalyst;
step two: putting the alpha, omega-dihydroxy polydimethylsiloxane (107 glue), MQ silicon resin, a cross-linking agent 1 and a cross-linking agent 2 in the step one into a planetary stirrer or a high-speed dispersion stirrer for uniform dispersion;
step three: and then the coupling agent and the catalyst are put into a planetary stirrer or a high-speed dispersion stirrer, and are stirred and dispersed for 40min under the vacuum degree of-0.1 MPa, so that the high-light-transmittance deketoxime type silicone sealant can be obtained.
Compared with the prior art, the invention has the beneficial effects that:
(1) the problem that the mutual solubility of the ketoxime type cross-linking agent and alpha, omega-dihydroxy polydimethylsiloxane (107 glue) is poor is solved;
(2) after ultraviolet accelerated aging, the light transmittance performance of the sealant meets the requirement that the T is more than or equal to 96% in GB/T2410-2008 test results, and the problem of poor light transmittance of the ketoxime-removing type silicone sealant can be well solved.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
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
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a ketoxime removing type silicone sealant with high light transmittance comprises the following preparation processes:
100 parts of 250000cps alpha, omega-dihydroxy polydimethylsiloxane, 50 parts of 10000cps MQ silicon resin, 10 parts of vinyl tributyrinoxime silane, 10 parts of methyl tributyrinoxime silane and 8 parts of propyl trimethoxy silane are put into a planetary stirrer or a high-speed dispersion stirrer to be uniformly dispersed, 2.5 parts of (N-N-propyl) aminopropyl trimethoxy silane and 0.5 part of dibutyl tin diacetylacetonate are added, and the mixture is stirred and dispersed for 40min under the vacuum degree of-0.1 MPa, so that the high-transmittance deketoxime type silicone sealant can be obtained.
Example 2
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a ketoxime removing type silicone sealant with high light transmittance comprises the following preparation processes:
100 parts of 50000cps alpha, omega-dihydroxy polydimethylsiloxane, 100 parts of 15000cps MQ silicon resin, 15 parts of vinyl tributyrinoxime silane, 15 parts of methyl tributyrinoxime silane and 10 parts of octyl trimethoxy silane are put into a planetary stirrer or a high-speed dispersion stirrer to be uniformly dispersed, 5 parts of (N-N-propyl) aminopropyl triethoxysilane and 1 part of dibutyltin dilaurate are added, and the mixture is stirred and dispersed for 40min under the vacuum degree of-0.1 MPa, so that the high-light-transmittance deketoxime type silicone sealant can be obtained.
Example 3
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a ketoxime removing type silicone sealant with high light transmittance comprises the following preparation processes:
100 parts of 250000cps alpha, omega-dihydroxy polydimethylsiloxane, 50 parts of 10000cps MQ silicon resin, 10 parts of vinyl tributyrinoxime silane, 10 parts of methyl tributyrinoxime silane and 8 parts of propyl trimethoxy silane are put into a planetary stirrer or a high-speed dispersion stirrer to be uniformly dispersed, 2.5 parts of (N-N-propyl) aminopropyl trimethoxy silane and 0.5 part of dibutyl tin diacetylacetonate are added, and the mixture is stirred and dispersed for 40min under the vacuum degree of-0.1 MPa, so that the high-transmittance deketoxime type silicone sealant can be obtained.
Example 4
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a ketoxime removing type silicone sealant with high light transmittance comprises the following preparation processes:
100 parts of 50000cps alpha, omega-dihydroxy polydimethylsiloxane, 75 parts of 1000cps MQ silicone resin, 25 parts of methyl tributyroximosilane, 1 part of propyl trimethoxy silane and 3 parts of octyl trimethoxy silane are put into a planetary stirrer or a high-speed dispersion stirrer to be uniformly dispersed, then 1 part of (N-N-propyl) aminopropyl triethoxy silane and 0.5 part of dibutyltin dilaurate are added, and stirred and dispersed for 40min under the vacuum degree of-0.1 MPa, so that the high-light-transmittance deoxo-ketone-oxime silicone sealant can be obtained.
Example 5
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a ketoxime removing type silicone sealant with high light transmittance comprises the following preparation processes:
100 parts of 200000cps alpha, omega-dihydroxy polydimethylsiloxane, 75 parts of 10000cps MQ silicon resin, 5 parts of vinyl tributyrinoxime silane, 25 parts of methyl tributyrinoxime silane and 3 parts of octyl triethoxysilane are put into a planetary mixer or a high-speed dispersion mixer to be uniformly dispersed, 1 part of (N-N-propyl) aminopropyl trimethoxysilane and 0.1 part of dibutyltin diacetate are added, and the mixture is stirred and dispersed for 40min under the vacuum degree of-0.1 MPa, so that the high-light-transmittance deketoxime type silicone sealant can be obtained.
Comparative example 1
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a ketoxime removing type silicone sealant with high light transmittance comprises the following preparation processes:
100 parts of 500000cps alpha, omega-dihydroxy polydimethylsiloxane, 50 parts of gas phase SiO2, 15 parts of vinyl tributyrinoxime silane and 10 parts of methyl tributyrinoxime silane are put into a planetary stirrer or a high-speed dispersion stirrer to be uniformly dispersed, 1 part of aminopropyl trimethoxysilane and 0.1 part of dibutyltin diacetate are added, and stirring and dispersion are carried out for 40min under the vacuum degree of-0.1 MPa, so as to obtain the high-light-transmittance deketoxime type silicone sealant.
Comparative example 2
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a ketoxime removing type silicone sealant with high light transmittance comprises the following preparation processes:
100 parts of 50000cps alpha, omega-dihydroxy polydimethylsiloxane, 60 parts of gas phase SiO2, 5 parts of vinyl tributyrinoxime silane and 25 parts of methyl tributyrinoxime silane are put into a planetary stirrer or a high-speed dispersion stirrer to be uniformly dispersed, 1 part of aminopropyltriethoxysilane and 1 part of dibutyltin dilaurate are added, and the mixture is stirred and dispersed for 40min under the vacuum degree of-0.1 MPa, so that the high-light-transmittance deketoxime type silicone sealant can be obtained.
And (3) testing and results:
the sample piece is prepared, maintained in an environment with 23 ℃ and 55% humidity for 28 days and then tested:
light transmittance test standard: GB/T2410-2008;
ultraviolet light aging test reference standard: ASTM C1442-2014;
color of the test piece: visual inspection was carried out.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A ketoxime removing type silicone sealant with high light transmittance is characterized in that: the adhesive consists of alpha, omega-dihydroxy polydimethylsiloxane (107 glue), MQ silicon resin, a crosslinking agent 1, a crosslinking agent 2, a coupling agent and a catalyst, and comprises the following components in parts by mass:
100 portions of alpha, omega-dihydroxy polydimethylsiloxane (107 glue)
50-100 parts of MQ silicon resin
115-30 parts of cross-linking agent
25-10 parts of cross-linking agent
1-5 parts of coupling agent
0.1-1 part of catalyst.
2. The high transmittance deoketiminate silicone sealant according to claim 1, wherein: the viscosity of the α, ω -dihydroxypolydimethylsiloxane (107 gum) ranged from 50000-500000 cps.
3. The high transmittance deoketiminate silicone sealant according to claim 1, wherein: the viscosity range of the MQ silicone resin is 1000-15000 cps.
4. The high transmittance deoketiminate silicone sealant according to claim 1, wherein: the cross-linking agent 1 is one or two of methyl tributyrinoxime silane, vinyl tributyrinoxime silane, phenyl tributyrinoxime silane and tetrabutoximino silane.
5. The high transmittance deoketiminate silicone sealant according to claim 1, wherein: the cross-linking agent 2 is one or two of propyl trimethoxy silane and oligomer thereof, propyl triethoxy silane and oligomer thereof, octyl trimethoxy silane and oligomer thereof, and octyl triethoxy silane and oligomer thereof.
6. The high transmittance deoketiminate silicone sealant according to claim 1, wherein: the coupling agent is one or two of (N-N-propyl) aminopropyltrimethoxysilane and (N-N-propyl) aminopropyltriethoxysilane.
7. The high transmittance deoketiminate silicone sealant according to claim 1, wherein: the catalyst is one or two of dibutyltin diacetate, dibutyltin dilaurate, dibutyltin diacetylacetonate and dibutyltin diacetyl ethyl acetate.
8. The method for preparing a ketoxime-removing silicone sealant with high light transmittance according to any one of claims 1 to 7, wherein: the preparation method comprises the following steps:
the method comprises the following steps: preparing raw materials: the adhesive comprises alpha, omega-dihydroxy polydimethylsiloxane (107 glue), MQ silicon resin, a crosslinking agent 1, a crosslinking agent 2, a coupling agent and a catalyst, and comprises the following components in parts by mass:
100 portions of alpha, omega-dihydroxy polydimethylsiloxane (107 glue)
50-100 parts of MQ silicon resin
115-30 parts of cross-linking agent
25-10 parts of cross-linking agent
1-5 parts of coupling agent
0.1-1 part of catalyst;
step two: putting the alpha, omega-dihydroxy polydimethylsiloxane (107 glue), MQ silicon resin, a cross-linking agent 1 and a cross-linking agent 2 in the step one into a planetary stirrer or a high-speed dispersion stirrer for uniform dispersion;
step three: and then the coupling agent and the catalyst are put into a planetary stirrer or a high-speed dispersion stirrer, and are stirred and dispersed for 40min under the vacuum degree of-0.1 MPa, so that the high-light-transmittance deketoxime type silicone sealant can be obtained.
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| CN202010302237.0A CN112778966A (en) | 2020-04-16 | 2020-04-16 | Ketoxime-removing type silicone sealant with high light transmittance and preparation method thereof |
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| CN202010302237.0A CN112778966A (en) | 2020-04-16 | 2020-04-16 | Ketoxime-removing type silicone sealant with high light transmittance and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196370A (en) * | 2021-11-14 | 2022-03-18 | 广东力伊祥新材料有限公司 | Alcoholic oxime crosslinking system fast curing silicone sealant |
| CN114854201A (en) * | 2022-05-20 | 2022-08-05 | 长春艾德斯新材料有限公司 | Single-component condensed type terminal protection liquid silicone rubber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102167965A (en) * | 2011-01-13 | 2011-08-31 | 霍尼韦尔综合科技(中国)有限公司 | Bi-component room-temperature cured silicone sealant |
| CN104388040A (en) * | 2014-10-23 | 2015-03-04 | 中国航空工业集团公司北京航空材料研究院 | Single-component flame-retardant ketoxime-removed/dealcoholized room temperature vulcanized organosilicon sealant and preparation method thereof |
| CN110669472A (en) * | 2019-11-01 | 2020-01-10 | 重庆天旗实业有限公司 | Transparent flame-retardant silicone sealant |
-
2020
- 2020-04-16 CN CN202010302237.0A patent/CN112778966A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167965A (en) * | 2011-01-13 | 2011-08-31 | 霍尼韦尔综合科技(中国)有限公司 | Bi-component room-temperature cured silicone sealant |
| CN104388040A (en) * | 2014-10-23 | 2015-03-04 | 中国航空工业集团公司北京航空材料研究院 | Single-component flame-retardant ketoxime-removed/dealcoholized room temperature vulcanized organosilicon sealant and preparation method thereof |
| CN110669472A (en) * | 2019-11-01 | 2020-01-10 | 重庆天旗实业有限公司 | Transparent flame-retardant silicone sealant |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196370A (en) * | 2021-11-14 | 2022-03-18 | 广东力伊祥新材料有限公司 | Alcoholic oxime crosslinking system fast curing silicone sealant |
| CN114854201A (en) * | 2022-05-20 | 2022-08-05 | 长春艾德斯新材料有限公司 | Single-component condensed type terminal protection liquid silicone rubber and preparation method thereof |
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