CN112175578A - Transparent UV (ultraviolet) in-situ curing organosilicon sealant and preparation method thereof - Google Patents
Transparent UV (ultraviolet) in-situ curing organosilicon sealant and preparation method thereof 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
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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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
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- C08G77/06—Preparatory processes
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- 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
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- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- 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
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/28—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen sulfur-containing groups
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- 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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- C08L2205/00—Polymer mixtures characterised by other features
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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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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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a transparent UV in-situ curing organosilicon sealant which comprises the following components in parts by weight: 75-95 parts of modified organic silicon resin, 1-10 parts of mercapto-functional organic silicon material, 1-10 parts of filler and 0.5-4 parts of photoinitiator. The invention has the beneficial effects that: the transparent UV in-situ curing organosilicon sealant belongs to single-component glue, can meet the requirements of automatic dispensing and rapid UV irradiation for in-situ curing, and achieves the effect of fully-automatically and rapidly shaping a sealing gasket in situ.
Description
Technical Field
The invention relates to the field of organic silica gel, in particular to a transparent UV in-situ curing organic silicon sealant and a preparation method thereof.
Background
Sealing gaskets required by common assembly of electronics and industry or direct assembly by adopting elastic sealing gaskets, but the problems of precision and tolerance of matched materials are involved, and the assembly is difficult to realize full automation, which often brings about the increase of additional cost and the reduction of production efficiency; or the problem of hot in-situ curing by adopting the sealant or the problem of room-temperature curing is solved, but the mode brings about the problems of energy consumption of high-temperature equipment or longer reaction time and limited productivity.
The UV curing material has the advantages of fast curing, energy conservation, normal temperature curing, less pollution and the like, and is more and more favored by various industries. The common UV curing is generally acrylate resin, which has excellent UV reaction activity, can be prepared into various materials with different hardness and elasticity according to different application requirements, and has wide market application. However, the traditional acrylic ester materials are difficult to use in harsh environments because of the limitations of the materials themselves, and are easily oxidized and cracked when the materials are kept at 120 ℃ or above for a long time, which causes the attenuation of the material performance.
The organosilicon material has been widely used in aerospace, electronics and electrical, chemical, transportation, medical and health, daily life and other fields because of its excellent high and low temperature resistance, weather resistance, aging resistance, corrosion resistance, low surface tension, physiological inertia and the like. The common curing mode of the organosilicon material is high-temperature curing or moisture curing, which limits the application of the organosilicon material and the improvement of downstream capacity to a certain extent.
Disclosure of Invention
Aiming at the problem of single curing mode of the existing organic silicon sealant, the invention provides a transparent UV (ultraviolet) in-situ curing organic silicon sealant which comprises the following components in parts by weight: 75-95 parts of modified organic silicon resin, 1-10 parts of mercapto-functional organic silicon material, 1-10 parts of filler and 0.5-4 parts of photoinitiator.
The data molecular weight of the modified organic silicon resin is 300-100000, and the structure is as follows:
(R1R2 2SiO1/2)x(R2 3SiO1/2)y(R1R2SiO2/2)a(R2 2SiO2/2)b(R2SiO3/2)m(SiO4/2)n，
in the formula, R1The structure is as follows:
the R is1The introduction of the structure refers to the introduction of two structural monomers as follows: ring body A and end sealing agent B:
each R2Independently selected from substituted or unsubstituted monovalent hydrocarbon groups of 1-10 carbon atoms; x, y, m and n are 0-4, and a and b are 10-50;
the structure of the mercapto-functionalized organosilicon material is:
(R2 3SiO1/2)x’(R3R2SiO2/2)a’(R2 2SiO2/2)b’(R3SiO3/2)m’，
in the formula, each R2Independently selected from substituted or unsubstituted monovalent hydrocarbon groups of 1-10 carbon atoms; r3Is a mercapto-functional group, which may be mercaptopropyl; x 'and m' are 0-10, and a 'and b' are 10-50.
The filler used in the invention is lipophilic white carbon black, and the photoinitiator used is one or a combination of more of 2-hydroxy-2-methyl-1-phenyl-1-acetone, (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide, phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-4' - (methylthio) -2-morpholine benzophenone or 2-isopropyl thioxanthone.
The preparation method of the transparent UV in-situ curing organosilicon sealant comprises the following steps:
1) preparation of modified Silicone resins
Mixing a sealing agent, a ring body, a dialkoxy silane monomer and a catalyst according to a corresponding molar ratio according to the structure of the target modified organic silicon resin, heating to 40-50 ℃, stirring for reaction for 0.5-1.5h, adding a multi-alkoxy silane monomer into a reaction bottle, slowly dropwise adding deionized water, heating to 100 plus 130 ℃ after heat preservation reaction for 30-60min, evaporating off byproduct ethanol and excessive water, keeping the internal temperature of the system above 90 ℃, and performing heat preservation reaction for 2-8h to obtain the modified organic silicon resin;
2) preparation of mercapto-functionalized organosilicon materials
Heating a sealing agent, a ring body, a dialkoxy silane monomer and a catalyst in a corresponding molar ratio to 40-50 ℃ according to the structure of the target mercapto-functionalized organosilicon, stirring for reaction for 0.5-1.5h, adding the trialkoxy silane monomer, slowly dropwise adding deionized water, carrying out heat preservation reaction for 30-60min, heating to 100-130 ℃, evaporating off by-product ethanol and excess water, keeping the internal temperature of the system above 90 ℃, and carrying out heat preservation reaction for 2-4h to obtain the mercapto-functionalized organosilicon;
3) preparation of the sealant
Weighing the components in parts by weight in a yellow light environment, adding the modified organic silicon resin, the mercapto-functionalized organic silicon material and the filler into a stirring kettle, uniformly stirring under the vacuum condition of less than 35 ℃ and more than 0.09MPa, adding the photoinitiator, and uniformly stirring to obtain the high-performance organic silicon/organic silicon composite material.
In the step 1) and the step 2), the addition amount of the catalyst is 0.5-1.5 per mill of the total mass of the end sealing agent, the small molecular ring body and the dialkoxy silane monomer, and the molar weight of the added deionized water is 0.5-1.5 times of that of the dialkoxy silane monomer;
the invention has the beneficial effects that: the preparation of the modified organic silicon resin adopts a hydrolysis mode to introduce acrylic acid groups, so that on one hand, the preparation of products with different structures and viscosities can be realized, and on the other hand, the modified organic silicon resin with determined target functionality and functional group positions can be easily obtained by adjusting the proportion of monomers, thereby being more beneficial to the adjustability of a formula crosslinking structure and performance. The mercapto-functionalized organosilicon material can improve the surface oxygen inhibition phenomenon of the UV organosilicon material, so that the surface of the product is dry and comfortable after being cured, the mercapto-functionalized organosilicon material synthesized by a hydrolysis method has good compatibility with main resin, the surface oxygen inhibition effect can be more effectively exerted by adjusting the position of the mercapto group, and meanwhile, the effects of adjusting the viscosity of the product and wetting a plasticizer can be realized in the formula. The transparent UV in-situ curing organosilicon sealant belongs to single-component glue, can meet the requirements of automatic dispensing and rapid UV irradiation for in-situ curing, and achieves the effect of fully-automatically and rapidly shaping a sealing gasket in situ.
Detailed Description
The present invention is described below with reference to examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Description of the drawings: in the examples of the present invention, Me represents a methyl group, and Ph represents a phenyl group.
Preparation of modified organic silicon resin
1. Modified Silicone resin (a)
154.4g of end capping agent B, 74.4g of ring body A, 1186g of octamethylcyclotetrasiloxane, 1.5g of concentrated sulfuric acid, 10g of ethanol and 10g of deionized water are added into a 2L three-neck flask, the temperature is raised to 50 ℃, stirring is carried out for reaction for 1 hour, 109g of methyltrimethoxysilane is added into a reaction bottle, 40g of deionized water is slowly dripped into the reaction bottle, after the dripping is finished, the reaction is carried out for 30 minutes under the condition of heat preservation, then the temperature is raised to 120 ℃, and by-product ethanol and excess water are removed by evaporation. When the temperature in the system rises to above 90 ℃, keeping the temperature for reaction for 3 hours, adding toluene for extraction, washing with distilled water to be neutral, and removing the solvent and micromolecules by reduced pressure distillation to obtain the target product modified organic silicon resin (a) with high photosensitive reaction activity, wherein the structural general formula of the target product is (R)1Me2SiO1/2)1(R1MeSiO2/2)0.5(Me2SiO2/2)20(MeSiO3/2)1。
2. Modified Silicone resin (b)
Adding 77.2g of end capping agent B, 1483g of octamethylcyclotetrasiloxane and 2g of tetramethylammonium hydroxide into a 2L three-neck flask under the protection of nitrogen, heating to 40 ℃, stirring for reaction for 0.5h, then heating to 100 ℃, keeping the temperature for reaction for 7h when the temperature in the system is raised to above 90 ℃, heating to 140 ℃ after the heat preservation reaction is finished, vacuumizing and stirring for reaction for 3h to obtain the modified organic silicon resin (B) with the target product having high photosensitive reaction activity, wherein the structural general formula of the target product is (R)1Me2SiO1/2)1(Me2SiO2/2)50。
3. Modified Silicone resin (c)
Adding 64.8g of hexamethyldisiloxane, 74.4g of ring body A, 1459g of methylphenyldimethoxysilane, 200g of deionized water and 3g of tetramethylammonium hydroxide into a 2L three-neck flask, heating to 50 ℃, stirring for reaction for 1h, heating to 100 ℃, evaporating to remove by-product ethanol and excess water, heating the interior of the system to 90 ℃, preserving heat for reaction for 2h, heating to 140 ℃ after the heat preservation reaction is finished, vacuumizing and stirring for reaction for 3h to obtain the target product (modified organic silicon resin (c) with high photosensitive reaction activity, wherein the structural general formula of the target product is (Me)3SiO1/2)1(R1MeSiO2/2)0.5(MePhSiO2/2)10。
4. Modified Silicone resin (d)
Adding 162.38g of hexamethyldisiloxane, 93g of ring body A, 741.55g of octamethylcyclotetrasiloxane, 1.5g of concentrated sulfuric acid, 10g of ethanol and 10g of deionized water into a 2L three-neck flask, heating to 45 ℃, stirring for reaction for 1.5h, then adding 417g of ethyl orthosilicate into a reaction bottle, slowly dropwise adding 100g of deionized water into the reaction bottle, after dropwise adding, keeping the temperature for reaction for 30min, subsequently heating to 120 ℃, and evaporating off by-product ethanol and excess water. Keeping the temperature to react for 2h when the internal temperature of the system rises to more than 90 ℃, adding toluene for extraction, washing the system with distilled water to be neutral, and removing the solvent and micromolecules by reduced pressure distillation to obtain the target product modified organic silicon resin (d) with high photosensitive reaction activity, wherein the structural general formula of the target product is (Me)3SiO1/2)2(R1MeSiO2/2)0.5(Me2SiO2/2)10(SiO4/2)2。
Preparation of di-and mercapto-functional organosilicon materials
1. Mercapto-functional silicone materials (. alpha.)
Adding 81.2g of hexamethyldisiloxane, 74.155g of octamethylcyclotetrasiloxane, 5g of concentrated sulfuric acid, 20g of ethanol and 8g of deionized water into a 1L three-neck flask, heating to 50 ℃, and stirring for reaction for 30min, adding 392.68g of mercaptopropyl trimethoxy silane into a reaction bottle, slowly adding 70g of deionized water dropwise into the reaction bottle, after the dropwise adding is finished, carrying out heat preservation reaction for 30min, then heating to 120 ℃, evaporating to remove by-product ethanol and redundant water, when the internal temperature of the system is raised to above 90 ℃, carrying out heat preservation reaction for 4h, adding methylbenzene for dilution, washing with distilled water to be neutral, carrying out reduced pressure distillation to remove solvent and micromolecules, and obtaining the target product, namely the mercapto-functionalized organosilicon material (alpha), wherein the structural general formula of the target product is (Me)3SiO1/2)1(Me2SiO2/2)1[HS(CH2)3SiO3/2]2。
2. Mercapto-functional silicone materials (. beta.)
Adding 81.2g of hexamethyldisiloxane, 721.36g of methylmercaptopropyldimethoxysilane, 733.08g of diphenyldimethoxysilane, 2g of tetramethylammonium hydroxide and 190g of water into a 2L three-neck flask, heating to 50 ℃, stirring for reaction for 1h, subsequently heating to 100 ℃, removing by-product ethanol and redundant water by evaporation, heating the interior of the system to 90 ℃, carrying out heat preservation reaction for 2h, heating to 140 ℃ after the heat preservation reaction is finished, vacuumizing and stirring for reaction for 3h to obtain the target product, namely, the mercapto-functionalized organosilicon material (beta), wherein the structural general formula of the target product is (Me)3SiO1/2)1[HS(CH2)3MeSiO2/2]4(Ph2SiO2/2)3。
Preparation of transparent UV in-situ curing organosilicon sealant
Example 1
In the environment of a yellow light lamp, 90g of modified organic silicon resin (a) with high photosensitive reaction activity, 3g of mercapto-functionalized organic silicon material (alpha) and 6g of hydrophobic meteorological silicon DM-20S are weighed and placed in a glue mixing device, are uniformly stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, are added with 1.2g of photoinitiator 1173, are uniformly mixed and stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, and are filled in a black rubber tube.
Example 2
In a yellow light lamp environment, 28g of modified organic silicon resin (b) with high photosensitive reaction activity, 50g of modified organic silicon resin (d) with high photosensitive reaction activity, 6.6g of mercapto-functionalized organic silicon material (alpha) and 15g of hydrophobic gas phase silicon H2000 are weighed and placed in a glue mixing device, are uniformly stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, then are added with 2g of photoinitiator 907 and 1g of photoinitiator 184 (ground into powder before use), are uniformly mixed and stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, and are filled in a black rubber tube.
Example 3
In the environment of a yellow light lamp, 85g of modified organic silicon resin (c) with high photosensitive reaction activity, 2g of mercapto-functionalized organic silicon material (beta) and 10g of hydrophobic meteorological silicon H2000 are weighed and placed in a glue mixing device, the materials are uniformly stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, then 2g of photoinitiator TPO (TPO) is added (the materials are ground into powder before use), and the materials are uniformly mixed and stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa and then filled in a black rubber tube.
The transparent UV in-situ curing organosilicon sealant obtained in the examples 1-3 is prepared into a 1.5mm adhesive film, LED-UV irradiation is carried out for 10s, after the irradiation is finished, the adhesive film is peeled off, and the test is carried out according to the standard (GB/T528-2009), and the results are shown in Table 1.
TABLE 1 test results of examples 1-3
| Example 1 | Example 2 | Example 3 | |
| Whether the surface is dry or not | Is that | Is that | Is that |
| Hardness of | 32A | 20A | 35D |
| Tensile strength | 1.2MPa | 0.75MPa | 2.3MPa |
| Elongation at break | 350％ | 400％ | 120％ |
From the test results it can be seen that: the transparent UV in-situ curing organosilicon sealant can realize rapid curing by UV irradiation (the curing can be completed within 10 s), and the surface is dry and comfortable after curing, so that the phenomenon of surface oxygen inhibition is overcome; secondly, after the glue is cured, the hardness can be changed to a large extent, and the sealing gasket has good deformation capacity and elasticity and has the effect of sealing the gasket. Within the scope of the patent, the preparation of products with different structures and viscosities can be realized, the modified organic silicon resin with determined target functionality and functional group positions can be easily obtained by adjusting the proportion of monomers, and the adjustability of the cross-linked structure and the performance of the formula is facilitated.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The transparent UV in-situ curing organosilicon sealant is characterized by comprising the following components in parts by weight:
75-95 parts of modified organic silicon resin, 1-10 parts of mercapto-functionalized organic silicon material, 1-10 parts of filler and 0.5-4 parts of photoinitiator;
the data molecular weight of the modified organic silicon resin is 300-100000, and the structure is as follows:
(R1R2 2SiO1/2)x(R2 3SiO1/2)y(R1R2SiO2/2)a(R2 2SiO2/2)b(R2SiO3/2)m(SiO4/2)n，
in the formula (I), the compound is shown in the specification,
R1the structure is as follows:
each R2Independently selected from substituted or unsubstituted monovalent hydrocarbon groups of 1-10 carbon atoms;
x, y, m and n are 0-4, and a and b are 10-50;
the structure of the mercapto-functionalized organosilicon material is as follows:
(R2 3SiO1/2)x’(R3R2SiO2/2)a’(R2 2SiO2/2)b’(R3SiO3/2)m’，
in the formula (I), the compound is shown in the specification,
each R2Independently selected from substituted or unsubstituted monovalent hydrocarbon groups of 1-10 carbon atoms;
R3is one of a mercapto-functional group or a mercaptopropyl group;
x 'and m' are 0-10, and a 'and b' are 10-50.
2. The transparent UV in situ curable silicone sealant according to claim 1, wherein the filler is oleophilic white carbon black.
3. The transparent UV in situ cure silicone sealant according to claim 1, wherein the photoinitiator is a combination of one or more of 2-hydroxy-2-methyl-1-phenyl-1-propanone, (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide, phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-4' - (methylthio) -2-morpholinobenzophenone, or 2-isopropylthioxanthone.
4. A method of preparing a transparent UV in situ curable silicone sealant according to any one of claims 1 to 3 comprising the steps of:
1) preparation of modified Silicone resins
Mixing a sealing agent, a ring body, a dialkoxy silane monomer and a catalyst according to a corresponding molar ratio according to the structure of the target modified organic silicon resin, heating to 40-50 ℃, stirring for reaction for 0.5-1.5h, adding a multi-alkoxy silane monomer into a reaction bottle, slowly dropwise adding deionized water, heating to 100-130 ℃ after heat preservation reaction for 30-60min, evaporating off by-product ethanol and excess water, keeping the internal temperature of the system above 90 ℃, and performing heat preservation reaction for 2-8h to obtain the modified organic silicon resin;
2) preparation of mercapto-functionalized organosilicon materials
Heating a sealing agent, a ring body, a dialkoxy silane monomer and a catalyst in a corresponding molar ratio to 40-50 ℃ according to the structure of the target mercapto-functionalized organosilicon, stirring for reaction for 0.5-1.5h, adding the trialkoxy silane monomer, slowly dropwise adding deionized water, carrying out heat preservation reaction for 30-60min, heating to 100-130 ℃, evaporating off by-product ethanol and excess water, keeping the internal temperature of the system above 90 ℃, and carrying out heat preservation reaction for 2-4h to obtain the mercapto-functionalized organosilicon;
3) preparation of the sealant
Weighing the components in parts by weight in a yellow light environment, adding the modified organic silicon resin, the mercapto-functionalized organic silicon material and the filler into a stirring kettle, uniformly stirring under the vacuum condition of less than 35 ℃ and more than 0.09MPa, adding the photoinitiator, and uniformly stirring to obtain the high-performance organic silicon/organic silicon composite material.
5. The method as claimed in claim 4, wherein in the step 1), the amount of the catalyst added is 0.5-1.5 per mill of the total mass of the end sealing agent, the small molecular ring body and the dialkoxy silane monomer, and the molar amount of the deionized water added is 0.5-1.5 times of the molar amount of the dialkoxy silane monomer; in the step 2), the addition amount of the catalyst is 0.5-1.5 per mill of the total mass of the end sealing agent, the small molecular ring body and the dialkoxy silane monomer, and the molar weight of the deionized water is 0.5-1.5 times of that of the dialkoxy silane monomer.
6. The method of claim 4, wherein in step 2), the ring body and the capping agent have the following structures represented by ring body A and capping agent B:
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604193A (en) * | 2021-09-06 | 2021-11-05 | 深圳市希顺有机硅科技有限公司 | Organosilicon sealant and preparation method thereof |
| CN113801628A (en) * | 2021-10-20 | 2021-12-17 | 烟台德邦科技股份有限公司 | UV-cured organic silicon coating adhesive and preparation method thereof |
| CN116144319A (en) * | 2022-11-28 | 2023-05-23 | 烟台德邦科技股份有限公司 | Rapid-curing single-component heat-conducting organopolysiloxane composition and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090192282A1 (en) * | 2008-01-25 | 2009-07-30 | National Science And Technology Development Agency | Synthetic method for preparing dual curable silicone compositions |
| CN102504270A (en) * | 2011-10-28 | 2012-06-20 | 中科院广州化学有限公司 | High-performance organic silicon electronic pouring sealant and preparation method and application thereof |
| JP2014001342A (en) * | 2012-06-20 | 2014-01-09 | Momentive Performance Materials Inc | Ultraviolet curable silicone resin composition and image display device using the same |
| CN105315675A (en) * | 2014-06-20 | 2016-02-10 | 上海交通大学 | Ultraviolet light-curing composition |
| CN107418505A (en) * | 2017-07-18 | 2017-12-01 | 江西绿洲环保新材料股份有限公司 | Ultraviolet light solidification sulfydryl/alkene organosilicon adhesive and preparation method thereof |
| CN109810516A (en) * | 2018-12-29 | 2019-05-28 | 山东大学 | A kind of ultraviolet light cure silicone rubber and preparation method thereof for DIW3D printing |
-
2020
- 2020-11-02 CN CN202011204264.0A patent/CN112175578A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090192282A1 (en) * | 2008-01-25 | 2009-07-30 | National Science And Technology Development Agency | Synthetic method for preparing dual curable silicone compositions |
| CN102504270A (en) * | 2011-10-28 | 2012-06-20 | 中科院广州化学有限公司 | High-performance organic silicon electronic pouring sealant and preparation method and application thereof |
| JP2014001342A (en) * | 2012-06-20 | 2014-01-09 | Momentive Performance Materials Inc | Ultraviolet curable silicone resin composition and image display device using the same |
| CN105315675A (en) * | 2014-06-20 | 2016-02-10 | 上海交通大学 | Ultraviolet light-curing composition |
| CN107418505A (en) * | 2017-07-18 | 2017-12-01 | 江西绿洲环保新材料股份有限公司 | Ultraviolet light solidification sulfydryl/alkene organosilicon adhesive and preparation method thereof |
| CN109810516A (en) * | 2018-12-29 | 2019-05-28 | 山东大学 | A kind of ultraviolet light cure silicone rubber and preparation method thereof for DIW3D printing |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604193A (en) * | 2021-09-06 | 2021-11-05 | 深圳市希顺有机硅科技有限公司 | Organosilicon sealant and preparation method thereof |
| CN113801628A (en) * | 2021-10-20 | 2021-12-17 | 烟台德邦科技股份有限公司 | UV-cured organic silicon coating adhesive and preparation method thereof |
| CN116144319A (en) * | 2022-11-28 | 2023-05-23 | 烟台德邦科技股份有限公司 | Rapid-curing single-component heat-conducting organopolysiloxane composition and preparation method thereof |
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