Organic silicon resin as well as preparation method and application thereof

A silicone and resin technology, applied in the field of silicone resin and its preparation, can solve the problems of affecting the release agent performance of the silicone resin, affecting the performance of the silicone resin, high viscosity of the silicone resin, etc., and achieving fast light curing speed. , Improve performance, good film-forming effect

Active Publication Date: 2018-06-29
SHANGHAI PHICHEM MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the process of realizing the present invention, the inventors have found that there are at least the following problems in the prior art: in the existing method for preparing a silicone resin containing double bonds by esterification, on the one hand, the Si-O bond is easy to undergo esterification. Fracture occurs in the process, which affects the performance of the final obtained silicone resin, and then affects the performance of the release agent of the obtained silicone resin; on the other hand, after the reaction finishes, it is necessary to wash with water or alkali to remove residual catalyst and excessive (formazine) base) acrylic acid, post-processing is more cumbersome
And utilize diisocyanate compound to prepare the organosilicon resin that contains double bond method to prepare the organosilicon resin viscosity that obtains is bigger, also can affect the performance of the release agent that uses this organosilicon resin

Method used

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  • Organic silicon resin as well as preparation method and application thereof
  • Organic silicon resin as well as preparation method and application thereof
  • Organic silicon resin as well as preparation method and application thereof

Examples

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preparation example Construction

[0065] In the second aspect, an embodiment of the present invention provides a method for preparing the above-mentioned silicone resin, which specifically includes the following steps:

[0066] Step 1, preparing polyether-modified silicone oil with a structure shown in formula (V);

[0067]

[0068] Wherein, n≥50, the structure of M is as shown in formula (II):

[0069]

[0070] Among them, m≥1, R 3 is an alkylene group;

[0071] Step 2, reacting the polyether-modified silicone oil obtained in step 1 with a compound having a structure shown in formula (VI) to obtain a silicone resin shown in formula (I);

[0072]

[0073] Among them, R 1 is an alkylene group, R 2 is hydrogen or methyl.

[0074] In the preparation method provided in the embodiment of the present invention, the silicone resin represented by formula (I) is prepared from polyether-modified silicone oil and a compound having a structure represented by formula (VI) as raw materials. Wherein, in the co...

Embodiment 1

[0106] This embodiment provides a silicone resin having a structure shown in formula (X), the preparation method of the silicone resin is as follows:

[0107] Step 101, add 5g of tetramethyldihydrodisiloxane (HMM, purchased from Dow Corning (Zhangjiagang) Silicone Co., Ltd., the same below) and 750g of octamethylcyclotetrasiloxane (D4 , purchased from Dow Corning (Zhangjiagang) Silicone Co., Ltd., the same below), and 37.75 g of amberlyst-35 solid acid catalyst (produced by Rohm and Haas Company, the same below) was added. The temperature was raised to 30°C for 12h. After the reaction finishes, remove the solid acid catalyst by filtration, and then add 0.5% NaHCO that accounts for the total mass of the filtrate in the resulting filtrate. 3 Neutralizes residual free acids. Afterwards, the unreacted D4 was distilled and extracted under the conditions of pressure -0.1MPa and temperature 130°C to obtain a clear and transparent hydrogen-terminated silicone oil represented by form...

Embodiment 2

[0116] This embodiment provides a silicone resin having a structure shown in formula (X), the preparation method of the silicone resin is as follows:

[0117] Step 201, prepare hydrogen-terminated silicone oil according to the method in step 101 in Example 1.

[0118] In step 202, weigh 100 g of the hydrogen-terminated silicone oil prepared in step 201, and add allyl polyether F6 (produced by Haian Petrochemical in Jiangsu Province, with a hydroxyl value of 45±8 mgKOH / g, the structure is shown in formula (XII), the same below ); Calculate the molar number of silicon-hydrogen bonds in the hydrogen-terminated silicone oil according to the measured hydrogen content, and the molar ratio of the silicon-hydrogen bonds in the allyl polyether F6 and the hydrogen-terminated silicone oil is 1.4:1.

[0119]

[0120] Then the temperature was raised to 100° C. under a nitrogen atmosphere, and then 10 ppm chloroplatinic acid solution in isopropanol was added to the reaction system, and t...

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Abstract

The invention discloses an organic silicon resin as well as a preparation method and the application thereof and belongs to the technical field of organic silicon resins. The organic silicon resin isof a structure of formula (I) as shown in the specification, in the formula, n is greater than or equal to 50; R1 is alkylene; R2 is hydrogen or methyl; M is of a structural formula (II) as shown in the specification, in the formula, m is greater than or equal to 1; R3 is alkylene. The organic silicon resin is relatively low in viscosity, rapid in photo-curing speed, good in filming property and in addition simple in preparation process; when the organic silicon resin is adopted as a host resin of a release agent, the properties of the release agent can be improved, and the release force of afilm formed after the release agent is cured can be reduced.

Description

technical field [0001] The invention relates to the technical field of silicone resins, in particular to a silicone resin and its preparation method and application. Background technique [0002] Silicone resin is an organic polymer material containing silicon atoms in the main chain of the molecule. The bond energy of the Si-O bond in its molecular structure is as high as 425kJ / mol, much higher than the bond energy of the C-C bond (375kJ / mol) and the C-O bond (351kJ / mol), so the silicone resin has a high degree of flexibility and good Excellent high temperature and low temperature resistance, good stability and oxidation resistance. Moreover, due to the small surface tension and large molecular volume of silicone resin, it has excellent weather resistance and water resistance. However, for organosiloxanes containing only Si-O bonds in their molecules, due to their low cohesive energy and density, their strength is low and their mechanical strength is poor. Adhesion to me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/388C08G81/00C09D183/04C09D183/08C09D183/12
CPCC08G77/38C08G77/388C08G81/00C08L2205/025C08L2205/035C09D183/04C08L83/08C08L83/12
Inventor 刘陈红张志鹏刘翘楚江彭胜吴胜密王海群孙培旸
Owner SHANGHAI PHICHEM MATERIAL CO LTD
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