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Preparation method for organic silicon resin

A silicone and resin technology, which is applied in the field of silicone resin preparation, can solve problems such as difficult to meet requirements, difficult filtration, calcium chloride agglomeration, etc., and achieve the effects of simplification of treatment process, high filtration efficiency and time saving

Inactive Publication Date: 2009-11-04
ZHUZHOU TIMES NEW MATERIALS TECH
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  • Application Information

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Problems solved by technology

This process is difficult to filter, there is a small amount of moisture remaining in the silicone toluene layer, and the resin has poor transparency; for the preparation of silicone resins containing little or no water, this process is difficult to meet the requirements
Someone once used anhydrous calcium chloride to remove water during the filtration process, but the effect was not satisfactory. CaCl2 can not only dissolve in water, but also easily cause calcium chloride to agglomerate, resulting in difficulty in filtration, and this filtration method is also very difficult. It is difficult to ensure that no water enters the silicone toluene layer
There are also hydrocarbyl trialkoxysilanes as starting materials, and the ratio is determined according to the silicone resin R / Si value of 0.7 to 1.5. At the same time, water, weak polar or non-polar solvents and 0.1N hydrochloric acid are added, and the reaction is carried out by heating and aging. To obtain a silicone resin solution, such as the method disclosed in the Chinese patent literature whose patent number is ZL200610020361.8 and named "Synthetic Method of Silicone Resin", but the silicone resin produced by this method is still difficult to obtain Silicone resin with little or no water content

Method used

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  • Preparation method for organic silicon resin

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Embodiment 1

[0016] A preparation process of a silicone resin containing no or little water, which adopts a conventional hydrolysis polycondensation reaction process to prepare the silicone resin. The pressure distillation oil-water separation process, the vacuum distillation oil-water separation operation is carried out before filtration, and the trace moisture remaining in the organosilicon toluene layer is removed by vacuum distillation oil-water separation. Preparation of 100% solid-containing silicone resin, the specific process is as follows:

[0017] a. Put the raw materials into the mixing tank and stir for 1 hour at 25-35°C;

[0018] b. Add the mixed monomers dropwise at 30-50°C, and finish adding within 5-7 hours;

[0019] c. Continue to stir for 1 hour after adding the materials, let stand to separate layers, and release the acidic water layer;

[0020] d. Under the condition of 40-50°C, wash with tap water for 4-6 times until the pH value is 7;

[0021] e. The organic silico...

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Abstract

A method for preparing a silicone resin. The silicone resin is prepared by conventional hydrolysis polycondensation reaction process, which is characterized in that: between the water washing and filtration process of conventional hydrolysis polycondensation reaction process, a conventional vacuum distillation oil-water separation process is added, and vacuum distillation oil-water separation is carried out before filtration Operation, the trace moisture remaining in the organosilicon toluene layer was removed by vacuum distillation oil-water separation. The process is simple, easy to operate, saves energy, and has high filtration efficiency. The filtration time of the original treatment process is shortened from 15 hours to about 2 hours, which greatly improves the problem of difficult filtration and simplifies the subsequent treatment process. This process fully meets the special needs of preparing silicone resins containing little or no water, especially for the preparation of 100% solid silicone resins.

Description

technical field [0001] The invention relates to a process for preparing silicone resin, in particular to a process for preparing 100% solid-containing silicone resin. Mainly used in the preparation of silicone resin. Background technique [0002] At present, the domestic production of silicone resins is basically carried out by direct filtration after washing, such as the technical content published in the Chinese patent literature with the patent number ZL200610097518.7 and the name "Preparation Method of High Temperature Resisting Silicone Resin". This process has problems such as difficult filtration, trace moisture remaining in the silicone toluene layer, and poor resin transparency; for the preparation of silicone resins containing little or no water, this process is difficult to meet the requirements. Someone once used anhydrous calcium chloride to remove water during the filtration process, but the effect was not satisfactory. CaCl2 can not only dissolve in water, bu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/00
Inventor 姜其斌衷敬和黎勇李强军
Owner ZHUZHOU TIMES NEW MATERIALS TECH