Method for preparing high-quality polythiol curing agent for epoxy resin

A high-quality technology for epoxy resin, applied in the direction of chemical recycling, etc., can solve the problems of large industrial-scale production and application limitations, high production and separation costs, not meeting green environmental protection, etc., and achieves good industrial application prospects and halogen residues. Low, mild effects

Active Publication Date: 2019-12-03
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Application Information

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Problems solved by technology

[0004] But, the polythiol curing agent that above-mentioned preparation method obtains, product is mostly yellow-green or light yellow, and transparency is poor, and mostly used in the above-mentioned preparation method is quaternary ammonium salt type phase-transfer catalyst, can remain in the product after use. Excessive residues of halogens, etc., such as the high content of chloride ions in the obtained product, do not meet the requirements of green environmental protection; and the catalyst is not easy to recycle, the cost of production and separation is high, and the limitations of industrial-scale production and application are large

Method used

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  • Method for preparing high-quality polythiol curing agent for epoxy resin
  • Method for preparing high-quality polythiol curing agent for epoxy resin
  • Method for preparing high-quality polythiol curing agent for epoxy resin

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preparation example Construction

[0030] The invention provides a kind of preparation method of high-quality polythiol curing agent for epoxy resin, comprising the following steps:

[0031] a) NaSH, catalyst, halogenated polyether polyol and water in H 2 React in the presence of S, and then separate the catalyst to obtain a crude product; the catalyst is a three-phase transfer catalyst;

[0032] b) washing and drying the crude product obtained in step a) successively to obtain a high-quality polythiol curing agent for epoxy resin.

[0033] The present invention at first NaSH, catalyzer, halogenated polyether polyalcohol and water in H 2 The reaction is carried out in the presence of S, and the catalyst is separated to obtain a crude product. The present invention has no special limitation on the source of the NaSH, and commercially available products or self-made products (mainly prepared by injecting hydrogen sulfide into an alkaline solution) well known to those skilled in the art can be used. In the pres...

Embodiment 1

[0065] (1) Adding 198.3g mass fraction in the reactor is 32% NaSH aqueous solution and 8.8g three-phase phase transfer catalyst PS-PEG-DBC-1, then add 177.7g chlorinated polyether and 132g deionized water, react After the kettle is closed, check the airtightness, and then inject H into the kettle. 2 S gas keeps the inside of the kettle at normal pressure, heats the reaction system to 90°C through an oil bath, and then keeps it warm for 6 hours, then opens the vent valve of the reactor and uses N 2 After replacement and filtration of the catalyst, the product was left to stand and separated to obtain the crude product A.

[0066] (2) Add the crude product A into 180g deionized water to wash once, adjust the pH of the organic phase to 5-7 with hydrochloric acid, let it stand for stratification after stabilization, and take out the lower layer material to be the crude product B; Add 180g of deionized water, mix well and let it stand for 12 hours, then cut out the product and rem...

Embodiment 2

[0071] Adopt the preparation method that embodiment 1 provides to obtain high-quality polythiol curing agent for epoxy resin; Phase transfer catalyst PS-PEG-DBC-1.

[0072]The product obtained by the preparation method provided in Example 2 of the present invention is colorless and transparent, with a chromaticity (Hazen) of 18 when tested by a Hunter chromaticity meter, and a halogen content (residual chlorine) of 173 ppm when tested by a coulometric chlorine meter.

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Abstract

The invention provides a method for preparing a high-quality polythiol curing agent for an epoxy resin. The method comprises the following steps: a) enabling NaSH, a catalyst, halogenated polyether polyhydric alcohol and water to react in the presence of H2S, and further separating the catalyst so as to obtain a crude product, wherein the catalyst is a three-phase transfer catalyst; and b) performing water washing and drying on the crude product obtained in the step a) in sequence, so as to obtain the high-quality polythiol curing agent for the epoxy resin. Compared with the prior art, the method adopts a specific type of catalysts, the high-quality polythiol curing agent for the epoxy resin is synthesized by using a specific preparation process through solvent-free method three-phase transfer catalysis, the prepared product is colorless and transparent and low in halogen residue, and in addition, the catalyst is easy to recycle, low in separation cost, recyclable and very good in industrial application prospects. Testing results show that the chromaticity of the high-quality polythiol curing agent which is prepared by using the preparation method provided by the invention and is adopted for the epoxy resin is 16-21, and the halogen content is within 176ppm.

Description

technical field [0001] The invention relates to the technical field of polythiol compounds, in particular to a method for preparing a high-quality polythiol curing agent for epoxy resins. Background technique [0002] The preparation method of known thiol compound has many kinds, for example: (1) disulfide compound reduction method; (2) use organic halide or alcohols to react with thiourea earlier to generate isothiourea salt, then isothiourea The method of urea hydrolysis; (3) the method via Bunte salt; (4) the method of using organic halides to react with metal salts such as sodium hydrogensulfide and potassium hydrogensulfide; (5) the method of hydrolysis by dithiocarbamate (6) A method of adding alkenes to hydrogen sulfide or thioacetic acid, etc. Among them, method (2) and method (4) are the most commonly used preparation methods of mercaptan compounds by organic halides as starting materials. Compared with other methods, these two methods have high yield, few by-produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00C08G65/326C08G59/66
CPCC08G59/66C08G65/00C08G65/326Y02P20/584
Inventor 费潇瑶梁万根张超崔卫华王树建
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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