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Polymercaptan curing agent, and preparation method and application thereof

A technology of curing agent and polythiol, which is applied in the field of polythiol curing agent and its preparation, can solve the problems of high chloride ion content, high requirement fields, unusable transparency and other problems, and achieve low halogen content and good Conversion rate, the effect of mild conditions

Active Publication Date: 2019-11-15
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the polythiol curing agent obtained by the preparation method disclosed in the prior art is mostly yellow-green or light yellow, with poor transparency, and the polymerizable composition obtained after mixing with epoxy resin will have coloring phenomenon, which cannot be obtained. It is used in fields requiring high transparency, and the resulting product has a high content of chloride ions, which limits its application fields

Method used

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  • Polymercaptan curing agent, and preparation method and application thereof
  • Polymercaptan curing agent, and preparation method and application thereof
  • Polymercaptan curing agent, and preparation method and application thereof

Examples

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preparation example Construction

[0031] The invention provides a kind of preparation method of polymercaptan curing agent, comprises the following steps:

[0032] a) NaSH, phase transfer catalyst, organic polyhalogenated polyether and water in H 2 React in the presence of S to obtain a crude product; the iron content of the NaSH is 0.005wt% to 1wt%;

[0033] b) washing and drying the crude product obtained in step a) successively to obtain a polythiol curing agent.

[0034] The present invention at first NaSH, phase transfer catalyst, organic polyhalogenated polyether and water in H 2 The reaction was carried out in the presence of S to obtain the crude product. In the present invention, the iron content of the NaSH is 0.005wt%-1wt%, preferably 0.06wt%-0.9wt%. The present invention does not have special restriction to the source of described NaSH, can adopt commercially available commodity or self-produced (mainly prepare by introducing hydrogen sulfide into alkali solution) well-known to those skilled in ...

Embodiment 1

[0073] (1) Adding 198.3g mass fraction is 32% NaSH (iron content is 0.08wt%) aqueous solution and 13.3g phase transfer catalyst tetrabutylammonium bisulfate in reactor, then adds 177.7g chlorinated polyether and 132g to Ionized water, check the airtightness after closing the reactor, and then inject H into the reactor 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, the product was left to stand and separated to obtain the crude product A.

[0074] (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 remove water ...

Embodiment 2

[0077] The preparation method provided in Example 1 was used to obtain a polythiol curing agent; the difference was that the iron content of NaSH was 0.06 wt%.

[0078]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 (Cl) content of 326 ppm when tested by a coulometric chlorine meter.

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Abstract

The invention provides a preparation method of a polymercaptan curing agent. The preparation method comprises the following steps: a) carrying out reacting on NaSH, a phase transfer catalyst, organicpolyhalogenated polyether and water in the presence of H2S to obtain a crude product, wherein the iron content of NaSH ranges from 0.005 wt% to 1 wt%; and b) sequentially washing the crude product obtained in the step a) by water, and carrying out drying to obtain the polymercaptan curing agent. Compared with the prior art, the preparation method has the advantages that the iron content of the rawmaterial NaSH is strictly controlled, the high-quality polymercaptan curing agent is obtained through a specific preparation process, and the product is colorless and transparent, is low in halogen content and meets the requirements of a novel green environment-friendly curing agent. When the polymercaptan curing agent is applied to preparation of optical materials such as lenses with good optical physical properties, the coloring problem cannot be caused. Experimental results show that the chromaticity of the polymercaptan curing agent obtained by the preparation method provided by the invention is 16-27, and the halogen content is within 700ppm.

Description

technical field [0001] The present invention relates to the technical field of polythiol compounds, more specifically, to a polythiol curing agent and its preparation method and application. 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-pr...

Claims

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Application Information

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IPC IPC(8): C08G65/326C08G59/66C08L63/00
CPCC08G59/66C08G65/326C08L63/00C08L2201/10
Inventor 费潇瑶梁万根崔卫华王树建张超
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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