Preparation method of polythiol compound for optical resin

A technology of polythiol compounds and polyol compounds, which is applied in the field of optical resins, can solve the problems of high chroma of polythiol compounds, which cannot meet the raw material requirements of optical resin lenses, etc.

Inactive Publication Date: 2017-11-03
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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Problems solved by technology

[0004] However, the chromaticity of the polythiol compound obtained by the preparation process of the prior art is relatively high, which cannot meet the raw material requirements for the preparation of optical resin lenses with excellent performance.

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  • Preparation method of polythiol compound for optical resin

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[0023] The invention provides a kind of preparation method of polythiol compound for optical resin, comprising the following steps:

[0024] a) carrying out a polyalcoholation reaction with mercaptoethanol and epichlorohydrin in an alkaline solution to obtain a reaction mixture with a polyol compound;

[0025] b) performing a thiolation reaction with the reaction mixture having a polyol compound obtained in step a) and thiourea in an acidic solution to obtain a reaction mixture having a polythiol compound;

[0026] c) performing a hydrolysis reaction on the reaction mixture having polythiol compounds obtained in step b), followed by washing with water and drying to obtain polythiol compounds for optical resins;

[0027] The iron content of the mercaptoethanol is greater than 0 and less than 10ppm; the iron content of the epichlorohydrin is greater than 0 and less than 10ppm.

[0028] In the present invention, the polyalcoholization reaction of mercaptoethanol and epichlorohyd...

Embodiment 1

[0045] (1) the 2-mercaptoethanol (2mol) that 156g iron content is 3ppm and the epichlorohydrin (0.8mol) that 74g iron content are 4ppm are added to 200g mass concentration successively and be 20% sodium hydroxide (1mol) In the solution, react at 10° C. for 1 h to obtain a reaction mixture with polyol compound;

[0046] (2) adding 228g thiourea (3mol) and 536.8g mass concentration to the reaction mixture with polyol compound obtained in step (1) is 34% hydrochloric acid (HCl is 5mol), and carries out thiolation reaction at 100°C for 3h , to obtain a reaction mixture with a polythiol compound;

[0047] (3) After cooling down to room temperature, 450 g of a mass concentration of 40% sodium hydroxide (4.5 mol) solution was added to the reaction mixture with polythiol compound obtained in step (2), and the hydrolysis reaction was carried out at 50° C. for 3 h, Obtain a reaction mixture with a crude product; finally, wash the reaction mixture with a crude product twice with water, ...

Embodiment 2

[0051] (1) the 2-mercaptoethanol (2mol) that 156g iron content is 5ppm and the epichlorohydrin (0.8mol) that 74g iron content are 2ppm are added to 200g mass concentration successively and be 20% sodium hydroxide (1mol) In the solution, react at 10° C. for 1 h to obtain a reaction mixture with polyol compound;

[0052] (2) adding 228g thiourea (3mol) and 536.8g mass concentration to the reaction mixture with polyol compound obtained in step (1) is 34% hydrochloric acid (HCl is 5mol), and carries out thiolation reaction at 100°C for 3h , to obtain a reaction mixture with a polythiol compound;

[0053] (3) After cooling down to room temperature, 450 g of a mass concentration of 40% sodium hydroxide (4.5 mol) solution was added to the reaction mixture with polythiol compound obtained in step (2), and the hydrolysis reaction was carried out at 50° C. for 3 h, A reaction mixture with a crude product was obtained; finally, the reaction mixture with the crude product was washed with...

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Abstract

The invention provides a preparation method of a polythiol compound for optical resin. The preparation method comprises the following steps: a), carrying out polyalcoholation reaction on mercaptoethanol and epoxy chloropropane in an alkaline solution to obtain a reaction mixture containing a polyalcohol compound; b), carrying out thiolation reaction on the reaction mixture containing the polyalcohol compound obtained in the step a) and thiourea in an acid solution to obtain a reaction mixture containing a polythiol compound; and c), carrying out hydrolysis reaction on the reaction mixture containing the polythiol compound obtained in the step b), and then washing and drying to obtain the polythiol compound for the optical resin, wherein the iron content of the mercaptoethanol is greater than 0 and less than 10 ppm and the iron content of the epoxy chloropropane is greater than 0 less than 10 ppm. According to the preparation method disclosed by the invention, by strictly controlling the iron content of raw materials, the polythiol compound with relatively low chroma is obtained by a specific preparation technology, and thereby the requirements on the raw materials for preparing an optical resin lens with excellent performance can be satisfied.

Description

technical field [0001] The invention relates to the technical field of optical resins, in particular to a preparation method of a polythiol compound for optical resins. Background technique [0002] Optical resin is a kind of organic material. The interior is a three-dimensional network structure connected by polymer chain structures. The intermolecular structure is relatively loose, and there is space for relative displacement between molecular chains. The light transmittance is 84%- 90%, good light transmittance, and the impact resistance of optical resin is strong. Optical resin has a wide range of applications, especially as an optical resin lens. Compared with traditional glass lenses, it has obvious advantages such as light weight, good impact resistance, and easy processing and molding. Therefore, the research on optical resin has broad applications. prospect. [0003] At present, the optical resins of optical resin lenses on the market are mainly polythiourethane r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/14C07C319/20C07C319/28C07C323/12C07C321/14C08G18/38
CPCC07C319/14C07C319/20C07C319/28C08G18/3876C07C323/12C07C321/14
Inventor 曹斌张超梁万根张宁任永平魏政王越先
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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