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Method for producing low chroma polythiol compound

A polythiol and compound technology, which is applied in the preparation of thioether, organic chemistry, etc., can solve the problems of chromaticity oligomeric thiol compounds, yellowing of optical resin lenses, poor chromaticity of thiol compounds, etc., and achieve low dosage , reducing the effect of chroma, large social and economic value

Active Publication Date: 2019-10-08
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Korean Patent No. 1993-0006918 discloses a preparation method of a thiourethane lens. Although this lens has excellent properties in terms of Abbe number and light transmittance, the synthetic optical resin lens suffers from poor chromaticity. Yellow, the product is unqualified
Korean Patent No. 10-2008-0090529 Analysis of impurities in raw materials will lead to poor color of thiol compounds
Patent CN104066716A found that the two kinds of impurities in the raw materials must be controlled at the same time to obtain polythiol compounds with low chroma. The control conditions are strict and difficult to operate
Patent CN107311898A mainly obtains polythiol compounds with lower chroma by strictly controlling the iron content in the reaction raw materials, so as to meet the raw material requirements for the preparation of excellent optical resin lenses. Strict control of iron content is required, and the operation is complicated and the process is cumbersome. high cost
Patent CN107311899A discloses a method for treating polythiol compounds with high chroma by reduction method, the steps are complicated, the cost is high, the cycle is long, and the energy consumption is high
There is still no method for obtaining low-color polythiol compounds by controlling the synthesis reaction steps

Method used

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  • Method for producing low chroma polythiol compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (a) Pour 190g of polyol A into a four-necked flask, add 115g (3mol) of thiourea and 152g of hydrochloric acid (3mol) with a mass fraction of 36%, and react at reflux at 100°C for 3.5h to form isothiuronium salt;

[0025] (b) After cooling down to room temperature, add sodium carbonate solution to adjust the pH of the system to 12, add 0.52 g of lauric acid at the same time, heat to 30 ° C, and carry out hydrolysis reaction for 2 hours to obtain a crude polythiol mixture;

[0026] (c) Mix and separate the crude product obtained in step (b), wash with water twice, dry and filter with 5% silica gel to obtain polythiol compound with low chroma.

[0027] The chromaticity of the polythiol product obtained in Example 1 of the present invention was detected by a high-precision multifunctional spectrophotometer, and the results showed that the chromaticity of the polythiol compound obtained in Example 1 of the present invention was 10 Hazen.

Embodiment 2

[0029] (a) Pour 200g of polyol B into a four-necked flask, add 123g of thiourea (3.2mol) and 177g of hydrochloric acid (3.5mol) with a mass fraction of 36%, and react at reflux at 110°C for 2h to form isothiourea salt;

[0030] (b) After cooling down to room temperature, add ammonia solution to adjust the pH of the system to 13, add 4g of sodium lauryl sulfate at the same time, heat to 45°C, and perform a hydrolysis reaction for 2.5 hours to obtain a crude polythiol mixture;

[0031] (c) mixing and separating the crude product obtained in step (b), washing with water twice, drying and filtering with 6% phosphorus pentoxide to obtain a polythiol compound with low chroma.

[0032] The chromaticity of the polythiol product obtained in Example 2 of the present invention was detected by a high-precision multifunctional spectrophotometer, and the results showed that the chromaticity of the polythiol compound obtained in Example 2 of the present invention was 9 Hazen.

Embodiment 3

[0034] (a) Pour 180g of polyol A into a four-necked flask, add 126g of thiourea (3.3mol) and 203g of hydrochloric acid (4mol) with a mass fraction of 36%, and react at reflux at 112°C for 2.5h to form isothiuronium salt;

[0035] (b) After cooling down to room temperature, add sodium hydroxide solution to adjust the pH of the system to 10, add 2 g of sodium dodecylbenzenesulfonate at the same time, heat to 70 ° C, and perform hydrolysis for 3.5 hours to obtain a crude polythiol mixture;

[0036] (c) mixing and separating the crude product obtained in step (b), washing with water twice, drying and filtering with 10% calcium oxide to obtain a polythiol compound with low chroma.

[0037] The chromaticity of the polythiol product obtained in Example 3 of the present invention was detected by a high-precision multifunctional spectrophotometer, and the results showed that the chromaticity of the polythiol compound obtained in Example 3 of the present invention was 8 Hazen.

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Abstract

The invention belongs to the technical field of optical resins, and particularly relates to a method for producing a low chroma polythiol compound. The specific preparation steps are as follows: a surfactant is added to an isothiourea salt in an alkaline solution to carry out a hydrolysis reaction to obtain a polythiol crude product mixture, and separating, washing with water, and drying are performed to obtain the low chroma polythiol compound. The production method has the advantages of simple operation, easy availability of raw materials, small use amount, low energy consumption, and no equipment investment, the obtained product can meet needs of industries such as fine chemical industry, the quality of downstream products is improved, and the product can be easily used to prepare optical resin lenses with excellent performance.

Description

technical field [0001] The invention belongs to the technical field of optical resins, in particular to a method for producing low chroma polythiol compounds. Background technique [0002] Compared with inorganic glass, optical resin has obvious advantages in the application of glasses. Polyurethane optical resin is an important development direction of new optical resin in recent years. It has the characteristics of high refractive index, high Abbe number, low specific gravity, high impact resistance, etc., and is especially suitable for the production of medium and high refractive ophthalmic lenses. The raw materials of this kind of resin are mainly prepared from polythiol compounds and isocyanates. Yellowness index is an important indicator of optical resin materials, and the key to determine the yellowness index of optical resins is the chromaticity of polythiol compounds. [0003] Korean Patent No. 1993-0006918 discloses a preparation method of a thiourethane lens. A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/20C07C321/14
CPCC07C319/20C07C321/14
Inventor 许倩倩郭龙龙张建林韩立霞马韵升
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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