Post-treatment method of multi-sulfhydryl compound crude product

A technology for polythiol compounds and polythiol compounds is applied in the field of post-processing of crude polythiol compounds, which can solve the problems of high chromaticity of products, unfavorable optical resins and the like, and achieve high light transmittance, low chromaticity, and yellowness index. low effect

Active Publication Date: 2017-10-10
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the chromaticity of the product obtained by this technology is still high, which is not conducive to the application of optical resins

Method used

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  • Post-treatment method of multi-sulfhydryl compound crude product
  • Post-treatment method of multi-sulfhydryl compound crude product
  • Post-treatment method of multi-sulfhydryl compound crude product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Mercaptoethanol (3.0 molar equivalents) and epichlorohydrin (1.2 molar equivalents) were added to 25% sodium hydroxide (1.6 molar equivalents) aqueous solution, and the temperature was controlled to -10°C and the addition time was 2 hours to obtain the triol . Then, thiourea (4.8 molar equivalent) and 35% hydrochloric acid (7.8 molar equivalent) were added and mixed, and heated to 100° C. for reaction for 3 hours to obtain an intermediate product. The intermediate product was added to 40% sodium hydroxide aqueous solution (6.6 molar equivalents) and hydrolyzed at 70°C for 2 hours to obtain a crude product, washed with water, leaving only the oil phase, adding 1% of the crude mass of sodium hydroxide, and vacuuming at 70°C Dehydrated. The dehydrated mixture was mixed with diatomaceous earth with a crude quality of 2%, stirred evenly, and filtered to obtain a colorless and transparent product. The color of the product was 8 Hazen.

[0053] Preparation of optical resin:

[0...

Embodiment 2

[0056] Mercaptoethanol (1.6 molar equivalent) and epichlorohydrin (0.8 molar equivalent) were added to a 38% aqueous solution of sodium hydroxide (1.0 molar equivalent) successively, and the temperature was controlled to 0° C. and the addition time was 2 hours to obtain the triol. Then thiourea (3.6 molar equivalent) and 25% hydrochloric acid (4.0 molar equivalent) were added and mixed, and heated to 115° C. for reaction for 5 hours to obtain an intermediate product. The intermediate product was added to a 30% sodium hydroxide aqueous solution (5.2 molar equivalent) to hydrolyze at 50°C for 3 hours to obtain a crude product, washed with water, leaving only the oil phase, added with 5% crude sodium sulfite, and dehydrated at 60°C under vacuum . The dehydrated mixture was mixed with activated carbon with a crude quality of 5%, stirred evenly, and filtered to obtain a colorless and transparent product. The color of the product was detected to be 12 Hazen.

[0057] Using this polyme...

Embodiment 3

[0059] Mercaptoethanol (3.5 molar equivalent) and epichlorohydrin (1.5 molar equivalent) were added to a 30% potassium hydroxide (1.7 molar equivalent) aqueous solution, and the temperature was controlled to 5° C. and the addition time was 3 hours to obtain the triol. Then, thiourea (6.6 molar equivalents) and 40% sulfuric acid (11 molar equivalents) were added and mixed, and heated to 150° C. to react for 4 hours to obtain an intermediate product. The intermediate product was added to a 40% potassium hydroxide aqueous solution (9.5 molar equivalent) to hydrolyze at 70°C for 2 hours to obtain a crude product, washed with water, leaving only the oil phase, adding 2% crude sodium bisulfite at 85°C Perform vacuum dehydration. The dehydrated mixture was mixed with attapulgite with a crude quality of 2%, stirred evenly, and filtered to obtain a colorless and transparent product, and the color of the product was 10 Hazen.

[0060] Using this polymercapto compound, an optical resin was...

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Abstract

The invention provides a post-treatment method of a multi-sulfhydryl compound crude product. The method comprises the following steps: A) the multi-sulfhydryl compound crude product with the structure shown in formula (I) is washed with water and then mixed with a reducing agent for vacuum dehydration, wherein the reducing agent is selected from one or more of sodium sulfite, sodium bisulfite, sodium hydrosulfite and sodium thiosulfate; B) the product obtained in step A) is mixed with an adsorbent and filtered, and a purified polythiol compound is obtained; the adsorbent is selected from one or more attapulgite, bentonite, diatomaceous earth and activated carbon.

Description

Technical field [0001] The invention belongs to the technical field of optical resins, and specifically relates to a post-treatment method for a crude product of a polysulfhydryl compound. Background technique [0002] Compared with inorganic glass, optical resin has obvious advantages in the application of glasses: light weight, good impact resistance and easy processing and molding. Currently, the optical resin materials on the market are mainly polythiourethane resins prepared from polythiol compounds and isocyanates. The refractive index of this type of resin is significantly higher than other types of resins on the market. The higher the refractive index of the resin, the lighter and thinner the prepared lens. Therefore, this type of resin is the key development direction of optical resins in recent years. [0003] The yellow index is an important indicator of optical resins, and the key factor that determines the yellow index is the chromaticity of the polythiol compound. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/28C07C321/14C08G18/38
CPCC07C319/28C08G18/3876C07C321/14
Inventor 曹斌张宁张超梁万根江德阳魏政王越先
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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