A kind of preparation method of 1,2,3-trimercaptopropane

A technology of trimercaptopropane and trichloropropane, which is applied in the field of chemical technology, can solve problems such as no relevant reports on synthesis technology, and achieve the effects of high added value of products, simple process, and easy availability of raw materials

Active Publication Date: 2020-09-25
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant report on the synthesis technology of 1,2,3-trimercaptopropane

Method used

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  • A kind of preparation method of 1,2,3-trimercaptopropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Into a 1000mL four-necked flask equipped with a glass stirring and thermometer was sequentially added 147.5g of trichloropropane, 700g of 32% sodium hydrosulfide and 1.47g of tetrabutylammonium chloride;

[0032] (2) Turn on the stirring, heat it to 90°C in an oil bath for 4 hours of heat preservation reaction;

[0033] (3) After the reaction is completed, transfer the product to a separatory funnel, let stand for 15 minutes, and cut the lower organic phase into a 500mL four-neck flask;

[0034] (4) Add 221g of deionized water to the organic phase, start stirring, add 50% sulfuric acid aqueous solution to adjust the pH of the system to 4, heat up to 50-60℃, stir for 15 minutes, and then transfer to the separatory funnel. , Let stand for 15min and cut the lower organic phase into a four-neck flask;

[0035] (5) Add 221g of deionized water to the four-necked flask, raise the temperature to 50-60℃ and stir for 15min for the first water washing. After completion, transfer to th...

Embodiment 2

[0040] (1) Into a 1000 mL four-necked flask equipped with a glass stirring and thermometer was sequentially added 147.5 g of trichloropropane, 876 g of 32% sodium hydrosulfide and 0.74 g of benzyl triethylammonium chloride;

[0041] (2) Turn on the stirring and heat it to 60°C in an oil bath for 5 hours of insulation reaction;

[0042] (3) After the reaction is completed, transfer the product to a separatory funnel, let stand for 15 minutes, and cut the lower organic phase into a 500mL four-neck flask;

[0043] (4) Add 221g of deionized water to the organic phase, start stirring, add 50% sulfuric acid aqueous solution to adjust the pH of the system to 5, heat up to 50-60℃, stir for 15 minutes, and then transfer to the separatory funnel. , Let stand for 15min and cut the lower organic phase into a four-neck flask;

[0044] (5) Add 221g of deionized water to the four-necked flask, raise the temperature to 50-60℃ and stir for 15min for the first water washing. After completion, transfer ...

Embodiment 3

[0049] (1) Into a 1000mL four-necked flask equipped with glass stirring and thermometer was sequentially added 147.5g of trichloropropane, 525.6g of 32% sodium hydrosulfide and 2.21g of tetrabutylammonium bromide;

[0050] (2) Turn on the stirring, heat it to 100°C in an oil bath, and conduct a heat preservation reaction for 3 hours;

[0051] (3) After the reaction is completed, transfer the product to a separatory funnel, let stand for 15 minutes, and cut the lower organic phase into a 500mL four-neck flask;

[0052] (4) Add 221g of deionized water to the organic phase, start stirring, add 50% sulfuric acid aqueous solution to adjust the pH of the system to 3, heat up to 50-60°C, stir for 15 minutes, and then transfer to a separatory funnel. , Let stand for 15min and cut the lower organic phase into a four-neck flask;

[0053] (5) Add 221g of deionized water to the four-necked flask, raise the temperature to 50-60℃ and stir for 15min for the first water washing. After completion, tra...

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Abstract

The invention discloses a preparation method of 1,2,3-trimercaptopropane. Trichloropropane and sodium hydrosulfide are used as raw materials to obtain 1,2,3-trimercaptopropane under the action of a catalyst. The product obtained by adopting the technical scheme of the invention has high mercapto group content and high refractive index, and can be used to prepare high refractive index lenses; and the preparation method has simple process, readily available raw materials, and high added value of the product.

Description

[0001] Invention field [0002] The invention belongs to the field of chemical technology, and specifically relates to a preparation method of 1,2,3-trimercaptopropane. Background technique [0003] Polyurethane material has excellent wear resistance, impact resistance and light transmission properties, so it has occupied a very important position in the field of optical plastics in recent years. Polyurethane is formed by the addition reaction of an active hydrogen-containing compound with a bifunctionality or higher and an isocyanate with a bifunctionality or higher. There are thermoplastic and thermosetting types. In order to destroy the crystalline properties of polyurethane and make the material have better light transmittance, cross-linking is a necessary measure, so the thermosetting type is mainly used. [0004] Isocyanate-containing compounds can be divided into two categories, namely, ordinary isocyanates containing NCO and isothiocyanates containing NCS. NCO compounds are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/02C07C319/28C07C321/04
CPCC07C319/02C07C319/28C07C321/04
Inventor 张超梁万根孙志利崔卫华费潇瑶许倩倩周芳晶靖培培
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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