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Polymercaptan compound as well as preparation method and application thereof

A compound and polythiol technology, applied in the field of preparation of polythiol compounds, can solve problems such as white turbidity and loss, and achieve the effects of solving white turbidity, being easy to control, and ensuring product quality

Inactive Publication Date: 2021-03-02
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 quality of raw materials and reaction impurities in the reaction have a great influence on the product index, which will further cause the composition containing these polythiol compounds to sometimes become cloudy when they are polymerized and solidified, resulting in huge losses.

Method used

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Examples

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preparation example Construction

[0034] The invention provides a kind of preparation method of polythiol compound, comprises the following steps:

[0035] A) reacting the epichlorohydrin solution, mercaptoethanol and the first basic compound solution to obtain a polyol mixed solution;

[0036] B) performing a salt-forming reaction on the polyol mixed solution, thiourea and the first acid solution to obtain an isothiouronium salt;

[0037] C) mixing the isothiouronium salt with the second basic compound solution, and performing a hydrolysis reaction to obtain a crude polythiol;

[0038] D) washing the crude polythiol with a second acid solution;

[0039] E) mixing the washed product with an organic solvent for extraction;

[0040] F) liquid separation and removal of solvent to obtain polythiol compound.

[0041] In the invention, the epichlorohydrin solution, the mercaptoethanol and the first basic compound solution are reacted to obtain the polyol mixed solution.

[0042] In some embodiments of the presen...

Embodiment 1

[0085] (1) preparation of polythiol, concrete steps are as follows:

[0086] (1) Synthesis of polyols:

[0087] 76.98g (0.98mol) mercaptoethanol is poured in the four-necked flask, dripping 62.5g concentration is the triethylamine solution (the amount of the substance of triethylamine is 0.19mol) of 30wt%, then according to epichlorohydrin addition is 46.30 g (0.5 mol) was added, epichlorohydrin solution (concentration: 99.85 wt%) was added and reacted at 45° C. for 20 min to obtain a polyol mixture.

[0088] (2) Salt-forming reaction:

[0089] Drop into 122g (1.59mol) thiourea and 198g concentration in the polyalcohol mixed solution in step (2) and be the hydrobromic acid (the amount of hydrogen bromide is 0.89mol) of 36wt%, reflux reaction 3h at 110 ℃, generate Isothiouronium salt.

[0090] (3) Hydrolysis reaction and post-treatment:

[0091] After cooling the isothiouronium salt in step (3) to 35°C, add 238g of sodium hydroxide solution (the amount of sodium hydroxide i...

Embodiment 2

[0098] (1) preparation of polythiol, concrete steps are as follows:

[0099] (1) Synthesis of polyols:

[0100] 77.37g (0.99mol) mercaptoethanol is poured in the four-necked flask, dripping 68.75g concentration is the potassium hydroxide solution (the amount of substance of potassium hydroxide is 0.37mol) of 30wt%, then according to the addition of epichlorohydrin 46.29 g (0.5 mol) was added into epichlorohydrin solution (concentration: 99.8 wt%) and reacted at 40° C. for 20 min to obtain a polyol mixture.

[0101] (2) Salt-forming reaction:

[0102] Add 122.5 g (1.6 mol) of thiourea and 197 g of hydrobromic acid (the amount of hydrogen bromide is 0.89 mol) with a concentration of 36 wt % to the polyol mixed solution in step (2), and react at reflux for 2.5 h at 110° C. , generating isothiouronium salt.

[0103] (3) Hydrolysis reaction and post-treatment:

[0104] After cooling the isothiouronium salt in step (3) to 20°C, add 330g of sodium hydroxide solution (the amount o...

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Abstract

The invention relates to the technical field of optical resin, in particular to a polymercaptan compound as well as a preparation method and application thereof. The preparation method of the polymercaptan compound comprises the following steps: A) reacting an epichlorohydrin solution, mercaptoethanol and a first alkaline compound solution to obtain a polyol mixed solution; B) carrying out salt forming reaction on the polyol mixed solution, thiourea and a first acid solution to obtain an isothiourea salt; E) mixing the isothiourea salt with a second alkaline compound solution, and carrying outhydrolysis reaction to obtain a polymercaptan crude product; D) washing the polymercaptan crude product with a second acid solution; E) mixing the washed product with an organic solvent, and conducting extracting; and F) separating the liquid, and removing the solvent to obtain the polymercaptan compound. According to the preparation method provided by the invention, the high-quality polymercaptan compound can be obtained, and polythiourethane resin with excellent hue is further obtained, so that the white turbidity phenomenon after the resin is cured is solved.

Description

technical field [0001] The invention relates to the technical field of optical resins, in particular to a polythiol compound, its preparation method and application. Background technique [0002] Plastic materials are lightweight, tough, and easy to dye. In recent years, they have been commonly used in the preparation of various optical materials. Corresponding to the field of spectacle lenses, low specific gravity, high transparency, low yellowness, high heat resistance, high strength, high refractive index and Abbe number are required. As a polythiourethane optical resin material with the above excellent properties is an important development direction in recent years, this type of resin material is mainly prepared from polythiol compounds and isocyanates as raw materials. [0003] When used in plastic lenses, polythiourethane-based resins must have excellent color tone and good transparency. However, the quality of raw materials and reaction impurities in the reaction h...

Claims

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Application Information

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IPC IPC(8): C08G75/04C08G18/64
CPCC08G18/6453C08G75/04
Inventor 许倩倩梁万根张超崔卫华孙志利费潇瑶卞文
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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