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Novel production process of thionocarbamate

A production process and thiourethane technology are applied in the new production process field of thiourethane, can solve the problems of incomplete reaction, environmental protection hazards, easy to use substandard, etc., and achieve less by-products, high safety, and sufficient reaction. Effect

Active Publication Date: 2022-04-26
QINGDAO LNT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: the process is more complex and discontinuous; the isomerization reaction of thiocyanate to isothiocyanate is not easy to carry out thoroughly, which limits the improvement of product yield; in the process of separating the aqueous phase from the organic phase The toxic intermediate isothiocyanate is easily entrained and discharged together with water, which deteriorates the operating environment and poses a hazard to environmental protection
[0004] In the existing production, the preparation of thiocarbamate is usually prepared in accordance with the standard YS / T 357-2015, that is, using xanthate, monochloroacetic acid, sodium carbonate and monoethylamine as raw materials to synthesize thiocarbamate , and there are various problems in this preparation process, a large amount of greenhouse gases will be produced, the reaction is incomplete, the organic phase and the aqueous phase are difficult to separate completely, and the thiourethane product obtained by the reaction is difficult to meet the use standard, etc., and the use of this process standard The appearance of the prepared thiourethane is yellow to reddish-brown. Due to its production process and its own nature, the color will become darker with time, resulting in subsequent use that is likely to fail to meet the standard

Method used

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  • Novel production process of thionocarbamate
  • Novel production process of thionocarbamate
  • Novel production process of thionocarbamate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of production technology of thiourethane, comprises the steps:

[0027] 1. Weigh 137g of water in a flask, dissolve 49.7g of chloroacetic acid solid in the water, start stirring, weigh 31.6g of soda ash, add soda ash to the flask, there will be a lot of CO when adding soda ash 2 Gas was generated; after adding soda ash, the reaction was stirred for 10 minutes to obtain a colorless transparent solution, pH=7.09.

[0028] 2. Add 97.1 g of xanthate several times in small amounts to the solution, the solution gradually becomes light yellow, and the temperature is 30-50°C.

[0029] 3. After stirring for 2 hours, add 35.3 g of monoethylamine to the solution at a temperature of 30-50°C, and stir for 3 hours after adding ethylamine.

[0030] 4. Let it stand for 12 hours to separate the liquid. Dark red tail liquid and light yellow turbid IPET are obtained, and a layer of gray-green mud-like intermediate layer will be formed between the tail liquid and thiourethane, whi...

Embodiment 2

[0033] A novel production process of thiourethane, comprising the steps of:

[0034] (1) Add 167ml of water to a 1L four-necked bottle, start stirring, and add 100g of 70% chloroacetic acid and 92.3g of 32% liquid caustic soda to the four-necked bottle at the same time at a controlled rate. After the reaction, a colorless and transparent solution is obtained, pH=7.23, continue Stir for 10 minutes;

[0035] (2) Add 138.5 g of xanthate to the solution of (1) several times in small amounts, control the reaction temperature to ≤45°C, and stir for 2.5 hours after adding the materials;

[0036] (3) Slowly add 52.3 g of ethylamine to the solution of (2), control the reaction temperature ≤ 45 ° C, stir for 3 hours after adding the material, and obtain an aqueous solution of thiourethane and sodium thioglycolate;

[0037] (4) The reacted material is settled in a separatory funnel, after 12 hours of natural settlement, the upper layer is taken to obtain a yellow turbid thiourethane sto...

Embodiment 3

[0040] A novel production process of thiourethane, comprising the steps of:

[0041] (1) Add 165ml of water to a 1L four-necked bottle, start stirring, and add 100g of 70% chloroacetic acid and 92.3g of 32% liquid caustic soda to the four-necked bottle at the same time under control, and obtain a colorless and transparent solution after the reaction, pH=7.25, continue Stir for 10 minutes;

[0042] (2) Add 138.5 g of xanthate several times in small amounts to the solution of (1), control the reaction temperature to ≤45° C., and stir for 2.5 hours after adding the materials; the solution after complete reaction is filtered through filter paper;

[0043](3) Slowly add 52.3 g of ethylamine to the solution of (2), control the reaction temperature ≤ 45 ° C, stir for 3 hours after adding the material, and obtain an aqueous solution of thiourethane and sodium thioglycolate;

[0044] (4) The reacted material is settled in a separatory funnel, after 8 hours of natural settlement, the u...

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Abstract

The invention provides a novel production process of thionocarbamate. The novel production process comprises the following steps: firstly, carrying out acid-base neutralization reaction on a monochloroacetic acid aqueous solution and liquid caustic soda in a reaction kettle; then xanthate is added into the reaction kettle for esterification reaction, and the reaction temperature is controlled to be 25-60 DEG C; conveying esterification liquid after complete reaction to a next reaction kettle, adding organic amine for reaction to obtain thionocarbamate and sodium thioglycolate aqueous solution, and adopting a horizontal flow and longitudinal flow combined stirring mode to guarantee complete reaction; the reacted material is settled in a settling tank, and after natural settling, the upper layer is taken to obtain a thionocarbamate stock solution; and refining the thionocarbamate stock solution. Compared with the traditional preparation method, the preparation process of the thionocarbamate provided by the invention has the advantages that sodium carbonate is changed into liquid caustic soda, the reaction process is changed from solid-liquid to acid-base dropwise adding reaction, the severe reaction is replaced by the gentle reaction, the reaction is more sufficient, a large amount of greenhouse gas is not generated, and the safety is higher.

Description

technical field [0001] The invention belongs to the technical field of environmental protection chemical industry, and in particular relates to a novel production process of thiourethane. Background technique [0002] Thiurethane refers to a class of compounds with the general formula ROCSNHR, which can be regarded as a derivative of xanthate (xanthate) (the sulfhydryl group in xanthate ROCSSH is replaced by alkylamine-RNH), usually oily Liquid, with special smell, less soluble in water. Excellent collector for copper sulfide, lead, zinc, molybdenum, nickel and other minerals. Thiurethane is the best collector for copper sulfide. It is highly efficient, non-toxic, and has good selectivity, and is widely used by countries all over the world. It also has a certain foaming performance, suitable for acidic or alkaline pulp. More importantly, thiourethane is an excellent collector of copper sulfide on the one hand, and sodium thioglycolate recovered from the tail liquid is the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/04
CPCC07C333/04
Inventor 李芳李洵匡凤文
Owner QINGDAO LNT CHEM
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