Method for resource full utilization of sodium chloride waste residue salt by esterification process

A sodium chloride and recycling technology, applied in the fields of alkali metal chlorides, organic chemistry, carboxylic acid halide preparation, etc., can solve the problems of inability to recover organic matter, qualitative and quantitative analysis, high water content of salt, etc. The effect of sustained and coordinated development

Inactive Publication Date: 2020-08-21
佛山经纬纳科环境科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods require pre-drying of waste salt slag and require the particles of waste salt slag to be uniform and as small as possible, and it is very easy to cause blockage and damage to the device
(2) Secondary concentration and crystallization treatment after dissolution and refining: This method is to redissolve the waste salt slag in fresh water, and recycle it after concentration and crystallization after chemical treatment. For example, CN 105883911 B molten salt chlorination slag recycling method, CN103979576 A method for evaporating and crystallizing salt slag from organic waste water containing ammonium sulfate; but these methods have high disposal costs, and secondary waste water is produced, and the effect of physical and chemical treatment after dissolution is difficult to guarantee. The water content of recrystallized salt is high, and some There is a large amount of crystal water, and the secondary use value is low
However, this method uses low-temperature roasting first to convert part of the organic impurities into carbon materials for recovery, but this will inevitably result in higher energy consumption; then, the remaining organic matter in the waste salt is further recovered by using an interface regulator. However, the qualitative and quantitative analysis of the organic matter in it is not carried out, and the organic matter that occupies the dominant position in it cannot be recovered in a targeted manner, resulting in a low recovery efficiency of the final organic matter

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Under normal temperature and pressure, slowly add 20 ml of acetyl chloride and 0.5 g of sodium hydroxide to 5 g of alcohol-containing sodium chloride waste salt residue, stir and mix for 30 minutes and then filter.

[0029] (2) Add 5ml of n-hexane into the solution obtained in step (1), stir and mix evenly, leave to stand for stratification, then separate the upper and lower liquids, and reclaim the upper liquid to obtain the esterification product;

[0030] (3) Get the lower floor solution obtained by step (2) separation, add 3ml of sodium carbonate solution (concentration is 10g / L) while stirring, then leave it for 6 minutes, it can be observed that fine precipitation occurs in the solution, filter; solid The precipitate is dried and recovered by nano-calcium carbonate.

[0031] (4) add 1.5ml hydrochloric acid solution (concentration is 1mol / L) to step (3) filtered gained solution, remove remaining sodium carbonate, leave standstill for 3 minutes and then be heate...

Embodiment 2

[0034] (1) Under normal temperature and pressure, slowly add 200 ml of benzoyl chloride and 5 g of sodium hydroxide to 52 g of alcohol-containing sodium chloride waste salt residue, stir and mix for 30 minutes and then filter.

[0035] (2) Add 50ml of n-hexane into the solution obtained in step (1), stir and mix evenly, let stand to separate layers, then separate the upper and lower liquids, and recover the upper liquid to obtain the esterification product.

[0036] (3) Get the lower floor solution obtained by step (2) separation, add 30ml of sodium carbonate solution (concentration is 10g / L) while stirring, then leave it for 6 minutes, it can be observed that fine precipitation occurs in the solution, filter; solid The precipitate is dried and recovered by nano-calcium carbonate.

[0037] (4) add 15ml hydrochloric acid solution (concentration is 1mol / L) in step (3) filtered gained solution, remove remaining sodium carbonate, leave standstill for 3 minutes and be heated to 60~90...

Embodiment 3

[0040] (1) Under normal temperature and pressure, slowly add 1000ml of oxalyl chloride and 25g of sodium hydroxide to 250g of alcohol-containing sodium chloride waste salt residue, stir and mix for 30min before filtering.

[0041] (2) Add 250ml of n-hexane into the solution obtained in step (1), stir and mix evenly, let stand to separate layers, then separate the upper and lower liquids, and recover the upper liquid to obtain the esterification product.

[0042] (3) Get the lower floor solution obtained by step (2) separation, add 150ml of sodium carbonate solution (concentration is 10g / L) while stirring, then let stand for 6 minutes, it can be observed that fine precipitation occurs in the solution, filter; solid The precipitate is dried and recovered by nano-calcium carbonate.

[0043] (4) add 75ml hydrochloric acid solution (concentration is 1mol / L) in step (3) filtered gained solution, remove remaining sodium carbonate, leave standstill for 3 minutes and be heated to 60~90...

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PUM

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Abstract

The invention belongs to the technical field of industrial waste salt slag treatment, and discloses a method for resource full utilization of sodium chloride waste slag salt by an esterification process. The method comprises the following steps: adding acyl chloride and an alkali catalyst into alcohol-containing sodium chloride waste salt slag, stirring and mixing, reacting, and filtering; addingn-hexane into the obtained solution, uniformly stirring and mixing, standing for layering, and recycling the obtained supernatant to obtain an esterification product; and adding a sodium carbonate solution into the obtained lower-layer solution, standing, filtering, drying and recycling obtained filter residues, adding hydrochloric acid into the filtrate, standing, heating for concentrating, separating separated crystals, and drying to obtain purified sodium chloride. According to the method disclosed by the invention, alcohol organic matters in the salt slag are efficiently and thoroughly esterified through normal-temperature treatment, so that the purpose of purifying sodium chloride is achieved, meanwhile, ester substances capable of being recycled are recycled, a technical support is provided for realizing energy conservation and emission reduction in the chemical industry, and sustainable coordinated development of the chemical industry is promoted.

Description

technical field [0001] The invention belongs to the technical field of industrial waste salt slag treatment, and in particular relates to a method for fully utilizing sodium chloride waste slag salt in the esterification method. Background technique [0002] In the production process of many fine chemicals and chemical pesticide products or intermediates, a large amount of by-product waste salt containing toxic and harmful chemicals is produced. For example, every ton of hydrazine hydrate produces 4 to 5 tons of by-products containing Alcohol sodium chloride waste salt slag produces 1.1 to 1.4 tons of by-product sodium chloride salt slag containing toxic and harmful chemicals for every ton of glyphosate pesticide produced, and the production of trimethyl orthoformate produces toxic and harmful chemical substances The by-product of alcohol-containing sodium chloride waste salt slag, the annual by-product of sodium chloride waste salt in the national chemical industry is more ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D3/06C07C67/14C07C69/14C07C69/63C07C69/78C07C69/36
CPCC01D3/06C01F11/18C07C67/14C07C69/14C07C69/63C07C69/78
Inventor 冯春全李政周含峰
Owner 佛山经纬纳科环境科技有限公司
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