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Method for converting dimethyl sulfate waste residue into dimethyl sulfate product

A technology for converting dimethyl sulfate into chemical instruments and methods, preparation of sulfur compounds and sulfonate esters, etc., can solve the problems of unusable, uneconomical, low content, etc., to eliminate environmental pollution and improve reaction speed. and conversion rate, the effect of improving economic efficiency

Inactive Publication Date: 2011-11-23
SHANDONG XINGHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its main disadvantages are: 1. Although the method of adding alkali neutralization after hydrolysis first has eliminated environmental pollution, the treatment cost will be greatly increased, which is very uneconomical
2. The ammonia water treatment method increases the consumption of ammonia water. Ammonium sulfate is sold as fertilizer, but the fertilizer is basically unusable due to its strong acidity.
The content of the produced methanol is 40%-50%, which is low, and it needs to be concentrated when used in large-scale production, which is uneconomical; the content of the produced sulfuric acid is 40%-50%, which is low, and it is difficult to reuse it as a chemical raw material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 9,750kg of dimethyl sulfate waste residue into the glass-lined reactor, slowly add 6,200kg of tap water, control the speed of tap water addition at a temperature of 70-140°C, and carry out hydrolysis and etherification reactions. The distilled gas is condensed through the condenser, and the water is condensed And a small amount of methanol, higher purity methyl ether gas and absorbed sulfur trioxide for esterification reaction, the esterification temperature is controlled at 70~140°C to produce dimethyl sulfate. Reclaim the dimethyl sulfate 3100kg of mass content 98.5%, reclaim the condensate and obtain the methanol 100kg that mass content is 40%, recover the raffinate in the reactor after distillation simultaneously and obtain 55~65% sulfuric acid 12500kg.

example 2

[0049]Add 9,750kg of dimethyl sulfate waste residue into the glass-lined reactor, slowly add 5,500kg of tap water, control the speed of tap water addition at a temperature of 70-140°C, and carry out hydrolysis and etherification reactions. The distilled gas is condensed through the condenser, and the water is condensed And a small amount of methanol, higher purity methyl ether gas and absorbed sulfur trioxide for esterification reaction, the esterification temperature is controlled at 70~140°C to produce dimethyl sulfate. Recover 2900kg of dimethyl sulfate with a mass content of 98.5%, recover the condensate to obtain 120kg of methanol with a mass content of 40%, and recover the residual liquid in the reactor after distillation to obtain 12200kg of sulfuric acid with a mass content of 55-65%.

example 3

[0051] Add 9600kg of dimethyl sulfate waste residue into the glass-lined reactor, slowly add 6200kg of tap water, control the speed of tap water addition at a temperature of 70-140°C, and carry out hydrolysis and etherification reactions. And a small amount of methanol, higher purity methyl ether gas and absorbed sulfur trioxide for esterification reaction, the esterification temperature is controlled at 70~140°C to produce dimethyl sulfate. Recover 2600kg of dimethyl sulfate with a mass content of 98.5%, recover the condensate to obtain 150 kg of methanol with a mass content of 40%, and recover the residual liquid in the reactor after distillation to obtain 13000 kg of 55-65% sodium sulfate.

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PUM

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Abstract

The invention discloses a method for converting dimethyl sulfate waste residue into a dimethyl sulfate product, belongs to a method for preparing sulfate, and in particular relates to a method for recycling waste residue generated by a dimethyl sulfate device in the production running process. The method is characterized by comprising the following steps of: hydrolyzing and etherifying dimethyl sulfate in the dimethyl sulfate waste residue to convert the dimethyl sulfate into dimethyl ether; and performing esterification on the generated dimethyl ether and sulfur trioxide to obtain the dimethyl sulfate product. The method comprises the following process steps of: hydrolysis, etherification, separation of distillates, esterification, and distillation. The invention provides a method for converting the dimethyl sulfate waste residue into the dimethyl sulfate product; and the dimethyl ether is recycled from the dimethyl sulfate waste residue and is further converted into the dimethyl sulfate product. The waste residue generated by the dimethyl sulfate device is recycled, and the environmental pollution of the dimethyl sulfate waste residue is eliminated. The purity of the recycled dimethyl ether gas is 99.0 to 99.75 percent; the dimethyl sulfate product has the dimethyl sulfate content of more than or equal to 99.5 percent and the acidity of less than or equal to 0.6 percent; and the content of a byproduct of sulfuric acid is 50 to 70 percent.

Description

technical field [0001] The invention relates to a method for converting dimethyl sulfate waste residue into a dimethyl sulfate product. The invention belongs to a method for preparing sulfuric acid ester, and in particular relates to a method for recycling waste residue generated in the production and operation of a dimethyl sulfate plant. Background technique [0002] A large amount of waste residue will be produced in the production of dimethyl sulfate, and the main components of the waste residue are dimethyl sulfate, sulfuric acid and black sludge. Direct discharge will cause serious pollution to the environment. At present, domestic methods for processing dimethyl sulfate waste residue mainly include: 1. adding water to hydrolyze the dimethyl sulfate waste residue, and then neutralizing it with liquid caustic soda. 2 Use ammonia water to neutralize to generate ammonium sulfate. Its main shortcoming has: 1. Though adopting the method for adding alkali to neutralize af...

Claims

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Application Information

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IPC IPC(8): C07C305/08C07C303/26C01B17/74
Inventor 高庆辉韩己强高源侯诗东
Owner SHANDONG XINGHUI CHEM
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