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Preparation process of dimethyl carbonate and catalyst thereof

A technology for the preparation of dimethyl carbonate and its preparation process, which is applied in the field of the preparation process of dimethyl carbonate and its catalyst, and can solve the problems of high catalyst preparation cost and unsatisfactory conversion rate of catalyst to methanol, etc.

Pending Publication Date: 2022-02-11
SHANDONG DEPU CHEM IND SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method needs the assistance of a catalyst to carry out, and it is still in the laboratory test stage
In addition, the preparation cost of this type of catalyst is high, and the conversion rate of the catalyst to methanol is not ideal

Method used

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  • Preparation process of dimethyl carbonate and catalyst thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of preparation technology of dimethyl carbonate, comprises the steps:

[0030] (1) Grind the sulfuric acid slag after drying at 50°C for 1 hour, pass through a 100-mesh sieve, and the sieve residue is less than 1.5%. Mix the obtained sulfuric acid slag with a sulfuric acid solution with a mass fraction of 10%, and add the sulfuric acid solution according to the ratio of 1g:1.5ml of sulfuric acid in the sulfuric acid slag and sulfuric acid solution, the temperature of the acid leaching treatment is 55°C, and the time is 105min , after completion, filter for solid-liquid separation to obtain pretreated sulfuric acid slag for future use.

[0031] (2) The sulfuric acid slag of described pretreatment is mixed with the sulfuric acid of mass fraction 35%, and the ratio of sulfuric acid slag and sulfuric acid is 1g: 3ml, and the temperature of described acid leaching treatment is 55 ℃, and the time is 180min, after finishing, filter and solidify Liquid separation, washi...

Embodiment 2

[0038] A kind of preparation technology of dimethyl carbonate, comprises the steps:

[0039] (1) Grind the sulfuric acid slag after drying at 50°C for 1 hour, pass through a 100-mesh sieve, and the sieve residue is less than 1.5%. Mix the obtained sulfuric acid slag with a sulfuric acid solution with a mass fraction of 5%, and add the sulfuric acid solution according to the ratio of sulfuric acid slag and sulfuric acid in the sulfuric acid solution: 1g: 1.7ml, the temperature of the acid leaching treatment is 65°C, and the time is 90min , after completion, filter for solid-liquid separation to obtain pretreated sulfuric acid slag for future use.

[0040] (2) The sulfuric acid slag of described pretreatment is mixed with the sulfuric acid of mass fraction 30%, and the ratio of sulfuric acid slag and sulfuric acid is 1g: 4ml, and the temperature of described acid leaching treatment is 65 ℃, and the time is 100min, after completion, filter and solidify Liquid-liquid separation, ...

Embodiment 3

[0047] A kind of preparation technology of dimethyl carbonate, comprises the steps:

[0048] (1) Grind the sulfuric acid slag after drying at 50°C for 1 hour, pass through a 90-mesh sieve, and the sieve residue is less than 1.5%. Mix the obtained sulfuric acid slag with a sulfuric acid solution with a mass fraction of 15%, and add the sulfuric acid solution according to the ratio of 1g:1.4ml of sulfuric acid in the sulfuric acid slag and sulfuric acid solution. The temperature of the acid leaching treatment is 40°C and the time is 120min , after completion, filter for solid-liquid separation to obtain pretreated sulfuric acid slag for future use.

[0049] (2) The sulfuric acid slag of described pretreatment is mixed with the sulfuric acid of mass fraction 45%, and the ratio of sulfuric acid slag and sulfuric acid is 1g: 2.5ml, and the temperature of described acid leaching treatment is 40 ℃, and the time is 240min, after finishing, filter and carry out Separation of solid and...

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Abstract

The invention discloses a preparation process of dimethyl carbonate and a catalyst thereof. The preparation process comprises the following steps: (1) drying sulfuric acid residues, grinding, carrying out acid leaching treatment, and carrying out solid-liquid separation to obtain pretreated sulfuric acid residues; (2) carrying out acid leaching treatment on the pretreated sulfuric acid residues again, and cleaning and drying solid residues obtained by solid-liquid separation; (3) adding excessive precipitant into the liquid phase obtained by solid-liquid separation to enable the iron element in the liquid phase to form precipitate, separating out the precipitate, and washing for later use; (4) uniformly mixing the precipitate with solid slag, calcium carbonate and water, granulating, and calcining the obtained particles in an air atmosphere to obtain a catalyst precursor; and (5) soaking the catalyst precursor in clear water, drying to obtain the catalyst, and catalyzing carbon dioxide and methanol to synthesize dimethyl carbonate by using the catalyst. According to the process, the catalyst prepared from industrial waste residues is used for catalyzing carbon dioxide and methanol to synthesize dimethyl carbonate, the conversion rate of methanol is increased, and the cost is low.

Description

technical field [0001] The invention relates to the technical field of dimethyl carbonate preparation, in particular to a preparation process of dimethyl carbonate and a catalyst thereof. Background technique [0002] As we all know, dimethyl carbonate is a chemical raw material with low toxicity, excellent environmental performance and wide application. It contains CH 3 -, CH 3 O-, CH 3 A variety of functional groups such as O-CO-, -CO-, are widely used as intermediates in organic synthesis, and are known as the "new cornerstone" of organic synthesis today. Dimethyl carbonate can be used as a raw material to prepare a variety of high value-added products. Fine specialty chemicals, such as pharmaceuticals, pesticides, synthetic materials, lubricating oil additives, etc. The earliest method of dimethyl carbonate is the phosgene method. Since the raw materials used in it are highly toxic, almost no enterprises have adopted this method to prepare dimethyl carbonate. The cur...

Claims

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Application Information

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IPC IPC(8): C07C68/04C07C69/96B01J23/78B01J35/10
CPCC07C68/04B01J23/78B01J35/60C07C69/96Y02P20/141
Inventor 卢伟谢厚正李飞张森杨芹芹姚平安
Owner SHANDONG DEPU CHEM IND SCI & TECH
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