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Process for catalytically synthesizing dimethyl carbonate

A dimethyl carbonate and process technology, which is applied in the field of catalytic synthesis of dimethyl carbonate, can solve the problems of difficult catalyst regeneration, complicated preparation process, and low overall cost performance, and achieve improved raw material utilization rate, product yield, and high catalytic activity , the effect of increasing the surface area

Active Publication Date: 2022-03-22
SHANDONG DEPU CHEM IND SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Carbon dioxide and methanol directly synthesize dimethyl carbonate. The reaction raw materials are cheap and easy to get, and the environmental hazards are minimal. It is a very economical and green process route with good application prospects. Effective progress has been made in this process, but It is still in the exploration and experimental stage, and there is still a long way to go before it has industrial application value. One of the reasons is that the reaction is difficult to carry out under conventional conditions, and catalysts need to be added to promote the reaction. Complicated problems, and problems such as low methanol conversion rate and difficult catalyst regeneration lead to low overall cost performance of the process, which needs to be further improved and optimized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of technique of catalytic synthesis dimethyl carbonate, comprises the steps:

[0029] (1) get the electroless nickel plating waste water of pH=4.4 to be acid waste liquid, wherein metal ion content is: Ni 2+ 14732mg / L, Fe 2+ 2.93mg / L, Cu 2+ 43.51mg / L, Zn 2+ 12.44mg / L. Add hydrogen peroxide to the electroless nickel-plating waste water to carry out decontamination treatment, and the concentration of the hydrogen peroxide in the waste water is 1200mmol / L as the criterion.

[0030] (2) Add sodium hydroxide powder to the electroless nickel-plating waste water that the step is processed through breaking network and make the metal ion wherein form hydroxide precipitation, treat to filter reaction solution with filter machine after no precipitate is formed, will obtain filter cake in Place in a cool place for 2 days, then pulverize into powder and pass through a 300-mesh sieve to obtain hydroxide powder, which is set aside.

[0031] (3) Mix the hydroxide powder, s...

Embodiment 2

[0035] A kind of technique of catalytic synthesis dimethyl carbonate, comprises the steps:

[0036] (1) get the electroless nickel plating waste water of pH=4.3 to be acid waste liquid, wherein metal ion content is: Ni 2+ 19004mg / L, Fe 2+ 3.51mg / L, Cu 2+ 24.87mg / L, Zn 2+ 7.94mg / L. Add hydrogen peroxide to the electroless nickel-plating waste water and carry out decontamination treatment, and described hydrogen peroxide is as the criterion with its concentration in waste water being 1300mmol / L.

[0037] (2) Add ammonia water to the electroless nickel-plating waste water that has been treated by breaking the network in the step to make the metal ions in it form hydroxide precipitates. After no precipitate is formed, use a filter to filter the reaction solution, and place the obtained filter cake in a cool place. 2 days, then pulverized into powder and passed through a 350-mesh sieve to obtain hydroxide powder for subsequent use.

[0038] (3) The hydroxide powder, silicon d...

Embodiment 3

[0042] A kind of technique of catalytic synthesis dimethyl carbonate, comprises the steps:

[0043] (1) get the electroless nickel plating waste water of pH=4.1 to be acid waste liquid, wherein metal ion content is: Ni 2+ 17218mg / L, Fe 2+ 2.25mg / L, Cu 2+ 59.96mg / L, Zn 2+ 15.1mg / L. Add hydrogen peroxide in this electroless nickel-plating waste water and carry out decontamination treatment, and described hydrogen peroxide is as the criterion with its concentration in waste water being 1250mmol / L.

[0044] (2) Add sodium hydroxide powder to the electroless nickel-plating waste water that the step is processed through breaking network and make the metal ion wherein form hydroxide precipitation, treat to filter reaction solution with filter machine after no precipitate is formed, will obtain filter cake in Place in a cool place for 1 day, then pulverize into powder and pass through a 300-mesh sieve to obtain hydroxide powder, which is set aside.

[0045] (3) Mix the hydroxide...

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Abstract

The invention discloses a process for catalytically synthesizing dimethyl carbonate, which comprises the following steps: (1) carrying out complex breaking treatment on chemical nickel-plating wastewater, then adding a precipitator, separating out precipitate, and crushing into hydroxide powder; (2) uniformly mixing the hydroxide powder, silicon dioxide powder, calcium oxide powder and a binder, granulating, and calcining the obtained particles in an air atmosphere to obtain a catalyst precursor; and (3) soaking the catalyst precursor in clear water, cleaning, repeatedly executing the step until the pH value of the cleaning solution is constant, taking out a solid product, and drying to obtain the porous catalyst. And (4) taking the porous catalyst as a catalyst, preparing dimethyl carbonate by adopting a methanol-carbon dioxide direct method, inserting an ultrasonic vibration rod into the liquid level of methanol during preparation, and separating out dimethyl carbonate after completion. According to the process disclosed by the invention, the industrial waste liquid is used as a raw material and is modified to prepare the catalyst, so that the cost of the catalyst is reduced, and the conversion rate of methanol is effectively improved.

Description

technical field [0001] The invention relates to the technical field of dimethyl carbonate preparation, in particular to a process for catalytically synthesizing dimethyl carbonate. Background technique [0002] Due to its low toxicity, dimethyl carbonate is an industrial raw material with excellent environmental performance and wide application, and has the characteristics of safe use, convenience, less pollution, and easy transportation. It is currently widely used in pesticides, medicines, chemicals, food, etc. In the preparation of additives, etc. At present, the mature preparation process of dimethyl carbonate includes phosgene method, oxidative carbonylation method and transesterification method. However, due to the use of highly toxic raw material phosgene in the phosgene method, the by-products pollute the environment and corrode equipment, and the chlorine content of the product Alcohol has been basically eliminated, and oxidative carbonylation and transesterificati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/04C07C69/96B01J23/78B01J23/80B01J37/03B01J37/08
CPCB01J23/80B01J37/03B01J37/082B01J23/78C07C68/04C07C69/96Y02P20/141
Inventor 卢伟李飞张新平王超李天磊姚平安
Owner SHANDONG DEPU CHEM IND SCI & TECH
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