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Response surface methodology-based method for optimizing high-yield preparation of dimethyl carbonate from ethylene carbonate and methanol

A technology of ethylene carbonate and dimethyl carbonate, applied in the field of carbonate preparation, can solve problems such as inefficiency

Inactive Publication Date: 2022-03-25
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Patent CN 109232250A discloses a method for improving production efficiency while maintaining high selectivity of dimethyl carbonate; Continuous and stable; patent CN 111848400A discloses a process of reactive distillation coupled with extractive distillation to produce dimethyl carbonate, which reduces the consumption of a large amount of steam and cooling capacity in the process; but the above large-scale process research for the preparation of dimethyl carbonate In the process, it is often necessary to determine the optimal reaction conditions through multiple full-process reactions, and the research method of only studying one influencing factor in one full-process reaction is extremely inefficient. In order to further improve the efficient dimethyl carbonate preparation process and master the reaction Theoretical calculations that affect the interaction of parameters and evaluate the response with a limited number of trials are particularly important

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  • Response surface methodology-based method for optimizing high-yield preparation of dimethyl carbonate from ethylene carbonate and methanol
  • Response surface methodology-based method for optimizing high-yield preparation of dimethyl carbonate from ethylene carbonate and methanol
  • Response surface methodology-based method for optimizing high-yield preparation of dimethyl carbonate from ethylene carbonate and methanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Single factor test (reaction temperature)

[0058] a.KF / γ-Al 2 o 3 Preparation of supported catalyst: use equal volume impregnation method, use analytical balance to weigh quantitative KF·2H 2 O was dissolved in a certain amount of deionized water to prepare a 0.5g / mL potassium fluoride solution, and a certain amount of solid γ-Al was added under stirring 2 o 3 Carrier, aging the mixed liquid at room temperature for 12 hours, drying in an oven at 110°C for 10 hours, then roasting at 550°C for 4 hours, and putting it into a drying tower for use after cooling;

[0059] B. in the experiment that ethylene carbonate and methanol transesterification prepare dimethyl carbonate, methyl alcohol and ethylene carbonate, catalyzer are joined in the 50ml round-bottom single-necked flask with water-cooled condenser according to the mol ratio of 8:1, catalyzer The concentration is 1‰, turn on the magnetic stirring, and adjust the speed to 300r / min. At the same time, six groups of...

Embodiment 2

[0063] Single factor test (alcohol to ester ratio)

[0064] a.KF / γ-Al 2 o 3 Preparation of supported catalyst: use equal volume impregnation method, use analytical balance to weigh quantitative KF·2H 2 O was dissolved in a certain amount of deionized water to prepare a 0.5g / mL potassium fluoride solution, and a certain amount of solid γ-Al was added under stirring 2 o 3 Carrier, aging the mixed liquid at room temperature for 12 hours, drying in an oven at 110°C for 10 hours, then roasting at 550°C for 4 hours, and putting it into a drying tower for use after cooling;

[0065] b. In the experiment of preparing dimethyl carbonate by transesterification of ethylene carbonate and methanol, the reaction temperature was fixed at 50°C, the magnetic stirring was turned on, and the speed was adjusted to 300r / min. Carry out four groups of parallel experiments simultaneously, methyl alcohol and ethylene carbonate are joined in the 50ml round bottom single-necked flask with water-cool...

Embodiment 3

[0069] Single factor test (catalyst concentration)

[0070] a.KF / γ-Al 2 o 3 Preparation of supported catalyst: use equal volume impregnation method, use analytical balance to weigh quantitative KF·2H 2 O was dissolved in a certain amount of deionized water to prepare a 0.5g / mL potassium fluoride solution, and a certain amount of solid γ-Al was added under stirring 2 o 3 Carrier, aging the mixed liquid at room temperature for 12 hours, drying in an oven at 110°C for 10 hours, then roasting at 550°C for 4 hours, and putting it into a drying tower for use after cooling;

[0071] B. in the experiment that ethylene carbonate and methanol transesterification prepare dimethyl carbonate, methyl alcohol and ethylene carbonate, catalyst are joined in the 50ml round-bottom single-necked flask with water-cooled condenser according to the molar ratio of 8:1, react The temperature was fixed at 50°C, the magnetic stirring was turned on, and the speed was adjusted to 300r / min. At the sam...

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Abstract

The invention relates to a method for optimizing high-yield preparation of dimethyl carbonate from ethylene carbonate and methanol based on a response surface method.The method comprises the steps that a KF / gamma-Al2O3 high-alkalinity supported catalyst prepared through an impregnation method is used for catalyzing an ester exchange reaction of ethylene carbonate and methanol, and qualitative and quantitative analysis is conducted on a reaction product through a gas chromatograph-mass spectrometer; the yield of dimethyl carbonate is calculated by applying an external standard curve method, optimization is performed by adopting a response surface method on the basis of a single factor test, and the optimal reaction conditions of transesterification in a reaction system applying the KF / gamma-Al2O3 high-alkalinity supported catalyst are obtained. According to the method disclosed by the invention, three factors which greatly influence the yield are selected as variables, a three-factor three-level response surface analysis test is designed, and then the optimal process condition is simulated and optimized through software, so that the yield of dimethyl carbonate can be effectively improved; meanwhile, a reference basis is provided for a method for preparing dimethyl carbonate from ethylene carbonate and methanol at high yield and application and development.

Description

technical field [0001] The invention belongs to the technical field of carbonate preparation, and relates to a method for preparing dimethyl carbonate at a high yield by optimizing ethylene carbonate and methanol based on a response surface method. Background technique [0002] Dimethyl carbonate, the chemical formula is C 3 h 6 o 3 , is a chemical raw material with low toxicity, excellent environmental protection performance and wide application. It is an important intermediate in organic synthesis. Its molecular structure contains functional groups such as carbonyl, methyl and methoxy, and has various reactivity. It has the characteristics of safe use, convenience, less pollution and easy transportation. At present, dimethyl carbonate is a green chemical that has attracted much attention in the world. On the one hand, dimethyl carbonate is expected to completely replace highly toxic or carcinogenic substances such as phosgene, dimethyl sulfate, methyl chloride and methy...

Claims

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Application Information

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IPC IPC(8): C07C68/065C07C69/96B01J27/12B01J37/02G01N30/02G01N30/72
CPCC07C68/065B01J27/12B01J37/0201G01N30/02G01N30/72G01N2030/025C07C69/96
Inventor 张文府李明燃任伟民吕小兵
Owner DALIAN UNIV OF TECH