Efficient and safe method for synthesizing carbonic ester by using oxidative carbonyl

A technology of oxo synthesis and oxidative carbonylation, applied in the direction of carbon monoxide and oxygen preparation, purification/separation of carbonate/haloformate, chemical instruments and methods, etc., can solve catalyst separation, recovery and corrosion, increase equipment Investment, operating costs, large-scale production equipment and other issues, to achieve the effect of great industrial application prospects, elimination of safety hazards, and efficient response

Active Publication Date: 2015-04-22
NANJING UNIV OF TECH +2
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Problems solved by technology

[0003] In the above-mentioned process method, it is not mentioned that in this system, the feed gas CO is in the O 2 The concentration in the concentration has the problem of potential safety hazard in the explosion limit range, while CO and O 2 The feed ratio has a great influence on the conversion rate, which restricts the development of the process to a certain extent; at the same time, there are still problems in the separation, recovery and corrosion of the catalyst in the slurry bed reactor, which increases equipment investment and operation. Cost; the amount of liquid held by the tubular reactor is small, and the gas-liquid reaction mass transfer

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  • Efficient and safe method for synthesizing carbonic ester by using oxidative carbonyl

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Embodiment 1

[0036] 8 kilograms of industrial-grade copper bromide, 4 kilograms of industrial-grade 4-methylquinolines are packed into a 300-liter reactor with packed tower, 110 kilograms of ethanol are packed into, ethylene carbonate 10L is added, and the compressor pressure is started. Enter CO, start the compressor and press O 2 , using a flow controller to control the amount of oxygen so that CO and O 2 The ratio of the intake air volume is 4:1, the total pressure is 3.5MPa, the reactor is heated to 100°C, the reaction starts, the liquid is collected in the gas condenser, and the catalyst solution separated by the flash tank enters the liquid outlet for recycling. After 1 hour, the system entered a steady state. In the separated liquid mixture, the DEC content was 21%. The crude product was separated into the next section to obtain a DEC content of 99.7%. After 15 hours of operation, the catalyst yield was 0.9g DEC / gcat.h, after running for 100 hours, the yield is 0.7 g DEC / gcat.h, an...

Embodiment 2

[0038] 8 kilograms of industrial-grade copper bromide, 110 kilograms of methanol, and 4 kilograms of industrial-grade quinoline are loaded into the reactor, and 10 L of ethylene carbonate is added, and the reaction is started according to the method described in Example 1. At 110 ° C, 3.0 MPa, it enters normal Reaction, after 1 hour, the DMC content in the crude product is 17%, after running for 10 hours, the catalyst yield is 0.6g DMC / gcat.h, after running for 100 hours, the productive rate is 0.7g DMC / gcat.h, after running for 200 hours , yield 0.65 g DMC / gcat.h.

Embodiment 3

[0040] 8 kilograms of industrial-grade copper bromide, 4 kilograms of industrial-grade 4-methylquinoline are packed into the reactor, 10 L of propylene carbonate is added, and the reaction is started according to the method described in Example 1. At 110 ° C, 3.0 MPa, the raw material is controlled The gas feed ratio is 3:1, and it enters the normal reaction. After 1 hour, the DEC content in the crude product is 15%. After running for 10 hours, the catalyst yield is 0.4g DEC / gcat.h. After running for 100 hours, the yield is 0.6 g DEC / gcat.h, yield 0.53 g DEC / gcat.h after 200 hours of operation.

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Abstract

The invention discloses an efficient and safe method for synthesizing carbonic ester by using oxidative carbonyl. The method comprises the steps of oxidative glycosylation reaction, flash separation, gas-liquid separation and product separation. The method can be used for overcoming the defects of heterogeneous catalytic system, complex process, poor recyclability and potential safety hazard of reaction process in the prior art; a novel process device is adopted; the feeding mole ratio of carbon monoxide (CO) to oxygen (O2) can be controlled; CO and O2 are taken as the reaction raw material gases; the catalyst solution is recyclable; a catalyst system applied to the reaction is a catalyst solution prepared from a solvent and a complex which is formed by homogeneous active components and ligands. The method has the advantages that the process is efficient, safe and simple, and the catalyst solution is easily recyclable; and the method has a good prospect of industrial application.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to an efficient and safe method for oxidative carbonyl synthesis of carbonate. Background technique [0002] Carbonate (dimethyl carbonate, diethyl carbonate, etc.) is an important green organic chemical raw material, and its molecule contains a variety of functional groups, which can be synthesized by reactions such as oxidative carbonylation. It can replace highly toxic phosgene and diethyl sulfate as a reaction solvent to react with various alcohols, phenols and esters to synthesize a series of high value-added downstream products. Therefore, the research on its synthetic method has gradually attracted people's attention. The traditional synthesis method is to react with alcohol and phosgene, the reactants of this method are highly toxic, and the HCl produced will severely corrode the reaction equipment. The transesterification method uses various carbonates and al...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/00C07C68/08
CPCC07C68/01C07C68/08C07C69/96Y02P20/584
Inventor 刘定华徐凯刘晓勤孙林兵万建龙崔德文
Owner NANJING UNIV OF TECH
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