Method and device for directly preparing diethyl carbonate by adopting one-step method

A diethyl carbonate, direct technology, applied in the field of diethyl carbonate preparation, can solve the problems of DEC decomposition, catalyst deactivation, low single-pass conversion rate, etc., to improve reaction conversion rate, follow-up separation convenience, and increase conversion rate Effect

Inactive Publication Date: 2015-03-25
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, since this reaction is not thermodynamically dominant and is accompanied by the formation of by-product water, the conversion rate of the reaction is very low
In particular, the water generated during the reaction will lead to catalyst deactivation and DEC decomposition, and the single-pass conversion rate based on ethanol is relatively low (<1%)
In order to improve the conversion rate of the reaction, some researchers tried to synthesize DEC by coupling reaction by adding acetonitrile or acetal, and achieved a higher yield of DEC, but the product was complicated by adding acetonitrile and many nitrogen-containing compounds were generated; while acetal The synthesis of aldehyde itself is difficult, which is not conducive to the scale-up of this reaction

Method used

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  • Method and device for directly preparing diethyl carbonate by adopting one-step method
  • Method and device for directly preparing diethyl carbonate by adopting one-step method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A method for directly preparing diethyl carbonate by one-step method, comprising the following steps:

[0026] 1) Put 20 mL of absolute ethanol in the reaction kettle, add 20 mL of propylene oxide, and add 0.3 g of two-component metal oxide catalyst K with a mass ratio of 1:0.4 2 O / ZrO 2 , cover and seal well;

[0027] The two-component metal catalyst K 2 O / ZrO 2 Prepared by impregnation method: at 70 ° C, zirconium nitrate was used as the precursor first, and NH 3 ·H 2 After precipitation occurs in O titration, reflux and aging for 6 hours, and ZrO is obtained after drying and roasting. 2 powder; then impregnated with potassium nitrate solution for 6h, then dried and roasted at 600 °C to obtain the catalyst K of double metal oxide 2 O / ZrO 2 ; Potassium nitrate and ZrO 2 The mass ratio of powder is 1:0.4.

[0028] 2) Pass CO 2 Purge and replace the air in the reactor, and then introduce CO 2 Gas to 5MPa, heated to a temperature of 150oC, and then CO 2 Pres...

Embodiment 2

[0034] A method for directly preparing diethyl carbonate by one-step method, comprising the following steps:

[0035] 1) Put 10 mL of absolute ethanol in the reaction kettle, add 30 mL of propylene oxide, and add 0.1 g of two-component metal oxide catalyst K with a mass ratio of 1:0.4 2 O / CeO 2 , cover and seal well;

[0036] Two-component metal oxide catalyst K 2 O / CeO 2 The preparation method is basically the same as Example 1, except that the transition metal is Ce;

[0037] 2) Pass CO 2 Purge and replace the air in the reactor, and then introduce CO 2 Gas to 4MPa, heated to a temperature of 150oC, and then CO 2 Pressurize to a reaction pressure of 7Mpa;

[0038] 3) Turn on the stirring controller, the stirring speed is 600rpm, and react for 8h;

[0039] 4) After the reaction is over, wait for the reactor to cool down to room temperature, release the pressure in the reactor to obtain diethyl carbonate and receive the product with ethanol.

[0040]Product detection ...

Embodiment 3

[0042] A method for directly preparing diethyl carbonate by one-step method, comprising the following steps:

[0043] 1) Put 30 mL of absolute ethanol in the reaction kettle, add 10 mL of propylene oxide, and at the same time add 0.5 g of a two-component metal oxide catalyst MgO / Nu with a mass ratio of 1:0.4 2 o 3 , cover and seal well;

[0044] Two-component metal oxide catalyst MgO / Nu 2 o 3 The preparation method is basically the same as in Example 1, except that the transition metal is Nu, and the alkali metal is Mg;

[0045] 2) Pass CO 2 Purge and replace the air in the reactor, and then introduce CO 2 Gas to 5MPa, heated to a temperature of 150oC, and then CO 2 Pressurize to a reaction pressure of 7Mpa;

[0046] 3) Turn on the stirring controller, the stirring speed is 700rpm, and react for 8h;

[0047] 4) After the reaction is over, wait for the reactor to cool down to room temperature, release the pressure in the reactor to obtain diethyl carbonate and receive t...

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Abstract

The invention discloses a method for directly preparing diethyl carbonate by adopting a one-step method. The method comprises the following steps: mixing absolute ethanol, epoxy propane and a double-component metal oxide catalyst and sealing by a cover; charging CO2 until the pressure is 4MPa to 6MPa, heating to the temperature of 150 to 250 DEG C, and then pressurizing CO2 to the pressure of 7MPa to 12MPa; starting a stirring controller, stirring and reacting for at least 2 hours; decompressing a reaction kettle after cooling the reaction kettle to room temperature to obtain diethyl carbonate and receiving diethyl carbonate by using ethanol. The method disclosed by the invention has the advantages of being simple in process and easy to operate by adopting the one-step method to prepare diethyl carbonate; the used reaction raw materials are low in price and easy to obtain; the catalyst is good in stability and quite convenient to separate subsequently; due to the added epoxy propane, the reaction conversion rate is effectively increased.

Description

technical field [0001] The invention relates to a preparation method of diethyl carbonate, in particular to a method and a device for directly preparing diethyl carbonate by adopting a one-step method. Background technique [0002] Diethyl carbonate (DEC) is an important organic synthesis intermediate, which can be used as a solvent, surfactant, lithium battery fluid additive, and oxygen-containing additive for gasoline and diesel fuel, and has a wide range of uses. [0003] DEC has a variety of preparation methods, mainly including: phosgene method, ethanol and CO 2 Direct synthesis method, urea alcoholysis method and oxidative carbonylation method, etc. Among them, ethanol and CO 2 DEC is directly synthesized, the raw material is the cheapest and easy to obtain, and it is also useful for solving CO 2 The resulting greenhouse effect is of great significance and is an attractive new green technology. The reaction equation is: 2C 2 h 5 OH+CO 2 → C. 2 h 5 OCOOC 2 h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06B01J23/04B01J23/10
CPCB01J23/002B01J23/04B01J23/10C07C68/065C07D317/36C07C69/96
Inventor 贾冬冬张雪征朱振孙永跃
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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