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Method for preparing ethyl methyl carbonate from dimethyl carbonate and diethyl carbonate

A technology of diethyl carbonate and dimethyl carbonate, applied in the field of preparation of chemical raw materials, which can solve problems such as separation and recovery difficulties, limited application, and difficult to meet raw material requirements

Inactive Publication Date: 2017-12-08
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the catalyst used can be recycled repeatedly, because the catalyst is a chloride-type Lewis acid, it is a homogeneous catalyst that is easy to absorb water and difficult to separate and recover. On the other hand, the use of chlorine-containing catalysts will cause organic chlorine impurities to be mixed into the product. Its post-purification and preparation of battery electrolyte grade products bring difficulties
[0014] Disclosed in CN1394847A is a kind of method that takes DMC and DEC as raw material synthetic EMC, and its used catalyst is the loaded metal oxide that is loaded on the aluminum oxide, comprises SnO 2 / Al 2 o 3 , Ga 2 o 3 / Al 2 o 3 , MoO 3 al 2 o 3 , ZrO 2 / Al 2 o 3 ,TiO 2 / Al 2 o 3 and V 2 o 5 / Al 2 O, under normal pressure, 104 ℃ of reaction 10h, the highest yield of ethyl methyl carbonate is only 43.6%, and the quality of the catalyst in this patent accounts for 8.4% of the total weight of the reaction raw materials, the catalyst consumption is large, and the product yield is low. its application in industry
[0015] In Japanese Patent JP2000281630, metal oxides such as lanthanum, actinium, scandium, and yttrium are used as the active components of the catalyst to catalyze the reaction of DMC and DEC to generate EMC. Although this kind of catalyst can be recycled and used and is not easy to deactivate, it requires the concentration of salt in the raw material The total content is less than 10ppm, and the content of inorganic salts is below 1ppm. The requirements for raw materials are very high, and it is difficult to meet such raw material requirements in actual production.
[0016] US Patent US5962720 adopts SmI 2 , Li, LiOCH 3 and CaH 2 As a catalyst, the reaction is carried out at normal temperature and pressure, and the reaction needs more than three days to reach equilibrium. This shows that this type of catalyst has a low catalytic rate and is not suitable for industrialization.
[0017] Based on the above-mentioned problems such as low product yield, difficult catalyst recovery, polluted products, large amount of catalyst used, harsh requirements on raw materials, and long reaction cycle, we have developed a new type of catalyst for the transesterification synthesis of DMC and DEC. EMC's response

Method used

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  • Method for preparing ethyl methyl carbonate from dimethyl carbonate and diethyl carbonate
  • Method for preparing ethyl methyl carbonate from dimethyl carbonate and diethyl carbonate
  • Method for preparing ethyl methyl carbonate from dimethyl carbonate and diethyl carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0071] In the fixed-bed reactor, self-made and single macroporous SiO 2 As a carrier, Ca(NO 3 ) 2 and Mg(SO 4 )2 25%Ca-5%Mg / SiO solution 2 Catalyst (1#), with single small hole SiO 2 As a carrier, Ca(NO 3 ) 2 and Mg(SO 4 ) 2 25%Ca-5%Mg / SiO solution 2 Catalyst (2#) and SiO composited with large and small pores 2 -Al 2 o 3 As a carrier, Ca(NO 3 ) 2 and Mg(SO 4 ) 2 25%Ca-5%Mg / SiO solution 2 Catalyst (3#) 50 g each, coprecipitation agents are KOH and NaHCO 3 dimethyl carbonate and ethanol were pumped into the reactor with a molar ratio of 1:1 using a constant-flow pump, and the reaction temperature was At 150°C, the mass space velocity of diethyl carbonate is 30h -1 After a stable reaction for 500 h under certain reaction conditions, samples were taken for chromatographic analysis and calculation, and the results are shown in Table 1.

[0072]

[0073] According to the reaction equation, dimethyl carbonate and diethyl carbonate react at an approximate molar r...

Embodiment 2

[0076] In the fixed bed reactor, the CaCl 2 and MgCl 2 25%Ca-5%Mg / SiO solution 2 Catalyst (4#), use Ca(NO 3 ) 2 and Mg(NO 3 ) 2 25%Ca-5%Mg / SiO solution 2 Catalyst (5#), use Ca(SO 4 ) 2 and Mg(SO 4 ) 2 25%Ca-5%Mg / SiO solution 2 Catalyst (6#), use CaCl during coprecipitation 2 and Mg(NO 3 ) 2 25%Ca-5%Mg / SiO solution 2 Catalyst (7#) and co-precipitation using Ca(NO 3 ) 2 and Mg(SO 4 ) 2 25%Ca-5%Mg / SiO solution 2 Catalyst (3#) 50 g each, coprecipitation agents are KOH and NaHCO 3 dimethyl carbonate and ethanol were pumped into the reactor with a molar ratio of 1:1 using a constant-flow pump, and the reaction temperature was At 150°C, the mass space velocity of diethyl carbonate is 30h -1 After 500 h of stable reaction under the reaction conditions, samples were taken for chromatographic analysis and calculation, and the results are shown in Table 2.

[0077]

[0078] As can be seen from Table 2, the use of Ca(NO 3 ) 2 and Mg(SO 4 ) 2 The mixed salt sol...

Embodiment 3

[0080] In the fixed-bed reaction tube, the co-precipitation prepared with different co-precipitation agents were loaded respectively, and Ca(NO 3 ) 2 and Mg(SO 4 ) 2 A mixed salt solution of 25%Ca-5%Mg / SiO as the source of active components 2 Catalyst 50 g, marked as NaOH (8#), KOH (9#), NH 3 ·H 2 O (10#), KOH and NaHCO 3 The mixed alkali (3#), NaOH and NH 3 ·H 2 Mixed base of O (11#), KOH and NH 3 ·H 2 The mixed alkali (12#) co-precipitation temperature of O was 70 °C, the co-precipitation pH was 11, and the aging time was 20 h. Use a constant flow pump to pump dimethyl carbonate and diethyl carbonate into the reactor at a molar ratio of 1:1. The reaction temperature is 150°C and the mass space velocity of diethyl carbonate is 30h. -1 After stable reaction for 500 h under the reaction conditions, samples were taken for chromatographic analysis and calculation, and the results are shown in Table 3.

[0081]

[0082] It can be seen from Table 3 that different co-p...

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Abstract

The invention discloses a method for preparing ethyl methyl carbonate from dimethyl carbonate and diethyl carbonate, and relates to a method for preparing a chemical raw material. According to the method, alkaline or acidic and alkaline metal oxide is supported by adopting a coprecipitation manner, and a single solution or a mixed solution of metal nitrate, hydrochloride and sulfate is utilized as a source of an active ingredient, so that the catalytic activity of a catalyst is further improved; when the catalyst is 20%Cs-10%Al-7.5%La / Al2O3-SiO2, the air speed is 10h<-1> and the temperature is 200 DEG C, the conversion rate can reach 71.90 percent, and the catalyst can be stably reacted for 5,000h without a deactivation phenomenon; during tank reaction, the reacted catalyst can be reutilized after being simply treated, and can still keep with relatively high activity after being reutilized for multiple times; the metal oxide in the active center of the catalyst prepared by a precipitation method is smaller in crystalline granularity, higher in dispersity and larger in surface area, and the catalytic effect of the prepared catalyst is higher than that of a catalyst prepared by an impregnation method.

Description

technical field [0001] The invention relates to a method for preparing chemical raw materials, in particular to a method for preparing ethyl methyl carbonate from dimethyl carbonate and diethyl carbonate. Background technique [0002] Ethylmethyl carbonate (EMC for short), molecular formula C 4 h 8 o 3 , with a molecular weight of 104.1, a colorless transparent liquid with a slightly pungent odor. Melting point -55°C, boiling point 109°C, insoluble in water, soluble in alcohol, ether and other organic solvents, it is an asymmetric carbonate. Because it contains both methyl and ethyl groups and has the characteristics of dimethyl carbonate and diethyl carbonate, EMC is also a solvent for special fragrances and intermediates, and has a wide range of uses. With the rapid development of the lithium-ion battery industry, the requirements on battery safety and service life are becoming more and more stringent, which brings challenges to the technological innovation of the batt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C69/96B01J23/02B01J29/08B01J29/10B01J32/00
CPCB01J23/02B01J29/084B01J29/088B01J29/106B01J2229/18B01J2523/00C07C68/06C07C69/96B01J2523/22B01J2523/23B01J2523/41Y02P20/50
Inventor 石磊姚杰张志刚陈飞王玉鑫
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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