One-step technology for synthesis of ethyl methyl carbonate and co-production of 1,2-propanediol

A technology of ethyl methyl carbonate and diethyl carbonate, which is applied in the technical field of synthesizing ethyl methyl carbonate, can solve the problems of increased operating costs, high energy consumption in industrial production processes, low conversion rate of reactants and low product selectivity, and achieves The effect of short synthetic route and clean reaction process

Inactive Publication Date: 2018-05-11
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0027] At present, in all above-mentioned synthesis methods of ethyl methyl carbonate, the transesterification method is mainly used as the mainstream synthetic route, but the raw material dimethyl carbonate of the transesterification method needs to be synthesized through methanol transesterification of ethylene carbonate or propylene carbonate, while ethylene carbonate Esters need to be prepared by ethylene oxide and carbon dioxide reaction, and propylene carbonate needs to be prepared by propylene carbonate reaction. The above-mentioned reaction route needs to be carried out in stages, and the conversion rate of reactants and product selectivity in each stage are low. Both require complex distillation and separation operations for each product, and the industrial production process consumes a lot of energy and increases operating costs.

Method used

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  • One-step technology for synthesis of ethyl methyl carbonate and co-production of 1,2-propanediol
  • One-step technology for synthesis of ethyl methyl carbonate and co-production of 1,2-propanediol
  • One-step technology for synthesis of ethyl methyl carbonate and co-production of 1,2-propanediol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Propylene carbonate, methanol and ethanol are used as raw materials to react to form ethyl methyl carbonate, the ratio of methanol to ethanol is 3:2, and the excess propylene carbonate is recycled.

[0049] The catalyst is an alkaline composite material 15%BaO-5%ZnO-3%La 2 o 3 / Cs-meso-EMT, the dosage is 3% of the total mass sum of the raw materials, and the ratio of the cross-sectional area of ​​the initial distillation section to the side line section is 1:1.

[0050] The operating conditions are as follows:

[0051] The first reactor T1: tower diameter 1000mm; tower height 19000mm; the number of trays in the public rectification section, initial distillation section, side line section, and public stripping section are 10, 20, 30, 15 respectively; the pressure inside the tower is 5MPa; The top temperature is 70°C; the bottom temperature of the common stripping section is 150°C; the bottom temperature of the side line section is 130°C.

[0052] Pressurized distillat...

Embodiment 2

[0060] Under the operating conditions of embodiment 1, the total raw material mass flow rate is 2500kg / h, and when the rectification pressure is 3MPa, the T2 pressurized rectification column reflux ratio is changed, and the change of the ethyl methyl carbonate mass fraction at the bottom of the tower still is as shown in Table 2 .

[0061] Table 2 Effects of different reflux ratios on the change of the mass fraction of ethyl methyl carbonate at the bottom of the T2 pressurized rectification column

[0062]

[0063] It can be seen from Table 2 that with the increase of reflux ratio, the mass fraction of EMC in the bottom of T2 pressurized distillation column first increases and then the rate of increase slows down obviously. The reason is that with the increase of the reflux ratio, more methanol, ethanol, DMC and the azeotrope of DMC and methanol at the top of the tower are taken away from the liquid phase, and the mass fraction of DMC in the bottom fraction of the tower dec...

Embodiment 3

[0065] Under the operating conditions of Example 1, when the total raw material mass flow rate is 2500kg / h, the pressure of the T2 pressurized rectification tower is changed, and the changes in the mass fractions of the components at the bottom of the tower are shown in Table 3.

[0066] Table 3 The influence of different pressures on the composition of the bottom of the T2 rectification column

[0067]

[0068]It can be seen from Table 3 that the mass fractions of methanol and ethanol in each liquid phase composition decrease as the reaction pressure increases, because the boiling point difference of the azeotrope composition increases at higher pressure, and the azeotrope is easier to separate. However, when the pressure is higher than 3MPa, the components remain basically unchanged. Because high pressure requires high equipment, it will greatly increase the input cost, so 3MPa is the best condition for this rectification process.

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Abstract

The invention provides a one-step technology for synthesis of ethyl methyl carbonate and co-production of 1,2-propanediol and relates to a technology for synthesizing ethyl methyl carbonate. Accordingto the technology, ethyl methyl carbonate, diethyl carbonate and 1,2-propanediol are directly synthesized in one step by catalysis of a multifunctional composite alkaline material catalyst. Azeotropic separation is performed synchronously while reactive distillation is performed, a solvent is not needed for extraction and separation of a product, and accordingly, the conventional technological process of synthesis of ethyl methyl carbonate is greatly simplified; meanwhile, multiple components are separated at a time, and the separation purity is high. The maximum selectivity of ethyl methyl carbonate in a crude product obtained by the reaction can reach 70%, and dimethyl carbonate and diethyl carbonate as byproducts can be taken as products to be separated directly and can also be recycled to be reacted continuously for generation of ethyl methyl carbonate, and the byproduct 1,2-propanediol can be taken as a bulk raw material to be separated by simple distillation. The whole reactionprocess is clean, efficient and pollution-free, and no waste is generated.

Description

technical field [0001] The invention relates to a process for synthesizing ethyl methyl carbonate, in particular to a process for synthesizing ethyl methyl carbonate in one step and co-producing 1,2-propanediol. Background technique [0002] Methyl Ethyl Carbonate (MEC for short), molecular formula: C 4 h 8 o 3 , colorless transparent liquid, density 1.01 g / mL, melting point -55 ° C, boiling point 107 ° C, flammable, can be mixed with organic solvents such as alcohols, ketones, esters in any proportion, is an excellent solvent, ethyl methyl carbonate is due to Its molecular structure has methyl and ethyl groups at the same time, so it has the characteristics of dimethyl carbonate and diethyl carbonate, and can be used as some special organic synthesis reagents, and it is also a solvent for special fragrances. [0003] Due to the low viscosity, large dielectric constant and strong solubility of lithium salts, ethyl methyl carbonate is an excellent lithium-ion battery elect...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96C07C29/36C07C31/20
CPCC07C29/36C07C68/065C07C69/96C07C31/205Y02P20/10
Inventor 石磊刘菊
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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