Method for synthesis of symmetrical carbonate and co-production of 1,2-propylene glycol

A technology of propylene glycol and propylene carbonate, applied in the direction of organic carbonate preparation, carbonate/haloformate preparation, chemical instruments and methods, etc., can solve the problems of increased operating cost, low conversion rate of reactants and low product selectivity, High energy consumption and other issues

Inactive Publication Date: 2018-06-08
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
  • Description
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  • 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 car

Method used

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  • Method for synthesis of symmetrical carbonate and co-production of 1,2-propylene glycol
  • Method for synthesis of symmetrical carbonate and co-production of 1,2-propylene glycol
  • Method for synthesis of symmetrical carbonate and co-production of 1,2-propylene glycol

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preparation example Construction

[0064] 1. Preparation method of mesoporous molecular sieve carrier:

[0065] In the present invention, orderly acid-base treatment is carried out on different carriers, and finally the molecular sieve carrier with the compound pore structure of mesoporous and micropores is prepared by high-temperature roasting. The purpose of the acid treatment is to remove the Al in the molecular sieve framework, so as to realize pore formation. The main function of the alkali treatment is to remove the Si in the molecular sieve framework to make the molecular sieve form a mesoporous structure. The preparation process includes the following steps:

[0066] 1) Dealumination: Add a certain mass of M-S carrier to a certain volume of acidic solution with a concentration of 0.11 mol / L, then stir and reflux in an oil bath at 100°C for 6 h, then filter, wash, and dry at 120°C for 8 h. The dealuminated M-S-DAl carrier is obtained.

[0067] 2) Desiliconization: Add the M-S-DAl carrier prepared in pro...

Embodiment 1

[0100] In the still of 50L slurry bed reactor, reaction pressure 2MPa, reaction raw material propylene carbonate: methyl alcohol=1:3, drop into each 1.2 kg of the basic catalyst that above-mentioned preparation method obtains respectively, the total volume of reaction solution is 40 L. The reaction was carried out with mechanical stirring, and the reaction temperature was 100°C. After 10 hours of reaction, samples were taken for chromatographic analysis and calculation. The conversion rate of raw materials and the yield of products are shown in Table 1.

[0101]

[0102] The reaction is catalyzed by a basic catalyst, and the reaction product is a single dimethyl carbonate and 1,2-propanediol. In addition to the generation of dimethyl carbonate (DMC) in the above table, a large amount of 1,2-propanediol is generated. Since 1,2-propanediol is derived from propylene carbonate (PC), if the product selectivity is calculated from propylene carbonate, 1 , The selectivity to 2-prop...

Embodiment 2

[0104] In a 50L slurry bed reactor, the reaction pressure is 2MPa, the reaction raw material propylene carbonate: various alcohols = 1:3, and 15%BaO-5%Cr 2 o 3 -3%La 2 o 3 / Zr-meso-ZSM-35 catalyst 1.2kg, the total volume of the reaction solution is 40 L. The reaction was mechanically stirred, the reaction temperature was 100°C, and after 10 hours of reaction, samples were taken for chromatographic analysis and calculation.

[0105]

[0106] It can be seen from Table 2 that when different alcohols are used as reaction raw materials to synthesize symmetrical carbonate esters, the reaction results are quite different. As the R group becomes more complex, the conversion rate of ROH gradually decreases, and the yield of symmetrical carbonate esters also gradually decreases. . The reason is that as the R group becomes more complex, the steric hindrance of ROH becomes larger, and it is difficult for the R group to approach propylene carbonate and replace it.

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Abstract

The invention discloses a method for synthesis of symmetrical carbonate and co-production of 1,2-propylene glycol, and relates to the method for synthesizing the symmetrical carbonate. According to the method provided by the invention, a high-efficiency basic catalyst with a composite pore structure is used for one-step synthesis of the symmetrical carbonate by using propylene carbonate and various alcohols (ROH, wherein the R can be selected from various alcohols such as straight-chain alcohols, iso-alcohols, aromatic alcohols, phenols, diols such as ethylene glycol and diethylene glycol, polyols, and the like). The obtained crude product obtained by a reaction only contains the symmetrical carbonate and the 1,2-propylene glycol, wherein the conversion rate of the propylene carbonate canbe up to 95%. The by-product 1,2-propylene glycol can be separated out through simple distillation as a bulk raw material. The whole reaction process is clean, efficient and free of pollution, and nowaste is generated. When the molar ratio of the propylene carbonate to the various alcohols is 1:3, the reaction pressure is 5 MPa, the reaction temperature is 100 DEG C, and the space velocity is 5 h<-1>, the catalyst is not deactivated and has good stability after being used for 5000 hours.

Description

technical field [0001] The invention relates to a method for synthesizing symmetrical carbonate esters, in particular to a method for synthesizing symmetrical carbonate esters 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 electro...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96C07C29/128C07C31/20B01J29/69B01J35/10
CPCY02P20/52C07C68/065B01J29/69B01J35/1004B01J35/1061B01J2229/18C07C29/1285C07C69/96C07C31/205
Inventor 石磊邓文杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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