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Method of one-step synthesis of asymmetric carbonate and co-production of 1,2-propylene glycol by using propylene oxide

A propylene oxide, asymmetric technology, used in the preparation of carbon dioxide or inorganic carbonate, chemical instruments and methods, products, etc., can solve the problem of increased operating costs, low reactant conversion and product selectivity, and high energy consumption. question

Inactive Publication Date: 2018-06-08
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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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 the reaction of ethylene oxide and carbon dioxide, and propylene carbonate needs to be prepared by the reaction of propylene oxide and carbon dioxide. The above reaction route needs to be carried out in stages. The process consumes a lot of energy and increases operating costs

Method used

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  • Method of one-step synthesis of asymmetric carbonate and co-production of 1,2-propylene glycol by using propylene oxide
  • Method of one-step synthesis of asymmetric carbonate and co-production of 1,2-propylene glycol by using propylene oxide
  • Method of one-step synthesis of asymmetric carbonate and co-production of 1,2-propylene glycol by using propylene oxide

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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

[0101] In the still of 50L slurry bed reactor, reaction pressure 10MPa, reaction raw material propylene oxide: carbon dioxide: methyl alcohol: ethanol=1:1:3:2, drop into each 1.2 kg of the neutral catalyst that above-mentioned preparation method obtains respectively, reaction solution The total volume is 40 L. The reaction was mechanically stirred at a reaction temperature of 100°C. After 10 hours of reaction, samples were taken for chromatographic analysis and calculation. The conversion rate of raw materials and product selectivity are shown in Table 1.

[0102] Table 1 Effects of different types of catalysts on feedstock conversion and product selectivity

[0103]

[0104] When the reaction is catalyzed by a neutral catalyst, the conversion rates of propylene oxide (PO) and carbon dioxide are basically the same, because propylene oxide only reacts with carbon dioxide to form propylene carbonate, and no other side reactions occur. In the following examples, neutral catal...

Embodiment 2

[0106] In a 50L slurry bed reactor, the reaction pressure is 10MPa, the reaction raw materials are propylene oxide: carbon dioxide: methanol: other alcohols = 1:1:3:2, and 15%PdO-8%GeO is added 2 -3%Ga 2 o 3 / Zr-meso-β catalyst 1.2 kg, the total volume of the reaction solution is 40L. The reaction was mechanically stirred at a reaction temperature of 100°C. After 10 hours of reaction, samples were taken for chromatographic analysis and calculation. The conversion rate of raw materials and product selectivity are shown in Table 2.

[0107] Table 2 Effects of different alcohols on feedstock conversion and product selectivity

[0108] It can be seen from Table 2 that when different alcohols are used as reaction raw materials to synthesize asymmetric carbonate esters, the reaction results are quite different. As the R group becomes complex, the conversion rate of ROH gradually decreases, and the selectivity of asymmetric carbonate esters also decreases. Gradually decreases. ...

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Abstract

The invention discloses a method of one-step synthesis of asymmetric carbonate and co-production of 1,2-propylene glycol by using propylene oxide, and relates to the method for synthesizing the asymmetric carbonate. A high-efficiency neutral catalyst with a composite pore structure is used for the one-step synthesis of the asymmetric carbonate by using the propylene oxide, carbon dioxide, methanoland various alcohols. The selectivity of the asymmetric carbonate in the crude product obtained by a reaction can be up to 70%. The by-products, dimethyl carbonate and dialkyl carbonates can be directly separated out as products, and can be recycled for continued reaction for generating the asymmetric carbonate; and the by-product 1,2-propylene glycol can be separated out through simple distillation as a bulk raw material. When the molar ratio of the propylene oxide to the carbon dioxide to the methanol to the other alcohols is 1:1:3:2, the reaction pressure is 5 MPa, the reaction temperatureis 100 DEG C, and the space velocity is 5 hours<-1>, the catalyst is not deactivated and has good stability after being used for 5000 hours. The whole reaction process is clean, efficient and free ofpollution, and no waste is generated.

Description

technical field [0001] The invention relates to a method for synthesizing an asymmetric carbonate ester, in particular to a method for synthesizing an asymmetric carbonate ester from propylene oxide in one step and co-producing 1,2-propanediol. Background technique [0002] Methyl Ethyl Carbonate (MPC 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 ex...

Claims

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Application Information

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IPC IPC(8): C07C29/128C07C68/04B01J29/74C07C69/96C07C31/20
CPCB01J29/7415B01J2229/20C07C29/128C07C68/04C07C69/96C07C31/205Y02P20/141Y02P20/52
Inventor 石磊姚杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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