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Method for one-step synthesis of carbonic acid symmetric ester and co-production of 1,2-propanediol through propylene oxide

A technology of propylene oxide and propylene glycol is applied in the preparation of carbon dioxide or inorganic carbonate, the preparation of oxygenated compounds, chemical instruments and methods, etc. increase, etc.

Inactive Publication Date: 2018-09-28
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 for one-step synthesis of carbonic acid symmetric ester and co-production of 1,2-propanediol through propylene oxide
  • Method for one-step synthesis of carbonic acid symmetric ester and co-production of 1,2-propanediol through propylene oxide
  • Method for one-step synthesis of carbonic acid symmetric ester and co-production of 1,2-propanediol through 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=1:1:3, drop into each 1.2 kg of the neutral catalyst that above-mentioned preparation method obtains respectively, reaction solution 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]

[0103] 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. But when the basic catalyst 10%BaO-20%CaO / Al 2 o 3 When the reaction is catalyzed, the selectivity of propylene oxide is significantly higher than that of carb...

Embodiment 2

[0105] In a 50L slurry bed reactor, the reaction pressure is 10MPa, the reaction raw material propylene oxide: carbon dioxide: various alcohols = 1:1:3, put in 15%PdO-8%SrO 2 -3%Ga 2 o 3 / Zn-meso-Y catalyst 1.2kg, the total volume of the reaction solution 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 2.

[0106]

[0107] 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 selectivity 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 i...

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Abstract

The invention relates to a method for one-step synthesis of a carbonic acid symmetric ester and co-production of 1,2-propanediol through propylene oxide, and relates to a method for synthesizing a carbonic acid symmetric ester. According to the present invention, the method is used for one-step synthesis of carbonic acid symmetric esters through propylene oxide, carbon dioxide and various alcohols(ROH can be a linear alcohol, an isomeric alcohol, an aromatic alcohol, a phenol, a diol such as 1,2-propylene glycol and diethylene glycol, polyol and various alcohols), the crude products obtainedthrough the reaction contain only the carbonic acid symmetric ester and the 1,2-propanediol, the selectivity of the carbonic acid symmetric ester can be up to 95%, and the by-product 1,2-propanediol as the bulk material can be separated through simple distillation, such that the whole reaction process is clean, efficient and non-polluting, and does not produce any waste; and the catalyst is not deactivated for 5000 h at the reaction temperature of 100 DEG C under the reaction pressure of 5 MPa at the space velocity of 5 h<-1> according to the molar ratio of propylene oxide to carbon dioxide tovarious alcohols of 1:1:3 so as to achieve good stability.

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 in one step from propylene oxide 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 exce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/04C07C69/96C07C29/128C07C31/20C07C27/00B01J29/04B01J29/12
CPCB01J29/044B01J29/126B01J2229/16B01J2229/18B01J2229/37B01J2229/38C07C29/128C07C68/04C07C69/96C07C31/205Y02P20/141Y02P20/52
Inventor 石磊胡亚威
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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