Production process of high-purity diethyl carbonate through direct catalysis of solid base catalyst

A solid base catalyst, the technology of diethyl carbonate, applied in the purification/separation of carbonate/haloformate, the preparation of organic carbonate, the production of bulk chemicals, etc., can solve the waste of raw materials, low solubility, Problems such as poor catalyst stability, to achieve the effects of high product selectivity and yield, simple process flow, and short synthesis path

Inactive Publication Date: 2019-02-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the homogeneous catalyst has little solubility in alcohol, and excessive concentration will cause precipitation and fouling of the catalyst, and even react with carbonate to form carbonate with poor solubility and reduce the conversion rate of ethylene carbonate , resulting in a waste of raw materials, so the catalyst has the disadvantages of poor stability and difficulty in recycling
[0031] There are a large number of reports on transesterification in China, such as the transesterification of dimethyl carbonate and ethanol to prepare diethyl carbonate, but the transesterification of dimethyl carbonate and ethanol is a reversible reaction in parallel series, which has serious selectivity problems. A large part of dimethyl carbonate is converted to ethyl methyl carbonate, thus wasting raw materials and energy
At the same time, the co-production is methanol, which is currently oversupplied in the market, and is not economically competitive.
And the report that prepares diethyl carbonate with ethylene carbonate (or propylene carbonate) and ethanol transesterification is seldom

Method used

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  • Production process of high-purity diethyl carbonate through direct catalysis of solid base catalyst
  • Production process of high-purity diethyl carbonate through direct catalysis of solid base catalyst
  • Production process of high-purity diethyl carbonate through direct catalysis of solid base catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Ethylene carbonate and excess ethanol are used as raw materials to react to produce diethyl carbonate and ethylene glycol at a ratio of 1:1, and the distilled ethanol is recycled.

[0074] The catalyst is an alkaline composite material 15%BaO-5%MgO-3%La 2 o 3 / Cs-meso-EMT, the cross-sectional area ratio of the initial distillation section and the side line section is 1:1.

[0075] The operating conditions of T1 and T2 towers are as follows:

[0076] The first reactive distillation column T1: column diameter 1000mm; column height 19000mm; the number of plates in the public rectification section, initial distillation section, side line section, and public stripping section are 10, 20, 30, 15 respectively; the internal pressure of the column is 0.5 MPa; tower top temperature 130°C; tower bottom temperature of common stripping section 190°C; tower bottom temperature of side line section 170°C.

[0077] Atmospheric distillation column T2: column diameter 4000mm; column he...

Embodiment 2

[0080] The operating conditions of T3 and T4 towers are as follows:

[0081] Vacuum distillation tower T3: tower diameter 3000mm; tower height 40000mm; the number of plates 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 0.1 MPa The temperature at the top of the tower is 90°C, and the temperature at the bottom of the common stripping section is 160°C; the temperature at the bottom of the side line section is 120°C.

[0082] Vacuum distillation tower T4: tower diameter 3000mm; tower height 40000mm; the number of plates 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 0.1 MPa ; The temperature at the top of the tower is 165°C, and the temperature at the bottom of the common stripping section is 180°C; the temperature at...

Embodiment 3

[0085] The 95% ethanol obtained from the top of the T2 atmospheric distillation tower is dewatered by a 13X molecular sieve dewatering device to obtain 99.99% ethanol and returned to the bottom of the T1 tower to continue the rectification reaction.

[0086] 95% ethanol is pumped into the molecular sieve water removal device at a certain speed to obtain 99.99% ethanol. Use a vacuum pump to pump a large amount of water and a small amount of ethanol above the molecular sieve into the vacuum distillation tower. A large amount of water can be obtained at the bottom of the tower, and 95% ethanol can be obtained at the top of the tower. % ethanol, which is pumped into the molecular sieve water removal device for recycling.

[0087] Diagram of molecular sieve water removal device figure 2 Shown:

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Abstract

The invention discloses a production process of high-purity diethyl carbonate through direct catalysis of a solid base catalyst and relates to a production process of chemical raw materials. The process disclosed by the invention comprises the following steps: performing atmospheric distillation on tower top liquid to obtain a high-purity diethyl carbonate solution by virtue of simple distillation, performing reduced pressure separation on tower bottoms to obtain lots of ethylene glycol, a tiny amount of diethyl carbonate and a small amount of ethylene carbonate, and directly taking the ethanol and ethylene carbonate as raw materials to circulate to a first reactive distillation column. A process route for synthesizing ethylene carbonate by taking ethylene carbonate and ethanol as raw materials is created. A technology of directly catalyzing the ethylene carbonate and ethanol to be simply separated in a catalytic distillation column by virtue of a multifunctional composite basic material is realized. The one-step production process for synthesizing diethyl carbonate is short in synthetic route, simple in process flow and high in product selectivity and yield, and is capable of effectively producing diethyl carbonate compared with the conventional process.

Description

technical field [0001] A chemical raw material production process relates to a production process in which a solid base catalyst directly catalyzes high-purity diethyl carbonate. Background technique [0002] Diethyl Carbonate (DEC for short) contains alkoxy and carbonyl groups in its molecule. It has active chemical properties and can react with a variety of alcohols, phenols, amines and esters. It is an important organic synthesis intermediate with excellent performance. It is widely used in pharmaceutical, pesticide and fiber industries. In addition, DEC is also an excellent gasoline additive and has a good market prospect. [0003] In terms of solvent, diethyl carbonate is used in electron tube cathode fixing paint and also used as surfactant; it is used in the synthesis of pyrethrins in pesticides; it is used as a solvent for plasticizers or directly as plasticizers in plastic processing; It is used to prepare electrolyte in capacitor battery and lithium battery indust...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06C07C68/08C07C31/20C07C29/128C07C29/80
CPCC07C29/1285C07C29/80C07C68/065C07C68/08C07C69/96C07C31/202Y02P20/10Y02P20/52
Inventor 石磊邓文杰许光文
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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