CN112479883A - Production device for dimethyl carbonate by ester exchange method and use method thereof - Google Patents

Production device for dimethyl carbonate by ester exchange method and use method thereof Download PDF

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CN112479883A
CN112479883A CN202011484989.XA CN202011484989A CN112479883A CN 112479883 A CN112479883 A CN 112479883A CN 202011484989 A CN202011484989 A CN 202011484989A CN 112479883 A CN112479883 A CN 112479883A
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ester exchange
methanol
outlet
reactor
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吴剑华
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C68/00Preparation of esters of carbonic or haloformic acids
    • C07C68/06Preparation of esters of carbonic or haloformic acids from organic carbonates
    • C07C68/065Preparation of esters of carbonic or haloformic acids from organic carbonates from alkylene carbonates
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C68/00Preparation of esters of carbonic or haloformic acids
    • C07C68/08Purification; Separation; Stabilisation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The dimethyl carbonate production device by the ester exchange method is provided with two tubular ester exchange reactors which are used in series, and a product separation tower is arranged between the two ester exchange reactors; the invention provides a device for producing dimethyl carbonate, which is characterized in that fresh raw material propylene (ethylene) carbonate enters a 1 st ester exchange reactor, fresh raw material methanol enters a 2 nd ester exchange reactor, both the two ester exchange reactors have higher reaction driving force, the device provided by the invention does not pursue the primary conversion rate of the raw materials, the reaction effect far exceeding the equilibrium conversion rate can be obtained by using the total feed composition close to the theoretical molar ratio, unconverted propylene (ethylene) carbonate and methanol are recycled after separation, and the defects of overhigh energy consumption and complex operation control caused by excessive methanol adopted in the process of pursuing the conversion rate of propylene (ethylene) carbonate in the dimethyl carbonate production operation by the traditional reaction rectification column ester exchange method are overcome. The device provided by the invention has the advantages of high production efficiency, good product quality, easy control of the production process, low energy consumption and large operation flexibility.

Description

Production device for dimethyl carbonate by ester exchange method and use method thereof
Technical Field
The invention relates to a production device of chemical products and a using method thereof, in particular to a production device for producing dimethyl carbonate by a transesterification method and a using method thereof.
Background
Dimethyl Carbonate (DCM) is a basic organic chemical raw material, known as a green organic chemical for the 21 st century. The method for producing the dimethyl carbonate comprises a methanol phosgene method, a sodium methoxide phosgene method, a methanol oxidation hydroxylation method, a methanol and carbon monoxide electrochemical reaction method, a carbon dioxide and methanol supercritical synthesis method, a urea alcoholysis method, an ester exchange method and the like. Some of the above methods have been industrialized, and some are still under development and exploration.
Propylene carbonate or ethylene carbonate is synthesized by taking propylene oxide or ethylene oxide and carbon dioxide as raw materials under the action of a catalyst, and then the propylene carbonate or the ethylene carbonate and methanol are subjected to ester exchange reaction to obtain dimethyl carbonate and byproduct propylene glycol or ethylene glycol, which is the currently adopted industrial production method of more dimethyl carbonate in China. Compared with other production methods, the ester exchange method for producing the dimethyl carbonate uses cheap raw materials and has low toxicity, and the byproduct propylene glycol or ethylene glycol also has good application. The transesterification reaction of propylene carbonate or ethylene carbonate and methanol is a reversible reaction, the conventional production method is to carry out the reaction in a reaction rectifying tower, in order to pursue higher conversion rate of propylene carbonate or ethylene carbonate, a large amount of excessive methanol is adopted for operation, the excessive methanol has high recovery energy consumption, the production efficiency of the device is low, and the operation control is complex.
The development of a new ester exchange reaction device has important significance for carrying out technical promotion and innovation on the traditional ester exchange method dimethyl carbonate production process, reducing the energy consumption in the production process, further reducing the production cost, improving the product quality and facilitating the operation.
Disclosure of Invention
The invention adopts a two-stage tubular reactor to carry out ester exchange reaction, combines the characteristics of reversible reaction, reasonably sets the feeding positions and modes of raw materials of ethylene carbonate and methanol, strengthens the mixed mass transfer of materials to be reacted and forms a novel dimethyl carbonate production device.
The invention is realized by the following technical scheme:
an apparatus for producing dimethyl carbonate by ester exchange method, comprising:
the device comprises a 1 st ester exchange reactor, a product separation tower, a second ester exchange reactor, a methanol recovery tower, a pressurized separation tower, a normal pressure separation tower, a propylene glycol light component removal tower, a propylene glycol rectifying tower, an auxiliary raw material tank, a product tank, a middle tank, a condenser, a reboiler, a material conveying device, a device room connecting pipeline, a control and display instrument and accessories. The 1 st ester exchange reactor and the 2 nd ester exchange reactor are tubular reactors with or without jackets, and movable and static flow disturbing elements which play a role in mixing media are arranged or not arranged in the reaction tubes.
The 1 st ester exchange reactor is provided with a material propylene carbonate, circulating methanol, a catalyst inlet and a primary reaction material outlet; the product separation tower is provided with a primary reaction material inlet, a tower top normal pressure product outlet and a tower kettle material outlet; the 2 nd ester exchange reactor is provided with a methanol inlet, a material inlet from the tower bottom of the product separation tower and a secondary reaction material outlet; the methanol recovery tower is provided with a secondary reaction material inlet, a tower top methanol and azeotrope recovery outlet and a tower kettle material outlet; the pressurized separation tower is provided with a normal-pressure azeotropic material inlet, a tower top pressurized azeotrope outlet and a tower kettle dimethyl carbonate outlet; the atmospheric separation tower is provided with a pressurized azeotropic material inlet, a tower top atmospheric azeotrope outlet and a tower kettle circulating methanol outlet; the propylene glycol lightness-removing tower is provided with a material inlet, a tower top light component outlet and a tower kettle material outlet; the propylene glycol rectifying tower is provided with a material inlet, a propylene glycol outlet at the top of the tower, unconverted propylene carbonate at the bottom of the tower and a catalyst outlet.
A primary reaction material outlet of the 1 st ester exchange reactor is communicated with a primary reaction material inlet of the product separation tower through a pipeline; the normal pressure product outlet at the top of the product separation tower is communicated with the normal pressure azeotropic material inlet of the pressurized separation tower or the pressurized azeotrope inlet of the normal pressure separation tower through a pipeline, and the material outlet at the bottom of the product separation tower is communicated with the material inlet of the 2 nd ester exchange reactor through a pipeline; the second reaction material outlet of the 2 nd ester exchange reactor is communicated with the second reaction material inlet of the methanol recovery tower through a pipeline; the outlet of the methanol recovery tower for recovering methanol and azeotrope at the top is communicated with the pressurized azeotropic material inlet of the normal pressure separation tower or the primary reaction material inlet of the product separation tower or the normal pressure azeotrope inlet of the pressurized separation tower through a pipeline, and the material outlet of the methanol recovery tower kettle is communicated with the material inlet of the propylene glycol lightness-removing tower through a pipeline; the outlet of the pressurized azeotrope at the top of the pressurized separation tower is communicated with the inlet of the pressurized azeotrope of the normal pressure separation tower through a pipeline; an atmospheric azeotrope outlet at the top of the atmospheric separation tower is connected with an atmospheric azeotropic material inlet of the pressurized separation tower through a pipeline, and a circulating methanol outlet at the tower bottom of the atmospheric separation tower is communicated with a circulating methanol inlet of the first ester exchange reactor through a pipeline; the material outlet of the bottom of the propylene glycol lightness-removing tower is communicated with the material inlet of the propylene glycol rectifying tower through a pipeline, and the material outlet of the bottom of the propylene glycol rectifying tower is communicated with the material inlet of the 1 st ester exchange reactor through a pipeline.
A method for using a dimethyl carbonate production device by a transesterification method comprises the following steps:
a. methanol, circulating methanol, propylene carbonate and a catalyst enter a 1 st ester exchange reactor and flow while being mixed and react to generate dimethyl carbonate and propylene glycol;
b. feeding the primary reaction material of the 1 st ester exchange reactor into a product separation tower, and feeding the tower bottom material into the 2 nd ester exchange reactor;
c. the material containing propylene glycol and unconverted propylene carbonate at the tower bottom of the product separation tower and the raw material methanol flow while mixing in the 2 nd ester exchange reactor, and further generate dimethyl carbonate and propylene glycol while reacting;
d. taking out of a methanol removal recovery tower of a secondary reaction material of the 2 nd ester exchange reactor, separating dimethyl carbonate and methanol azeotrope and unconverted methanol from the tower top, and sending the dimethyl carbonate and methanol azeotrope and unconverted methanol to a normal pressure separation tower or a product separation tower or a pressurization separation tower;
e. feeding the normal pressure product separated from the top of the product separation tower and the normal pressure azeotrope separated from the top of the normal pressure separation tower into a pressure separation tower, and feeding the pressure azeotrope separated from the top of the pressure separation tower into the normal pressure separation tower; the normal pressure product separated from the top of the product separating tower enters a normal pressure separating tower;
f. pressurizing the tower bottom of the separation tower to obtain dimethyl carbonate, and circularly feeding the methanol at the tower bottom of the normal-pressure separation tower to the 1 st ester exchange reactor;
g. separating heavy components in a tower kettle of the methanol recovery tower into a propylene glycol lightness removing tower, separating water and residual methanol and dimethyl carbonate from the tower top of the propylene glycol lightness removing tower, and feeding materials in the tower kettle into a propylene glycol rectifying tower; the materials at the top of the propylene glycol lightness-removing tower are further separated, and the separated methanol and dimethyl carbonate are sent to a product separation tower or a normal pressure separation tower or a pressurized separation tower;
h. the propylene glycol is obtained at the top of the propylene glycol rectifying tower, the unconverted propylene carbonate and the catalyst at the bottom of the tower are sent to the 1 st ester exchange reactor, and the unconverted propylene carbonate and the catalyst at the bottom of the tower are respectively sent to the 1 st ester exchange reactor through separation.
A production device of dimethyl carbonate by a transesterification method and a use method thereof are provided, wherein a catalyst and methanol are premixed or the catalyst and propylene carbonate are premixed and then enter a 1 st ester exchange reactor, or a methanol, propylene carbonate and catalyst blending device is arranged before the first ester exchange reaction.
The device for producing the dimethyl carbonate by the ester exchange method comprises a 1 st ester exchange reactor, a 2 nd ester exchange reactor or a jet reactor, a pump type reactor, a stirring reactor, a circulating reactor, a tower type reactor, a reaction rectifying tower, a super-gravity reactor, a micro-channel reactor, an impinging stream reactor or a tubular reactor and different combinations of the reactors.
A ester exchange method dimethyl carbonate apparatus for producing and its operation method, said apparatus and operation method do not set up 2 ester exchange reactor, product knockout tower bottom material methanol removal recovery tower, the top of the tower retrieves methanol and residual dimethyl carbonate and goes to the atmospheric separation column or goes to the pressurized separation column; or the 2 nd ester exchange reactor and the methanol recovery tower are not arranged, the material at the bottom of the product separation tower enters a propylene glycol light component removal tower, water, methanol and residual dimethyl carbonate are separated from the top of the tower, and the material at the bottom of the tower enters a propylene glycol rectifying tower; the materials at the top of the propylene glycol lightness-removing tower are further separated, and the separated methanol and dimethyl carbonate are sent to a product separation tower or an atmospheric separation tower or a pressurized separation tower.
A device for producing dimethyl carbonate by a transesterification method and a using method thereof are suitable for producing dimethyl carbonate and byproduct ethylene glycol by using ethylene carbonate as a raw material to replace propylene carbonate.
The invention has the advantages and effects that:
1. compared with the traditional reaction rectification tower reactor, the tubular reactor with the built-in turbulence element is adopted for ester exchange reaction, the materials are fully mixed and contacted in the reactor, the interface is rapidly updated, and the reaction speed is high;
2. a product separation tower is arranged between two ester exchange reactors used in series, and a reaction product generated in the 1 st ester exchange reactor is removed in time, so that the reaction in the 2 nd ester exchange reactor can be effectively carried out in the positive direction;
3. adjusting the feeding molar ratio of propylene (ethylene) carbonate to methanol in the 1 st ester exchange reactor and the 2 nd ester exchange reactor, wherein fresh raw material propylene (ethylene) carbonate enters from the 1 st ester exchange reactor, fresh raw material methanol enters from the 2 nd ester exchange reactor, and both reactors have higher reaction driving force;
4. the design and operation guiding idea of the ester exchange reaction in the traditional reaction rectifying tower is to pursue that the primary conversion rate of the dimethyl carbonate is as high as possible. Because the transesterification process of propylene (ethylene) carbonate and methyl ester is a reversible reaction, the pursuit of higher propylene carbonate primary conversion rate can cause a large amount of excess methanol, and the feeding molar ratio of the methanol to the propylene (ethylene) carbonate is far higher than the theoretical molar ratio of the reaction process; the design and operation of the invention have the guiding ideas that the one-way conversion rate of the reaction raw materials is not pursued, the effect of far exceeding the equilibrium conversion rate is realized by adopting the feed composition close to the theoretical molar ratio of the reaction process, and the energy consumption is obviously reduced in the ester exchange reaction process with a large amount of excessive methanol in the traditional reaction rectifying tower;
5. the device provided by the invention does not pursue the primary conversion rate of the raw materials, unconverted raw materials of propylene (ethylene) carbonate and methanol circularly return to the first ester exchange reactor to participate in the reaction again, and the utilization rate of the raw materials is high;
6. the device provided by the invention has the advantages of high production efficiency, large production capacity, low energy consumption, good product quality, easy control of the production process and large operation flexibility.
Description of the drawings:
FIG. 1 is a schematic diagram of a production apparatus for performing an ester exchange reaction between propylene carbonate and methanol by using two tubular reactors connected in series.
The specific embodiment is as follows:
example 1
The production device of dimethyl carbonate by ester exchange method used in this embodiment includes a 1 st ester exchange reactor 1-1, a product separation tower 2-1, a second ester exchange reactor 1-2, a methanol recovery tower 2-2, a pressurized separation tower 3, an atmospheric separation tower 4, a propylene glycol light component removal tower 5, a propylene glycol rectification tower 6, an auxiliary raw material tank, a product tank, an intermediate tank, a condenser, a reboiler, a material conveying device, a device-to-device connecting pipeline, a control and display instrument and accessories. The 1 st ester exchange reactor 1-1 and the 2 nd ester exchange reactor 1-2 are tubular reactors with or without jackets, and movable and static flow disturbing elements which play a mixing role for media are arranged or not arranged in the reaction tubes.
The 1 st ester exchange reactor 1-1 is provided with a material propylene carbonate, circulating methanol, a catalyst inlet and a primary reaction material outlet; the product separation tower 2-1 is provided with a primary reaction material inlet, a tower top normal pressure product outlet and a tower kettle material outlet; the 2 nd ester exchange reactor 1-2 is provided with a methanol inlet, a material inlet from the bottom of the product separation tower 2-1 and a secondary reaction material outlet; the methanol recovery tower 2-2 is provided with a secondary reaction material inlet, a tower top methanol recovery and azeotrope outlet and a tower kettle material outlet; the pressure separation tower 3 is provided with a normal pressure azeotropic material inlet, a tower top pressure azeotrope outlet and a tower kettle dimethyl carbonate outlet; the atmospheric separation tower 4 is provided with a pressurized azeotropic material inlet, a tower top atmospheric azeotrope outlet and a tower kettle circulating methanol outlet; the propylene glycol lightness-removing tower 5 is provided with a material inlet, a tower top light component outlet and a tower kettle material outlet; the propylene glycol rectifying tower 6 is provided with a material inlet, a propylene glycol outlet at the top of the tower, unconverted propylene carbonate at the bottom of the tower and a catalyst outlet.
A primary reaction material outlet of the 1 st ester exchange reactor 1-1 is communicated with a primary reaction material inlet of the product separation tower 2-1 through a pipeline; an atmospheric product outlet at the top of the product separation tower 2-1 is communicated with an atmospheric azeotropic material inlet of the pressurized separation tower 3 through a pipeline, and a tower bottom material outlet of the product separation tower 2-1 is communicated with a material inlet of the 2 nd ester exchange reactor 1-2 through a pipeline; the secondary reaction material outlet of the 2 nd ester exchange reactor 1-2 is communicated with the secondary reaction material inlet of the methanol recovery tower 2-2 through a pipeline; the outlet of the methanol recovery tower 2-2 for recovering methanol and azeotrope is communicated with the pressurized azeotropic material inlet of the atmospheric separation tower 4 through a pipeline, and the material outlet of the tower bottom of the methanol recovery tower 2-2 is communicated with the material inlet of the propylene glycol lightness-removing tower 5 through a pipeline; the outlet of the pressurized azeotrope at the tower top of the pressurized separation tower 3 is communicated with the inlet of the pressurized azeotrope of the normal pressure separation tower 4 through a pipeline; an atmospheric azeotrope outlet at the top of the atmospheric separation tower 4 is connected with an atmospheric azeotropic material inlet of the pressurized separation tower 3 through a pipeline, and a circulating methanol outlet at the bottom of the atmospheric separation tower 4 is communicated with a circulating methanol inlet of the first ester exchange reactor 1-1 through a pipeline; the material outlet of the tower bottom of the propylene glycol lightness-removing tower 5 is communicated with the material inlet of the propylene glycol rectifying tower 6 through a pipeline, and the material outlet of the tower bottom of the propylene glycol rectifying tower 6 is communicated with the material inlet of the 1 st ester exchange reactor 1-1 through a pipeline. The device of the embodiment is shown in figure 1.
The application method of the dimethyl carbonate production device by the ester exchange method provided by the embodiment comprises the following steps:
a. methanol, circulating methanol, propylene carbonate and a catalyst enter the 1 st ester exchange reactor 1 and flow while mixing and reacting to generate dimethyl carbonate and propylene glycol;
b. the primary reaction material of the 1 st ester exchange reactor 1-1 enters a product separation tower 2-1, and the tower bottom material enters the 2 nd ester exchange reactor 1-2;
c. the material containing propylene glycol and unconverted propylene carbonate at the bottom of the product separation tower 2-1 and the raw material methanol enter a 2 nd ester exchange reactor 1-2 to flow while being mixed, and the mixture reacts while further generating dimethyl carbonate and propylene glycol;
d. taking out the secondary reaction material methanol-removing recovery tower 2-2 of the second ester exchange reactor 1-2, separating dimethyl carbonate, methanol azeotrope and unconverted methanol from the tower top, and sending to a normal pressure separation tower 4;
e. the azeotropic mixture of the normal pressure dimethyl carbonate and the methanol separated from the top of the product separation tower 2-1 and the azeotropic mixture of the normal pressure dimethyl carbonate and the methanol separated from the top of the normal pressure separation tower 4 enter a pressure azeotropic tower 3, and the pressure azeotropic mixture separated from the top of the pressure azeotropic tower 3 enters a normal pressure separation tower 4;
f. pressurizing the tower bottom of the separation tower 3 to obtain dimethyl carbonate, and circularly feeding the methanol at the tower bottom of the normal pressure separation tower 4 to the 1 st ester exchange reactor 1-1;
g. separating heavy components in a tower bottom of the methanol recovery tower 2-2 into a propylene glycol lightness-removing tower 5, separating water and residual methanol and dimethyl carbonate from the tower top of the propylene glycol lightness-removing tower 5, and feeding materials in the tower bottom into a propylene glycol rectifying tower 6;
h. propylene glycol is obtained at the top of the propylene glycol rectifying tower 6, and the unconverted propylene carbonate and the catalyst at the bottom of the tower are sent to the 1 st ester exchange reactor 1-1.
Example 2
Example 2 is essentially the same as example 1 except that the 1 st transesterification reactor 1-1 and the 2 nd transesterification reactor 1-2 are commercially available static mixers.
Example 3
This example is substantially the same as example 1 except that the apparatus is not provided with the 2 nd ester exchange reactor 1-2, the bottom material of the product separation column 2-1 is sent to the methanol recovery column 2-2, and the top recovered methanol and the residual dimethyl carbonate are sent to the atmospheric separation column 4 or the unpressurized separation column 3.
Example 4
This example is substantially the same as example 1 except that the apparatus is not provided with a 2 nd ester exchange reactor 1-2 and a methanol recovery column 2-2, the bottom material of the product separation column 2-1 is sent to a propylene glycol lightness-removing column 5, water and residual methanol and residual dimethyl carbonate are separated from the top of the column, the bottom material of the column is sent to a propylene glycol rectification column 6, and the top separated material of the propylene glycol lightness-removing column 5 is further separated into methanol and dimethyl carbonate and sent to the product separation column 2-1.
Example 5
This example is substantially the same as example 1 except that the bottom material of the propylene glycol rectification column 6 is further separated, the unconverted propylene carbonate is sent to the 1 st transesterification reactor 1-1, and the catalyst is regenerated and sent to the 1 st transesterification reactor 1-1.
Example 6
This example is essentially the same as example 1 except that an atmospheric blend of dimethyl carbonate and methanol is separated overhead from product separation column 2-1 to pressure separation column 3.
Example 7
This example is substantially the same as example 1 except that the overhead separation from the propylene glycol lightness-removing column 5 is further separated into methanol and dimethyl carbonate, which are sent to the atmospheric separation column 4.

Claims (5)

1. A production device of dimethyl carbonate by a transesterification method is characterized by comprising:
the system comprises a 1 st ester exchange reactor (1-1), a product separation tower (2-1), a second ester exchange reactor (1-2), a methanol recovery tower (2-2), a pressure separation tower (3), an atmospheric separation tower (4), a propylene glycol lightness-removing tower (5), a propylene glycol rectifying tower (6), an auxiliary raw material tank, a product tank, an intermediate tank, a condenser, a reboiler, a material conveying device, a connecting pipeline between devices, a control and display instrument and accessories; the 1 st ester exchange reactor (1-1) and the 2 nd ester exchange reactor (1-2) are tubular reactors with or without jackets, and a dynamic and static flow disturbing element which has a mixing effect on a medium is arranged or not arranged in a reaction tube;
the 1 st ester exchange reactor (1-1) is provided with a material propylene carbonate, circulating methanol, a catalyst inlet and a primary reaction material outlet; the product separation tower (2-1) is provided with a primary reaction material inlet, a tower top normal pressure product outlet and a tower kettle material outlet; the 2 nd ester exchange reactor (1-2) is provided with a methanol inlet, a tower kettle material inlet from the product separation tower (2-1) and a secondary reaction material outlet; the methanol recovery tower (2-2) is provided with a secondary reaction material inlet, a tower top methanol and azeotrope outlet and a tower kettle material outlet; the pressure separation tower (3) is provided with a normal-pressure azeotropic material inlet, a tower top pressure azeotrope outlet and a tower kettle dimethyl carbonate outlet; the atmospheric separation tower (4) is provided with a pressurized azeotropic material inlet, a tower top atmospheric azeotrope outlet and a tower kettle circulating methanol outlet; the propylene glycol lightness-removing tower (5) is provided with a material inlet, a light component outlet at the top of the tower and a material outlet at the bottom of the tower; the propylene glycol rectifying tower (6) is provided with a material inlet, a propylene glycol outlet at the top of the tower, unconverted propylene carbonate at the bottom of the tower and a catalyst outlet;
the primary reaction material outlet of the 1 st ester exchange reactor (1-1) is communicated with the primary reaction material inlet of the product separation tower (2-1) through a pipeline; an atmospheric product outlet at the top of the product separation tower (2-1) is communicated with an atmospheric azeotropic material inlet of the pressurized separation tower (3) or a pressurized azeotrope inlet of the atmospheric separation tower (4) through a pipeline, and a tower kettle material outlet of the product separation tower (2-1) is communicated with a material inlet of the 2 nd ester exchange reactor (1-2) through a pipeline; the secondary reaction material outlet of the 2 nd ester exchange reactor (1-2) is communicated with the secondary reaction material inlet of the methanol recovery tower (2-2) through a pipeline; the outlet of the methanol recovery tower (2-2) for recovering methanol and azeotrope at the top of the tower is communicated with the pressurized azeotropic material inlet of the normal pressure separation tower (4) or the primary reaction material inlet of the product separation tower (2-1) or the normal pressure azeotrope inlet of the pressurized separation tower (3) through a pipeline, and the material outlet of the methanol recovery tower (2-2) at the bottom of the tower is communicated with the material inlet of the propylene glycol lightness-removing tower (5) through a pipeline; the outlet of the pressurized azeotrope at the tower top of the pressurized separation tower (3) is communicated with the inlet of the pressurized azeotrope of the normal pressure separation tower (4) through a pipeline; an atmospheric azeotrope outlet at the top of the atmospheric separation tower (4) is connected with an atmospheric azeotropic material inlet of the pressurized separation tower (3) through a pipeline, and a circulating methanol outlet at the tower bottom of the atmospheric separation tower (4) is communicated with a circulating methanol inlet of the first ester exchange reactor (1-1) through a pipeline; the material outlet of the bottom of the propylene glycol lightness-removing tower (5) is communicated with the material inlet of the propylene glycol rectifying tower (6) through a pipeline, and the material outlet of the bottom of the propylene glycol rectifying tower (6) is communicated with the material inlet of the 1 st ester exchange reactor (1-1) through a pipeline.
2. The use method of the apparatus for producing dimethyl carbonate by ester exchange method according to claim 1, wherein the method comprises:
a. methanol, circulating methanol, propylene carbonate and a catalyst enter a 1 st ester exchange reactor (1) and flow while mixing and reacting to generate dimethyl carbonate and propylene glycol;
b. the first reaction material of the 1 st ester exchange reactor (1-1) enters a product separation tower (2-1), and the tower bottom material enters the 2 nd ester exchange reactor (1-2);
c. the material containing propylene glycol and unconverted propylene carbonate at the bottom of the product separation tower (2-1) and the raw material methanol flow in the 2 nd ester exchange reactor (1-2) while mixing, and further generate dimethyl carbonate and propylene glycol while reacting;
d. a methanol removal recovery tower (2-2) for secondary reaction materials of the second ester exchange reactor (1-2) is taken out, azeotrope of dimethyl carbonate and methanol and unconverted methanol separated from the tower top are sent to a normal pressure separation tower (4), a product separation tower (2-1) or a pressurization separation tower (3);
e. the normal pressure product separated from the top of the product separation tower (2-1) and the normal pressure azeotrope separated from the top of the normal pressure separation tower (4) enter a pressure separation tower (3), and the pressure azeotrope separated from the top of the pressure separation tower (3) enters the normal pressure separation tower (4); the normal pressure product separated from the top of the product separation tower (2-1) enters a normal pressure separation tower (4);
f. pressurizing the tower bottom of the separation tower (3) to obtain dimethyl carbonate, and circularly feeding the methanol at the tower bottom of the normal-pressure separation tower (4) to the 1 st ester exchange reactor (1-1);
g. separating heavy components in the tower bottom of the methanol recovery tower (2-2) into a propylene glycol lightness-removing tower (5), separating water and residual methanol and dimethyl carbonate from the tower top of the propylene glycol lightness-removing tower (5), and feeding materials in the tower bottom into a propylene glycol rectifying tower (6); materials at the top of the propylene glycol lightness-removing tower (5) are further separated, and the separated methanol and dimethyl carbonate are sent to a product separation tower (2-1), an atmospheric separation tower (4) or a pressurized separation tower (3);
h. propylene glycol is obtained at the top of the propylene glycol rectifying tower (6), the unconverted propylene carbonate and the catalyst at the bottom of the tower are sent to the 1 st ester exchange reactor (1-1), and the unconverted propylene carbonate and the catalyst at the bottom of the tower are respectively sent to the 1 st ester exchange reactor after separation.
3. The use method of the production device of dimethyl carbonate by ester exchange method according to claim 2, characterized in that the catalyst is premixed with methanol or premixed with propylene carbonate and then enters the 1 st ester exchange reactor (1-1), or a methanol, propylene carbonate and catalyst blending device is arranged before the first ester exchange reaction.
4. The apparatus for producing dimethyl carbonate by ester exchange method according to claim 1, wherein the 1 st ester exchange reactor (1-1), the 2 nd ester exchange reactor (1-2) or the jet reactor, the pump reactor, the stirring reactor, the circulating reactor, the tower reactor, the reactive distillation column, the supergravity reactor, the microchannel reactor, the impinging stream reactor, or the tubular reactor and different combinations of the aforementioned reactors.
5. The apparatus for producing dimethyl carbonate by ester exchange method according to claim 1, wherein the apparatus is adapted to produce dimethyl carbonate and ethylene glycol as a byproduct by using ethylene carbonate as a raw material instead of propylene carbonate.
CN202011484989.XA 2020-12-16 2020-12-16 Production device for dimethyl carbonate by ester exchange method and use method thereof Pending CN112479883A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113731320A (en) * 2021-09-30 2021-12-03 沈阳工业大学 Dimethyl carbonate production device and method based on resource utilization
CN114159816A (en) * 2021-12-03 2022-03-11 铜陵金泰化工股份有限公司 Processing device and process for preparing dimethyl carbonate and co-producing propylene glycol

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113731320A (en) * 2021-09-30 2021-12-03 沈阳工业大学 Dimethyl carbonate production device and method based on resource utilization
CN113731320B (en) * 2021-09-30 2023-11-21 沈阳工业大学 Dimethyl carbonate production device and method based on resource utilization
CN114159816A (en) * 2021-12-03 2022-03-11 铜陵金泰化工股份有限公司 Processing device and process for preparing dimethyl carbonate and co-producing propylene glycol

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