CN210314061U - Rectification and purification device for synthesizing dimethyl oxalate by carbonylation of coal-made ethylene glycol - Google Patents

Rectification and purification device for synthesizing dimethyl oxalate by carbonylation of coal-made ethylene glycol Download PDF

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CN210314061U
CN210314061U CN201920666668.8U CN201920666668U CN210314061U CN 210314061 U CN210314061 U CN 210314061U CN 201920666668 U CN201920666668 U CN 201920666668U CN 210314061 U CN210314061 U CN 210314061U
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tower
vacuum
communicated
dimethyl oxalate
rectifying tower
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张超奇
桑良玉
田旭
安东亮
李金金
李俊杰
王昕昕
陈帅
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Anyang Yongjin Chemical Co ltd
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Anyang Yongjin Chemical Co ltd
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Abstract

The utility model relates to a can improve dimethyl oxalate product purity, reduce the energy consumption and practice thrift manufacturing cost's synthetic dimethyl oxalate rectification purification device of coal system ethylene glycol carbonylation, including dimethyl oxalate feeding heat exchanger, the vacuum rectification tower of putting through with dimethyl oxalate feeding heat exchanger, be equipped with the reboiler at the bottom of the tower cauldron, the overhead condenser communicates with each other with the vacuum rectification tower top through the evaporation vapor outlet, the overhead condenser communicates with reflux drum and tail cooler respectively, the reflux drum communicates with the backwash pump, the backwash pump communicates with each other with vacuum rectification tower top and overhead extraction flow control valve; the bottom of the rectifying tower is communicated with a heavy component discharge pump, and the heavy component discharge pump is communicated with a discharge hole of the tower kettle through a dimethyl oxalate feeding heat exchanger through a pipeline and a tower kettle liquid level regulating valve; a backflow flow regulating valve is arranged on an outlet pipeline of the backflow pump; the vacuum operation reduces the boiling point of each component, reduces the consumption of medium-pressure steam, reduces the cost, continuously extracts the components in the tower kettle and the light components at the tower top, realizes the effective recycling of heat and materials, and has no discharged materials.

Description

Rectification and purification device for synthesizing dimethyl oxalate by carbonylation of coal-made ethylene glycol
Technical Field
The utility model belongs to coal system ethylene glycol chemical industry field especially relates to a can improve dimethyl oxalate product purity, reduces the energy consumption and practices thrift manufacturing cost's coal system ethylene glycol carbonylation synthesis dimethyl oxalate rectification purification device.
Background
Ethylene glycol is an important chemical raw material and is mainly used as a solvent, an antifreezing agent, a raw material for synthesizing polyester resin and the like. At present, ethylene glycol is mainly prepared by a direct hydration method of ethylene oxide. Since ethylene is used as a raw material for the production of ethylene oxide, the mass production mainly depends on petroleum resources. The total energy characteristics of China are rich in coal, gas and little in oil, so that coal is efficiently converted into chemical raw materials such as ethylene glycol, dependence of the chemical raw materials on petroleum resources is reduced, the optimization of energy and resource structures is facilitated, and the method has important significance.
In recent years, with the gradual maturity of the technology for preparing ethylene glycol from coal, a large number of enterprises for preparing ethylene glycol from coal are built domestically. According to reliable statistics, the capacity of producing ethylene glycol by coal in China can reach more than 800 ten thousand tons in the coming years. Dimethyl oxalate is an intermediate product in the production process of ethylene glycol prepared from coal and is prepared by carbonylation synthesis reaction, a carbonylation synthesis device has complex reaction, the main target product is dimethyl oxalate, a series of side reactions are also included, the products comprise dimethyl carbonate, methyl formate, methyl acetate and the like, and the products have high resistance of a catalyst bed layer and short service life and the like due to the fact that impurity components are various and complex and cause great negative influence on a subsequent hydrogenation process catalyst. The prior treatment device basically adopts a conventional normal-pressure rectification device, a pressure rectification device or an extraction rectification device, has the defects of low product purity, high energy consumption and the like, adopts a vacuum rectification device, not only can obtain a high-purity dimethyl oxalate product, but also reduces the energy consumption of the device and saves the production cost of the device.
Disclosure of Invention
The utility model aims to solve the problem of low purity of the target product dimethyl oxalate caused by the carbonylation synthesis side reaction in the production process of the coal-based ethylene glycol in the prior art, and provides a rectification and purification device for synthesizing dimethyl oxalate through carbonylation of coal-based ethylene glycol, which reduces consumption, purifies and prolongs the effective service life of a hydrogenation catalyst.
In order to achieve the above purpose, the present invention adopts the following technical solutions:
a rectification and purification device for synthesizing dimethyl oxalate through carbonylation of coal-made glycol comprises a dimethyl oxalate feeding heat exchanger and a vacuum rectifying tower communicated with the dimethyl oxalate feeding heat exchanger, wherein a reboiler is arranged at the bottom of a tower kettle of the vacuum rectifying tower, a liquid phase inlet of the reboiler is communicated with the bottom of the vacuum rectifying tower, and a liquid phase outlet of the reboiler is communicated with the upper part of the bottom of the vacuum rectifying tower; the top of the vacuum rectifying tower is provided with an evaporation vapor outlet for providing rising steam for the vacuum rectifying tower, a tower top condenser is communicated with the top of the vacuum rectifying tower through the evaporation vapor outlet, the tower top condenser is communicated with a reflux tank and a tail cooler through pipelines respectively, the reflux tank and the tail cooler are communicated with each other, condensate falls back to the reflux tank by using gravity, noncondensable gas is pumped out through the tail cooler through vacuum equipment, the reflux tank is communicated with a reflux pump, the reflux pump is communicated with the top of the vacuum rectifying tower through a pipeline, and is communicated with a tower top extraction flow regulating valve through a pipeline; the pressure of the rectifying device is adjusted by a vacuum degree adjusting valve communicated with vacuum equipment; a part of the liquid phase of the reflux tank returns to the top of the vacuum rectifying tower through a reflux pump, and the other part of the liquid phase is communicated with a liquid level adjusting and extracting device through an extracting flow adjusting valve at the top of the tower; a heavy component discharging pump is communicated with the bottom of a rectifying tower of the vacuum rectifying tower through a pipeline, and the heavy component discharging pump is communicated with a discharging port of a tower kettle through a pipeline and a tower kettle liquid level regulating valve through a dimethyl oxalate feeding heat exchanger; a backflow flow regulating valve is arranged on an outlet pipeline of the backflow pump; the inlet pipeline of the vacuum equipment is provided with a vacuum degree regulating valve, and the pressure stability of the rectifying tower is controlled by regulating the air inlet amount of the vacuum equipment.
The vacuum rectifying tower is a main device, and a tower tray and a packing layer are arranged in the vacuum rectifying tower.
The technical scheme of the utility model the positive effect that produces as follows: the utility model discloses a rectification and purification device for synthesizing dimethyl oxalate through carbonylation of coal-made ethylene glycol, which adopts a vacuum rectification device to remove light component impurities in dimethyl oxalate mixed liquid to obtain a high-purity dimethyl oxalate intermediate product; meanwhile, the boiling point of each component is reduced by vacuum operation, the medium-pressure steam consumption is reduced, the production cost is reduced, and the market competitiveness is improved; the components at the bottom of the tower and the light components at the top of the tower are continuously extracted, and the effective recycling of heat and materials is realized without discharging materials.
The utility model discloses a dimethyl oxalate rectification purification device runs through practice, has greatly solved the problem that dimethyl oxalate purity is low, harmful impurity is many in the coal system ethylene glycol production process, has very big benefit to the effective life who prolongs hydrogenation catalyst; meanwhile, taking a device for producing 20 ten thousand tons of ethylene glycol per year as an example, the consumption of medium pressure steam is reduced by 8 tons/h, the unit price of the steam is 160 yuan/ton, the annual operation period is 8000 hours, and the steam cost can be saved by 1024 ten thousand yuan per year.
Drawings
FIG. 1 is a schematic view of the connection structure of a rectification and purification apparatus for the carbonylation synthesis of dimethyl oxalate from ethylene glycol by using coal of the present invention.
The labels in the figures are: 1. dimethyl oxalate feeding heat exchanger; 2. a vacuum rectification column; 3. a reboiler; 4. a tower top condenser; 5. a tail cooler; 6. a reflux tank; 7. a reflux pump; 8. a kettle liquid discharging pump; 9. a liquid level regulating valve of the tower kettle; 10. a reflux flow regulating valve; 11. a flow regulating valve is extracted from the tower top; 12. and a vacuum degree adjusting valve.
Detailed Description
The present invention will be further illustrated and described with reference to the following specific embodiments and the accompanying drawings.
As shown in fig. 1, a rectification and purification device for synthesizing dimethyl oxalate by carbonylation of coal-made ethylene glycol comprises a dimethyl oxalate feeding heat exchanger 1 and a vacuum rectifying tower 2 communicated with the dimethyl oxalate feeding heat exchanger 1, wherein the bottom of a tower kettle of the vacuum rectifying tower 2 is provided with a reboiler 3, a liquid phase inlet of the reboiler 3 is communicated with the bottom of the vacuum rectifying tower 2, and a liquid phase outlet of the reboiler 3 is communicated with the upper part of the bottom of the vacuum rectifying tower 2; an evaporation vapor outlet for providing rising vapor for the vacuum rectifying tower is formed in the top of the vacuum rectifying tower 2, a tower top condenser 4 is communicated with the top of the vacuum rectifying tower 2 through the evaporation vapor outlet, the tower top condenser 4 is communicated with a reflux tank 6 and a tail gas cooler 5 through pipelines respectively, the reflux tank 6 and the tail gas cooler 5 are communicated with each other, condensate falls back to the reflux tank 6 by utilizing gravity, noncondensable gas is pumped out through the tail gas cooler 5 through vacuum equipment, the reflux tank 6 is communicated with a reflux pump 7, the reflux pump 7 is communicated with the top of the vacuum rectifying tower 2 through a pipeline, and is communicated with a flow regulating valve 11 at the top of a recovery tower through a pipeline; the pressure of the rectifying device is adjusted by a vacuum degree adjusting valve 12 communicated with vacuum equipment; a part of the liquid phase of the reflux tank 6 returns to the top of the vacuum rectifying tower 2 through a reflux pump 7, and the other part of the liquid phase is communicated with a liquid level adjusting and extracting device through an extracted flow adjusting valve 11 at the top of the tower; a heavy component discharging pump 8 is communicated with the bottom of a rectifying tower of the vacuum rectifying tower 2 through a pipeline, the heavy component discharging pump 8 is communicated with a discharging port of a tower kettle through a dimethyl oxalate feeding heat exchanger 1 through a pipeline and a tower kettle liquid level regulating valve 9, the dimethyl oxalate feeding heat exchanger 1 adopts a rectifying heat coupling principle to exchange heat between a low-temperature feeding dimethyl oxalate liquid phase and a high-temperature pure dimethyl oxalate discharging port of the tower kettle, so that the feeding temperature is increased, and the discharging temperature is reduced; a reflux flow regulating valve 10 is arranged on an outlet pipeline of the reflux pump 7 and used for regulating the reflux ratio of the rectification operation and stabilizing the operation temperature and the product quality at the top of the tower, and a produced flow regulating valve 11 arranged at the top of the tower controls the liquid level stability of the reflux tank by regulating the produced quantity; the inlet pipeline of the vacuum equipment is provided with a vacuum degree regulating valve 12, and the pressure stability of the rectifying tower is controlled by regulating the air inlet quantity of the vacuum equipment.
The heat source of the reboiler adopts medium-pressure steam for heating to provide rising steam required by rectification, and the stability and constancy of the rectifying tower kettle are controlled by adjusting the steam addition amount according to the processing load.
The dimethyl oxalate feeding heat exchanger does not additionally increase heat supply, and adopts feeding and discharging of the vacuum rectifying tower for heat exchange.
The vacuum device is provided with vacuum equipment, and vacuum suction is utilized to maintain a certain vacuum degree in the rectifying tower and the reflux tank, so that the boiling point of each component is reduced, and the steam investment of the reboiler is saved.
The reflux device is one of the necessary conditions for the rectification process, light components are cooled by a condenser and a tail gas cooler, condensate reaches a certain temperature and is recycled to a reflux tank, part of condensate is used as reflux of a rectification tower to realize mass transfer and heat transfer processes, and the other part of condensate is taken as a tower top product and is returned to a device before synthesis for reuse.
The vacuum rectifying tower is a main device, a tower tray and a packing layer are arranged in the vacuum rectifying tower, ascending steam and descending liquid generate mass transfer and heat transfer processes for many times under the condition of certain vacuum degree, the purification of a dimethyl oxalate product is realized, and a refined product passes through a kettle liquid pump extraction device.
A rectification and purification device for coal-made ethylene glycol carbonylation synthetic product dimethyl oxalate comprises a vacuum rectifying tower 2, a dimethyl oxalate feeding heat exchanger 1, a vacuum device, an evaporation device and a condensation reflux device, wherein the dimethyl oxalate feeding preheating mainly aims at improving the feeding temperature and reducing the steam consumption; the vacuum device utilizes vacuum equipment to maintain a certain vacuum degree in the rectifying tower, reduces the boiling point of liquid phase components, reduces the operating temperature and reduces the steam consumption; the evaporation device is characterized in that a reboiler 3 is arranged at the bottom of the rectifying tower to provide rising steam for the top of the rectifying tower; the condensing reflux device is characterized in that a tower top condenser 4 and a tail gas cooler 5 are arranged at the tower top, steam rising from the tower top firstly passes through the tower top condenser 4 to condense part of gas phase materials into liquid phase and flows into a reflux tank 6, the uncondensed part of gas phase passes through the tail gas cooler 5, condensate liquid falls back into the reflux tank 6, and noncondensable gas is treated by vacuum equipment. The main working principle is as follows: dimethyl oxalate feeding is preheated by a dimethyl oxalate feeding heat exchanger 1 and enters a vacuum rectifying tower 2, a liquid phase is heated by a reboiler 3 and then evaporated into ascending steam to exchange heat with reflux liquid jetted from the top of the tower, a light component gas phase is cooled by a condenser from the top of the tower, a condensate liquid falls back to a reflux tank 6, an uncondensed light component gas phase is cooled by a tail gas cooler 5, a condensate liquid phase falls back to the reflux tank 6, uncondensed gas is extracted by vacuum equipment, the vacuum degree of the rectifying tower is controlled by the vacuum equipment, a part of the condensate liquid in the reflux tank 6 returns to the top of the tower through a reflux pump to serve as reflux, a part of the condensate liquid is extracted from a rectifying device, and refined dimethyl oxalate extracted from a tower bottom is pumped to a product storage tank through a kettle liquid pump to be.
The dimethyl oxalate feeding heat exchanger does not additionally increase heat supply, adopts feeding and vacuum rectifying tower discharging to exchange heat, achieves the purposes of improving feeding temperature, reducing steam input and reducing discharging temperature, and saves production cost.
The vacuum device is provided with vacuum equipment, and vacuum suction is utilized to maintain a certain vacuum degree in the rectifying tower and the reflux tank, so that the boiling point of each component is reduced, and the steam investment of the reboiler is saved.
The evaporation device is characterized in that a reboiler is arranged at the bottom of the vacuum rectification tower, and rising steam required by rectification is provided by heating medium-pressure steam.
The reflux device is one of the necessary conditions for the rectification process, light components are cooled by a condenser and a tail gas cooler, condensate reaches a certain temperature and is recycled to a reflux tank, part of condensate is used as reflux of a rectification tower to realize mass transfer and heat transfer processes, and the other part of condensate is taken as a tower top product and is returned to a device before synthesis for reuse.
The vacuum rectifying tower is a main device, a tower tray and a packing layer are arranged in the vacuum rectifying tower, ascending steam and descending liquid generate mass transfer and heat transfer processes for many times under the condition of certain vacuum degree, the purification of a dimethyl oxalate product is realized, and a refined product is extracted by a kettle liquid pump.
Embodiment 1 a device for rectifying and purifying dimethyl oxalate as a coal-based ethylene glycol carbonylation synthetic product, as shown in fig. 1, comprises a dimethyl oxalate feeding heat exchanger 1, a vacuum rectifying tower 2, a reboiler 3, a tower top condenser 4, a tail gas cooler 5, a reflux tank 6, a reflux pump 7, a heavy component discharging pump 8, a tower bottom liquid level regulating valve 9, a reflux flow regulating valve 10, a tower top extraction flow regulating valve 11 and a vacuum degree regulating valve 12.
The vacuum rectifying tower is one of main devices for rectifying operation, a tower kettle of the vacuum rectifying tower is provided with a reboiler, a liquid phase inlet of the reboiler is connected with the bottom of the rectifying tower, and an evaporation vapor outlet is connected with the upper part of the rectifying tower kettle to provide rising vapor for the rectifying tower; a discharge pump of the tower kettle is connected with the bottom of the rectifying tower, and the extraction flow is controlled by an outlet regulating valve; the feeding heat exchanger adopts a rectification heat coupling principle, namely, a low-temperature feeding dimethyl oxalate liquid phase exchanges heat with a tower kettle high-temperature pure dimethyl oxalate discharging material, the feeding temperature is increased, and the discharging temperature is reduced; a tower top condenser is connected with the top of a rectifying tower, steam of the rectifying tower exchanges heat with circulating water through the condenser, condensate falls to a reflux tank by using gravity, uncondensed gas phase exchanges heat with chilled water through a tail gas cooler, the condensate falls back to the reflux tank by using gravity, non-condensable gas is pumped out through vacuum equipment, and the pressure of a rectifying device is adjusted by the vacuum equipment; and a part of the liquid phase of the reflux tank returns to the top of the rectifying tower through a reflux pump, and a part of the liquid phase passes through a liquid level adjusting extraction device.
And a liquid level regulating valve is arranged on a pipeline behind the discharge pump of the rectifying tower kettle, and the liquid level of the rectifying tower kettle is controlled to be stable by adjusting the discharge amount. And a reflux pump outlet pipeline is provided with a reflux flow regulating valve for regulating the reflux ratio of rectification operation, stabilizing the operation temperature and the product quality at the top of the tower, and a light component extraction flow regulating valve at the top of the tower is arranged to control the liquid level stability of the reflux tank by adjusting the extraction amount. And a pressure regulating valve is arranged on an inlet pipeline of the vacuum equipment, and the pressure stability of the rectifying tower is controlled by regulating the air inlet amount of the vacuum equipment. The heat source of the reboiler adopts medium-pressure steam, and the stability and constancy of the rectifying tower kettle are controlled by adjusting the steam addition amount according to the treatment load.

Claims (3)

1. The utility model provides a coal system ethylene glycol carbonylation synthesizes dimethyl oxalate rectification purification device, includes dimethyl oxalate feeding heat exchanger (1), with vacuum rectifying column (2) that dimethyl oxalate feeding heat exchanger (1) was put through mutually, its characterized in that: a reboiler (3) is arranged at the bottom of the tower kettle of the vacuum rectifying tower (2), a liquid phase inlet of the reboiler (3) is communicated with the bottom of the vacuum rectifying tower (2), and a liquid phase outlet of the reboiler (3) is communicated with the upper part of the bottom of the vacuum rectifying tower (2); an evaporation vapor outlet for providing rising vapor for the vacuum rectifying tower is formed in the top of the vacuum rectifying tower (2), a tower top condenser (4) is communicated with the top of the vacuum rectifying tower (2) through the evaporation vapor outlet, the tower top condenser (4) is communicated with a reflux tank (6) and a tail gas cooler (5) through pipelines respectively, the reflux tank (6) and the tail gas cooler (5) are communicated with each other, condensate falls back to the reflux tank (6) by utilizing gravity, non-condensable gas is pumped out through the tail gas cooler (5) through vacuum equipment, the reflux tank (6) is communicated with a reflux pump (7), the reflux pump (7) is communicated with the top of the vacuum rectifying tower (2) through a pipeline, and is communicated with a tower top extraction flow regulating valve (11) through a pipeline simultaneously; the pressure of the rectification system is adjusted by a vacuum degree adjusting valve (12) communicated with vacuum equipment; a part of the liquid phase of the reflux tank (6) returns to the top of the vacuum rectifying tower (2) through a reflux pump (7), and the other part is communicated with a liquid level regulating and extracting system through an extracting flow regulating valve (11) at the top of the tower; a heavy component discharge pump (8) is communicated with the bottom of a rectifying tower of the vacuum rectifying tower (2) through a pipeline, and the heavy component discharge pump (8) is communicated with a discharge hole of the tower kettle through a dimethyl oxalate feeding heat exchanger (1) through a pipeline and a tower kettle liquid level regulating valve (9); a reflux flow regulating valve (10) is arranged on an outlet pipeline of the reflux pump (7); the inlet pipeline of the vacuum equipment is provided with a vacuum degree regulating valve (12).
2. The rectification and purification device for the oxo synthesis of dimethyl oxalate through coal glycol according to claim 1,
the method is characterized in that: the reboiler (3) adopts medium-pressure steam for heating to provide rising steam required by rectification, and the distillation tower kettle is controlled by adjusting the steam addition amount according to the treatment load.
3. The rectification and purification device for the oxo synthesis of dimethyl oxalate through coal glycol according to claim 1 is characterized in that: a tower tray and a packing layer are arranged inside the vacuum rectifying tower (2), and ascending steam and descending liquid generate mass transfer and heat transfer processes for multiple times, so that the purification of the dimethyl oxalate product is realized.
CN201920666668.8U 2019-05-10 2019-05-10 Rectification and purification device for synthesizing dimethyl oxalate by carbonylation of coal-made ethylene glycol Active CN210314061U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848349A (en) * 2020-07-01 2020-10-30 桐昆集团股份有限公司 Continuous refining plant of ethylene glycol

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848349A (en) * 2020-07-01 2020-10-30 桐昆集团股份有限公司 Continuous refining plant of ethylene glycol

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