CN110833701A - Device for purifying acetic acid in vinyl acetate production by ethylene method - Google Patents

Device for purifying acetic acid in vinyl acetate production by ethylene method Download PDF

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Publication number
CN110833701A
CN110833701A CN201911143665.7A CN201911143665A CN110833701A CN 110833701 A CN110833701 A CN 110833701A CN 201911143665 A CN201911143665 A CN 201911143665A CN 110833701 A CN110833701 A CN 110833701A
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China
Prior art keywords
acetic acid
rectifying tower
heat exchanger
outlet
tower
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CN201911143665.7A
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Chinese (zh)
Inventor
任国瑜
任佳乐
黄志伟
王宝强
王金玺
刘树繁
曹曈斌
宋紫薇
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Yulin University
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Yulin University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/43Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
    • 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

Abstract

A device for purifying acetic acid in vinyl acetate production by an ethylene method comprises an acetic acid rectifying tower top condenser, an acetic acid rectifying tower, a heat exchanger and a gas-liquid separation tank, wherein a top outlet of the acetic acid rectifying tower is connected with a top inlet of the heat exchanger through a compressor, a bottom outlet of the heat exchanger is connected with a bottom inlet of the acetic acid rectifying tower top condenser, and a top outlet of the acetic acid rectifying tower top condenser is connected with the acetic acid rectifying tower; the bottom outlet of the acetic acid rectifying tower is connected with the side wall inlet of the heat exchanger, the side wall outlet of the heat exchanger is connected with the inlet of the gas-liquid separation tank, and the top outlet of the gas-liquid separation tank is connected with the reflux inlet of the acetic acid rectifying tower. By arranging the heat exchanger, the heat transfer effect is improved, the energy consumption of the tower bottom reboiler is effectively reduced, and the energy utilization rate is improved. Through set up the dull and stereotyped internals of vortex in the heat exchanger, increased heat transfer efficiency, promoted the utilization ratio of energy.

Description

Device for purifying acetic acid in vinyl acetate production by ethylene method
Technical Field
The invention belongs to the technical field of separation of acetic acid and water, and relates to a device for purifying acetic acid in vinyl acetate production by an ethylene method.
Background
Vinyl acetate is an important organic chemical raw material, and with the continuous development of coal-to-olefin in China, the ethylene method for producing vinyl acetate gradually replaces the highly-polluted acetylene method. Vinyl acetate is widely used for producing a series of chemical products such as polyvinyl acetate, polyvinyl alcohol, coating, adhesive and the like, the demand of vinyl acetate is increased year by year along with the continuous development of downstream products, but the energy consumption for purifying and separating acetic acid in reaction liquid accounts for about 16 percent of the whole production, and how to effectively reduce the energy consumption for separating acetic acid is a problem which needs to be solved urgently in the production of vinyl acetate by an ethylene method in China.
Since vinegar/water is a typical non-ideal system, most of the current methods adopt constant boiling rectification, and the added azeotropic components must be distilled out from the top of the tower, condensed and recycled. And thus consumes more heat energy and electric energy.
Aiming at the existing problems, how to economically, energy-saving and efficiently realize the refining of the acetic acid and reduce the investment cost of equipment and materials becomes a key problem which is urgently needed to be solved in the current industrial production.
Disclosure of Invention
The invention aims to provide a device for purifying acetic acid in vinyl acetate production by an ethylene method, which has novel and reasonable design, the energy is recycled after the hot steam at the top of the tower is heated for the second time by a compressor and exchanges heat with the material flow at the bottom of the tower, and a discontinuous flow disturbing flat plate inner member is added into a heat exchanger. The heat transfer efficiency of the heat exchanger is increased, and the loss of energy consumption in the separation process is effectively reduced; the economic benefit of enterprises is improved.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
a device for purifying acetic acid in vinyl acetate production by an ethylene method comprises an acetic acid rectifying tower top condenser, an acetic acid rectifying tower, a heat exchanger and a gas-liquid separation tank, wherein a top outlet of the acetic acid rectifying tower is connected with a top inlet of the heat exchanger through a compressor, a bottom outlet of the heat exchanger is connected with a bottom inlet of the acetic acid rectifying tower top condenser, and a top outlet of the acetic acid rectifying tower top condenser is connected with the acetic acid rectifying tower;
the bottom outlet of the acetic acid rectifying tower is connected with the side wall inlet of the heat exchanger, the side wall outlet of the heat exchanger is connected with the inlet of the gas-liquid separation tank, and the top outlet of the gas-liquid separation tank is connected with the reflux inlet of the acetic acid rectifying tower.
The invention is further improved in that the heat exchanger is a tubular heat exchanger.
The invention has the further improvement that the heat exchanger comprises a cylinder body, and the two ends of the cylinder body are provided with end sockets; the total length of the heat exchanger is 5.5 meters, the total length of the cylinder is 4.4 meters, and the diameter of the cylinder is 0.5 meter.
The invention has the further improvement that the cylinder body of the heat exchanger comprises a shell pass and a tube pass, the bottom of the acetic acid rectifying tower is connected with the shell pass inlet of the heat exchanger, and the shell pass outlet of the heat exchanger is connected with the gas-liquid separator;
the inlet of a compressor at the top of the acetic acid rectifying tower is connected, the outlet of the compressor is connected with the tube pass inlet of the heat exchanger, and the tube pass outlet of the heat exchanger is connected with the condenser.
The invention is further improved in that a plurality of turbulence three-blade type inner components are arranged in the tube pass.
The invention is further improved in that the spoiler-type three-blade inner member comprises a sleeve, and 3 blades are uniformly arranged on the sleeve.
The invention has the further improvement that a support rod is arranged in the tube pass, a plurality of turbulence three-blade type internal components are sleeved on the support rod, and the turbulence three-blade type internal components can rotate under the impact action of fluid.
The invention is further improved in that auxiliary heat exchangers are arranged at the inlet and the outlet of the heat exchanger.
The invention has the further improvement that the bottom outlet of the acetic acid rectifying tower is connected with the side wall inlet of the heat exchanger through a discharging pump of the acetic acid rectifying tower kettle; the bottom outlet of the gas-liquid separation tank is connected with a pipeline, and a tower kettle outlet flow control valve is arranged on the pipeline; the bottom outlet of the heat exchanger is connected with a stop valve through the outlet of the heat exchanger and is connected with the bottom inlet of a condenser at the top of the acetic acid rectifying tower; the top outlet of the condenser at the top of the acetic acid rectifying tower is divided into two paths, one path is connected with the acetic acid rectifying tower through a flow control valve returned from the top outlet of the first acetic acid rectifying tower, and the other path is provided with a flow control valve at the top outlet of the second acetic acid rectifying tower.
The further improvement of the invention is that the acetic acid rectifying tower is a plate rectifying tower, and the total number of actual tower plates in the acetic acid rectifying tower is 30-42;
the total height of the plate type rectifying tower is 26 meters, the diameter of the tower is 1.2 meters, a sieve plate tower is arranged inside the plate type rectifying tower, the diameter of an inner hole of the tower is 12.7 millimeters, the width of a side wall downcomer inside the plate type rectifying tower is 0.78 meter, the height of an internal weir of the plate type rectifying tower is 70 millimeters, and the distance between tower plates is 0.8 meter; the acetic acid rectifying tower is internally provided with a high-temperature polytetrafluoroethylene lining.
Compared with the prior art, the invention has the following beneficial effects: by arranging the heat exchanger, the heat transfer effect is improved, the energy consumption of the tower bottom reboiler is effectively reduced, and the energy utilization rate is improved. Through set up the dull and stereotyped internals of vortex in the heat exchanger, increased heat transfer efficiency, promoted the utilization ratio of energy. The device can replace the traditional azeotropic distillation and is used for separating water in acetic acid, thereby obviously reducing energy loss and increasing the economic benefit of enterprise production.
Furthermore, the invention adopts a new rectification mode, and adopts a plate-type rectification tower, wherein the material flow extracted from the top of the rectification tower is compressed by a compressor and then heated, and exchanges heat with the material flow at the bottom of the rectification tower, so that the energy in the system is recycled, and the energy consumption of separation is reduced.
Drawings
FIG. 1 is a flow diagram of the rectification mode of the present invention.
FIG. 2 is a schematic diagram of the structure of a turbulent three-blade type internal component of the heat exchanger of the present invention.
FIG. 3 is a graph comparing the energy consumption of a conventional rectification and the apparatus of the present invention.
Fig. 4 is a schematic view of the internal structure of the heat exchanger of the present invention.
Fig. 5 is a comparison diagram of a three-blade type inner member heat exchanger and a common heat exchanger Nu.
FIG. 6 is a graph of pressure drop comparison of a three-blade type internals heat exchanger with a conventional heat exchanger.
In the figure: the device comprises a turbulent three-blade type inner component 1, a heat pump rectifying tower raw material pump 29, a boiler water regulating valve 30, a feed flow control valve 31, an acetic acid rectifying tower 32, a second acetic acid rectifying tower top outlet flow control valve 33, a first acetic acid rectifying tower top outlet reflux control valve 34, a compressor 35, a heat exchanger 36, a gas-liquid separation tank 37, a tower kettle outlet flow control valve 38, an acetic acid rectifying tower kettle discharge pump 39, a stop valve 40 and an acetic acid rectifying tower top condenser 41.
Detailed Description
The present invention will now be described in detail with reference to the drawings, which are provided for purposes of illustration and not limitation.
Referring to fig. 1, the invention is a device for purifying acetic acid in vinyl acetate production by ethylene method, comprising an acetic acid rectifying tower top condenser 41, an acetic acid rectifying tower 32, a heat exchanger 36 and a gas-liquid separation tank 37, wherein the top outlet of the acetic acid rectifying tower 32 is connected with the top inlet of the heat exchanger 36 through a compressor 35, and the bottom outlet of the heat exchanger 36 is connected with the bottom inlet of the acetic acid rectifying tower top condenser 41 through a heat exchanger outlet connection stop valve 40. The top outlet of the condenser 41 at the top of the acetic acid rectifying tower is divided into two paths, one path is connected with the acetic acid rectifying tower 32 through the flow control valve 34 at the top outlet of the first acetic acid rectifying tower, and the other path is provided with the flow control valve 33 at the top outlet of the second acetic acid rectifying tower.
The bottom outlet of the acetic acid rectifying tower 32 is connected with the side wall inlet of the heat exchanger 36 through an acetic acid rectifying tower kettle discharge pump 39, and the side wall outlet of the heat exchanger 36 is connected with the inlet of the gas-liquid separation tank 37. The top outlet of the gas-liquid separation tank 37 is connected with the reflux inlet of the acetic acid rectification tower 32, the bottom outlet of the gas-liquid separation tank 37 is connected with a pipeline, and the pipeline is provided with a tower kettle outlet flow control valve 38.
The hot steam material flow on the top of the tower is heated up through compression and exchanges heat with the material flow on the bottom of the tower, so that the energy utilization rate is improved.
Wherein, the acetic acid rectifying tower 32 is a plate rectifying tower, the total number of actual plates in the acetic acid rectifying tower 32 is 30-42, and the optimal number of plates is 35.
The total number of actual tower plates of the plate-type rectifying section of the plate-type rectifying tower is 22, and the total number of stripping sections is 13.
The total height of the plate rectifying tower is 26 meters, and the diameter of the tower is 1.2 meters.
The inside of the plate rectifying tower is a sieve plate tower, and the diameter of an inner hole of the tower is 12.7 mm.
The width of a side wall downcomer inside the plate rectifying tower is 0.78 m.
The height of the internal weir of the plate-type rectifying tower is 70 mm, and the distance between the tower plates is 0.8 m.
The acetic acid rectifying tower 32 is internally provided with a high-temperature polytetrafluoroethylene lining.
The heat exchanger 36 comprises a cylinder body, seal heads are arranged at two ends of the cylinder body, the total length of the heat exchanger 36 is 5.5 meters, the total length of the cylinder body is 4.4 meters, the total length of the seal heads at two ends is 1.1 meters, and the diameter of the cylinder body is 0.5 meter. The heat exchanger 36 is a tube heat exchanger. A cold-heat exchange system is arranged in the heat exchanger 36, the cold-heat exchange system comprises a cold-heat fluid input system and a heat exchange system, a cold fluid passes through a tube pass, and a hot fluid passes through a shell pass. Cold and hot fluid is subjected to countercurrent heat exchange, cold fluid is input from a connecting pipe at one side of the end socket, hot fluid is input from a connecting pipe at one side of the cylinder, and the cold and hot fluids are respectively output from corresponding sides after countercurrent heat exchange in the heat exchanger.
Air is input by the fan, and enters the inner pipe of the heat exchanger 36 after the flow is measured by the air flow meter, so as to exchange heat with the water vapor on the pipe pass. The vapor enters the shell side of the heat exchange tube from the outlet of the compressor 35, and the acetic acid at the bottom of the acetic acid rectifying tower 32 enters the tube side of the heat exchanger.
The heat exchanger 36 comprises a tube side and a shell side, the bottom of the acetic acid rectifying tower 32 is connected with a shell side inlet of the heat exchanger, a shell side outlet of the heat exchanger is connected with a gas-liquid separator 37, the top of the acetic acid rectifying tower 32 is connected with an inlet of a compressor 25, an outlet of the compressor 25 is connected with a tube side inlet of the heat exchanger 36, and a tube side outlet of the heat exchanger is connected with a condenser 41. The tube pass is acetic acid solution at the bottom of the tower, the shell pass is hot steam at the top of the tower, and a plurality of turbulence three-blade type inner components 1 are arranged in the tube pass. Referring to fig. 2, the spoiler-type inner member 1 includes a sleeve on which 3 blades are uniformly disposed. Specifically, a support rod is arranged in the tube pass, a plurality of turbulence three-blade type inner components 1 are sleeved on the support rod, and the turbulence three-blade type inner components 1 can rotate under the impact action of fluid. When all fluid in the tube pass flows, the fluid can drive the blades of the three-blade type inner component 1 to rotate at a high speed in the tube to disturb the fluid, particularly the heat transfer resistance on the side with smaller heat exchange coefficient of the inner wall of the tube is reduced, and the total heat transfer coefficient is greatly improved.
In the invention, the auxiliary heat exchangers are arranged at the inlet and the outlet of the heat exchanger 36, and the minimum energy consumption is achieved through dynamic adjustment so as to achieve the purpose of reducing energy consumption.
In the prior art, an acetic acid aqueous solution and an entrainer n-butyl acetate enter an azeotropic distillation tower, the n-butyl acetate and water enter a reflux tank from the top of the tower through condensation, the acetic acid with the purity of 99.8% is produced at the bottom of the tower and sent to a storage tank, the n-butyl acetate and the water are sent to an entrainer recovery tower through a pump, the entrainer n-butyl acetate is further separated from the top of the tower through conventional distillation, the n-butyl acetate is cooled and recycled, and the wastewater at the bottom of the tower is sent to a subsequent section for treatment.
In the traditional process of separating acetic acid from water, azeotropic distillation is adopted, and after an entrainer is added into the acetic acid and water, the entrainer is regenerated for recycling. The device provided by the invention is used for simulating the process, and then the Aspen plus (chemical process simulation) software is used for simulating. In the case of treating a mixture of acetic acid and water of the same composition and mass per unit time. The total energy consumption of the traditional separation of acetic acid and water is 57275.00 kW. The total energy consumption of the device is about 44166.67kW, compared with the traditional rectification, the energy utilization rate is improved, the device is changed from double towers to single tower, the equipment cost is saved, the energy consumption is reduced by about 22.8%, the economic benefit is improved, and the technical effect of the device is better.
Referring to fig. 4, 6 groups of three-blade spoiler type internals are added in the heat exchanger to collect experimental data of a normal heat exchanger, and two groups of experimental results are shown in fig. 5 and 6; the Knoop Seir number of the turbulent three-blade type inner component is 186, and the pressure drop of the heat exchanger is 2310 Pa; the Knoop quasi number of the common heat exchanger is 104, the pressure drop of the heat exchanger is 4364Pa, so that the heat transfer performance of the heat exchanger can be effectively improved by the self-rotating turbulent three-blade type inner member, and most importantly, the increase of the pressure drop of the heat exchanger is obviously reduced.
As can be seen from the combination of FIG. 3, FIG. 5 and FIG. 6, the apparatus of the present invention has the advantages of energy saving and equipment saving compared with the conventional rectification. And because the heat exchanger is adopted, the comprehensive performance of the heat exchanger is improved, the cost is saved, the heat exchange efficiency is improved, and the energy utilization rate is improved. And the comprehensive performance of the rectification is better than that of the traditional rectification, and the energy loss is saved while the separation efficiency is improved.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (10)

1. A device for purifying acetic acid in vinyl acetate production by an ethylene method is characterized by comprising a condenser (41) at the top of an acetic acid rectifying tower, the acetic acid rectifying tower (32), a heat exchanger (36) and a gas-liquid separation tank (37), wherein the outlet at the top of the acetic acid rectifying tower (32) is connected with the inlet at the top of the heat exchanger (36) through a compressor (35), the outlet at the bottom of the heat exchanger (36) is connected with the inlet at the bottom of the condenser (41) at the top of the acetic acid rectifying tower, and the outlet at the top of the condenser (41) at the top of the acetic acid rectifying tower is connected with the acetic acid rectifying tower (32);
the bottom outlet of the acetic acid rectifying tower (32) is connected with the side wall inlet of the heat exchanger (36), the side wall outlet of the heat exchanger (36) is connected with the inlet of the gas-liquid separation tank (37), and the top outlet of the gas-liquid separation tank (37) is connected with the reflux inlet of the acetic acid rectifying tower (32).
2. The apparatus for purifying acetic acid in the production of vinyl acetate by the ethylene process according to claim 1, wherein the heat exchanger (36) is a tubular heat exchanger.
3. The device for purifying acetic acid in the vinyl acetate production by the ethylene method according to claim 1 or 2, characterized in that the heat exchanger (36) comprises a cylinder body, and sealing heads are arranged at two ends of the cylinder body; the total length of the heat exchanger (36) is 5.5 meters, the total length of the cylinder is 4.4 meters, and the diameter of the cylinder is 0.5 meter.
4. The apparatus for purifying acetic acid in vinyl acetate production by ethylene process according to claim 1, wherein the barrel of the heat exchanger (36) comprises a shell side and a tube side, the bottom of the acetic acid rectifying tower (32) is connected with the shell side inlet of the heat exchanger, and the shell side outlet of the heat exchanger is connected with the gas-liquid separator (37);
the top of the acetic acid rectifying tower (32) is connected with an inlet of a compressor (25), an outlet of the compressor (25) is connected with a tube pass inlet of a heat exchanger (36), and a tube pass outlet of the heat exchanger is connected with a condenser (41).
5. An apparatus for purifying acetic acid in the production of vinyl acetate by ethylene process according to claim 1, characterized in that a plurality of flow-disturbing three-blade type internals (1) are installed in the tube side.
6. An apparatus for purifying acetic acid in vinyl acetate production by ethylene process according to claim 5, characterized in that the three-bladed flow disturbing internal member (1) comprises a sleeve on which 3 blades are uniformly arranged.
7. The apparatus for purifying acetic acid in the ethylene process of producing vinyl acetate as claimed in claim 6, wherein the tube pass is provided with a support bar, the support bar is sleeved with a plurality of flow-disturbing three-blade type internals (1), and the plurality of flow-disturbing three-blade type internals (1) can rotate under the impact of the fluid.
8. The apparatus for purifying acetic acid in the production of vinyl acetate by the ethylene process according to claim 6, characterized in that the inlet and the outlet of the heat exchanger (36) are provided with auxiliary heat exchangers.
9. The device for purifying acetic acid in vinyl acetate production by the ethylene method according to claim 1, characterized in that the bottom outlet of the acetic acid rectifying tower (32) is connected with the side wall inlet of the heat exchanger (36) through a tower bottom discharge pump (39) of the acetic acid rectifying tower; the bottom outlet of the gas-liquid separation tank (37) is connected with a pipeline, and a tower kettle outlet flow control valve (38) is arranged on the pipeline; the bottom outlet of the heat exchanger (36) is connected with the inlet at the bottom of a condenser (41) at the top of the acetic acid rectifying tower through a heat exchanger outlet connection stop valve (40); the top outlet of the condenser (41) at the top of the acetic acid rectifying tower is divided into two paths, one path is connected with the acetic acid rectifying tower (32) through a reflux quantity control valve (34) at the top outlet of the first acetic acid rectifying tower, and the other path is provided with a flow control valve (33) at the top outlet of the second acetic acid rectifying tower.
10. The apparatus for purifying acetic acid in vinyl acetate production by ethylene process according to claim 1, wherein the acetic acid rectifying tower (32) is a plate rectifying tower, and the total number of actual plates in the acetic acid rectifying tower (32) is 30-42;
the total height of the plate type rectifying tower is 26 meters, the diameter of the tower is 1.2 meters, a sieve plate tower is arranged inside the plate type rectifying tower, the diameter of an inner hole of the tower is 12.7 millimeters, the width of a side wall downcomer inside the plate type rectifying tower is 0.78 meter, the height of an internal weir of the plate type rectifying tower is 70 millimeters, and the distance between tower plates is 0.8 meter; the acetic acid rectifying tower (32) is internally provided with a high-temperature polytetrafluoroethylene lining.
CN201911143665.7A 2019-11-20 2019-11-20 Device for purifying acetic acid in vinyl acetate production by ethylene method Pending CN110833701A (en)

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CN113968782A (en) * 2021-11-24 2022-01-25 南通醋酸纤维有限公司 Method for removing impurities in recycled acetic acid
CN114632343A (en) * 2022-05-18 2022-06-17 北京化工大学 MVR heat pump rectification system and method
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Cited By (4)

* Cited by examiner, † Cited by third party
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CN114939363A (en) * 2021-02-06 2022-08-26 上海霞飞日化有限公司 Perfume stirring device
CN113968782A (en) * 2021-11-24 2022-01-25 南通醋酸纤维有限公司 Method for removing impurities in recycled acetic acid
CN114632343A (en) * 2022-05-18 2022-06-17 北京化工大学 MVR heat pump rectification system and method
CN114632343B (en) * 2022-05-18 2022-12-02 北京化工大学 MVR heat pump rectification system and method

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