CN113528197A - Method for recovering hydrocarbons and acetonitrile by acetonitrile method butadiene extraction device - Google Patents
Method for recovering hydrocarbons and acetonitrile by acetonitrile method butadiene extraction device Download PDFInfo
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- CN113528197A CN113528197A CN202010314938.6A CN202010314938A CN113528197A CN 113528197 A CN113528197 A CN 113528197A CN 202010314938 A CN202010314938 A CN 202010314938A CN 113528197 A CN113528197 A CN 113528197A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/04—Liquid carbonaceous fuels essentially based on blends of hydrocarbons
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- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to the technical field of ethylene cracking C4 fraction separation, and discloses a method for recovering hydrocarbons and acetonitrile by an acetonitrile method butadiene extraction device, which comprises the following steps: part of the washing tower water is sent to a dimer washing tower to be used as washing water to remove dimers in a regeneration solvent, the dimers are discharged to a liquefaction fuel tank from the tower top, washing wastewater in the tower bottom is sent to a buffer tank for flash evaporation, the wastewater after flash evaporation in the buffer tank enters a solvent recovery tower after heat exchange, the buffer tank exhaust gas is converged with the solvent recovery tower top exhaust gas, the liquid phase is condensed by a heat exchanger, the liquid phase enters the lower part of the dimer washing tower together with the regeneration solvent and liquefied hydrocarbon, after the liquid phase is in countercurrent contact with the washing water for water washing, hydrocarbons in the condensed liquid phase, dimers in the regeneration solvent and the liquefied hydrocarbon are discharged to the liquefaction fuel tank from the tower top, and the solvent is dissolved in the washing water and then discharged to the buffer tank from the tower bottom. The method can effectively improve the yield of products and byproducts, reduce the loss of the solvent and improve the economic benefit of the device.
Description
Technical Field
The invention relates to the technical field of separation of ethylene cracking C4 fractions, in particular to a method for recovering hydrocarbons and acetonitrile by an acetonitrile method butadiene extraction device.
Background
The process for extracting butadiene by acetonitrile method takes mixed C4 by-product of an ethylene cracking device as a raw material, takes acetonitrile as a solvent, and produces a polymer-grade 1, 3-butadiene product by two-stage extractive distillation and two-stage common distillation. The acetonitrile solvent is extracted and rectified to become rich solvent, then stripped to become poor solvent, and then recycled in the device after being recovered by a series of reboiler heat.
As is known to all, because the saturated vapor pressure of acetonitrile solvent is lower and is more volatile, three water washing towers, namely a raffinate water washing tower, a butadiene water washing tower and a dimer water washing tower, are arranged in the acetonitrile method butadiene extraction device. In the acetonitrile method butadiene extraction device, raffinate extracted from the top of a first extraction rectifying tower and crude butadiene extracted from the top of a second extraction rectifying tower contain a certain amount of solvent acetonitrile, and acetonitrile in the raffinate and the crude butadiene is removed in a water washing mode by generally using the principle that water is similar to acetonitrile and is dissolved mutually in operation, so that the acetonitrile content in products and byproducts is ensured to be below a specified range; and part of the washing wastewater discharged from the two water washing tower kettles is sent to a dimer water washing tower to be used as washing water to remove dimer in the circulating solvent, and the dimer is removed from the top of the dimer water washing tower and is sent out of a battery limit as liquefied fuel. Washing wastewater containing the solvent and discharged from the three water washing tower kettles is converged into a buffer tank which is close to normal pressure and normal temperature, hydrocarbons and acetonitrile carried in the wastewater are flashed out in the buffer tank, and the flashed wastewater enters the middle part of the solvent recovery tower after being heated by a feeding heat exchanger through a feeding pump. The hydrocarbon, acetonitrile and water are separated in the solvent recovery tower, the acetonitrile and a small amount of hydrocarbon and water form an azeotrope which is separated from the top of the solvent recovery tower and then recycled, and the tower kettle is a wastewater discharge device.
However, the above method of removing acetonitrile by washing the C4 fraction with water and recycling acetonitrile in the waste water has a disadvantage. That is, the loss of C4 hydrocarbons and solvent in the overhead gas from the buffer tank and the solvent recovery column is large. When three strands of tower cauldron waste water that have the higher pressure join and get into the buffer tank that is close the ordinary pressure, because the reduction of pressure, the flash distillation can be carried out to tower cauldron waste water in the buffer tank. C4 hydrocarbons dissolved in the tower bottom wastewater under the high pressure condition can be flashed and resolved in the buffer tank, the quick flashing and resolving of the C4 component can also carry part of acetonitrile and water, and finally the buffer tank exhausts through an exhaust line discharge device of the buffer tank top pressure split system. The buffer tank exhaust generally contains high C4 content and a small amount of acetonitrile, which can cause the waste of device products, byproducts and solvents, reduce the hydrocarbon recovery rate of the device, increase the loss rate of the device solvents and further reduce the economic benefit of the device. Similarly, the normal-temperature tower washing wastewater after flash evaporation in the buffer tank enters the middle part of the solvent recovery tower through a feed pump and a feed heat exchanger after temperature rise, and hydrocarbons, acetonitrile and water are separated in the solvent recovery tower. The C4 hydrocarbon is still dissolved in the normal temperature waste water after flash evaporation in the buffer tank, the hydrocarbon is heated by steam in the solvent recovery tower, the hydrocarbon gas solubility is reduced along with the increase of the temperature, the hydrocarbon can be further analyzed from the waste water, and finally the hydrocarbon can pass through an exhaust line discharge device of the tower top reflux tank split system. Similarly, acetonitrile in the wastewater at normal temperature in the buffer tank is treated by the solvent recovery tower to form acetonitrile water to form an azeotrope (regenerated solvent) which is separated from the top of the solvent recovery tower, but the temperature of the regenerated solvent at the top of the solvent recovery tower is generally higher than the normal temperature of the buffer tank, the higher temperature can cause higher saturated vapor pressure of the acetonitrile, and part of the acetonitrile changes from liquid phase to gas phase in order to reach the saturated vapor pressure and finally is discharged out of the device along with the secondarily resolved hydrocarbons through an exhaust line of a tower top reflux tank split-pass system. The tower top exhaust gas of the solvent recovery tower generally contains higher C4 content and part of acetonitrile, which can cause the waste of device products, byproducts and solvents, reduce the hydrocarbon recovery rate of the device, increase the loss rate of the device solvents and further reduce the economic benefit of the device.
Therefore, the technology for reasonably recovering the hydrocarbons and the solvent of the acetonitrile method butadiene extraction device becomes a key technology for improving the yield of products and byproducts, reducing the solvent loss and improving the economic benefit of the device of the acetonitrile method butadiene extraction device.
Disclosure of Invention
In order to solve the problem of loss of hydrocarbons and solvents of an acetonitrile butadiene extraction device, the invention aims to provide a method for recovering hydrocarbons and solvents of the acetonitrile butadiene extraction device.
The invention provides a method for recovering hydrocarbons and acetonitrile by an acetonitrile method butadiene extraction device, which comprises the following steps: the method comprises the following steps that washing tower water parts of three washing towers in an acetonitrile butadiene extraction device are sent to a dimer washing tower to serve as washing water to remove dimers in a regeneration solvent, the dimers are discharged from the top of the dimer washing tower and serve as liquefied fuel to be sent to a liquefied fuel tank, washing wastewater in a dimer washing tower kettle and other washing tower water are sent to a buffer tank to be flashed, the wastewater flashed in the buffer tank enters a solvent recovery tower after heat exchange through a feed and discharge heat exchanger, the wastewater in the solvent recovery tower kettle is discharged as regeneration water after heat exchange through the feed and discharge heat exchanger, gas at the top of the solvent recovery tower enters a solvent recovery tower reflux tank after being condensed through a solvent recovery tower condenser, and liquid in the solvent recovery tower reflux tank reflows to the solvent recovery tower or serves as the regeneration solvent to be extracted; the method comprises the steps of merging the buffer tank exhaust gas with the solvent recovery tower top exhaust gas, condensing the liquid phase through a heat exchanger, then feeding the liquid phase, the regenerated solvent and the liquefied hydrocarbon into the lower part of a dimer water washing tower, carrying out countercurrent contact with washing water, washing, discharging the hydrocarbons in the condensed liquid phase, the dimers in the regenerated solvent and the liquefied hydrocarbon from the top of the dimer water washing tower together to serve as liquefied fuel, sending the liquefied fuel to a liquefied fuel tank, dissolving the solvent in the washing water, and then discharging the liquefied fuel from the bottom of the dimer water washing tower to a buffer tank.
The traditional butadiene extraction device adopting the acetonitrile method adopts a method of removing acetonitrile by washing C4 components and recycling acetonitrile in waste water, but the process of removing acetonitrile by washing C4 components and recycling acetonitrile can cause a large amount of C4 and acetonitrile loss. The method comprises the steps of merging the buffer tank exhaust gas with the solvent recovery tower top exhaust gas, condensing the mixture into a liquid phase through a heat exchanger, feeding the liquid phase into the lower part of a dimer water washing tower, and discharging hydrocarbons in the liquid phase from the top of the dimer water washing tower after washing the liquid phase to be used as a liquefied fuel product. The method effectively improves the yield of products and byproducts, reduces the loss of solvent and improves the economic benefit of the device.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without limiting the invention.
FIG. 1 is a schematic diagram of a process flow for recovering hydrocarbons and solvents in an extraction plant for butadiene by acetonitrile method according to an embodiment of the present invention.
Description of the reference numerals
1-buffer tank, 2-buffer tank discharge gas, 3-wastewater after flash evaporation in the buffer tank, 4-feed and discharge heat exchanger, 5-solvent recovery tower, 6-solvent recovery tower condenser, 7-solvent recovery tower reflux tank, 8-solvent recovery tower top discharge gas, 9-heat exchanger, 10-refrigerant, 11-liquid phase after condensation, 12-dimer water washing tower, 13-liquefied fuel tank, 14-liquefied fuel extraction pump, 15-liquefied fuel, 16-buffer tank feed, 17-regenerated water, 18-regenerated solvent, 19-liquefied hydrocarbon and 20-washing tower water.
Detailed Description
In order that the present invention may be more readily understood, the following detailed description of the invention is given with reference to the accompanying drawings and embodiments, which are given by way of illustration only and are not intended to limit the invention.
The invention provides a method for recovering hydrocarbons and acetonitrile by an acetonitrile method butadiene extraction device, which comprises the following steps: the method comprises the steps of sending water parts of washing towers of three washing towers in an acetonitrile butadiene extraction device to a dimer washing tower to serve as washing water to remove dimers in a regeneration solvent, discharging dimers from the top of the dimer washing tower to serve as liquefied fuel to be sent to a liquefied fuel tank, sending washing wastewater in a kettle of the dimer washing tower and other washing tower water to a buffer tank for flash evaporation, sending the wastewater subjected to flash evaporation in the buffer tank to a solvent recovery tower after heat exchange through a feed and discharge heat exchanger, sending the wastewater in the kettle of the solvent recovery tower to a feed and discharge heat exchanger to serve as regeneration water, condensing gas at the top of the solvent recovery tower through a condenser of the solvent recovery tower to enter a reflux tank of the solvent recovery tower, returning the liquid in the reflux tank of the solvent recovery tower to the solvent recovery tower or taking the liquid as the regeneration solvent, merging gas in the buffer tank with gas discharged from the top of the solvent recovery tower, condensing the gas into a liquid phase through the heat exchanger, and sending the liquid phase together with the regeneration solvent and liquefied hydrocarbon to the lower part of the dimer washing tower, after the washing water is brought into countercurrent contact with the washing water, hydrocarbons in the condensed liquid phase, dimers in the regenerated solvent and liquefied hydrocarbons are discharged from the top of the dimer water washing column together as liquefied fuel and sent to a liquefied fuel tank, and the solvent is dissolved in the washing water and then discharged from the bottom of the dimer water washing column and sent to a buffer tank.
In the invention, the buffer tank is used for collecting wastewater discharged from each washing tower kettle of the acetonitrile method butadiene device. Preferably, the buffer tank vent gas operating pressure: 10-100kPaG, operating temperature: 30-50 ℃, hydrocarbon content in buffer tank discharge gas: 10-99.9 wt%, and the balance of acetonitrile, water and nitrogen.
In the invention, the solvent recovery tower is used for refining the butadiene regeneration solvent by the acetonitrile method. Preferably, the solvent recovery overhead gas operating pressure is: 5-500kPaG, operating temperature: 60-150 ℃, hydrocarbon content in the vent gas at the top of the solvent recovery tower: 0.1-60 wt%, and the balance of acetonitrile, water and nitrogen. In addition, the vent gas at the top of the solvent recovery tower is discharged from the top of the reflux tank of the solvent recovery tower.
According to the invention, the heat exchanger condenses the buffer tank discharge gas and the solvent recovery tower top discharge gas into a liquid phase by using a refrigerant, wherein the refrigerant can use hydrocarbons such as propylene and the like, and the condensation temperature of the hydrocarbons is 0.1-20 ℃. Preferably, the process side operating pressure of the heat exchanger is: 5-100kPaG, operating temperature: 0.1-20 ℃.
Preferably, the dimer water-washing plate number is 30 to 50 plates, the operating pressure is 0.2 to 0.4MPaG, and the operating temperature is 30 to 45 ℃.
Preferably, the upper part of the dimer water-washing column is introduced into the regeneration water or fresh water discharged from the bottom of the solvent recovery column as washing water together with the washing water. The washing water can better recover the hydrocarbons and the solvent in the condensed liquid phase, the addition amount of the regeneration water or the fresh water and the washing water is that the solvent in the condensed liquid phase and the regeneration solvent is completely dissolved, the hydrocarbons, the dimers and the liquefied hydrocarbons are discharged, and the specific amount is determined according to the requirement and belongs to the conventional selection.
The process parameters which are not limited in the invention can be selected conventionally according to the prior art.
The present invention will be described in detail by way of examples.
Examples
This example illustrates the recovery of hydrocarbons and acetonitrile in an acetonitrile butadiene extraction unit of the present invention.
As shown in fig. 1, data of a 12-ten-thousand-ton/year acetonitrile butadiene extraction apparatus are taken as examples:
buffer tank vent gas 2, operating pressure: 70kPaG, operating temperature: 38.5 ℃, wherein the hydrocarbon content: 93.4% (by weight); acetonitrile content: 5.1 percent (weight ratio), and the balance of nitrogen and water; the flow rate is as follows: 120 kg/h;
solvent recovery overhead vent gas 8, operating pressure: 70kPaG, operating temperature: 82.8 ℃, wherein the hydrocarbon content: 39.7% (weight ratio); acetonitrile content: 48.8 percent (weight ratio), and the balance of nitrogen and water; the flow rate is as follows: 30 kg/h;
the two exhaust gases are converged and then enter a heat exchanger 9 for condensation, and the process side operating pressure of the heat exchanger 9 is as follows: 60kPaG, operating temperature: 2 ℃, and the refrigerant 10 is propylene;
the liquid phase 11 after condensation enters a dimer water washing column 12, the number of the trays of the dimer water washing column 12 is 40, and the operation pressure at the top of the column is as follows: 0.31MPaG, operating temperature: at 40 ℃.
The specific process comprises the following steps:
The buffer tank exhaust gas 2 and the solvent recovery tower top exhaust gas 8 are converged and then sent to a heat exchanger 9, and the heat exchanger 9 uses propylene as a refrigerant 10 to condense the two exhaust gases to a liquid phase. The condensed liquid phase 11 enters the lower part of the dimer water-washing column 12 together with the liquefied hydrocarbon 19 and the regeneration solvent 18.
In the dimer water-washing column 12, the condensed liquid phase 11, the regenerated solvent 18 and the liquefied hydrocarbon 19 are brought into countercurrent contact with the washing water, the hydrocarbons in the condensed liquid phase 11, the dimer in the regenerated solvent 18 and the liquefied hydrocarbon 19 are discharged from the top of the dimer water-washing column 12 together as the liquefied fuel 15 and sent to the liquefied fuel tank 13, and the solvent is dissolved in the washing water and then discharged from the bottom of the dimer water-washing column 12 and sent to the buffer tank 1.
The effect is as follows:
according to the data, the operation time of the 12 ten thousand tons/year acetonitrile method butadiene extraction device is 8000 hours per year, compared with the traditional acetonitrile method butadiene extraction device, the method can recover about 992 tons of liquefied fuel per year, reduce the loss of acetonitrile by about 166 tons, effectively improve the yield of products and byproducts, reduce the loss of solvent and improve the economic benefit of the device.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.
Claims (6)
1. A method for recovering hydrocarbons and acetonitrile by an acetonitrile method butadiene extraction device comprises the following steps: the method comprises the following steps that washing tower water parts of three washing towers in an acetonitrile butadiene extraction device are sent to a dimer washing tower to serve as washing water to remove dimers in a regeneration solvent, the dimers are discharged from the top of the dimer washing tower and serve as liquefied fuel to be sent to a liquefied fuel tank, washing wastewater in a dimer washing tower kettle and other washing tower water are sent to a buffer tank to be flashed, the wastewater flashed in the buffer tank enters a solvent recovery tower after heat exchange through a feed and discharge heat exchanger, the wastewater in the solvent recovery tower kettle is discharged as regeneration water after heat exchange through the feed and discharge heat exchanger, gas at the top of the solvent recovery tower enters a solvent recovery tower reflux tank after being condensed through a solvent recovery tower condenser, and liquid in the solvent recovery tower reflux tank reflows to the solvent recovery tower or serves as the regeneration solvent to be extracted; characterized in that the method further comprises: the method comprises the steps of merging the buffer tank exhaust gas with the solvent recovery tower top exhaust gas, condensing the liquid phase through a heat exchanger, then feeding the liquid phase, the regenerated solvent and the liquefied hydrocarbon into the lower part of a dimer water washing tower, carrying out countercurrent contact with washing water, washing, discharging the hydrocarbons in the condensed liquid phase, the dimers in the regenerated solvent and the liquefied hydrocarbon from the top of the dimer water washing tower together to serve as liquefied fuel, sending the liquefied fuel to a liquefied fuel tank, dissolving the solvent in the washing water, and then discharging the liquefied fuel from the bottom of the dimer water washing tower to a buffer tank.
2. The method for recovering hydrocarbons and acetonitrile by using the acetonitrile butadiene extraction device according to claim 1, wherein the operation pressure of the buffer tank vent gas is as follows: 10-100kPaG, operating temperature: 30-50 ℃, hydrocarbon content in buffer tank discharge gas: 10-99.9 wt%, and the balance of acetonitrile, water and nitrogen.
3. The method for recovering hydrocarbons and acetonitrile by using the acetonitrile butadiene extraction device according to claim 1, wherein the operation pressure of the solvent recovery overhead gas is as follows: 5-500kPaG, operating temperature: 60-150 ℃, hydrocarbon content in the vent gas at the top of the solvent recovery tower: 0.1-60 wt%, and the balance of acetonitrile, water and nitrogen.
4. The method for recovering the hydrocarbons and the acetonitrile by the acetonitrile butadiene extraction device according to claim 1, wherein the operation pressure of the process side of the heat exchanger is as follows: 5-100kPaG, operating temperature: 0.1-20 ℃.
5. The method for recovering hydrocarbons and acetonitrile by an acetonitrile butadiene extraction apparatus according to claim 1, wherein the dimer washing stage number is 30 to 50 plates, the operation pressure is 0.2 to 0.4MPaG, and the operation temperature is 30 to 45 ℃.
6. The method for recovering hydrocarbons and acetonitrile by an acetonitrile butadiene extraction apparatus according to claim 1, wherein the upper part of the dimer water washing column is introduced into the regenerated water or fresh water discharged from the bottom of the solvent recovery column as washing water together with the washing water.
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CN113956126A (en) * | 2021-10-26 | 2022-01-21 | 中国石油化工股份有限公司 | Butadiene separation method by recycling acetonitrile |
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CN103864551A (en) * | 2012-12-10 | 2014-06-18 | 中国石油化工集团公司 | Method for increasing acetonitrile method 1,3-butadiene extraction equipment raffinate product specification |
CN108218657A (en) * | 2018-01-08 | 2018-06-29 | 惠生工程(中国)有限公司 | A kind of method for recovering tail gas in acetonitrile method Butadiene extraction process |
CN108727150A (en) * | 2017-04-25 | 2018-11-02 | 中国石化工程建设有限公司 | A method of dimer content in the system circulation solvent of control acetonitrile method butadiene extraction device |
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CN103864551A (en) * | 2012-12-10 | 2014-06-18 | 中国石油化工集团公司 | Method for increasing acetonitrile method 1,3-butadiene extraction equipment raffinate product specification |
CN108727150A (en) * | 2017-04-25 | 2018-11-02 | 中国石化工程建设有限公司 | A method of dimer content in the system circulation solvent of control acetonitrile method butadiene extraction device |
CN108218657A (en) * | 2018-01-08 | 2018-06-29 | 惠生工程(中国)有限公司 | A kind of method for recovering tail gas in acetonitrile method Butadiene extraction process |
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CN113956126A (en) * | 2021-10-26 | 2022-01-21 | 中国石油化工股份有限公司 | Butadiene separation method by recycling acetonitrile |
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