CN109879720B - Method and equipment for separating and recovering difluoro dichloromethane in tetrafluoroethylene production - Google Patents
Method and equipment for separating and recovering difluoro dichloromethane in tetrafluoroethylene production Download PDFInfo
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Abstract
The invention provides a method for separating and recovering difluorodichloromethane in tetrafluoroethylene production, which comprises the following steps: 1) rectifying and separating a fraction a obtained after rectification and separation of tetrafluoroethylene pyrolysis gas in a tetrafluoroethylene monomer recovery tower, wherein one part of a mixture at the top of the tower is used as a fraction c to enter a tower kettle of a tail gas absorption tower, and the other part of the mixture is used as a fraction d to be continuously recovered to a gas holder; 2) continuously feeding the fraction c into a tower kettle of a tail gas absorption tower, enabling a tower top spray absorbent to be in countercurrent contact with the fraction c rising from the tower kettle in the absorption tower, then discharging the mixture into a tail gas desorption tower, and 3) discharging the mixture into the tail gas desorption tower, and heating and desorbing. The method for recovering the difluorodichloromethane from the tetrafluoroethylene production process has the advantages of simple process flow, convenient operation, full-closed operation of the whole production process, safety, energy conservation and environmental protection.
Description
Technical Field
The invention belongs to the field of organic compounds, and particularly relates to a method for separating fluorine-containing components in a tetrafluoroethylene production process.
Background
At present, the industrial production technology for preparing tetrafluoroethylene (C2F4) by cracking difluorochloromethane (F22) mainly comprises two types of air tube cracking and superheated steam dilution cracking, and in the two industrial production technologies, compared with the air tube cracking, the superheated steam dilution cracking has the advantages of low unit consumption of production raw materials, low energy consumption, less three-waste discharge, obvious reduction of production cost and the like. Therefore, the superheated steam dilution cracking technology is widely applied in China, and the scale of production devices is gradually enlarged. With the increasing market competition, the quality of tetrafluoroethylene monomer directly influences the market competitiveness of the downstream polytetrafluoroethylene product.
Difluorodichloromethane is a by-product of the cracking of F22 to produce tetrafluoroethylene. Although the amount of byproducts generated after the tetrafluoroethylene is prepared by diluting and cracking with steam is greatly reduced relative to the empty tube cracking in the domestic tetrafluoroethylene production process, difluorodichloromethane is difficult to effectively separate in the currently mature tetrafluoroethylene rectification and purification process, part of the byproducts enter residual liquid to be treated as waste liquid in the rectification and separation process, but part of the byproducts still enter the front end of the production process through the recovery and circulation of tetrafluoroethylene so as to form accumulation.
In order to ensure the quality of tetrafluoroethylene polymer products, after the content of difluorodichloromethane in a tetrafluoroethylene production process is accumulated to a certain degree, the treatment needs to be carried out by increasing the discharge amount of waste liquid, planned emptying and the like, so that the process has great potential safety hazard and environmental protection risk, and the unit consumption of a production system is high.
At present, although the tetrafluoroethylene production process is gradually mature and complete, no related technology is disclosed in China in the aspect of solving the difficult problem of separation of difluorodichloromethane in the tetrafluoroethylene production process. Therefore, the method and the process for continuously and stably operating, safely and efficiently recovering the difluorodichloromethane from the tetrafluoroethylene are developed, and the optimization of a tetrafluoroethylene production industrial device and the stability of the product quality are facilitated.
Disclosure of Invention
Aiming at the defects in the field and aiming at an industrial tetrafluoroethylene production device, the invention discloses a practical method for recovering difluorodichloromethane from a tetrafluoroethylene production process.
The second purpose of the invention is to provide a device for separating and recovering difluoro dichloromethane in tetrafluoroethylene production.
The above purpose of the invention is realized by the following technical scheme:
a method for separating and recovering difluorodichloromethane in tetrafluoroethylene production is characterized by comprising the following steps:
1) rectifying and separating a fraction a obtained after rectification and separation of tetrafluoroethylene pyrolysis gas in a tetrafluoroethylene monomer recovery tower, discharging a tower bottom fraction b (entering a subsequent rectification tower), taking a part of a mixture containing tetrafluoroethylene, hexafluoropropylene and difluorodichloromethane at the tower top as a fraction c to enter a tower bottom of a tail gas absorption tower, and continuously recovering the other part of the mixture as a fraction d to a gas holder;
2) continuously feeding the fraction c into a tower kettle of a tail gas absorption tower, enabling a tower top spray absorbent to be in countercurrent contact with the fraction c rising from the tower kettle in the absorption tower, enabling the difluorodichloromethane in the fraction c absorbed by the absorbent to return to the tower kettle to form a mixture, discharging the mixture to enter a tail gas desorption tower, and recovering components (gas phase) at the top of the absorption tower to a low-pressure system;
the mixture g of tetrafluoroethylene and the like which is not absorbed in the fraction c is accumulated at the top of the absorption tower and is recovered from the top to a low-pressure system for continuous rectification.
3) And discharging the mixture into a tail gas desorption tower, desorbing the difluorodichloromethane contained in the mixture by heating, and then recovering the difluorodichloromethane to a difluorodichloromethane storage tank, wherein the desorbed absorbent is recycled.
And (3) continuously recovering and rectifying the components in the gas holder in the step 1) in a low-pressure system. The method means that the components in the gas holder enter a series of equipment before the tetrafluoroethylene monomer recovery tower to be rectified and then enter the tetrafluoroethylene monomer recovery tower. The technology mainly solves the problem that the difluorodichloromethane is accumulated in the internal circulation process for a long time, and the separated fraction c breaks through the accumulation of the difluorodichloromethane in the original circulation process.
The tetrafluoroethylene pyrolysis gas is pyrolysis gas obtained after dilution and cracking by using water vapor of difluorochloromethane (F22), and the residual fraction obtained after purification, dehydration, pressurization, removal of non-condensable gas and rectification and recovery of a tetrafluoroethylene product is used as fraction a.
The fraction b is a fraction containing components such as chlorodifluoromethane, hexafluoropropylene, octafluorocyclobutane and the like; the fraction c and the fraction d have the same composition and are fractions containing components such as tetrafluoroethylene, perfluoropropylene, difluorodichloromethane and the like.
Preferably, in the step 1), the top pressure of the monomer recovery tower is 0.8-1.0 MPa, the temperature at the top of the tower is-20-0 ℃, and the reflux ratio is 8-20: 1.
In the step 1), the liquid level of the tower bottom of the monomer recovery tower and the discharge amount of the tower bottom fraction are subjected to linkage control, the liquid level of the tower bottom is maintained at 1/2-2/3, and the tower bottom fraction b is discharged to a subsequent rectifying device.
Wherein the mass ratio of the fraction c discharged from the top of the tetrafluoroethylene recovery tower in the step 1) to the fraction d is controlled as follows: fraction c: the fraction d is 1:8 to 1: 25.
Wherein, in the step 2), the temperature of the tower kettle of the tail gas absorption tower is 40-70 ℃, the temperature of the tower top is-30 to-10 ℃, the pressure of the tower top is 0.2-0.4 MPa, and the liquid-gas ratio is as follows: 5-15: 1; the absorbent sprayed on the top of the tail gas absorption tower is a polar solvent, and is selected from one or more of methanol, ethanol, chloroform, isopropanol and diethyl ether.
Wherein, in the step 3), the temperature of the bottom of the tail gas desorption tower is 50-85 ℃, the temperature of the top of the tower is-30 to-10 ℃, and the pressure of the top of the tower is 0.02-0.15 MPa.
And 3) detecting and analyzing the purity of the difluorodichloromethane in the desorbed product in the step 3), and if the purity is lower than 90%, discharging the product from the difluorodichloromethane storage tank to the tail gas absorption tower for repeated absorption and separation until the purity of the difluorodichloromethane in the product is higher than 90%, and then comprehensively utilizing the product as a recovered product.
A device for separating and recovering difluorodichloromethane in tetrafluoroethylene production comprises a tetrafluoroethylene monomer recovery tower, a tail gas absorption tower, a tail gas desorption tower, a difluorodichloromethane storage tank and a gas holder;
the top of the tetrafluoroethylene monomer recovery tower is respectively connected with the tail gas absorption tower and the gas holder through pipelines, the tower kettle of the tail gas absorption tower is connected with the tail gas desorption tower, and the desorption agent pipeline at the bottom of the tail gas desorption tower is connected with the top of the tail gas absorption tower; the top of the tail gas desorption tower is connected with the 5-stage difluoro methylene dichloride storage tank; and the top of the difluoro dichloromethane storage tank is provided with a pipeline connected to the tail gas absorption tower.
Preferably, an absorbent delivery pump is arranged on the desorption agent pipeline, and a wire mesh filler or a mesh wave filler is filled in the tetrafluoroethylene monomer recovery tower; the tail gas absorption tower is filled with one or more of pall rings, saddle rings, raschig rings and calendering hole rings.
The invention has the beneficial effects that:
the method and the process for recovering the difluorodichloromethane from the tetrafluoroethylene production process have the characteristics of simple process flow, convenient operation, full-closed operation of the whole production process, safety, energy conservation and environmental protection. Meanwhile, in the process of absorbing and separating the difluorodichloromethane by adopting the polar absorbent, the invention recovers a large amount of tetrafluoroethylene and perfluoropropylene, and simultaneously can ensure that the recovered difluorodichloromethane reaches the purity of more than 90 percent, thereby obviously reflecting the reutilization value of the difluorodichloromethane.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention,
wherein, 1 is a tetrafluoroethylene monomer recovery tower, 2 is a tail gas absorption tower, 3 is an absorbent delivery pump, 4 is a tail gas desorption tower, 5 is a difluoro methylene dichloride storage tank, and 6 is a gas holder.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention.
Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Example 1
The equipment adopted by the invention is shown in figure 1, and the equipment for separating and recovering difluorodichloromethane in tetrafluoroethylene production comprises a tetrafluoroethylene monomer recovery tower 1, a tail gas absorption tower 2, a tail gas desorption tower 4, a difluorodichloromethane storage tank 5 and a gas holder 6;
the top of the tetrafluoroethylene monomer recovery tower 1 is respectively connected with the tail gas absorption tower 2 and the gas holder 6 through pipelines, the bottom of the tail gas absorption tower 2 is connected with the tail gas desorption tower 4, and the desorption agent pipeline at the bottom of the tail gas desorption tower 4 is connected with the top of the tail gas absorption tower; the top of the tail gas desorption tower is connected with a difluoro dichloromethane storage tank 5; and the top of the difluoro dichloromethane storage tank is provided with a pipeline connected to the tail gas absorption tower. The absorbent conveying pump 3 is arranged on the analysis agent pipeline.
Equipment parameters:
the inner diameter of the monomer recovery tower is 600mm, stainless steel mesh wave packing with the diameter of 597mm multiplied by 100mm is filled in the monomer recovery tower, and the height of the packing is 25000 mm. The internal diameter of the tail gas absorption tower is 200mm, stainless steel pall ring packing with the diameter of 25mm multiplied by 25mm is filled in the tail gas absorption tower, and the height of the packing is 15000 mm. The internal diameter of the tail gas desorption tower is phi 150mm, stainless steel pall ring packing with phi 25mm multiplied by 25mm is filled in the tail gas desorption tower, and the height of the packing is 15000 mm.
The device operating conditions are as follows: f22, continuously feeding residual fraction a of cracked gas diluted and cracked by water vapor into a monomer recovery tower after the steps of purifying, dehydrating, pressurizing, removing non-condensable gas and rectifying and recovering a tetrafluoroethylene product, controlling the feeding amount to be 2000-2500 kg/h, starting a kettle heat tracing and a tower top refrigerant of the monomer recovery tower, controlling the tower top pressure of the monomer recovery tower to be 0.8-1.0 MPa, and controlling the tower top temperature to be-20-0 ℃. After the liquid-phase materials appear in the tower kettle through the liquid level meter, the liquid level of the tower kettle of the tetrafluoroethylene recovery tower and the discharge amount of the fraction b of the tower kettle are subjected to linkage control, the liquid level is controlled at 1/2-2/3 of the measuring range of the liquid level of the tower kettle, and the fraction b is discharged to a subsequent rectifying device. With the stable pressure of the tower top, the reflux ratio is controlled as follows: and 8-20: 1, firstly, recovering all materials at the top of the tower as a fraction d according to 900kg/h to a gas holder for continuous rectification, and after the monomer recovery tower process is stable, performing distillation according to a specific gravity fraction c: and (4) conveying the fraction c to a tail gas absorption tower at a ratio of 90kg/h, and recovering the fraction d to a gas holder at a ratio of 810kg/h for continuous rectification, wherein the ratio of the fraction d is 1: 9.
When the fraction c continuously enters the tower bottom of the tail gas absorption tower, the tower top spraying absorbent e and the fraction c rising from the tower bottom are in countercurrent contact in the absorption tower, and the liquid-gas ratio is as follows: 8:1. And then, with the rise of the tower top pressure of the absorption tower, performing linkage control on the tower top pressure of the absorption tower and the recovery amount of the mixture g, wherein the tower top pressure is controlled to be 0.2-0.4 MPa. Meanwhile, with the increase of the liquid level of the tower kettle, the tower kettle is opened to carry out heat tracing and tower top refrigerant, the tower kettle temperature of the tail gas absorption tower is controlled to be 40-70 ℃, the tower top temperature is controlled to be-30-10 ℃, then the discharge amount of the mixture f and the liquid level of the tower kettle of the tail gas absorption tower are controlled in a linkage mode, and the liquid level of the tower kettle is controlled to be 1/2-2/3 of the measuring range of the liquid level of the tower kettle. In the implementation process, the absorbent e sprayed by the tail gas absorption tower is methanol.
And after the mixture f is discharged and enters a tail gas desorption tower, opening a tower kettle of the tail gas desorption tower for heat tracing and tower top refrigerant, controlling the tower kettle temperature of the tail gas desorption tower to be 50-85 ℃, the tower top temperature to be-30-10 ℃, desorbing a mixture h of difluorodichloromethane and the like contained in the mixture f to the tower top for accumulation, and then controlling the tower top pressure of the desorption tower and the recovery amount of a desorbed product h to a difluorodichloromethane storage tank in a linkage manner along with the rise of the tower top pressure of the tail gas desorption tower, wherein the tower top pressure is controlled to be 0.02-0.15 MPa. After the operation is stabilized for 24 hours, the desorbed product h containing the difluorodichloromethane is collected for a total of 180kg, wherein the purity of the difluorodichloromethane is as follows: 42 percent. And (3) conveying the desorbed product h to a tail gas absorption tower, controlling the feeding amount to be 30kg/h, and controlling the liquid-gas ratio to be: 8:1, controlling the processes of the stable tail gas absorption tower and the tail gas analysis tower for 6 hours, and collecting products h containing the difluoro dichloromethane to account for 88kg in total, wherein the purity of the difluoro dichloromethane is 93 percent.
Example 2
Under the condition that residual materials are remained during the previous operation of the device, the parameters of each device are consistent with those of the embodiment 1, the residual fraction a obtained after the pyrolysis gas obtained after F22 steam dilution and pyrolysis is subjected to the steps of purification, dehydration, pressurization, non-condensable gas removal and tetrafluoroethylene product recovery continuously enters a monomer recovery tower, the feeding amount is still controlled to be 2000-2500 kg/h, the monomer recovery tower kettle heat tracing and the tower top refrigerant are started, the monomer recovery tower top pressure is controlled to be 0.8-1.0 MPa, and the tower top temperature is-20-0 ℃. After the liquid-phase materials appear in the tower kettle through the liquid level meter, the liquid level of the tower kettle of the tetrafluoroethylene recovery tower and the discharge amount of the fraction b of the tower kettle are subjected to linkage control, the liquid level is controlled at 1/2-2/3 of the measuring range of the liquid level of the tower kettle, and the fraction b is discharged to a subsequent rectifying device. With the stable pressure of the tower top, the reflux ratio is controlled as follows: and 8-20: 1, firstly, recovering all materials at the top of the tower as a fraction d according to 900kg/h to a gas holder for continuous rectification, and after the monomer recovery tower process is stable, performing distillation according to a specific gravity fraction c: and (4) conveying the fraction c to a tail gas absorption tower at a rate of 60kg/h, and recovering the fraction d to a gas holder at a rate of 840kg/h for continuous rectification.
The tail gas absorption tower still adopts methanol as an absorbent, the tail gas absorption tower and the tail gas desorption tower are still controlled according to the process parameters, after the operation is carried out for 24 hours, a mixture h containing the difluoro dichloromethane is collected for totally 180kg, and the purity of the difluoro dichloromethane in the mixture h is as follows: 42 percent. Conveying the mixture h to a tail gas absorption tower, controlling the feeding amount to be 30kg/h, and controlling the liquid-gas ratio to be: 8:1, after the process control of the tail gas absorption tower and the tail gas analysis tower is stabilized for 6 hours, collecting the desorbed product h containing the difluoro dichloromethane, wherein the total amount of the desorbed product h is 85kg, and the purity of the difluoro dichloromethane in the desorbed product h is as follows: 61 percent. Conveying the product h to a tail gas absorption tower, controlling the feeding amount to be 20kg/h, and controlling the liquid-gas ratio to be: 1:8, after the process control of the tail gas absorption tower and the tail gas analysis tower is stabilized for 5 hours, collecting products h containing difluoro dichloromethane, wherein the total amount of the products h is 61kg, and the purity of the difluoro dichloromethane in the products h is as follows: 94 percent.
Example 3
Under the condition that residual materials are reserved during the previous driving of the device, the equipment parameters are consistent with those of the embodiment 1.
F22, continuously feeding residual fraction a of cracked gas diluted and cracked by water vapor into a monomer recovery tower after the steps of purifying, dehydrating, pressurizing, removing non-condensable gas and recovering a tetrafluoroethylene product, controlling the feeding amount to be 2000-2500 kg/h, starting a tower kettle heat tracing and a tower top refrigerant of the monomer recovery tower, controlling the tower top pressure of the monomer recovery tower to be 0.8-1.0 MPa, and controlling the tower top temperature to be-20-0 ℃. After the liquid-phase materials appear in the tower kettle through the liquid level meter, the liquid level of the tower kettle of the tetrafluoroethylene recovery tower and the discharge amount of the fraction b of the tower kettle are subjected to linkage control, the liquid level is controlled at 1/2-2/3 of the measuring range of the liquid level of the tower kettle, and the fraction b is discharged to a subsequent rectifying device. With the stable pressure of the tower top, the reflux ratio is controlled as follows: and 8-20: 1, firstly, recovering all materials at the top of the tower as a fraction d according to 900kg/h to a gas holder for continuous rectification, and after the monomer recovery tower process is stable, performing distillation according to a specific gravity fraction c: and (3) conveying the fraction c to a tail gas absorption tower at a ratio of 45kg/h, and recovering the fraction d to a gas holder at a ratio of 855kg/h for continuous rectification, wherein the fraction d is 1: 19.
The tail gas absorption tower still adopts methanol as an absorbent, the tail gas absorption tower and the tail gas desorption tower are still controlled according to the process parameters, after the operation is carried out for 24 hours, the total amount of products h which contain the difluorodichloromethane and are desorbed is 180kg, and the purity of the difluorodichloromethane in the products h is 42%. Conveying the product h to a tail gas absorption tower, controlling the feeding amount to be 30kg/h, and controlling the liquid-gas ratio to be: 8:1, after the process control of the tail gas absorption tower and the tail gas analysis tower is stabilized for 6 hours, collecting a mixture h containing difluoro dichloromethane, wherein the total amount of the mixture h is 55kg, and the purity of the difluoro dichloromethane in a product h is as follows: 74 percent. Conveying the mixture h to a tail gas absorption tower, controlling the feeding amount to be 20kg/h, and controlling the liquid-gas ratio to be: 8:1, after the process control of the tail gas absorption tower and the tail gas analysis tower is stabilized for 3 hours, collecting the desorbed products h containing the difluoro dichloromethane, wherein the total amount of the desorbed products h is 45kg, and the purity of the difluoro dichloromethane is 96 percent.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (7)
1. A method for separating and recovering difluorodichloromethane in tetrafluoroethylene production is characterized by comprising the following steps:
1) rectifying and separating a fraction a obtained after rectification and separation of tetrafluoroethylene pyrolysis gas in a tetrafluoroethylene monomer recovery tower, discharging a tower kettle fraction b, taking a part of a mixture containing tetrafluoroethylene, hexafluoropropylene and difluorodichloromethane at the tower top as a fraction c to enter a tail gas absorption tower kettle, and continuously recovering the other part of the mixture as a fraction d to a gas holder;
2) continuously feeding the fraction c into a tower kettle of a tail gas absorption tower, enabling a spray absorbent at the tower top to be in countercurrent contact with the fraction c rising from the tower kettle in the absorption tower, enabling the difluorodichloromethane in the fraction c absorbed by the absorbent to return to the tower kettle to form a mixture, discharging the mixture to enter a tail gas desorption tower, and recovering components at the tower top of the absorption tower to a low-pressure system;
3) discharging the mixture, feeding the mixture into a tail gas desorption tower, heating the mixture to desorb difluorodichloromethane contained in the mixture, recycling the difluorodichloromethane to a difluorodichloromethane storage tank, and recycling the desorbed absorbent;
wherein, in the step 2), the temperature of the tower kettle of the tail gas absorption tower is 40-70 ℃, the temperature of the tower top is-30 to-10 ℃, the pressure of the tower top is 0.2-0.4 MPa, and the liquid-gas ratio is as follows: 5-15: 1; the absorbent sprayed on the top of the tail gas absorption tower is methanol.
2. The method of claim 1, wherein: the tetrafluoroethylene pyrolysis gas is pyrolysis gas obtained after dilution and cracking by using monochlorodifluoromethane water vapor, and the residual fraction of the pyrolysis gas after purification, dehydration, pressurization, removal of non-condensable gas and recovery of a tetrafluoroethylene product by rectification is fraction a.
3. The method of claim 1, wherein: in the step 1), the top pressure of the monomer recovery tower is 0.8-1.0 MPa, the temperature of the top of the tower is-20-0 ℃, and the reflux ratio is 8-20: 1.
4. The method of claim 1, wherein: in the step 1), the liquid level of the tower bottom of the monomer recovery tower and the discharge amount of the tower bottom fraction are subjected to linkage control, the liquid level of the tower bottom is maintained at 1/2-2/3, and the tower bottom fraction b is discharged to a subsequent rectifying device.
5. The method of claim 1, wherein: the mass ratio of the fraction c discharged from the top of the tetrafluoroethylene recovery tower in the step 1) to the fraction d is controlled as follows: fraction c: the fraction d is 1:8 to 1: 25.
6. The method according to any one of claims 1 to 5, wherein: in the step 3), the temperature of the bottom of the tail gas desorption tower is 50-85 ℃, the temperature of the top of the tower is-30 to-10 ℃, and the pressure of the top of the tower is 0.02-0.15 MPa.
7. The method according to any one of claims 1 to 5, wherein: and 3) detecting and analyzing the purity of the difluorodichloromethane in the desorbed product in the step 3), and if the purity is lower than 90%, discharging the product from the difluorodichloromethane storage tank to the tail gas absorption tower for repeated absorption and separation until the purity of the difluorodichloromethane in the product is higher than 90%, and then comprehensively utilizing the product as a recovered product.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4249917A (en) * | 1979-11-21 | 1981-02-10 | Union Carbide Corporation | Sterilization gas separation process |
| RU2063952C1 (en) * | 1994-03-22 | 1996-07-20 | Российский научный центр "Прикладная химия" | Method of isolation of difluorochloromethane and hexafluoropropene |
| US6488817B1 (en) * | 1998-03-31 | 2002-12-03 | Alliedsignal Inc. | Purification of hydrofluorocarbons |
| CN104817424A (en) * | 2015-03-17 | 2015-08-05 | 中昊晨光化工研究院有限公司 | Method for separation of difluoromethane from tetrafluoroethylene product |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100540517C (en) * | 2007-12-29 | 2009-09-16 | 山东东岳高分子材料有限公司 | The method of separating trifluoroethylene during tetrafluoroethylene is produced |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4249917A (en) * | 1979-11-21 | 1981-02-10 | Union Carbide Corporation | Sterilization gas separation process |
| RU2063952C1 (en) * | 1994-03-22 | 1996-07-20 | Российский научный центр "Прикладная химия" | Method of isolation of difluorochloromethane and hexafluoropropene |
| US6488817B1 (en) * | 1998-03-31 | 2002-12-03 | Alliedsignal Inc. | Purification of hydrofluorocarbons |
| CN104817424A (en) * | 2015-03-17 | 2015-08-05 | 中昊晨光化工研究院有限公司 | Method for separation of difluoromethane from tetrafluoroethylene product |
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