CN101157595B - Method for preparing pentafluoroethane - Google Patents
Method for preparing pentafluoroethane Download PDFInfo
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- CN101157595B CN101157595B CN2007100905348A CN200710090534A CN101157595B CN 101157595 B CN101157595 B CN 101157595B CN 2007100905348 A CN2007100905348 A CN 2007100905348A CN 200710090534 A CN200710090534 A CN 200710090534A CN 101157595 B CN101157595 B CN 101157595B
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Abstract
The invention discloses a method for preparing the pentafluoroethane (HFC-125).In the method, the hydrogen fluoride (HF) and the perchlorethylene (PCE) are adopted as the raw materials, and two reactors and two steps of gas phase catalysis fluorination reaction are taken to prepare the HFC-125. A first reactor fluorinates the PCE and synthesizes 2, 2-dichlor-1, 1, 1-trifluoroethane (HCFC-123) and 2-chlorin-1, 1, 1, 2-tetrafluorothane (HCFC-124), and a second reactor fluorinates HCFC-123 and HCFC-124 and synthesizes HFC-125. The unreacted PCE in the resultant flow of the first reactor is separated by a first distillation tower and then is circulated to the first reactor; the HF, HCFC-126, HCFC-124, HFC-125 and HCL in the resultant flow of the first reactor and the second reactor are separated by a second distillation tower and a third distillation tower, and then the separated HF circulates to the first reactor and the second reactor, while the HCFC-123, the HCFC-124 and the HFC-134a circulate to the second reactor. The invention can prolong the service life of the catalyst and improve the one-way conversion of PCE as well as remarkably reduce the content of chloropentafluoroethane (CFC-115) in the desired product HFC-125.
Description
Technical field
The present invention relates to the preparation method of a kind of pentafluoride ethane (HFC-125), relate in particular to and a kind ofly obtain 2 by hydrogen fluoride gas phase catalytic fluorination zellon (PCE), 2-two chloro-1,1,1-Halothane (HCFC-123) and 2-chloro-1,1,1,2-Tetrafluoroethane (HCFC-124), further then catalytic fluorination HCFC-123 and HCFC-124 obtain the preparation method of pentafluoride ethane.
Background technology
Pentafluoride ethane is a kind of fluorinated hydrocarbons compound to atmospheric ozone layer safety, mainly as the substitute of monochlorodifluoromethane (HCFC-22) refrigeration agent, in addition, also is widely used as whipping agent, solvent, propellant, fire-fighting medium and dry etching agent.
At present, in the currently known methods of industrial preparation HFC-125, be raw material with hydrogen fluoride and PCE, the preparation method of the synthetic HFC-125 of gas-phase reaction is most widely used in the presence of catalyzer.It is raw material with PCE that Chinese patent CN1057516C discloses a kind of, in the presence of fluorination catalyst, carries out gas phase fluorination in single fluorination reactor, the preparation method of synthetic HFC-125.In this method, fluoridizing PCE generates the reaction of HCFC-123, HCFC-124 and fluoridizes in the same reactor of the synthetic HFC-125 of HCFC-123, HCFC-124 and carry out, be subjected to the influence of intermediate product HCFC-123 and HCFC-124, the reaction of fluoridizing PCE generation HCFC-123, HCFC-124 is restricted, and causes the per pass conversion of PCE relatively low.In order to improve the space-time yield of HFC-125, reaction needed is carried out under the high temperature about 350 ℃ in addition, because the polyreaction of PCE easily takes place down high temperature, has accelerated the coking rate of catalyzer, influences life of catalyst.And the content of the C2ClF5 in the product (CFC-115) is higher, because of the azeotropism of CFC-115 and HFC-125, brings difficulty for the purification of HFC-125, has increased production cost.
Summary of the invention
The invention provides a kind ofly overcome the deficiency that exists in the background technology, increased the PCE per pass conversion, prolonged catalyst life, the preparation method of pentafluoride ethane that CFC-115 content is low.
With PCE is raw material, and the principal reaction of the synthetic HFC-125 of gas phase fluorination is as follows:
The main side reaction that takes place is as follows:
(6)
The present invention adopts two reactors, mainly reacts (1) in first reactor, and the HCFC-123 that does not recycle in first reactor makes just to obtain the PCE per pass conversion identical with existing HFC-125 technology of preparing under lower temperature of reaction.Owing to reduced temperature of reaction, slowed down the speed of the catalyst surface coking that causes owing to the PCE high temperature polymerization, prolonged catalyst life.Second reactor mainly reacts (2) and (3), does not have raw material PCE in second reactor, and therefore, reaction can be carried out under higher temperature, has increased the transformation efficiency of HCFC-123 and HCFC-124.But the increase temperature of reaction helps the carrying out of side reaction (4), (5), (6), causes the content of CFC-115 in the reaction product to increase, and is unfavorable for the purification of HFC-125.The present invention will react the HFC-134a that generates and be circulated in second reactor, and the balance of reaction (5) is moved to the direction that generates HCFC-133a, suppress the disproportionation reaction of HFC-123, reduce the content of the CFC-115 in the product.
The invention provides a kind of is the preparation method of the pentafluoride ethane of raw material with PCE and HF, may further comprise the steps:
A. hydrogen fluoride and zellon enter first reactor, fluoridation takes place in the presence of fluorination catalyst, 200 ℃～350 ℃ of temperature of reaction, comprise 2 of reaction generation in the product stream, 2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1,2-Tetrafluoroethane, pentafluoride ethane, hydrogenchloride and unreacted hydrogen fluoride and zellon;
B. hydrogen fluoride and 2,2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1, the 2-Tetrafluoroethane enters second reactor, further fluoridation in the presence of fluorination catalyst is reacted and is 250 ℃～400 ℃ of temperature, comprises pentafluoride ethane, hydrogenchloride, a spot of C2ClF5,1 of generation in the product stream of second reactor, 1,1,2-Tetrafluoroethane and unreacted hydrogen fluoride, 2,2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1, the 2-Tetrafluoroethane;
C. the product of step a flows to into first distillation tower and separates, and the zellon that the first distillation Tata still is contained low amount of fluorinated hydrogen is circulated to first reactor;
D. the product stream of second reactor is mixed into second column and separates among the step c first distillation tower cat head component and the step b, and the HF part of after-fractionating Tata still is circulated to first reactor, and another part is circulated to second reactor;
E. the pentafluoride ethane of steps d after-fractionating column overhead, hydrogenchloride, 2,2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1,2-Tetrafluoroethane, 1,1,1,2-Tetrafluoroethane and low amount of fluorinated hydrogen enter that the 3rd distillation tower separates, the 3rd distillation Tata still 2,2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1,2-Tetrafluoroethane, 1,1,1,2-Tetrafluoroethane and low amount of fluorinated hydrogen are circulated to second reactor reaction, and are circulated in the above-mentioned material of second reactor 1,1,1, the molar content of 2-Tetrafluoroethane is 1%～3%;
F. step e the 3rd distillation tower cat head component pentafluoride ethane, hydrogenchloride and a spot of 1,1,1,2-Tetrafluoroethane, C2ClF5 enter the purifying products system, after deacidification, dehydration, rectification process, obtain the target product pentafluoride ethane.
Among the present invention, for the HF that controls reactive system and the mol ratio of organic materials, a large amount of HF circulate in reactive system, and fresh HF raw material can or enter reactive system by first reactor, second reactor simultaneously by any one reactor in first reactor, second reactor.
The type of reactor that is used for fluoridation is not crucial, and the present invention can use tubular reactor, fluidized-bed reactor etc.In addition, adiabatic reactor or isothermal reactor also can be used to the present invention.
The present invention uses the chromic oxide that contains multiple metal (as Zn, Co, Ni, Ge, In etc.), also can use chromic oxide, chromium fluoride, fluorizated chromic oxide, aluminum fluoride, fluorizated aluminum oxide, be carried on the fluorination catalysts such as chromic oxide on gac, aluminum fluoride, the magnesium fluoride.
The fluorizated reaction conditions can be selected according to catalyzer and catalytic activity level thereof.The temperature of reaction of first reactor is 200 ℃～350 ℃, preferred 250 ℃～300 ℃; Reaction pressure is 0MPa～2.0MPa, preferred 0.5MPa～1.5MPa, more preferably 0.8MPa～1.2MPa; Be 5 seconds～30 seconds duration of contact, preferred 10 seconds～20 seconds; The mol ratio of HF and PCE is 3～15: 1, preferred 6～10: 1.The temperature of reaction of second reactor is 250 ℃～400 ℃, preferred 300 ℃～350 ℃; Reaction pressure is 0MPa～2.0MPa, preferred 0.5MPa～1.5MPa, more preferably 0.8MPa～1.2MPa; Be 1 second～20 seconds duration of contact, is preferably 5 seconds～10 seconds; The mol ratio of HF and HCFC-123 and HCFC-124 is 3～10: 1, is preferably 6～8: 1.The pressure of first reactor and second reactor can be the same or different, and for easy operation, the reaction pressure of preferred two reactors of the present invention is identical.
The main hydrogen fluoride that takes place is fluoridized the reaction that PCE synthesizes HCFC-123 in first reactor, contains in the reacting product stream outside HFC-125, HCFC-123, HCFC-124, the HCl, also contains unreacted PCE and HF.
The reaction that hydrogen fluoride is fluoridized HCFC-123, HCFC-124 mainly takes place in second reactor, contain outside the target product HFC-125 in the product stream, also contain HCFC-124, HCFC-123 as reaction raw materials or reaction product, HCl, HF etc. and as HFC-134a, the CFC-115 of impurity.
The product of first reactor flows to into first distillation tower and separates, the working pressure of first distillation tower is 0.8MPa～1.2MPa, tower top temperature is 70 ℃～100 ℃, tower still temperature is 100 ℃～150 ℃, the cat head component is HCFC-123, HCFC-124, HFC-125, HCl and HF, and tower still component is the PCE that contains small amount of H F.The tower still material of first distillation tower is circulated to first reactor again as part of raw materials.
The cat head component of first distillation tower and the product stream of second reactor are mixed, enter second column then and separate.Tower still component HF and other compositions of second column are separated, and the HF after the separation is circulated to first reactor and second reactor.The cat head component is HCFC-123, HCFC-124, HFC-125, HCl, CFC-115, HFC-134a and a spot of HF.The working pressure of second column is 0.8MPa～1.2MPa, and tower top temperature is 30 ℃～60 ℃, and tower still temperature is 80 ℃～110 ℃.
The after-fractionating cat head component that will contain HCFC-123, HCFC-124, HFC-125, HCl, CFC-115, HFC-134a and a spot of HF enters the 3rd distillation tower, the tower still component that further is separated into the cat head component that contains HFC-125, HCl, CFC-115, small amount of H FC-134a and contains HCFC-123, HCFC-124, HF and HFC-134a.The 3rd distillation tower working pressure be 0.8MPa～1.2MPa, tower top temperature is 20 ℃～-10 ℃, tower still temperature is 40 ℃～80 ℃.
The tower still component of the 3rd distillation tower is circulated to second reactor as reaction raw materials.HFC-134a is circulated to second reactor, reduces the content of CFC-115 in the product.The molar content that the present invention is circulated to the HFC-134a of second reactor be the organic materials total amount 1%～3%.
The 3rd distillation tower cat head component pentafluoride ethane, hydrogenchloride and a spot of 1,1,1,2-Tetrafluoroethane, C2ClF5 enter the purifying products system, after deacidification, dehydration, rectification process, obtain the target product pentafluoride ethane.
Generally speaking, the operational condition of distillation tower can be selected according to the working pressure of the level of equipment, general facilities, reactive system and the isolating composition of desire etc.Among the present invention, the selection of the operating parameters of distillation tower is one of key of feed separation and stable reaction operation.The present invention relates to three distillation towers altogether, and their working pressure can be the same or different, for easy operation, the working pressure of preferred three distillation towers of the present invention is identical, working pressure is 0.2MPa～2.0MPa, preferred 0.5MPa～1.5MPa, more preferably 0.8MPa～1.2MPa.The working pressure of distillation tower and the working pressure of reactive system can be the same or different, and equally for easy operation, the working pressure of the preferred distillation tower of the present invention is consistent with reactive system.The service temperature of distillation tower is formed decision by working pressure and desire are isolating, when the working pressure of three distillation towers is 0.8MPa～1.2MPa, the tower top temperature of first distillation tower is 70 ℃～100 ℃, tower still temperature is 100 ℃～150 ℃, the cat head component is HCFC-123, HCFC-124, HFC-125, HCl and HF, and tower still component is the PCE that contains small amount of H F; The tower top temperature of second column is 30 ℃～60 ℃, and tower still temperature is 80 ℃～110 ℃, and the cat head component is HCFC-123, HCFC-124, HFC-125, HCl, CFC-115, HFC-134a and a spot of HF, and tower still component is HF; The tower top temperature of the 3rd distillation tower is 20 ℃～-10 ℃, and tower still temperature is 40 ℃～80 ℃, and the cat head component is HFC-125, HCl, CFC-115 and small amount of H FC-134a, and the tower still consists of HCFC-123, HCFC-124, a spot of HF and HFC-134a.
By implementing the present invention, fluoridize PCE and generate the reaction of HCFC-123, HCFC-124 and fluoridize the synthetic HFC-125 of HCFC-123, HCFC-124 respectively when different reactor is carried out, the transformation efficiency of PCE per pass conversion and HCFC-123, HCFC-124 all is improved.Simultaneously,, especially fluoridize PCE in lower temperature of reaction because different temperature of reaction are adopted in two reactions, slowed down catalyst surface coking rate, prolonged catalyst life.And HFC-134a is circulated to the molecular balance that the disproportionation reaction that has suppressed HCFC-123 in second reactor generates CFC-115, reduce the content of CFC-115 in the product.The amount of contained CFC-115 changes with working condition in the HFC-125 of gained, but is reduced to 0.5% or lower significantly usually, thereby can produce highly purified HFC-125.
Description of drawings
Accompanying drawing is preparation technology's schema of pentafluoride ethane.
Label meaning in the accompanying drawing is as follows:
Pipeline: 1,2,4,6,7,8,10,11,13,14,15,16,17 and 19; First reactor: 3; First distillation tower: 5; Second column: 9; The 3rd distillation tower: 12; Second reactor: 18.
Embodiment
Embodiment
The present invention is described in more detail with reference to accompanying drawing.The mixture of fresh PCE or PCE and HF is through pipeline 1, enter by pipeline 2 in first reactor 3 that is filled with fluorination catalyst with the HF logistics that recycles through pipeline 10 with through the PCE logistics that pipeline 6 recycles and to react, 280 ℃～330 ℃ of temperature of reaction, reaction pressure 0.8MPa～1.2MPa, 10 seconds～20 seconds duration of contact, mol ratio 6～the 10:1 of hydrogen fluoride and zellon, the reaction product pipeline 4 of flowing through enters first distillation tower 5 and separates, the working pressure of first distillation tower is 0.8MPa～1.2MPa, tower top temperature is 70 ℃～100 ℃, tower still temperature is 100 ℃～150 ℃, the PCE that tower still component contains small amount of H F enters first reactor, cat head component HCFC-123 by pipeline 6 circulations, HCFC-124, HFC-125, HF and HCl are by pipeline 7,8 enter second column 9 separates.The working pressure of second column is 0.8MPa～1.2MPa, tower top temperature is 30 ℃～60 ℃, tower still temperature is 80 ℃～110 ℃, the cat head component of second column 9 is HCFC-123, HCFC-124, HFC-125, HCl, CFC-115, HFC-134a and small amount of H F, enters the 3rd distillation tower by pipeline 11; The tower still component of second column is HF, and its part enters first reactor by pipeline 10 circulations, and its another part enters second reactor 18 by pipeline 15 circulations.The 3rd distillation tower working pressure is 0.8MPa～1.2MPa, tower top temperature is 20 ℃～-10 ℃, tower still temperature is 40 ℃～80 ℃, the 3rd distillation tower cat head component is HFC-125, HCl and section H FC-134a, enter the purifying products system by pipeline 14, by obtaining the HFC-125 product after deacidification, dehydration, the rectification process; The tower still component of the 3rd distillation tower is HCFC-123, HCFC-124, a spot of HF and section H FC-134a, enters second reactor 18 by pipeline 13 circulations.HF, the HCFC-123, HCFC-124 and the small amount of H FC-134a that enter second reactor 18 react under the effect of fluorination catalyst, reaction is 300 ℃～350 ℃ of temperature, reaction pressure 0.8MPa～1.2MPa, 5 seconds～10 seconds duration of contact, hydrogen fluoride and 2-two chloro-1,1,1-Halothane and 2-chloro-1,1,1, the mol ratio 6～8:1 of 2-Tetrafluoroethane, reacting product stream enter second column 9 by pipeline 19,8 to be separated.The fresh PCE that adds enters first reactor through pipeline 1, and the fresh HF that adds enters first reactor and second reactor respectively through pipeline 1,16.
The main streams composition sees Table 1 among the embodiment.
Table 1
| The pipeline logistics | 1 | 4 | 6 | 7 | 10 | 11 | 13 | 14 | 15 | 16 | 19 |
| HF | 50 | 403 | 18 | 385 | 396 | 41 | 41 | ? | 620 | 40 | 672 |
| PCE | 150 | 72 | 72 | ? | ? | ? | ? | ? | ? | ? | ? |
| HCFC-123 | ? | 73 | ? | 73 | 3 | 272 | 272 | ? | 5 | ? | 207 |
| HCFC-124 | ? | 57 | ? | 57 | 1 | 241 | 241 | ? | 2 | ? | 187 |
| HFC-125 | ? | 5 | ? | 5 | ? | 104 | ? | 104 | ? | ? | 99 |
| CFC-115 | ? | ? | ? | ? | ? | 1 | ? | 1 | ? | ? | 1 |
| HFC-134a | ? | ? | ? | ? | ? | 6 | 5 | 1 | ? | ? | 6 |
| HCl | ? | 79 | ? | 79 | ? | 133 | ? | 133 | ? | ? | 54 |
| Other | ? | 1 | ? | 1 | ? | 1 | 1 | ? | ? | ? | ? |
| Total amount (kg/h) | 200 | 690 | 90 | 600 | 400 | 799 | 560 | 239 | 627 | 40 | 1227 |
Claims (3)
1. the preparation method of a pentafluoride ethane is a raw material with hydrogen fluoride and zellon, may further comprise the steps:
A. hydrogen fluoride and zellon enter first reactor, fluoridation takes place in the presence of fluorination catalyst, 200 ℃～350 ℃ of temperature of reaction, comprise 2 of reaction generation in the product stream, 2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1,2-Tetrafluoroethane, pentafluoride ethane, hydrogenchloride and unreacted hydrogen fluoride and zellon;
B. hydrogen fluoride and 2,2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1, the 2-Tetrafluoroethane enters second reactor, further fluoridation in the presence of fluorination catalyst is reacted and is 250 ℃～400 ℃ of temperature, comprises pentafluoride ethane, hydrogenchloride, a spot of C2ClF5,1 of generation in the product stream of second reactor, 1,1,2-Tetrafluoroethane and unreacted hydrogen fluoride, 2,2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1, the 2-Tetrafluoroethane;
C. the product of step a flows to into first distillation tower and separates, and the zellon that the first distillation Tata still is contained low amount of fluorinated hydrogen is circulated to first reactor;
D. the product stream of second reactor is mixed into second column and separates among the step c first distillation tower cat head component and the step b, and the HF part of after-fractionating Tata still is circulated to first reactor, and another part is circulated to second reactor;
E. the pentafluoride ethane of steps d after-fractionating column overhead, hydrogenchloride, 2,2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1,2-Tetrafluoroethane, 1,1,1,2-Tetrafluoroethane and low amount of fluorinated hydrogen enter that the 3rd distillation tower separates, the 3rd distillation Tata still 2,2-two chloro-1,1,1-Halothane, 2-chloro-1,1,1,2-Tetrafluoroethane, 1,1,1,2-Tetrafluoroethane and low amount of fluorinated hydrogen are circulated to second reactor reaction, and are circulated in the above-mentioned material of second reactor 1,1,1, the molar content of 2-Tetrafluoroethane is 1%～3%;
F. step e the 3rd distillation tower cat head component pentafluoride ethane, hydrogenchloride and a spot of 1,1,1,2-Tetrafluoroethane, C2ClF5 enter the purifying products system, after deacidification, dehydration, rectification process, obtain the target product pentafluoride ethane.
2. pentafluoride ethane preparation method according to claim 1 is characterized in that fresh hydrogen fluoride raw material enters first reactor and/or second reactor.
3. pentafluoride ethane preparation method according to claim 1 and 2 is characterized in that the first distillation tower working pressure of step c is 0.8MPa～1.2MPa, and tower top temperature is 70 ℃～100 ℃, and tower still temperature is 100 ℃～150 ℃; The second column working pressure of steps d is 0.8MPa～1.2MPa, and tower top temperature is 30 ℃～60 ℃, and tower still temperature is 80 ℃～110 ℃; The 3rd distillation tower working pressure of step e is 0.8MPa～1.2MPa, and tower top temperature is 20 ℃～-10 ℃, and tower still temperature is 40 ℃～80 ℃.
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| CN107311836A (en) * | 2017-06-09 | 2017-11-03 | 浙江三美化工股份有限公司 | A kind of method that tetrachloro-ethylene prepares pentafluoroethane |
| CN109053365A (en) * | 2018-08-31 | 2018-12-21 | 浙江蓝天环保高科技股份有限公司 | A kind of separator and separation method of fluorine carbon alkane |
| CN108997080B (en) * | 2018-09-11 | 2019-12-24 | 福建省清流县东莹化工有限公司 | Production process for synthesizing pentafluoroethane by two-step gas-phase catalytic fluorination |
| CN109053366B (en) * | 2018-09-18 | 2019-10-11 | 福建省清流县东莹化工有限公司 | A kind of purifying process of a chloropentafluoroethane |
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Address after: 710065 Shaanxi province Xi'an Yanta District Zhang eight road No. 168 Patentee after: Xi'an Inst. of Modern Chemistry Patentee after: Shandong Huaan New Material Co., Ltd. Address before: 710065 Shaanxi province Xi'an Yanta District Zhang eight road No. 168 Patentee before: Xi'an Inst. of Modern Chemistry Patentee before: Zibo Huaan Chemical Co., Ltd. |