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CN102001910B - Method for preparing 2,3,3,3-tetrafluoropropene - Google Patents

Method for preparing 2,3,3,3-tetrafluoropropene Download PDF

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CN102001910B
CN102001910B CN 201010286960 CN201010286960A CN102001910B CN 102001910 B CN102001910 B CN 102001910B CN 201010286960 CN201010286960 CN 201010286960 CN 201010286960 A CN201010286960 A CN 201010286960A CN 102001910 B CN102001910 B CN 102001910B
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CN102001910A (en
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王博
吕剑
张伟
曾纪珺
马洋博
杜咏梅
袁俊
徐强
封利民
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Shandong Huaan Modern Environmental Protection Technology Co., Ltd.
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Xian Modern Chemistry Research Institute
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Abstract

The invention discloses a method for preparing 2,3,3,3-tetrafluoropropene, comprising the following steps: a. in the presence of a fluorinated catalyst, hydrogen fluoride and 1,1,2,3-tetrafluoropropene enter into a first reactor to react; b. in the presence of the fluorinated catalyst, 2-chloro-3,3,3 trifluoropropene, 2-chloro-1,1,1,2-tetrafluoropropane, 1,1,1,2,2-pentafluoropropane and hydrogen fluoride enter into a second reactor to react; c. the product flows obtained in the steps a and b enter into a first distillation tower to be separated; the tower top components are hydrogen chloride and 2,3,3,3-tetrafluoropropene which break away from the system and others are column reactor components; and d. the column reactor components in the step c enter into a second distillation tower to be separated; the column reactor components include 2-chloro-3,3,3 trifluoropropene and 2-chloro-1,1,1,2-tetrafluoropropane which are recycled to the second reactor; and the tower top components, including hydrogen fluoride and 1,1,1,2,2-pentafluoropropane, are recycled to the first reactor or/and the second reactor to be used.

Description

The preparation method of 2,3,3,3-tetrafluoeopropene
Technical field
The present invention relates to a kind of 2,3,3, the preparation method of 3-tetrafluoeopropene (HFO-1234yf) relates in particular to a kind of under the existence of fluorination catalyst, with 1,1,1,2,2-pentachloropropane (HCC-240ab) or 2,3,3,3-tetrachloro propylene is raw material, obtains 2,3 through two step gas phase fluorination, the preparation method of 3,3-tetrafluoeopropene.
Background technology
At present, HFA 134a (HFC-134a) is widely used in the mobile air conditioner refrigeration system, because the latent value (GWP) of its Greenhouse effect is 1430, can cause global warming, needs the new needs of substitute to conform of exploitation.
2,3,3,3-tetrafluoeopropene, the ozone depletion value (ODP) of diving is zero, and GWP is 4, and atmospheric lifetime is only 11 days, has good physical and chemical performance, is considered to directly substitute the economical scheme of HFC-134a.US Patent No. 2009024009 discloses the method for synthetic HFO-1234yf a kind of.The method is raw material with 1,1,2,3-tetrachloro propylene or HCC-240db, at first at Cr 2O 3Under the existence of catalyzer, carry out HF gas phase fluorination 1,1,2 in the first reactor, 3-tetrachloro propylene obtains 2-chloro-3,3,3 ,-trifluoropropene (HCFC-1233xf), then at SbCl 5Under effect, liquid-phase fluorination HCFC-1233xf obtains 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) in the second reactor, at last in the 3rd reactor HCFC-244bb at CsCl/MgF 2Under existence, 350 ℃～550 ℃ dehydrochlorinations obtain HFO-1234yf.But the method reactions steps is more, total three-step reaction, and also the second step reaction is liquid phase reaction, needs isolation of intermediate products HCFC-244bb, as the raw material of three-step reaction.。
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiency that exists in background technology, provides a kind of with 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene are raw material, need not the separation of intermediate product, reactions steps less 2,3,3, the preparation method of 3-tetrafluoeopropene.
In order to solve the problems of the technologies described above, the present invention is raw material with 1,1,1,2,2-pentachloropropane (HCC-240ab) or 2,3,3,3-tetrachloro propylene, adopts the standby HFO-1234yf of gas phase catalytic fluorination legal system, and the principal reaction of generation is as follows:
CCl 3CCl 2CH 3+3HF——→CF 3CCl＝CH 2+4HCl (1)
CCl 3CCl＝CH 2+3HF——→CF 3CCl＝CH 2+3HCl (2)
CF 3CCl＝CH 2+HF→CF 3CFClCH 3 (3)
CF 3CFClCH 3→CF 3CF＝CH 2+HCl (4)
The main side reaction that occurs:
CF 3CFClCH 3+HF→CF 3CF 2CH 3+HCl (5)
Figure DEST_PATH_GSB00001088610300011
The present invention adopts two reactors, and the first reactor mainly carries out hydrogen fluoride (HF) and fluoridizes HCC-240ab or 2,3,3, the reaction of 3-tetrachloro propylene, react (1) and (2) is under suitable reaction conditions, HCC-240ab or 2, the transformation efficiency of 3,3,3-tetrachloro propylene 〉=90%, even can reach 100%, primary product is HCFC-1233xf; The second reactor mainly carries out the reaction of reaction that HF fluoridizes HCFC-1233xf and HCFC-244bb, HFC-245cb dehydrochlorination, (3) and (4) react, HCFC-244bb can occur simultaneously fluoridize generation 1,1,1, the side reaction (5) of 2,2-pentafluoropropane (HFC-245cb) and HFO-1234yf and HF addition generate the side reaction (6) of HFC-245cb.The present invention loops back in the second reactor reaction to generate more HFO-1234yf with intermediate product HCFC-244bb and HFC-245cb.
The invention provides a kind ofly 2,3,3, the preparation method of 3-tetrafluoeopropene comprises the following steps:
A. hydrogen fluoride, 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene enters the first reactor, reacts under the existence of fluorination catalyst, and reaction conditions is: reaction pressure 0.1MPa～1.0MPa, hydrogen fluoride and 1,1, the mol ratio 5～20 of 1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene; 2 seconds～30 seconds duration of contact; 220 ℃～350 ℃ of temperature of reaction; The product stream that obtains comprises 2-chloro-3,3,3 trifluoro propenes, the 2-chloro-1,1,1,2-tetrafluoropropane, 1,1,1,2 that reaction generates, 2-pentafluoropropane, hydrogenchloride and unreacted hydrogen fluoride and 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene;
B.2-chloro-3,3, and 3 trifluoro propenes, 2-chloro-1,1,1,2-tetrafluoropropane and 1,1,1,2,2-pentafluoropropane and hydrogen fluoride enter the second reactor, react under the existence of fluorination catalyst, and reaction conditions is: reaction pressure 0.1MPa～1.0MPa; The mol ratio 2～15 of hydrogen fluoride and 2-chloro-3,3,3 trifluoro propenes, 2-chloro-1,1,1,2-tetrafluoropropane and 1,1,1,2,2-pentafluoropropane total amount; 5 seconds～30 seconds duration of contact; 300 ℃～380 ℃ of temperature of reaction; Product stream comprises 2,3,3,3-tetrafluoeopropene, 1,1,1,2,2-pentafluoropropane, 2-chloro-1,1,1,2-tetrafluoropropane, 2-chloro-3,3,3 ,-trifluoropropene and hydrogenchloride and hydrogen fluoride;
C. the product stream of step a enters the first distillation tower separation, the tower reactor component comprises hydrogen fluoride, HCFC-1233xf, HCFC-244bb, HFC-245cb, HFO-1234yf and unreacted 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene, the tower top component is hydrogenchloride, breaks away from reactive system, enters acid making system and makes hydrochloric acid;
D. the tower reactor component of step c enters phase separator and is separated, phase separation temperature is-30 ℃～10 ℃, 1,1,1 of phase separator lower floor, 2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene is circulated to the first reactor, and hydrogen fluoride, HCFC-1233xf, HCFC-244bb, HFC-245cb and the HFO-1234yf on phase separator upper strata enters second column together with the product stream of step b separates;
E. second column tower reactor component 2-chloro-3,3,3 ,-trifluoropropene, 2-chloro-1,1,1,2-tetrafluoropropane and hydrogen fluoride are circulated to the second reactor, tower top component hydrogenchloride, 1,1,1,2,2-pentafluoropropane and 2,3,3,3-tetrafluoeopropene enter the 3rd distillation tower and separate;
F. the 3rd distillation tower tower reactor component 1,1,1,2, the 2-pentafluoropropane is circulated to the second reactor, tower top component hydrogenchloride and 2,3,3,3-tetrafluoeopropene break away from reactive system, enter the purifying products system, through deacidification, dehydration, rectification process, obtain target product 2,3,3, the 3-tetrafluoeopropene.
The reaction conditions of the present invention's the first reactor is preferably: the mol ratio 10～15 of reaction pressure 0.3～0.6MPa, hydrogen fluoride and 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene; 6 seconds～10 seconds duration of contact; 260 ℃～300 ℃ of temperature of reaction; The reaction conditions of the second reactor is preferably: reaction pressure 0.3MPa～0.6MPa; The mol ratio 5～8 of hydrogen fluoride and 2-chloro-3,3,3 ,-trifluoropropene, 2-chloro-1,1,1,2-tetrafluoropropane and 1,1,1,2,2-pentafluoropropane total amount; 10 seconds～15 seconds duration of contact; 330 ℃～360 ℃ of temperature of reaction.
The operational condition not restriction of the present invention to distillation tower can suitably be selected according to the level of equipment, general facilities, the working pressure of reactive system and the composition that wish is separated etc.Working pressure is 0.1MPa～1.0MPa, preferred 0.3MPa～0.6MPa.Generally, for easy and simple to handle, the working pressure of distillation tower is consistent with reactive system.Tower top temperature and tower reactor temperature are determined by working pressure and material component thereof.
In the present invention, fresh HF raw material can or enter reactive system by the first reactor, the second reactor simultaneously by any one reactor in the first reactor, the second reactor.
The present invention is to not restriction of the catalyzer in fluoridation, any known fluorination catalyst all is applicable to the present invention, such as: chromic oxide, chromium fluoride, the chromic oxide of fluoridizing, aluminum fluoride, the aluminum oxide of fluoridizing, be carried on chromic oxide on gac, aluminum fluoride, magnesium fluoride, contain chromic oxide and the activated carbon supported SbCl of various metals (as Zn, Co, Ni, Ge, In etc.) 5Or TiCl 4Deng.The fluorination catalyst that adopts is different, and reaction conditions is different, comprises the mol ratio of temperature of reaction, reaction pressure, duration of contact and material.The preferential chromium-based fluorination catalyst that contains Al, Zn, Mg, Ni metal powder that adopts of the present invention, catalytic activity is good, and selectivity is high, and regenerability is good, and entire life is long.Chinese patent CN1651137A is seen in the preparation that contains the chromium-based catalysts of Al, Zn, Mg, Ni metal powder.
The type of reactor that the present invention is used for fluoridation is not crucial, any suitable gas phase fluorination device all is applicable to the present invention, and the present invention preferentially selects the material calandria type fixed bed reactor made of nickel and alloy (comprising Hastelloy, Inconel, Incoloy and Monel) thereof for example with anti-hydrogen fluoride corrosion effect.
Advantage of the present invention:
Of the present invention 2,3,3,3-tetrafluoeopropene preparation method is with 1,1,1,2,2-pentachloropropane (HCC-240ab) or 2,3,3,3-tetrachloro propylene is raw material, the gas phase catalytic fluorination successive reaction, avoided the second step liquid-phase fluorination process of prior art and the sepn process of intermediate product HCFC-244bb, reactions steps is less, and reactions steps of the present invention was two steps.And the reactions steps of the method for documents was three steps.
Description of drawings
Fig. 1 represents preparation technology's schema of 2,3,3,3-tetrafluoeopropene.
Label meaning in Fig. 1 is as follows.Pipeline: 1,2,4,6,7,9,11,13,14,15,16,17,19 and 20; The first reactor: 3; The first distillation tower: 5; Phase separator: 8; Second column: 10; The 3rd distillation tower: 12; The second reactor: 18.
Embodiment
The present invention is described in more detail with reference to accompanying drawing.Fresh HCC-240ab or 2, the mixture of 3,3,3-tetrachloro propylene and HF is through pipeline 1, enter in the first reactor 3 that is filled with fluorination catalyst by pipeline 2 together with the logistics that recycles through pipeline 20 and react, the reaction product pipeline 4 of flowing through enters the first distillation tower 5 and separates.
The first distillation tower tower top component is that HCl enters acid making system by pipeline 6 and makes hydrochloric acid, the tower reactor component is HF, HCFC-1233xf, HCFC-244bb, HFC-245cb, HFO-1234yf and unreacted HCC-240ab or 2,3,3,3-tetrachloro propylene, by pipeline 7, enter phase separator 8 and be separated; The unconverted HCC-240ab of phase separator lower floor or 2,3,3,3-tetrachloro propylene, enter the first reactor via pipeline 21 circulations and continue reaction, the phase separator upper materials comprises HF, HCFC-1233xf and a small amount of HCFC-244bb, HFC-245cb, HFO-1234yf, enters second column 10 by pipeline 9 together with the second reactor outlet material pipeline 19 and separates.
The tower reactor component of second column is that HF, HCFC-1233xf, HCFC-244bb and a small amount of HFC-245cb enter the second reactor reaction by pipeline 15; The tower top component of second column is HFC-245cb, HFO-1234yf, HCl and a small amount of HF, enters the 3rd distillation tower 12 by pipeline 11 and separates.
The 3rd distillation tower tower top component is HFO-1234yf and HCl, enters the purifying products system by pipeline 14, by obtaining the HFO-1234yf product after deacidification, dehydration, rectification process; The 3rd distillation tower tower reactor component is HFC-245cb, a small amount of HF and part HFO-1234yf, enters the second reactor 18 after the logistics of the tower reactor by pipeline 13 and second column by pipeline 15 circulations mixes and carries out second step and react.Reacting product stream enters second column 10 by pipeline 19 to be separated.The fresh HCC-240ab that adds or 2,3,3,3-tetrachloro propylene enter the first reactor through pipeline 1, and the fresh HF that adds enters respectively the first reactor and the second reactor through pipeline 1,16.
Embodiment 1
Add 60 milliliters of chromium-based fluorination catalysts that contain Al, Zn, Mg, Ni in internal diameter is the carbon steel pipe of 38mm, method for preparing catalyst is seen Chinese patent CN1651137A.The first reactor is warming up to 260 ℃, passes into HF and 1,1,1,2,2-pentachloropropane (HCC-240ab) is reacted, and the mol ratio of controlling HF and HCC-240ab is 10, be 6 seconds duration of contact, reaction pressure 0.1MPa, after reaction 20h, reaction product is after washing, alkali cleaning, alkali drying are removed HCl and HF, with organic composition in the gas chromatographic analysis reaction product, the results are shown in Table 1.
Embodiment 2
Operation substantially the same manner as Example 1, difference are that the temperature of reaction with the first reactor changes 220 ℃ into, the results are shown in Table 1.
Embodiment 3
Operation substantially the same manner as Example 1, difference are that the temperature of reaction with the first reactor changes 300 ℃ into, the results are shown in Table 1.
Embodiment 4
Operation substantially the same manner as Example 1, difference are that the temperature of reaction with the first reactor changes 350 ℃ into, the results are shown in Table 1.
Embodiment 5
Operation substantially the same manner as Example 1, difference are to change 2 seconds duration of contact into, to the results are shown in Table 1.
Embodiment 6
Operation substantially the same manner as Example 1, difference are to change 10 seconds duration of contact into, to the results are shown in Table 1.
Embodiment 7
The operation identical with embodiment basic 1, difference are to change 30 seconds duration of contact into, to the results are shown in Table 1.
Embodiment 8
Operation substantially the same manner as Example 1, difference are that the mol ratio with HF and HCC-240ab changes 5 into, the results are shown in Table 1.
Embodiment 9
Operation substantially the same manner as Example 1, difference are that the mol ratio with HF and HCC-240ab changes 15 into, the results are shown in Table 1.
Embodiment 10
Operation substantially the same manner as Example 1, difference are that the mol ratio with HF and HCC-240ab changes 20 into, the results are shown in Table 1.
Embodiment 11
Operation substantially the same manner as Example 1, difference are to change reaction pressure into 0.3MPa, the results are shown in Table 1.
Embodiment 12
Operation substantially the same manner as Example 1, difference are to change reaction pressure into 0.6MPa, the results are shown in Table 1.
Embodiment 13
Operation substantially the same manner as Example 1, difference are to change reaction pressure into 1.0MPa, the results are shown in Table 1.
Embodiment 14
Operation substantially the same manner as Example 1, difference are with raw material 1,1,1,2, and the 2-pentachloropropane changes 2,3,3,3-tetrachloro propylene into and reacts, and the results are shown in Table 1.
Table 1
Figure BSA00000276848900061
Other product comprises CF 3CFClCH 3(HCFC-244bb), CF 3CF 2CH 3(HFC-245cb) and the trace CF 3CHClCHF 2(HCFC-244db), CF 3CHFCH 2F (HFC-245eb) etc.
Embodiment 15
In being the carbon steel pipe of 38mm, internal diameter adds 50 milliliters of chromium-based fluorination catalysts that contain Al, Zn, Mg, Ni, method for preparing catalyst is seen Chinese patent CN1651137A, the second reactor is warming up to 360 ℃, pass into HF and HCFC-1233xf reacts, the mol ratio of controlling HF and HCFC-1233xf is 5, be 10 seconds duration of contact, reaction pressure 0.1MPa, after reaction 20h, reaction product is after HCl and HF are removed in washing, alkali cleaning, with organic composition in the gas chromatographic analysis reaction product, the results are shown in Table 2.
Embodiment 16
The operation identical with embodiment basic 15, difference are that the temperature of reaction with the second reactor changes 300 ℃ into, the results are shown in Table 2.
Embodiment 17
The operation identical with embodiment basic 15, difference are that the temperature of reaction with the second reactor changes 330 ℃ into, the results are shown in Table 2.
Embodiment 18
The operation identical with embodiment 15, difference are that the temperature of reaction with the second reactor changes 380 ℃ into, the results are shown in Table 2.
Embodiment 19
The operation identical with embodiment basic 15, difference are to change 5 seconds duration of contact into, to the results are shown in Table 2.
Embodiment 20
The operation identical with embodiment basic 15, difference are to change 15 seconds duration of contact into, to the results are shown in Table 2.
Embodiment 21
The operation identical with embodiment basic 15, difference are to change 30 seconds duration of contact into, to the results are shown in Table 2.
Embodiment 22
The operation identical with embodiment basic 15, difference changes the mol ratio of HF and HCFC-1233xf into 2 and the results are shown in Table 2.
Embodiment 23
The operation identical with embodiment basic 15, difference changes the mol ratio of HF and HCFC-1233xf into 8, the results are shown in Table 2.
Embodiment 24
The operation identical with embodiment basic 15, difference changes the mol ratio of HF and HCFC-1233xf into 15, the results are shown in Table 2.
Embodiment 25
The operation identical with embodiment basic 15, difference changes reaction pressure into 0.3MPa, the results are shown in Table 2.
Embodiment 26
Operation substantially the same manner as Example 15, difference changes reaction pressure into 0.6MPa, the results are shown in Table 2.
Embodiment 27
Operation substantially the same manner as Example 15, difference changes reaction pressure into 1.0MPa, the results are shown in Table 2.
Table 2
Figure BSA00000276848900081
Other product comprises CF 3CFClCH 3(HCFC-244bb), CF 3CF 2CH 3(HFC-245cb) and the trace CF 3CHClCHF 2(HCFC-244db), CF 3CHFCH 2F (HFC-245eb) etc.
Embodiment 27
in being the carbon steel pipe of 38mm, internal diameter add 50 milliliters to contain Al, Zn, Mg, the chromium-based fluorination catalyst of Ni, method for preparing catalyst is seen Chinese patent CN1651137A, be warming up to 360 ℃, pass into HCFC-1233xf, HCFC-244bb, HFC-245cb and HF react, control HFC-245cb, the molar ratio of HCFC-244bb and HCFC-1233xf 0.1: 0.2: 1, HF and mol ratio (HCFC-1233xf+HCFC-244bb+HFC-245cb) are 5, be 10 seconds duration of contact, reaction pressure 0.1MPa, after reaction 20h, reaction product is through washing, after HCl and HF are removed in alkali cleaning, with organic composition in the gas chromatographic analysis reaction product, the results are shown in Table 3.
Embodiment 28
Operation substantially the same manner as Example 27, difference changes the molar ratio of HFC-245cb, HCFC-244bb and HCFC-1233xf into 0.2: 0.5: 1, the results are shown in Table 3.
Embodiment 29
Operation substantially the same manner as Example 27, difference changes the molar ratio of HFC-245cb, HCFC-244bb and HCFC-1233xf into 0.5: 0.1: 1, the results are shown in Table 3.
Embodiment 30
Operation substantially the same manner as Example 27, difference changes the molar ratio of HF ℃-245cb, HCFC-244bb and HCFC-1233xf into 0.5: 0.5: 1, the results are shown in Table 3.
Table 3
Figure BSA00000276848900091
Other product comprises CF 3CFClCH 3(HCFC-244bb), CF 3CF 2CH 3(HFC-245cb) and the trace CF 3CHClCHF 2(HCFC-244db), CF 3CHFCH 2F (HFC-245eb) etc.

Claims (2)

1. one kind 2,3,3, the preparation method of 3-tetrafluoeopropene, the method is raw material with 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene, comprises the following steps:
A. hydrogen fluoride, 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene enters the first reactor, reacts under the existence of fluorination catalyst, and reaction conditions is: reaction pressure 0.1MPa～1.0MPa, hydrogen fluoride and 1,1, the mol ratio 5～20 of 1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene; 2 seconds～30 seconds duration of contact; 220 ℃～350 ℃ of temperature of reaction; The product stream that obtains comprises 2-chloro-3,3,3 trifluoro propenes, the 2-chloro-1,1,1,2-tetrafluoropropane, 1,1,1,2 that reaction generates, 2-pentafluoropropane, hydrogenchloride and unreacted hydrogen fluoride and 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene;
B.2-chloro-3,3, and 3 trifluoro propenes, 2-chloro-1,1,1,2-tetrafluoropropane and 1,1,1,2,2-pentafluoropropane and hydrogen fluoride enter the second reactor, react under the existence of fluorination catalyst, and reaction conditions is: reaction pressure 0.1MPa～1.0MPa; The mol ratio 2～15 of hydrogen fluoride and 2-chloro-3,3,3 trifluoro propenes, 2-chloro-1,1,1,2-tetrafluoropropane and 1,1,1,2,2-pentafluoropropane total amount; 5 seconds～30 seconds duration of contact; 300 ℃～380 ℃ of temperature of reaction; Product stream comprises 2,3,3,3-tetrafluoeopropene, 1,1,1,2,2-pentafluoropropane, 2-chloro-1,1,1,2-tetrafluoropropane, 2-chloro-3,3,3 ,-trifluoropropene and hydrogenchloride and hydrogen fluoride;
C. the product stream of step a enters the first distillation tower separation, the tower reactor component comprises hydrogen fluoride, HCFC-1233xf, HCFC-244bb, HFC-245cb, HFO-1234yf and unreacted 1,1,1,2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene, the tower top component is hydrogenchloride, breaks away from reactive system, enters acid making system and makes hydrochloric acid;
D. the tower reactor component of step c enters phase separator and is separated, phase separation temperature is-30 ℃～10 ℃, 1,1,1 of phase separator lower floor, 2,2-pentachloropropane or 2,3,3,3-tetrachloro propylene is circulated to the first reactor, and hydrogen fluoride, HCFC-1233xf, HCFC-244bb, HFC-245cb and the HFO-1234yf on phase separator upper strata enters second column together with the product stream of step b separates;
E. second column tower reactor component 2-chloro-3,3,3 ,-trifluoropropene, 2-chloro-1,1,1,2-tetrafluoropropane and hydrogen fluoride are circulated to the second reactor, tower top component hydrogenchloride, 1,1,1,2,2-pentafluoropropane and 2,3,3,3-tetrafluoeopropene enter the 3rd distillation tower and separate;
F. the 3rd distillation tower tower reactor component 1,1,1,2, the 2-pentafluoropropane is circulated to the second reactor, tower top component hydrogenchloride and 2,3,3,3-tetrafluoeopropene break away from reactive system, enter the purifying products system, through deacidification, dehydration, rectification process, obtain target product 2,3,3, the 3-tetrafluoeopropene.
2. according to claim 12,3,3, the preparation method of 3-tetrafluoeopropene, the reaction conditions that it is characterized in that the first reactor described in step a is: reaction pressure 0.3MPa～0.6MPa, hydrogen fluoride and 1,1,1,2, the mol ratio 10～15 of 2-pentachloropropane or 2,3,3,3-tetrachloro propylene; 6 seconds～10 seconds duration of contact; 260 ℃～300 ℃ of temperature of reaction; The reaction conditions of the second reactor described in step b is: reaction pressure 0.3MPa～0.6MPa; The mol ratio 5～8 of hydrogen fluoride and 2-chloro-3,3,3 ,-trifluoropropene, 2-chloro-1,1,1,2-tetrafluoropropane and 1,1,1,2,2-pentafluoropropane total amount; 10 seconds～15 seconds duration of contact; 330 ℃～360 ℃ of temperature of reaction.
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