CN87209610U - Perfluoropropene reaction device - Google Patents

Perfluoropropene reaction device Download PDF

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Publication number
CN87209610U
CN87209610U CN 87209610 CN87209610U CN87209610U CN 87209610 U CN87209610 U CN 87209610U CN 87209610 CN87209610 CN 87209610 CN 87209610 U CN87209610 U CN 87209610U CN 87209610 U CN87209610 U CN 87209610U
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Prior art keywords
reaction
reactor
tetrafluoroethylene
perfluoropropene
tubular reactor
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CN 87209610
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Chinese (zh)
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季静佳
毕世元
李世雄
吴兴旺
陆钦
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SHANGHAI ORGANIC FLUORINE MATERIAL INST
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SHANGHAI ORGANIC FLUORINE MATERIAL INST
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Priority to CN 87209610 priority Critical patent/CN87209610U/en
Publication of CN87209610U publication Critical patent/CN87209610U/en
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Abstract

The utility model discloses an improved reaction device for preparing the perfluoropropene. The device comprises a pipe type reactor B which can make the tetrafluoroethene and the octafluorocyclobutane change into the perfluoropropene. The utility model is characterized in that a tank type reactor A which is in order to carry out a reversible reaction between the tetrafluoroethene and the octafluorocyclobutane, and the type reactor A positioned at the front of the pipe type reactor B is connected with the pipe type reactor B in series. The device of the utility model is adopted for preparing the perfluoropropene, the self polymerization of the tetrafluoroethene can be reduced to eliminate the 'temperature runaway ' and cemented carbon phenomena in the pipe type reactor B. Thereby, the rate of production of the perfluoropropene is improved 5-10%.

Description

Perfluoropropene reaction device
The utility model relates to a kind of reaction unit for preparing alkenes compounds, particularly relates to a kind of reaction unit for preparing perfluoro propylene.
Perfluoro propylene is one of basic raw material of synthetic fluorine material, especially makes the main raw material of viton, its source easily whether and the price cheap viton industrial expansion prospect that is directly connected to whether.
At present, produce perfluoro propylene and mostly adopt blank pipe (tubular reactor) thermo-cracking tetrafluoroethylene, mainly there is following shortcoming aborning in this class device: the one, and tetrafluoroethylene is at the easy autohemagglutination of thermal decomposition tube ingress, the 2nd, pyrolysis gas is tied carbon easily in the thermal decomposition tube exit, and the 3rd, the poor selectivity of perfluoro propylene.For the productive rate that improves perfluoro propylene and prolong the continuous production cycle, successively proposed low pressure pyrolysis (United States Patent (USP) 2758138) abroad, in tetrafluoroethylene, mixed fluorine carbon high boiling material mixed pyrolysis (United States Patent (USP) 2970176), F 22Single stage method prepares perfluoro propylene (United States Patent (USP) 3306940), injects F in thermal decomposition tube ingress 22With HC1(United States Patent (USP) 3578721) and with the method for water vapor or carbonic acid gas dilution pyrolysis (United States Patent (USP) 1016016 and 1384036).The characteristics of these methods all are to eliminate the productive rate of autohemagglutination and knot carbon phenomenon and then raising perfluoro propylene in the process of preparation perfluoro propylene by the concentration that reduces tetrafluoroethylene.Although these methods can both be improved pyrolytical condition more or less,, therefore can not tackle the problem at its root owing to do not set about improving (form that is still keeping original single tubular reactor) from reaction unit simultaneously.The fact is verified, and these methods have all been brought disadvantages such as the increase of energy consumption and isolating difficulty.
The purpose of this utility model is will provide a kind of can overcome perfluoro propylene reaction unit above-mentioned shortcoming, that improved, so that under the prerequisite of not introducing any thinner, eliminate the autohemagglutination of reactant, the phenomenons such as knot carbon of pyrolysis gas, and then improve the productive rate of perfluoro propylene.
The utility model is to constitute like this, it is a kind of reaction unit for preparing perfluoro propylene, comprise a tubular reactor that makes tetrafluoroethylene change into perfluoro propylene, a tank reactor for carrying out reversible reaction between tetrafluoroethylene and the Perfluorocyclobutane is characterized in that also connecting before this tubular reactor.
Come reaction unit of the present utility model for a more detailed description below in conjunction with the preparation process of accompanying drawing and perfluoro propylene.
Accompanying drawing is the sectional view of the utility model reaction unit.
According to the ultimate principle of chemical reaction engineering, designed the reaction unit that forms by two dissimilar combination of reactors, first reactor is tank reactor A, and second reactor is tubular reactor B, and two reactors link for series connection.Tank reactor A is the reactor that carries out reversible reaction between tetrafluoroethylene and the Perfluorocyclobutane, and tubular reactor B makes tetrafluoroethylene change into the reactor of perfluoro propylene, also is to make Perfluorocyclobutane change into the reaction unit of perfluoro propylene simultaneously.Here the diameter of tank reactor A approximates height, preferably is ball-type, and the volume ratio of this tank reactor A and tubular reactor B is (47~70): (0.67~1).Employed nozzle 3 when the top of tank reactor A is provided with a reactant gases and enters, its external packets are covered with one and are used for coating shape electric furnace 4 that the still reactant gases is heated.The outside of tubular reactor B is also coating a heating electric furnace 5.
Being gaseous phase as the tetrafluoroethylene of reactant or the mixture 1(of tetrafluoroethylene and Perfluorocyclobutane) speed about spinner-type flowmeter 2 and nozzle 3 are with 100 meter per seconds is introduced into tank reactor A.What carry out among the tank reactor A is reversible reaction between tetrafluoroethylene and the Perfluorocyclobutane, but the trend of reaction is to impel Perfluorocyclobutane to increase, its objective is the dividing potential drop of utilizing Perfluorocyclobutane to reduce tetrafluoroethylene in the reaction system, thereby suppress the autohemagglutination of tetrafluoroethylene by the concentration that reduces tetrafluoroethylene.Perfluorocyclobutane itself also can change into perfluoro propylene in addition.Temperature of reaction among the tank reactor A is 300~500 ℃, and the residence time of reactant gases in still is 40~80 seconds.When temperature rose to more than 300 ℃, tetrafluoroethylene can dimerization become Perfluorocyclobutane.This dimerization reaction is strong exothermal reaction, when Perfluorocyclobutane reach a certain amount of after, the reaction heat that this strong exothermal reaction is emitted just is enough to the unstripped gas temperature under the normal temperature is increased to temperature of reaction.High flow rate when these characteristics of tetrafluoroethylene dimerization reaction and unstripped gas enter reactor has been created condition (diameter of tank reactor A approximates highly and preferably is this design of ball-type and then more helps mixing in the still) to reaching the full operating mode of mixing in the tank reactor A.
Then, to enter second reactor be the reaction that tubular reactor B changes into perfluoro propylene to the mixture of tetrafluoroethylene and Perfluorocyclobutane.Tetrafluoroethylene and Perfluorocyclobutane change into perfluoro propylene simultaneously in tubular reactor B, and wherein near the invert point the exit is controlled in 800~950 ℃, and the total residence time of reactant gases in this tubular reactor then was controlled in 0.5~1.2 second.This tubular reactor is a high temperature reaction zone, but the temperature of each point is inconsistent, and the temperature of ingress is lower, and about 600 ℃, the temperature in exit is higher, about 1000 ℃, a temperature distribution that progressively increases progressively is arranged between two-end-point.Because tetrafluoroethylene and the Perfluorocyclobutane temperature when leaving tank reactor and enter tubular reactor can reach 500 ℃, therefore, they just can be heated to rapidly more than 700 ℃ in high temperature reaction zone, thereby their residence time in high temperature reaction zone were foreshortened in 1.2 seconds.Experimental results show that.In tubular reactor B, with regard to the productive rate that the selectivity that improves perfluoro propylene promptly improves perfluoro propylene, the high temperature short residence time(SRT) is better than the low temperature long residence time.This is because at high temperature cascade reaction can take place tetrafluoroethylene, if do not shorten the residence time of tetrafluoroethylene as far as possible in the high-temperature zone, just can not suppress a large amount of generations of other by products, thereby just be difficult to improve the productive rate (volume ratio of tank reactor A and tubular reactor B is (47~70): (0.67~1) can satisfy the requirement of residence time aspect) of perfluoro propylene.
On the other hand, the type of heating of general tubular reactor is the outer heating of pipe, so exists radial temperature profile in the thermal decomposition tube.And tetrafluoroethylene to be reacted into perfluoro propylene be an exothermic process, and this exothermic process aggravated the radial temperature profile of reaction tubes, thereby is easy to generate " temperature runaway " and knot carbon phenomenon.And in reaction unit of the present utility model, the material that enters tubular reactor B has contained the Perfluorocyclobutane of higher proportion, the reaction that utilizes Perfluorocyclobutane to change into perfluoro propylene is these characteristics of thermo-negative reaction, can relax the radial temperature profile of tubular reactor B greatly, thereby reduce the possibility that " temperature runaway " and knot carbon take place among the tubular reactor B.
At last, product gas 6 leads to cooling and refining step.
The entire reaction system is that the reaction pressure among tank reactor A and the tubular reactor B is 30~80 mmhg (gauge pressures), slightly exists pressure difference in the system, but this pressure difference is exceeded towards the direction of regulation is mobile automatically with the reaction gas physical efficiency.
Perfluoropropene reaction unit of the present utility model compares to traditional reaction unit can demonstrate following advantage:
1. the autohemagglutination phenomenon of tetrafluoroethene in pyrolysis system as reactant greatly reduces.
2. relax the temperature runaway phenomenon in the tubular reactor, guaranteed the safe operation of reaction unit.
Basically eliminate the knot carbon phenomenon in tubular reactor exit.
4. the productive rate of perfluoro propylene has improved 5~10%
Process has been carried out series of experiments in this reaction unit as described above, and its result is as shown in the table.
Figure 87209610_IMG2
Annotate: employed unstripped gas only is tetrafluoroethene among the embodiment of table 1.
Figure 87209610_IMG3
Annotate: employed unstripped gas is the mixed feeding of tetrafluoroethene and octafluorocyclobutane among the embodiment of table 2. Temperature among the tank reactor A is 400 ℃, and the time of staying is 70 seconds, and the reaction temperature of tubular reactor B is 850 ℃, and the time of staying is 1 second.

Claims (3)

1, a kind of reaction unit for preparing perfluoro propylene, comprise a tubular reactor B who makes tetrafluoroethylene change into perfluoro propylene, a tank reactor A for carrying out reversible reaction between tetrafluoroethylene and the Perfluorocyclobutane is characterized in that also connecting before this tubular reactor B.
2, reaction unit according to claim 1 is characterized in that the diameter of tank reactor A approximates height, preferably is ball-type.
3, reaction unit according to claim 1 is characterized in that the volume ratio of tank reactor A and tubular reactor B is (47~70): (0.67~1).
CN 87209610 1987-06-26 1987-06-26 Perfluoropropene reaction device Withdrawn CN87209610U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 87209610 CN87209610U (en) 1987-06-26 1987-06-26 Perfluoropropene reaction device

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Application Number Priority Date Filing Date Title
CN 87209610 CN87209610U (en) 1987-06-26 1987-06-26 Perfluoropropene reaction device

Publications (1)

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CN87209610U true CN87209610U (en) 1988-05-11

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CN 87209610 Withdrawn CN87209610U (en) 1987-06-26 1987-06-26 Perfluoropropene reaction device

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CN (1) CN87209610U (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101255092B (en) * 2008-04-09 2011-10-05 宁波巨化化工科技有限公司 Reactor for producing tetrachloroethylene

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101255092B (en) * 2008-04-09 2011-10-05 宁波巨化化工科技有限公司 Reactor for producing tetrachloroethylene

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