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US5243105A Expired / Lapsed US ⏱️ 0.0 years remaining

Chemical process

Assignee: Ineos Fluor Holdings Ltd
•
Filing: 1991-12-11
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Granted: 1993-09-07
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Expires: 2011-12-11
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Abstract

Abstract 1,1,1,2-tetrafluoroethane (HFA 134a) is manufactured from trichloroethylene by a two-stage process comprising reacting trichloroethylene with hydrogen fluoride under superatmospheric pressure in a first reaction zone to form 1,1,1-trifluoro-2-chloroethane (133a) and reacting the 1,1,1-trifluoro-2-chloroethane with hydrogen fluoride in a second reaction zone to form 1,1,1,2-tetrafluoroethane; the entire product stream from the 133a reaction zone together with additional HF of required is fed through the 134a reaction zone. The two reaction zones may be provided within a single reaction vessel.

Inventors

  • 👤 John D. Scott
  • 👤 Rachel A. Steven

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-04 22:29
CPC Classifications
C; C07; C07C; C07C19/00; C07C19/08; C07C17/00; C07C17/093; C07C17/20; C07C17/202; C07C17/206; C07C17/21

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 160 words
A method for the manufacture of 1,1,1,2-tetrafluoroethane which comprises the steps of: (A) contacting a mixture of trichloroethylene and hydrogen fluoride with a fluorination catalyst under superatmospheric pressure at a temperature in the range of about 200° to 400° C. in a first reaction zone to form a product containing 1,1,1-trifluoro-2-chloroethane and hydrogen chloride together with unreacted starting materials, (B) passing product of step (A) together with hydrogen fluoride to a second reaction zone containing a fluorination catalyst at a temperature in the range of about 280°-450° C. but higher than the temperature in step (A) to form a product containing 1,1,1,2-tetrafluoroethane, 1,1,1-trifluoro-2-chloroethane and hydrogen chloride, (C) treating the product of step (B) to separate 1,1,1,2-tetrafluoroethane and hydrogen chloride from 1,1,1-trifluoro-2-chloroethane and unreacted hydrogen fluoride, (D) feeding the 1,1,1-trifluoro-2-chloroethane mixture obtained from step (C) together with trichloroethylene and hydrogen fluoride to said first reaction zone (step (A)), and (E) recovering the 1,1,1,2-tetrafluoroethane and hydrogen chloride separated out in step (C).
Claim 2
Independent Claim 160 words
A method for the manufacture of 1,1,1,2-tetrafluoroethane which comprises the steps of: (A) contacting a mixture of trichloroethylene and hydrogen fluoride with a fluorination catalyst under superatmospheric pressure at a temperature in the range of about 200° to 400° C. in a first reaction zone to form a product containing 1,1,1-trifluoro-2-chloroethane and hydrogen chloride together with unreacted starting materials, (B) passing product of step (A) together with hydrogen fluoride to a second reaction zone containing a fluorination catalyst at a temperature in the range of about 280°-450° C. but higher than the temperature in step (A) to form a product containing 1,1,1,2-tetrafluoroethane, 1,1,1-trifluoro-2-chloroethane and hydrogen chloride, (C) treating the product of step (B) to separate 1,1,1,2-tetrafluoroethane and hydrogen chloride from 1,1,1-trifluoro-2-chloroethane and unreacted hydrogen fluoride, (D) feeding the 1,1,1-trifluoro-2-chloroethane mixture obtained from step (C) together with trichloroethylene and hydrogen fluoride to said first reaction zone (step (A)), and (E) recovering the 1,1,1,2-tetrafluoroethane and hydrogen chloride separated out in step (C).
Claim 3
Dependent Claim 29 words
A method as claimed in claim 1, wherein 15 to 60 moles of hydrogen fluoride per mole of trichloroethylene are fed into the first reaction zone in step (A).
Claim 4
Dependent Claim 32 words
A method as claimed in claim 1 or claim 2 wherein the temperature in the first reaction zone in step A is in the range of from 220° C. to 350° C.
Claim 5
Dependent Claim 29 words
A method as claimed in claim 1 wherein 2 to 6 moles of hydrogen fluoride per mole of 1,1,1-trifluoro-2-chloroethane are fed into the second reaction zone in step (B).
Claim 6
Dependent Claim 29 words
A method as claimed in claim 1 wherein the temperature in the second reaction zone in step (B) is in the range of from 305° C. to 385° C.
Claim 7
Dependent Claim 25 words
A method as claimed in claim 1 wherein the contact time in step (A) and in step (B) is from 5 seconds to 30 seconds.
Claim 8
Dependent Claim 29 words
A method as claimed in claim 1 wherein the reactions in step (A) and step (B) are carried out at a pressure of from 5 bars to 20 bars.
Claim 9
Dependent Claim 11 words
A method as claimed in claim 1 which is operated continuously.
Claim 10
Dependent Claim 19 words
A method as claimed in claim 1 wherein said first and second reaction zones are provided by adiabatic reactors.
Claim 11
Dependent Claim 54 words
A method as claimed in claim 1 wherein the trichloroethylene fed into the first reaction zone in step (A) together with the product stream from step (B) is added to said product stream from step (B) in order to heat the trichloroethylene and cool the product stream in advance of the first reaction zone.
Claim 12
Independent Claim 143 words
A method for the manufacture of 1,1,1,2-tetrafluoroethane which comprises the steps of: (A) contacting a mixture of trichloroethylene and hydrogen fluoride with a fluorination catalyst under superatmospheric pressure at a temperature in the range of about 200° to 400° C. in a first reaction zone to form a product containing 1,1,1-trifluoro-2-chloroethane and hydrogen chloride together with unreacted starting materials, (B) passing the 1,1,1-trifluoro-2-chloroethane obtained in step (A) together with hydrogen fluoride to a second reaction zone containing a fluorination catalyst at a temperature in the range of about 280°-450° C. but higher than the temperature in step (A) to form a product containing 1,1,1,2-tetrafluoroethane, 1,1,1-trifluoro-2-chloroethane and hydrogen chloride, (C) treating the product of step (B) to separate 1,1,1,2-tetrafluoroethane from 1,1,1-trifluoro-2-chloroethane and unreacted hydrogen fluoride, and (D) feeding the 1,1,1-trifluoro-2-chloroethane obtained from step (C) and hydrogen fluoride to said first reaction zone step (A).
Claim 13
Independent Claim 143 words
A method for the manufacture of 1,1,1,2-tetrafluoroethane which comprises the steps of: (A) contacting a mixture of trichloroethylene and hydrogen fluoride with a fluorination catalyst under superatmospheric pressure at a temperature in the range of about 200° to 400° C. in a first reaction zone to form a product containing 1,1,1-trifluoro-2-chloroethane and hydrogen chloride together with unreacted starting materials, (B) passing the 1,1,1-trifluoro-2-chloroethane obtained in step (A) together with hydrogen fluoride to a second reaction zone containing a fluorination catalyst at a temperature in the range of about 280°-450° C. but higher than the temperature in step (A) to form a product containing 1,1,1,2-tetrafluoroethane, 1,1,1-trifluoro-2-chloroethane and hydrogen chloride, (C) treating the product of step (B) to separate 1,1,1,2-tetrafluoroethane from 1,1,1-trifluoro-2-chloroethane and unreacted hydrogen fluoride, and (D) feeding the 1,1,1-trifluoro-2-chloroethane obtained from step (C) and hydrogen fluoride to said first reaction zone step (A).
Claim 14
Dependent Claim 102 words
In a method for producing 1,1,1,2-tetrafluoroethane in two reaction stages involving (1) the reaction of trichloroethylene and hydrogen fluoride to produce 1,1,1-trifluoro-2-chloroethane and (2) the reaction of 1,1,1-trifluoro-2-chloroethane with hydrogen fluoride to produce 1,1,1,2-tetrafluoroethane, the improvement which comprises carrying out the reaction (2) between 1,1,1-trifluoro-2-chloroethane and hydrogen fluoride at superatmospheric pressure and at a temperature in the range of 280°-450° C., carrying out the reaction (1) between trichloroethylene and hydrogen fluoride at a temperature in the range of 200°-400° C. and below that used in reaction (2), and recycling unconverted 1,1,1-trifluoro-2-chloroethane with hydrogen fluoride for further reaction in the presence of trichloroethylene.
Claim 15
Dependent Claim 102 words
In a method for producing 1,1,1,2-tetrafluoroethane in two reaction stages involving (1) the reaction of trichloroethylene and hydrogen fluoride to produce 1,1,1-trifluoro-2-chloroethane and (2) the reaction of 1,1,1-trifluoro-2-chloroethane with hydrogen fluoride to produce 1,1,1,2-tetrafluoroethane, the improvement which comprises carrying out the reaction (2) between 1,1,1-trifluoro-2-chloroethane and hydrogen fluoride at superatmospheric pressure and at a temperature in the range of 280°-450° C., carrying out the reaction (1) between trichloroethylene and hydrogen fluoride at a temperature in the range of 200°-400° C. and below that used in reaction (2), and recycling unconverted 1,1,1-trifluoro-2-chloroethane with hydrogen fluoride for further reaction in the presence of trichloroethylene.
Claim 16
Dependent Claim 98 words
In a method for producing 1,1,1,2-tetrafluoroethane in two reaction stages involving (1) the reaction of trichloroethylene and hydrogen fluoride to produce 1,1,1-trifluoro-2-chloroethane and (2) the reaction of 1,1,1-trifluoro-2-chloroethane with hydrogen fluoride to produce 1,1,1,2-tetrafluoroethane, the improvement which comprises carrying out the reaction (2) between 1,1,1-trifluoro-2-chloroethane and hydrogen fluoride at a temperature in the range of 280°-450° C., carrying out the reaction (1) between trichloroethylene and hydrogen fluoride at a temperature in the range of 200°-400° C. and below that used in reaction (2), and recycling unconverted 1,1,1-trifluoro-2-chloroethene with hydrogen fluoride for further reaction in the presence of trichloroethylene.
Claim 17
Dependent Claim 98 words
In a method for producing 1,1,1,2-tetrafluoroethane in two reaction stages involving (1) the reaction of trichloroethylene and hydrogen fluoride to produce 1,1,1-trifluoro-2-chloroethane and (2) the reaction of 1,1,1-trifluoro-2-chloroethane with hydrogen fluoride to produce 1,1,1,2-tetrafluoroethane, the improvement which comprises carrying out the reaction (2) between 1,1,1-trifluoro-2-chloroethane and hydrogen fluoride at a temperature in the range of 280°-450° C., carrying out the reaction (1) between trichloroethylene and hydrogen fluoride at a temperature in the range of 200°-400° C. and below that used in reaction (2), and recycling unconverted 1,1,1-trifluoro-2-chloroethene with hydrogen fluoride for further reaction in the presence of trichloroethylene.

References Cited (Backward Citations)

US2005710A Cited
US2637747A Cited
US4158675A Cited
US4605798A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1996-09-06 1997-03-08 1997-09-07 $2000.00 Window Closed / Lapsed
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