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GB646219A - Improvements in and relating to the dehydration of aqueous solutions of formic acid - Google Patents

Improvements in and relating to the dehydration of aqueous solutions of formic acid

Info

Publication number
GB646219A
GB646219A GB35052/47A GB3505247A GB646219A GB 646219 A GB646219 A GB 646219A GB 35052/47 A GB35052/47 A GB 35052/47A GB 3505247 A GB3505247 A GB 3505247A GB 646219 A GB646219 A GB 646219A
Authority
GB
United Kingdom
Prior art keywords
column
pipe
formic acid
per cent
entrainer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
GB35052/47A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Usines de Melle SA
Original Assignee
Usines de Melle SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Usines de Melle SA filed Critical Usines de Melle SA
Publication of GB646219A publication Critical patent/GB646219A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/43Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/43Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
    • C07C51/46Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by azeotropic distillation

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Formic acid is dehydrated in a two-stage distillation system, the aqueous feed-acid being supplied at a point in the system where formic acid of the same concentration is present; one stage comprises the concentration of 77 per cent acid (i.e. the C.B.M. of formic acid and water) to 85-95 per cent by rectification in the presence of a water-entrainer, with reflux of entrainer and also part of the water, which separate in the usual decanter, keeping several plates at the base of the column free of entrainer, and the other stage comprises fractionating without an entrainer, the 85-95 per cent acid from the entrainer-distillation stage to give substantially anhydrous formic acid as head-product, and 77 per cent acid as residue; this residue is passed to the entrainer-distillation stage. Suitable entrainers are butyl, isobutyl, amyl and isoamyl formates; also butyl oxide and methylpropyl ketone. In an example 77 per cent formic acid is fed from tank 1 through pipes 2 and 2a into column 3 which is charged with butyl formate. The base of the column is maintained at 103.5 DEG C. The butyl formate/water binary taken off at the head of <PICT:0646219/III/1> the column, is condensed and the condensate is passed to decanter 5. The formate-layer is completely refluxed through pipe 6; and the water-layer is partly withdrawn from the system through pipe 7, and partly returned to the column through pipe 8. Formic acid of about 90 per cent strength and almost free from butyl formate, is withdrawn from the base of column 3 and passed through pipe 11 into column 10. Anhydrous formic acid is withdrawn from column 10 through pipe 12, while the 77 per cent acid which collects at the base, is passed to tank 13 and then pumped to tank 1 through pipe 15. A draw-off pipe 16 is provided on the reflux vessel of column 10 in order to remove any small quantities of butyl formate and water which may have inadvertently passed into column 10. The mixture withdrawn through pipe 16 is returned to column 3 through pipe 17. In another example, the feed is 95 per cent formic acid. This is introduced directly into column 10 through pipes 18 and 18b, and column 3 is charged with butyl oxide. The whole or any part of the process may be carried out at a pressure different from atmospheric. Specification 303,742, [Class 32], is referred to.
GB35052/47A 1941-04-04 1947-12-31 Improvements in and relating to the dehydration of aqueous solutions of formic acid Expired GB646219A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR646219X 1941-04-04

Publications (1)

Publication Number Publication Date
GB646219A true GB646219A (en) 1950-11-15

Family

ID=9001258

Family Applications (1)

Application Number Title Priority Date Filing Date
GB35052/47A Expired GB646219A (en) 1941-04-04 1947-12-31 Improvements in and relating to the dehydration of aqueous solutions of formic acid

Country Status (1)

Country Link
GB (1) GB646219A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112386938A (en) * 2020-12-03 2021-02-23 山东恒信科技发展有限公司 Dehydration system and dehydration method for N-formylmorpholine and cyclic interval hydrocarbon

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112386938A (en) * 2020-12-03 2021-02-23 山东恒信科技发展有限公司 Dehydration system and dehydration method for N-formylmorpholine and cyclic interval hydrocarbon

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