GB802522A - Improvements in or relating to recovery of citric acid - Google Patents

Improvements in or relating to recovery of citric acid

Info

Publication number
GB802522A
GB802522A GB21002/55A GB2100255A GB802522A GB 802522 A GB802522 A GB 802522A GB 21002/55 A GB21002/55 A GB 21002/55A GB 2100255 A GB2100255 A GB 2100255A GB 802522 A GB802522 A GB 802522A
Authority
GB
United Kingdom
Prior art keywords
calcium
citrate
acid
citric acid
mol
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
GB21002/55A
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.)
Pfizer Inc
Original Assignee
Pfizer Inc
Charles Pfizer and Co Inc
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 Pfizer Inc, Charles Pfizer and Co Inc filed Critical Pfizer Inc
Publication of GB802522A publication Critical patent/GB802522A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C59/00Compounds having carboxyl groups bound to acyclic carbon atoms and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups
    • C07C59/235Saturated compounds containing more than one carboxyl group
    • C07C59/245Saturated compounds containing more than one carboxyl group containing hydroxy or O-metal groups
    • C07C59/265Citric acid
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part

Landscapes

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

Abstract

Calcium mono-acid citrate is precipitated from an aqueous solution of citric acid by heating the solution at a temperature of at least 40 DEG C. either in the presence of calcium hydroxide, calcium oxide or calcium carbonate, wherein the amount of calcium present in the reaction mixture is not greater than two-thirds of that theoretically required for the complete neutralization of the citric acid to form tricalcium citrate, or in the presence of tricalcium citrate in an amount not exceeding one mol. per mol. of free citric acid present. Citric acid may be regenerated from the calcium mono-acid citrate, e.g. by treating the latter with a stoichiometric amount of sulphuric acid. It is preferred to use reaction temperatures of above 70 DEG C., e.g. temperatures of 80 DEG to 95 DEG C. and improved results are obtained if the mixture to be converted to calcium mono-acid citrate is seeded with calcium mono-acid citrate. The amount of calcium added in the form of calcium monoacid citrate for seeding is not to be considered in calculating the maximum amount of calcium which may be present in the reaction mixture to form the calcium mono-acid citrate. In one method of operation a citric acid solution is divided into two parts, the first part, about two-thirds of the total, may be completely neutralized with calcium hydroxide, calcium oxide, or calcium carbonate, and the tricalcium citrate which precipitates may be filtered off and added to the remaining part of the original citric acid solution and the mixture heated to at least 40 DEG C. to precipitate calcium mono-acid citrate. In examples, calcium acid citrate is precipitated by (1) adding tricalcium citrate (1 mol.) to a solution of citric acid (1 mol.) in two litres of water and heating the mixture at 40 DEG C. for 23 hours; (2) adding calcium hydroxide (1 mol) (or the equivalent amounts of calcium oxide or calcium carbonate) to a solution of one mol. citric acid in 1 litre of water and heating at 90 DEG C. for 2 hours; (3) adding 0.6 mol. of calcium hydroxide to citric acid (1 mol.) dissolved in 1 litre of water and heating the mixture at 40 DEG C. for 2 1/2 hours. In other examples: (4) and (5) about 5 per cent of the calcium hydroxide required to produce complete neutrality is added to a fermentation liquor in which citric acid has been prepared and the resulting precipitate of oxalic acid is filtered off and calcium mono-acid citrate is precipitated by adding tricalcium citrate to the filtrate while maintaining the mixture at 90 DEG C. in (4) (or 85-90 DEG C. in (5)) and adding some calcium mono-acid citrate as seed.
GB21002/55A 1954-07-28 1955-07-20 Improvements in or relating to recovery of citric acid Expired GB802522A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US802522XA 1954-07-28 1954-07-28

Publications (1)

Publication Number Publication Date
GB802522A true GB802522A (en) 1958-10-08

Family

ID=22156186

Family Applications (1)

Application Number Title Priority Date Filing Date
GB21002/55A Expired GB802522A (en) 1954-07-28 1955-07-20 Improvements in or relating to recovery of citric acid

Country Status (1)

Country Link
GB (1) GB802522A (en)

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