Process for reducing formation of gypsum scale durng the washing of calcium sulphate hemihydrate crystals

• US 4,049,774 A
• Filed: 11/08/1974
• Issued: 09/20/1977
• Est. Priority Date: 11/12/1970
• Status: Expired due to Term

• Current Assignee: Fisons Limited (Sanofi )
• Original Assignee: Fisons Limited (Sanofi )
• Inventors: Robinson, Norman, Janikowski, Stanislaw Maria, Harper, Douglas Charles
• Primary Examiner(s): Vertiz, O. R.
• Assistant Examiner(s): Langel, Wayne A.
• Application Number:
  US05/522,265
• Time in Patent Office: 1,047 Days
• Field of Search: 423/167, 423/266, 423/267, 423/268, 423/317, 423/319, 423/320, 423/321, 423/555
• US Class Current: 423/157.4
• CPC Class Codes: C01B 25/226 Hemihydrate process
• CPC Class Codes: C01F 11/46 Sulfates dehydration of gypsum for the production of calcium sulfate cements C04B11/02
• CPC Class Codes: C23F 15/005 Inhibiting incrustation

Abstract

A process for reducing formation of calcium sulphate scale during the washing of calcium sulphate hemihydrate crystals by washing the crystals with a liquor containing certain surface-active agents in sufficient amount to give a concentration of from 0.0002 to 1% by weight of surface-active agent in the wash liquors.

Claims

1. In a process for producing phosphoric acid wherein phosphate rock is acidulated with a mineral acid and crystals of calcium sulphate hemihydrate are formed, separated off from the phosphoric acid and thereafter washed, the improvement which comprises washing the calcium sulphate hemihydrate crystals with an aqueous wash liquor which prior to contact with the crystals, contains P₂ O₅ in amounts less than 30% and H₂ SO₄ in amounts of less than 10 parts by weight per 100 parts by weight of H₃ PO₄ present in the aqueous wash liquor and contains from 0.0002 to 1.0% by weight of an additive selected from the group consisting of compounds of the empirical general formula:

space="preserve" listing-type="equation">R.sup.1 R.sup.2 S(O).sub.n I

wherein n has a value of 3 or 4 and when n is 3 R² is hydrogen and R¹ is an alkyl or aralkyl group and when n is 4 R¹ is an alkyl or aralkyl group and R² is hydrogen or an R¹ group;

alkylene oxide condensates of an alcohol, phenol or an alkyl phenol and mixtures and salts, esters and amides of said compounds whereby the deposition of calcium sulphate dihydrate scale due to the recrystallisation of the calcium sulphate hemihydrate to calcium sulfate dihydrate is reduced;

the total contact time between the calcium sulphate hemihydrate crystals and the wash liquor during washing being less than 10 minutes.

2. A process as claimed in claim 1 wherein the additive comprises a mixture of an alkylbenzene sulphonic acid, or alkali-metal salt thereof, with an ethylene oxide condensate of an alkylphenol.

3. A process as claimed in claim 2 wherein the mixture comprises from 50 to 80 parts by weight of the sulphonic acid or salt thereof and from 50 to 20 parts by weight of the condensate.

4. A process as claimed in claim 3 wherein the alkyl group in the alkylbenzene sulphonic acid contains from 9 to 11 carbon atoms and the condensate is a condensate of from 5 to 15 molar proportions of ethylene oxide with octyl- or nonylphenol.

5. A process according to claim 1 wherein the additive is used in the form of an alkali-metal or ammonium salt thereof.

6. A process as claimed in claim 1 wherein R¹ is an alkyl group containing from 8 to 18 carbon atoms, optionally interrupted by one or more ether linkages.

7. A process as claimed in claim 1 wherein the additive is an ethylene oxide condensate of an alkyl phenol or of a monohydric or dihydric alkanol.

8. A process as claimed in claim 1 wherein the compound of formula 1 is selected from alkylbenzene sulphonic acids;

monoalkyl sulphate esters;

dialkyl sulphate esters;

sulphate mono-esters of alkylene oxide condensates with alcohols, glycols or alkylphenols;

alkane sulphonates; and

mixtures of these.

9. A process as claimed in claim 1 wherein the washing is carried out in a number of stages and the additive is added to the wash liquors in two or more of the wash stages.

10. A process as claimed in claim 1 wherein the crystals are washed in situ on the filter in which the crystals are separated from the phosphoric acid.