METHOD FOR THE PREPARATION OF CALCIUM MONOHYDROGEN PHOSPHATE

• US 20190322530A1
• Filed: 06/27/2017
• Published: 10/24/2019
• Est. Priority Date: 06/28/2016
• Status: Abandoned Application

• Current Assignee: Prayon Technologies
• Original Assignee: Prayon Technologies
• Inventors: THEYS, Tibaut, HENRY, Thomas
• Application Number:
  US16/311,626
• Publication Number:
  US 20190322530A1
• Time in Patent Office: Days
• CPC Class Codes: A23L 33/16 Inorganic salts, minerals or trace elements
• CPC Class Codes: C01B 25/22 Preparation by reacting phosphate-containing material with an acid, e.g. wet process
• CPC Class Codes: C01B 25/322 Preparation by neutralisation of orthophosphoric acid
• CPC Class Codes: C01B 25/324 Preparation from a reaction solution obtained by acidifying with an acid other than orthophosphoric acid
• CPC Class Codes: C05B 11/04 using mineral acid
• CPC Class Codes: C05B 11/12 using aqueous hydrochloric acid
• CPC Class Codes: C05B 3/00 Fertilisers based essentially on di-calcium phosphate C05B11/00 takes precedence

Abstract

This present invention disclosure relates to a method for the preparation of calcium monohydrogen phosphate comprising an etching in an aqueous medium, during a predetermined time period, of a phosphate source with an acid with formation of a pulp comprising an aqueous phase containing calcium phosphate in solution and a solid phase containing impurities, a first separation between said aqueous phase and said solid phase, during a predetermined time period, a neutralization of said aqueous phase at a sufficient pH to obtain a precipitation of said calcium monohydrogen phosphate, a second separation between said aqueous medium and said calcium monohydrogen phosphate, characterized in that said first separation of said step b) is carried out at a filtration rate of at least 0.1 ton of P₂O₅/√ΔP/m²/day.

Claims

1. A method for the preparation of calcium monohydrogen phosphate comprising the steps of:

a) digesting in an aqueous medium, during a predetermined time period, a phosphate source by an acid with formation of a pulp comprising an aqueous phase containing calcium phosphate in solution and a solid phase containing impurities,

b) separating said aqueous phase containing calcium phosphate in solution and said solid phase containing impurities, for a predetermined time period to provide a separated aqueous phase containing calcium phosphate in solution,

c) neutralizing said separated aqueous phase containing calcium phosphate in solution at a sufficient pH to obtain a precipitation in an aqueous medium of insoluble calcium phosphate as aforementioned calcium monohydrogen phosphate, and

d) separating said aqueous medium and said calcium monohydrogen phosphate,

wherein step b) is carried out at a filtration rate of at least 0.1 ton of P₂O₅/√

Δ

P/m²/day, between 0.1 and 5 tons of P₂O₅/√

Δ

P/m²/day, between 0.15 and 3 tons of P₂O₅/√

Δ

P/m²/day, between 0.3 and 0.9 tons of P₂O₅/√

Δ

P/m²/day, or between 0.4 and 0.7 tons of P₂O₅/√

Δ

P/m²/day, said filtration rate being calculated according to the following equation;

2. The method according to claim 1, wherein said predetermined time period of said step a) of digestion is greater than, less than or equal to that of the aforementioned first separation step b).

3. The method according to claim 1, wherein the aforementioned steps a) and b) are carried out in a predetermined duration of less than 2 hours, between 30 and 100 minutes, 30 and 70 minutes, or between 40 and 65 minutes.

4. The method according to claim 1, wherein said phosphate source and said acid are introduced into a first reactor comprising said aqueous medium simultaneously or successively, in order to carry out said step a) of digestion and wherein said pulp comprising said aqueous phase containing calcium phosphate in solution and said solid phase containing impurities is transferred from the first reactor to a separation means for carrying out said first separation referred to in the aforementioned step b).

5. The method according to claim 4, wherein said separation means is located between said first reactor and a second reactor.

6. The method according to claim 4, wherein said separation means is present in a second reactor into which said pulp comprising an aqueous phase containing calcium phosphate in solution and a solid phase containing impurities is introduced, to carry out said first separation referred to in the aforementioned step b).

7. The method according to claim 4, wherein said separation means is a filter selected from the group consisting of a rotary filter, a rotary filter with tilting cell, a press filter, a belt filter, a drum filter.

8. The method according to claim 1, wherein said acid is selected from the group consisting of hydrochloric acid (HCl), nitric acid, sulfuric acid, phosphoric acid and mixtures thereof.

9. The method according to claim 8, wherein said acid is an aqueous solution of acid having an acid concentration of less than or equal to 15% by weight.

10. The method according to claim 1, wherein steps a) and b) are carried out at a temperature of between 50°

C. and 70°

C. or equal to 60°

C.

11. The method according to claim 1, wherein said phosphate source is selected from the group consisting of a phosphate rock, a phosphate ore, and secondary phosphate sources.

12. The method according to claim 1, wherein the neutralization step is carried out using a neutralization agent selected from the group consisting of calcium-based compounds.

13. The calcium monohydrogen phosphate obtained according to claim 1, wherein the calcium monohydrogen phosphate is suitable for producing phosphoric acid.

14. The calcium monohydrogen phosphate obtained according to claim 1, wherein the calcium monohydrogen phosphate has a purity level suitable for use in the food industry in the agricultural sector, or horticultural sector.

15. The method according to claim 11, wherein the secondary phosphate sources are selected from ash, sewage sludge, bone slurry, pig slurry, or mixtures thereof.

16. The method according to claim 12, wherein said calcium-based compounds are selected from the group consisting of calcium oxide, calcium hydroxide, calcium carbonate, and water-soluble calcium salts.