Process for manufacturing MGDA/GLDA granules, granules, and their use

Patent metadata

Field	Value
Publication number	US-10865362-B2
Application number	US-201716316266-A
Country	US
Kind code	B2
Filing date	Jul 5, 2017
Priority date	Jul 15, 2016
Publication date	Dec 15, 2020
Grant date	Dec 15, 2020

Abstract

Process for manufacturing granules of salts of at least two aminopolycarboxylic acids (A), com-prising the steps of (a) providing an aqueous solution of (A1) at least one alkali metal salt of a mixture of L- and D-enantiomers of methyl glycine diacetic acid (MGDA), said mixture containing predominantly the respective L-isomer with an enantiomeric excess (ee) in the range of from 10 to 95%, (A2) at least one alkali metal salt of L- and D-enantiomers of glutamic acid diacetic acid (GLDA) or of enantiomerically pure L-GLDA, the weight ratio of (A1) and (A2) being in the range of from 1:9 to 9:1, (b) spray granulating said solution with a gas inlet temperature of at least 125° C. Additionally, the present invention relates to granules and to their use.

First claim

The invention claimed is:

1. A process for manufacturing granules of salts of at least two aminopolycarboxylic acids (A), the process comprising:
spray granulating, with a gas inlet temperature of at least 125° C., an aqueous solution comprising (A1) an alkali metal salt of a mixture of L- and D-enantiomers of methyl glycine diacetic acid (MGDA), the mixture comprising predominantly the L-enantiomer with an enantiomeric excess (ee) in a range of from 10 to 95%, and (A2) an alkali metal salt of a mixture of L- and D-enantiomers of glutamic acid diacetic acid (GLDA) or of enantiomerically pure L-GLDA,
wherein a weight ratio of (A1) and (A2) is in a range of from 1:9 to 9:1.

2. The process of claim 1 , wherein the aqueous solution has a concentration of the aminopolycarboxylic acids (A) in a range of from 45 to 65% by weight.

3. The process of claim 1 , wherein the spray granulating is performed in a fluidized bed or a spouted bed.

4. The process of claim 1 , wherein the alkali metal salts comprise fully neutralized sodium and potassium salts of MGDA and GLDA.

5. The process of claim 3 , wherein the spray granulating is performed in a fluidized bed comprising particles having an average diameter (D50) in a range of from 100 to 800 μm.

6. The process of claim 1 , wherein the aqueous solution subjected to spray-granulation further comprises silica, a silicate, an organic polymer, an organic copolymer, or a mixture of two or more of these.

7. The process of claim 1 , wherein the alkali metal salt of (A1) comprises a compound of formula (I)
[CH 3 —CH(COO)—N(CH 2 —COO) 2 ]M 3-x H x   (I),

wherein
M is an alkali metal cation, and
x is in a range of from 0 to 1.

8. A granule, comprising, in molecular disperse form:
(A1) an alkali metal salt of a mixture of L- and D-enantiomers of methyl glycine diacetic acid (MGDA), said mixture comprising predominantly the L-enantiomer with an enantiomeric excess (ee) in a range of from 10 to 95%, and
(A2) an alkali metal salt of L- and D-enantiomers of glutamic acid diacetic acid (GLDA) or of enantiomerically pure L-GLDA,
wherein a weight ratio of (A1) and (A2) is in a range of from 1:9 to 9:1, and
wherein the granule has a residual moisture content in a range of from 5 to 15% by weight.

9. The granule of claim 8 , having an average diameter (D50) in a range of from 350 to 900 μm.

10. A solid hard surface cleaner, comprising the granule of claim 8 in a range of from 1 to 50 wt. %.

11. The hard surface cleaner of claim 10 , which is an automatic dishwashing detergent.

12. A process for making tablets, the process comprising:
pelletizing a mixture comprising the granule of claim 8 .

13. The process of claim 1 , wherein the aqueous solution has a pH value in a range of from 8 to 14.

14. The process of claim 1 , wherein the aqueous solution has a pH value in a range of from 9 to 13.5.

15. The process of claim 1 , wherein the alkali metal salts comprise fully neutralized potassium salts of MGDA and GLDA.

16. The process of claim 1 , wherein the alkali metal salts comprise fully neutralized sodium salts of MGDA and GLDA.

17. The process of claim 1 , wherein the granules have an average particle diameter (D50) in a range of from 0.1 mm to 2 mm.

18. The process of claim 1 , wherein the aqueous solution has a total solids contents in a range of from 30 to 70 wt. %.

19. The process of claim 1 , wherein the aqueous solution has a total solids contents in a range of from 45 to 65%.

20. The process of claim 1 , wherein the spray-drying comprises removing 51 to 75 wt. % of the water present in the aqueous solution.

21. A solid laundry detergent, comprising the granule of claim 8 in a range of from 1 to 30 wt. %.

Assignees

• Basf Se

Inventors

• Reinoso Garcia Marta
• Mueller Michael Klemens
• Sueling Carsten
• Mormul Verena

Classifications

• C11D17/06

  Powder; Flakes; Free-flowing mixtures; Sheets · CPC title

• C11D11/02

  Preparation in the form of powder by spray drying · CPC title

• C11D3/33 Primary

  Amino carboxylic acids · CPC title

• C07C227/36

  Racemisation of optical isomers · CPC title

• C11D17/0073 Primary

  Tablets · CPC title