# US 10,865,362 B2 · Process for manufacturing MGDA/GLDA granules, granules, and their use

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- Number: US 10,865,362 B2
- Document ID: US10865362B2
- Status: Granted
- Kind: B2
- Application number: 16/316,266
- Filed: 2017-07-05
- Published: 2020-06-11
- Granted: 2020-12-15
- Earliest claimed: 2016-07-15
- Assignees: BASF SE
- Applicants: BASF SE
- Inventors: Marta Reinoso Garcia; Michael Klemens Mueller; Carsten Sueling; Verena Mormul
- Web page: https://patentgrep.com/patent/US10865362B2

## CPC

- C11D 3/33: Amino carboxylic acids
- C11D 7/3245: {Aminoacids}
- C11D 11/02: Preparation in the form of powder by spray drying
- C11D 17/0073: {Tablets}
- C11D 17/06: Powder; Flakes; Free-flowing mixtures; Sheets
- C11D: DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL

## 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.

## Claims

### Claim 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.

### Claim 2 (depends on 1)

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.

### Claim 3 (depends on 1)

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

### Claim 4 (depends on 1)

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

### Claim 5 (depends on 3)

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.

### Claim 6 (depends on 1)

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.

### Claim 7 (depends on 1)

The process of claim 1, wherein the alkali metal salt of (A1) comprises a compound of formula (I)
[CH3—CH(COO)—N(CH2—COO)2]M3-xHx (I),
wherein
M is an alkali metal cation, and
x is in a range of from 0 to 1.

### Claim 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.

### Claim 9 (depends on 8)

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

### Claim 10 (depends on 8)

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

### Claim 11 (depends on 10)

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

### Claim 12 (depends on 8)

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

### Claim 13 (depends on 1)

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

### Claim 14 (depends on 1)

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

### Claim 15 (depends on 1)

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

### Claim 16 (depends on 1)

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

### Claim 17 (depends on 1)

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.

### Claim 18 (depends on 1)

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

### Claim 19 (depends on 1)

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

### Claim 20 (depends on 1)

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

### Claim 21 (depends on 8)

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