Powders and granules and process for making such powders and granules

Abstract

Process for making a powder or granule containing at least one chelating agent selected from alkali metal salts of methyl glycine diacetic acid (MGDA) and glutamic acid diacetate (GLDA) and iminodisuccinic acid (IDS), said process comprising the steps of (a) introducing an aqueous solution or aqueous slurry of the respective chelating agent (A) into a spray-dryer or spray-granulator, and removing most of said water by spray-drying or spray granulation using a gas with an inlet temperature of 125 to 250° C., (b) withdrawingpowder or granules, respectively, from the spray-dryer or spray-granulator, respectively, (c) separating off fines from said powder or granules, wherein said fines have a maximum particle diameter of 350 μm, (d) separating off lumps from said powder or granules, wherein said lumps have a particle diameter of 1,500 μm or more, (e) milling said lumps to a maximum particle diameter of 500 μm, (f) re-introducing said fines from step (c) and milled lumps from step (e) into the spray-dryer or spray-granulator, wherein the share of fines is in the range of from 0.5 to 20% by weight of the total chelating agent (A) withdrawn in step (b) and the share of milled lumps is in the range of from 5 to 60% by weight of the total chelating agent (A) withdrawn in step (b).

Claims

1. A process for making a powder or granule comprising at least one chelating agent selected from the group consisting of an alkali metal salt of methyl glycine diacetic acid (MGDA), an alkali metal salt of glutamic acid diacetate (GLDA), and an alkali metal salt of iminodisuccinic acid (IDS), wherein the alkali metal salt has a formula selected from the group consisting of formula (I a), (I b) and (I c):
[CH.sub.3—CH(COO)—N(CH.sub.2—COO).sub.2]M.sub.3-xH.sub.x  (I a) wherein in formula (I a), M is, independently at each occurrence, an alkali metal cation, and x is from zero to 1.0,
[OOC—CH.sub.2CH.sub.2C—CH(COO)—N(CH.sub.2—COO).sub.2]M.sub.4-xH.sub.x  (I b) wherein in formula (I b), M is, independently at each occurrence, an alkali metal cation, and x is from zero to 2.0,
[H—N—(CH(COO)—CH.sub.2COO).sub.2]M.sub.4-xH.sub.x  (I c) wherein in formula (I c), M is, independently at each occurrence, an alkali metal cation, and x is from zero to 2.0, the process comprising: (a) introducing an aqueous solution or aqueous slurry of the chelating agent into a spray-dryer or spray-granulator, and removing most of the water by spray-drying or spray granulation using a gas with an inlet temperature of 125 to 250° C., (b) withdrawing powder or granules, from the spray-dryer or spray-granulator, (c) separating off fines from the powder or granules, wherein the fines have a maximum particle diameter of 30 μm in the case of powders and a maximum particle diameter of 350 μm in the case of granules, (d) separating off lumps from the powder or granules, wherein the lumps have a particle diameter of 250 μm in the case of powders and 1,000 μm or more in the case of granules, respectively, (e) milling the lumps to a maximum particle diameter of 500 μm in the case of granules or to 40 μm in the case of powders, and (f) re-introducing the fines from (c) and milled lumps from (e) into the spray-dryer or spray-granulator, wherein the amount of fines is in a range of from 4 to 18% by total weight of the chelating agent withdrawn in (b), and the amount of milled lumps from (e) is in a range of from 20 to 40% by total weight of the chelating agent withdrawn in (b).

2. The process according to claim 1, wherein in (c) a range of from 80 to 99% by weight of the fines is separated off.

3. The process according to claim 1, wherein the aqueous solution or slurry in (a) comprises at least one (co)polymer (B) selected from the group consisting of homo- and copolymers of (meth)acrylic acid and polyalkylenimines that may be polyalkoyxylated or substituted with carboxymethyl groups.

4. The process according to claim 3, wherein the powder or granule comprises in a range of from 80 to 99.9% by weight of the chelating agent and 0.1 to 20% by weight of the (co)polymer (B), wherein percentages refer to a solids content of the powder or granule.

5. The process according to claim 1, wherein the chelating agent is at least one selected from the group consisting of the trisodium salt of MGDA and the tetrasodium salt of GLDA.

6. The process according to claim 3, wherein the (co)polymer (B) is a per-sodium salt of polyacrylic acid.

7. The process according to claim 3, wherein the (co)polymer (B) is a polyethylenimine that may be polyethoxylated.

8. The process according to claim 3, wherein the (co)polymer (B) has an average molecular weight M.sub.w in a range of from 1,200 to 30,000 g/mol, determined by gel permeation chromatography and referring to the respective free acid.

Description

EXAMPLE 1

(1) Step (a.1): an aqueous solution of (A.1) was heated to 80° C.

(2) A vessel containing a fluidized bed from 1 kg of solid MGDA-Na.sub.3 granule, initial average particle diameter 550 μm, was provided. The fluidization was accomplished by entering a so-called fluidization gas at the bottom of the vessel, said fluidization gas being air with an inlet temperature of 150° C.

(3) As soon as the bed temperature of at least 105° C. was reached, an amount of 2 kg/h of the above aqueous solution of (A.1) was sprayed onto the fluidized bed with the help of a nozzle. The spraying—and thus atomizing—was accomplished with air with a gas inlet temperature of 150° C.

(4) Step (b.1): Every 30 minutes, an aliquot of granule was withdrawn from the vessel through a discharge screw at the side.

(5) Steps (c.1) and (d.1): The aliquot withdrawn in accordance with step (b.1) was classified by sieving in a sieving machine with two sieves, mesh 350 μm and 1,250 μm. Shares of 25% by weight lumps having a minimum diameter of 1,250 μm, and 7% by weight of fines having a maximum diameter of 350 μm were separated off.

(6) Step (e.1): The lumps obtained in step (d.1) were milled down in a hammer mill, type Kinematica Polymix System PM-MFC 90 D. Milled particles with a maximum diameter 500 μm were collected and transferred to step (f).

(7) Step (f.1) The milled lumps obtained in step (e.1) were combined with the fines from step (c.1) and returned portion-wise into the granulator.

(8) A free-flowing granule of (A.1) was obtained that had excellent properties such as, but not limited to excellent percarbonate stability and low hygroscopicity. No hot spots were observed during processing. No sticky material was obtained. A free flowing granule was obtained, and the hygroscopicity was low.

EXAMPLE 2

(9) Basically, example 1 was repeated, with following differences:

(10) In step (a.2), an aqueous solution of (A.1), concentration 40% by weight, and (B.1), 0.25% by weight, was heated to 80° C. and then spray granulated.

(11) In step (c.2), 13% by weight fines were removed. In step (d.2), 28% by weight lumps were removed.

(12) The subsequent steps were repeated mutatis mutandis.

(13) A free-flowing co-granule of (A.1) and (B.1) was obtained that had excellent properties such as, but not limited to excellent percarbonate stability and low hygroscopicity. No hot spots were observed during processing. No sticky material was obtained. The hygroscopicity was low.

EXAMPLE 3

(14) Basically, example 1 was repeated, with following differences:

(15) In step (a.3), an aqueous solution of (A.1), concentration 40% by weight, and (B.1), 10% by weight, was heated to 80° C. and then spray granulated.

(16) In step (c.3), 8% by weight fines were removed. In step (d.3), 26% by weight lumps were removed.

(17) The subsequent steps were repeated mutatis mutandis.

(18) A free-flowing co-granule of (A.1) and (B.1) was obtained that had excellent properties such as, but not limited to excellent percarbonate stability and low hygroscopicity. No hot spots were observed during processing. No sticky material was obtained. The hygroscopicity was low.

EXAMPLE 4

(19) Step (a.4): an aqueous solution of (A.1) was heated to 55° C.

(20) A vessel containing a fluidized bed from 1 kg of solid MGDA-Na.sub.3 granule, initial average particle diameter 550 μm, was provided. The fluidization was accomplished by entering a so-called fluidization gas at the bottom of the vessel, said fluidization gas being air with an inlet temperature of 150° C.

(21) As soon as the bed temperature of at least 99° C. was reached, an amount of 2 kg/h of the above aqueous solution of (A.1) was sprayed onto the fluidized bed with the help of a nozzle. The spraying—and thus atomizing—was accomplished with air with a gas inlet temperature of 160° C. and a pressure of 2.8 bar.

(22) Step (b.4): Every 30 minutes, an aliquot of granule was withdrawn from the vessel through a discharge screw at the side. Residual moisture content was 9.5% by weight.

(23) Steps (c.4) and (d.4): The aliquot withdrawn in accordance with step (b.4) was classified by sieving in a continuously operated sieving machine with two sieves, mesh 350 μm and 1,250 μm. Shares of 5% by weight lumps having a minimum diameter of 1,250 μm, and 37% by weight of fines having a maximum diameter of 350 μm were separated off.

(24) Step (e.4): The lumps obtained in step (d.4) were milled down in a bolting machine with 1435 rounds per minute. Milled particles with a maximum diameter 500 μm were collected and transferred to step (f).

(25) Step (f.4) The milled lumps obtained in step (e.4) were combined with the fines from step (c.4) and returned portion-wise into the granulator.

(26) A free-flowing granule of (A.1) was obtained that had excellent properties such as, but not limited to excellent percarbonate stability and low hygroscopicity. No hot spots were observed during processing. No sticky material was obtained. A free flowing granule was obtained, and the hygroscopicity was low.

EXAMPLE 5

(27) Step (a.5): an aqueous solution of (A.1) was heated to 55° C.

(28) A vessel containing a fluidized bed from 1 kg of solid MGDA-Na.sub.3 granule, initial average particle diameter 550 μm, was provided. The fluidization was accomplished by entering a so-called fluidization gas at the bottom of the vessel, said fluidization gas being air with an inlet temperature of 150° C.

(29) As soon as the bed temperature of at least 93° C. was reached, an amount of 2 kg/h of the above aqueous solution of (A.1) was sprayed onto the fluidized bed with the help of a nozzle. The spraying—and thus atomizing—was accomplished with air with a gas inlet temperature of 171° C. and a pressure of 3.2 bar.

(30) Step (b.5): Every 30 minutes, an aliquot of granule was withdrawn from the vessel through a discharge screw at the side. Residual moisture content was 11.1% by weight.

(31) Steps (c.5) and (d.5): The aliquot withdrawn in accordance with step (b.5) was classified by sieving in a continuously operated sieving machine with two sieves, mesh 350 μm and 1,250 μm. Shares of 35% by weight lumps having a minimum diameter of 1,250 μm, and 4% by weight of fines having a maximum diameter of 350 μm were separated off.

(32) Step (e.5): The lumps obtained in step (d.5) were milled down in a bolting machine with 1435 rounds per minute. Milled particles with a maximum diameter 500 μm were collected and transferred to step (f).

(33) Step (f.5) The milled lumps obtained in step (e.5) were combined with the fines from step (c.5) and returned portion-wise into the granulator.

(34) A free-flowing granule of (A.1) was obtained that had excellent properties such as, but not limited to excellent percarbonate stability and low hygroscopicity. No hot spots were observed during processing. No sticky material was obtained. A free flowing granule was obtained, and the hygroscopicity was low.

(35) The results are summarized in Table 2.

(36) TABLE-US-00002 TABLE 2 process parameters of the exemplified granules fines lumps granule % [wt %] [wt %] [wt %] (D50) crystallinity Experiment 1 7 25 68 n.d. Experiment 2 13 28 59 n.d. Experiment 3 8 26 66 n.d. Experiment 4 37 5 58 436 80 Experiment 5 4 35 61 740 86 The (D50) refers to the granule.