Process and device for manufacturing organometallic complexes in powder form
View Patent ↗According to the invention, powders of low hygroscopicity are prepared by granulation of an aqueous solution ( 1 ) in a fluidized bed ( 140 ). A compound formed from crystalline grains whose moisture content is defined and stable is obtained. The invention applies especially to organometallic complexes of glycine with a metal.
1. Process for producing a crystalline organometallic complex in powder form, comprising the steps of:
a) preparing an aqueous solution of the organometallic complex,
b) granulating and drying said solution by spraying in a fluidized bed by circulation of air,
c) extracting the powder grains from the fluidized bed when they have reached a size greater than a predetermined lower size limit and a moisture content below a predetermined maximum moisture content,
wherein said predetermined lower size limit is about 25 μm,
and wherein the predetermined maximum moisture content is between 2% and 20% by weight.
2. Process according to claim 1 wherein, during the step of granulation and drying in a fluidized bed, the temperature and flow rate parameters of the aqueous solution and of the air are chosen so as to obtain, at the end of the step, powder grains having a moisture content below said predetermined maximum moisture content.
3. Process according to claim 1 , wherein:
said solution is granulated and dried continuously by spraying in an air-fluidized bed,
the temperature and flow rate parameters of the aqueous solution and of the air are continuously adapted so as to obtain in the fluidized bed a moisture content below said predetermined maximum moisture content,
the powder grains having a size greater than said predetermined lower size limit are continuously extracted from the fluidized bed.
4. Process according to claim 3 wherein, during a preliminary training step, inlet air, outlet air and inlet aqueous solution flow rates and temperatures are determined, making it possible to produce a flow of outlet powder grains having a moisture content, measured by collecting samples, that is substantially equal to said predetermined maximum moisture content, and said flow rate and temperature values are then maintained throughout the process.
5. Process according to claim 1 wherein:
a batch of material is granulated and dried by spraying said solution in a fluidized-air bed,
after the powder grains in the fluidized bed have reached a size larger than the predetermined lower size limit, the spraying is stopped while continuing maintenance in the fluidized bed to perform drying until a moisture content below the predetermined maximum moisture content is reached,
the mass of powder grains having this size and this moisture content is extracted.
6. Process according to claim 1 wherein, during the step of preparation of the organometallic complex, the mixture temperature is maintained in the range from about 55° C. to 80° C.
7. Process according to claim 1 wherein, during step a), water, amino acid and a water-soluble metal salt are mixed together with heating in a mixer until a temperature of 80° C. is reached, for at least 15 minutes.
8. Process according to claim 7 wherein the water is introduced and is heated first in the mixer, then the amino acid and the metal salt are added, and the mixture is stirred and heated until a temperature of 80° C. is reached, for at least 15 minutes.
9. Process according to claim 1 wherein, to prepare an anhydrous iron glycinate, glycine is used as amino acid, iron II sulfate heptahydrate is used as metal salt, and the moisture content is about 6%.
10. Process according to claim 1 wherein, to prepare copper glycinate dihydrate, glycine is used as amino acid, copper sulfate pentahydrate is used as metal salt, and the moisture content is about 13%.
11. Process according to claim 1 wherein, to prepare anhydrous zinc glycinate, glycine is used as amino acid, zinc sulfate monohydrate is used as metal salt, and the moisture content is about 2%.
12. Process according to claim 1 wherein, to prepare zinc glycinate dihydrate, glycine is used as amino acid, zinc sulfate monohydrate is used as metal salt, and the moisture content is about 13%.
13. Process according to claim 1 wherein, to prepare zinc glycinate trihydrate, glycine is used as amino acid, zinc sulfate monohydrate is used as metal salt, and the moisture content is about 17%.
14. Process for producing a crystalline organometallic complex in powder form, comprising the steps of:
a) preparing an aqueous solution of the organometallic complex,
b) granulating and drying said solution by spraying in a fluidized bed by circulation of air,
c) extracting the powder grains from the fluidized bed when they have reached a size greater than a predetermined lower size limit and a moisture content below a predetermined maximum moisture content,
wherein said predetermined lower size limit is about 80 μm,
and wherein the predetermined maximum moisture content is between 2% and 20% by weight.