Process of manufacturing 2-(4'-diethylamino-2'-hydroxybenzoyl)benzoic acid hexyl ester
US-2024109838-A1 · Apr 4, 2024 · US
US9908842B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9908842-B2 |
| Application number | US-201515501869-A |
| Country | US |
| Kind code | B2 |
| Filing date | Aug 7, 2015 |
| Priority date | Aug 8, 2014 |
| Publication date | Mar 6, 2018 |
| Grant date | Mar 6, 2018 |
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The present invention relates to a method for obtaining crystalline L-alanine from an aqueous solution of L-alanine, in particular from an aqueous solution of L-alanine, which is obtained from a fermentation process.
Opening claim text (preview).
We claim: 1. A method for obtaining crystalline L-alanine from an aqueous solution of L-alanine containing 100 to 30,000 ppm, based on L-alanine, of one or more α-amino acids different from L-alanine, comprising a) providing an aqueous solution of L-alanine containing at least 100 ppm, based on L-alanine, of one or more α-amino acids different from L-alanine; b) subjecting the solution of L-alanine to a crystallization by inducing conditions of a controlled supersaturation in a manner that the ratio c:c* of the concentration c of dissolved L-alanine to the equilibrium solubility c* of L-alanine under the conditions of controlled supersaturation is in a range from > 1:1 to 1.5:1, thereby affecting the crystallization of L-alanine; and c) separating crystalline L-alanine from the mother liquor. wherein the aqueous solution of L-alanine is fed to a continuously operated crystallization apparatus, which contains an aqueous suspension of L-alanine crystals. 2. The method of claim 1 , where the concentration of dissolved L-alanine under the conditions of supersaturation is from 150 to 400 g/L. 3. The method of claim 1 , where the controlled supersaturation is induced at a temperature of at least 30° C. 4. The method of claim 1 , where the controlled supersaturation is induced by removing water and/or by cooling. 5. The method of claim 4 , where the water is removed by evaporation. 6. The method of claim 1 , where step b) comprises b1) continuously feeding the aqueous solution of L-alanine to a crystallisation apparatus containing an aqueous suspension of L-alanine; b2) continuously removing water from the aqueous suspension of L-alanine contained in the crystallisation apparatus to maintain conditions of controlled supersaturation; b3) continuously removing the aqueous suspension of L-alanine from the crystallisation apparatus. 7. The method of claim 6 , where a portion of the aqueous suspension of L-alanine removed in step b3) is mixed with the aqueous solution of L-alanine of step b1) and the mixture is fed back it into the crystallization apparatus. 8. The method of claim 7 , where the mass ratio of the mixture which is fed back it into the crystallization apparatus and the aqueous solution of L-alanine, mixed with the suspension, is at least 4:1. 9. The method of claim 1 , where the solid content of the aqueous suspension is from 5 to 30% by weight, based on the weight of the suspension. 10. The method of claim 1 , where the crystallization is effected in a crystallizer, selected from a forced circulation crystallizer, draft tube crystallizer, a draft tube baffled crystallizer, an Oslo-type crystallizer, and an induced forced circulation crystallizer. 11. The method of claim 1 , where the crystallization of L-alanine comprises at least two subsequent crystallization steps. 12. The method of claim 11 , where the crystalline L-alanine obtained in a precedent crystallization step is dissolved in a mixture of the mother liquor of the subsequent crystallization step with water to obtain an aqueous solution of L-alanine, from which L-alanine is crystallized in the subsequent crystallization step. 13. The method of claim 1 , where the aqueous solution of L-alanine provided in step a) does not contain more than 100 ppm of solid insoluble material. 14. The method of claim 1 , where the aqueous solution of L-alanine provided in step a) has been filtered to remove solid insoluble material. 15. The method of claim 1 , where the aqueous solution of L-alanine provided in step a) contains at least one amino acid selected from the group consisting of D-alanine, L-valine, L-leucine, L-lysine, L-asparagine, L-glutamine, and L-arginine. 16. The method of claim 1 , where the aqueous solution of L-alanine provided in step a) is obtained by a fermentation process. 17. The method of claim 9 , where a solid content of the aqueous suspension is from 20 to 25%, by weight, based on the weight of the suspension.
Crystallisation · CPC title
Crystalline forms, e.g. polymorphs · CPC title
having only one amino and one carboxyl group bound to the carbon skeleton · CPC title
Alpha- or beta- amino acids {(other amino acids C12P13/005)} · CPC title
the nitrogen atom of the amino group being further bound to hydrogen atoms · CPC title
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