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Process for purifying difructose dianhydride III

Патентный поиск по классам МПК-8:

Класс C12P19/12 дисахариды

Класс C07H1/06 выделение; очистка

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Класс C07H3/10 ангидросахара, например эпоксиды

Класс C12N9/10 трансферазы (2)

Класс C12P1/00 Получение соединений или композиций, не отнесенных к группам  3/00

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Класс C12P19/44 получение O-гликозидов, например глюкозидов


Классы МПК:C12P19/12 дисахариды
C07H1/06 выделение; очистка
C07H3/10 ангидросахара, например эпоксиды
C12N9/10 трансферазы (2)
C12P1/00 Получение соединений или композиций, не отнесенных к группам  3/00
C12P1/02 микробных грибков
C12P19/44 получение O-гликозидов, например глюкозидов
Автор(ы): Kikuchi, Hiroto (Hokkaido, JP)
Sakurai, Hiroaki (Hokkaido, JP)
Takagi, Norimitsu (Hokkaido, JP)
Aritsuka, Tsutomu (Hokkaido, JP)
Senba, Yoshihiro (Hokkaido, JP)
Tomita, Fusao (Hokkaido, JP)
Asano, Kozo (Hokkaido, JP)
Патентообладатель(и): Nippon Beet Sugar Mfg., Co., Ltd. (Tokyo, JP)
Приоритеты:
подача заявки
02.03.2004
публикация патента
16.08.2011

РЕФЕРАТ (Abstract)

In the invention, highly pure crystals of difructose dianhydride III (di-D-fructofuranose-1,2′:2,3′-dianhydride; hereinafter referred to as DFA III) are produced by adding 5% or less of powdered active carbon to a DFA III containing purified solution containing DFA III of 90% or more purity at a concentration of R-Bx 10-60, preferably 40-55, and after stirring, applying the mixture to solid-liquid separation (filtration with diatomaceous, filtration through a membrane filter, ultrafiltration, or continuous centrifugal separation) and concentrating the separated liquid part, followed by immediate crystallization.

In the process of the invention, DFA III crystals can be produced efficiently and industrially, and the resulting crystals can be used for various purposes in pharmaceuticals or food and drink since they have no smell. This is characteristics of the invention different from the prior art products.

Полный текст Патента US 7998710 + PDF


ФОРМУЛА ИЗОБРЕТЕНИЯ (CLAIMS)

The invention claimed is:

1. A process for purifying difructose dianhydride III (DFA III) having a purity based on dry weight of at least 70% (w/w), comprising: contacting under aeration (i) a solution containing DFA III having a DFA III purity based on dry weight of at least 60% (w/w) and less than 70% (w/w) and having an R-Bx of 10 or more, with (ii) a yeast that acts on disaccharides or monosaccharides other than DFA III to degrade or incorporate said disaccharides or monosaccharides other than DFA III into the yeast, and with (iii) active carbon particles for a time and under conditions sufficient for impurities to adsorb on the active carbon particles, wherein said active carbon particles are added in amount of 5% (w/w) or less based on the dry weight of the DFA III containing solution, and wherein the activated carbon particles have an average particle size from 15 to 200 microns, thereby providing a contacted solution; separating the contacted solution into a solid phase and a liquid phase; and recovering from the liquid phase DFA III having a purity based on dry weight of at least 70% (w/w), thereby purifying DFA III.

2. The process of claim 1, wherein the recovering the DFA III having a purity of 70% (w/w) or more based on dry weight comprises separating the DFA III having a purity of 70% (w/w) or more based on dry weight chromatographically.

3. The process of claim 2, wherein the recovering comprises obtaining a chromatographically purified DFA III by chromatographically separating DFA III from the DFA III containing liquid phase or from the DFA III having a purity of at least 70% (w/w) based on dry weight.

4. The process of claim 1, comprising filtering the contacted solution thereby separating the solid and liquid phases.

5. The process of claim 1, wherein the recovering comprises crystallizing DFA III having a purity of at least 95% (w/w) based on dry weight from the DFA III having a purity based on dry weight of at least 70% (w/w), wherein said crystallized DFA III lacks the smell of DFA III crystals produced by a method not employing the active carbon particles.

6. The process of claim 1, wherein the recovering comprises crystallizing DFA III having a purity of at least 99% (w/w) based on dry weight from the DFA III having a purity based on dry weight of at least 70% (w/w), wherein said crystallized DFA III lacks the smell of DFA III crystals produced by a method not employing the active carbon particles.

7. The process of claim 1, wherein said DFA III containing solution is obtained by treating inulin with a fructosyltransferase, wherein the polymerization degree of fructose in said inulin is 10 or more.

8. The process of claim 1, wherein said DFA III containing solution is obtained by treating inulin with inulin fructotransferase, wherein the polymerization degree of fructose in said inulin is 10 or more.

9. The process of claim 1, wherein said DFA III containing solution is a solution produced by action of a fructosyltransferase on a fructose polymer or a material containing fructose polymer.

10. The process of claim 1, wherein said DFA III containing solution is a syrup suitable for crystallization and separation.

11. A process for producing difructose dianhydride III (DFA III) having a purity of at least 70% (w/w) based on dry weight, comprising: producing a crude solution containing DFA III having a DFA III purity based on dry weight of less than 70% (w/w) but more than 60% (w/w) by contacting a DFA III containing solution with a yeast under conditions suitable for removing disaccharides other than DFA III and/or monosaccharides from the DFA III containing solution; contacting the crude solution with 0.1% (w/w) to 5% (w/w), based on the dry weight of the DFA III containing solution, of activated carbon particles, wherein said particles have an average particle size from 15 to 200 microns, for a time and under conditions sufficient for impurities to adsorb on the activated carbon particles, thereby providing a contacted solution; separating the contacted solution into a solid phase and a liquid phase; and recovering from the liquid phase DFA III having a purity based on dry weight of at least 70% (w/w), thereby producing DFA III having a purity of at least 70% (w/w) based on dry weight.

12. The process of claim 11, wherein said crude solution is a DFA III containing fraction obtained by chromatographically removing said saccharides other than DFA III from the DFA III containing solution.

13. The process of claim 11, wherein the producing the crude solution further comprises defecating and filtering the DFA III containing solution.

14. The process of claim 11, wherein said crude solution has a concentration of R-Bx of 60 or more.

15. The process of claim 11, wherein the recovering further comprises recovering colorless and odorless DFA III crystals having a purity of at least 95% (w/w) based on dry weight.

16. A process for producing a purified difructose dianhydride III (DFA III) comprising: providing a crude DFA III solution containing DFA III and impurities, said crude DFA III solution having a DFA III purity of at least 60% (w/w) based on dry weight; adding to said crude DFA III solution up to 5% (w/w) of activated carbon particles, wherein said particles have an average particle size from 15 to 200 microns, for a time and under conditions sufficient for the impurities to adsorb onto the activated carbon particles thereby providing a treated crude DFA III solution; separating the treated solution into a liquid phase and a solid phase; and recovering from the liquid phase said purified DFA III as a purified DFA III solution.

17. The process of claim 16, wherein the crude DFA III solution is an extract obtained from Jerusalem artichoke, burdock, or chicory.

18. The process of claim 16, wherein the crude DFA III solution is produced by contacting a solution containing inulin with inulin hydrolase to produce DFA III and then deactivating the inulin hydrolase.

19. The process of claim 16, wherein the crude DFA III solution has an R-Bx of at least 60.

20. The process of claim 16, further comprising filtering the treated crude DFA III solution through diatomaceous earth and through a membrane filter prior to separating the liquid and solid phases.

21. The process of claim 16, further comprising concentrating the purified DFA III solution to form a liquid condensate, and then crystallizing the condensate, thereby obtaining a crystal or granule of said purified DFA III.


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