CN108129345A - A kind of preparation method of D-VB5 calcium - Google Patents
A kind of preparation method of D-VB5 calcium Download PDFInfo
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- CN108129345A CN108129345A CN201810022854.8A CN201810022854A CN108129345A CN 108129345 A CN108129345 A CN 108129345A CN 201810022854 A CN201810022854 A CN 201810022854A CN 108129345 A CN108129345 A CN 108129345A
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- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- C07D307/26—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D307/30—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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- C12P17/00—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms
- C12P17/02—Oxygen as only ring hetero atoms
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Abstract
The present invention relates to biotechnologies and synthesis technical field, specifically disclose a kind of preparation method of D calcium pantothenates.The preparation method, includes the following steps：L pantoic acid lactone hydrolases are added in into DL pantoic acid lactone aqueous solutions, is hydrolyzed, obtains the feed liquid of the pantoic acid lactone containing D；After the filtered processing of feed liquid, extraction processing is carried out with esters solvent, takes organic phase, after washing, obtain D pantoic acid lactone solution；By the D pantoic acid lactones solution after decolorization, dehydration, distillation and concentration processing is carried out, obtains D pantoic acid lactone concentrates；Alanine calcium is added in into the D pantoic acid lactones concentrate, after insulation reaction, D pantothenic acid calcium solutions are obtained by filtration, crystallized processing, filtration treatment, drying process obtain D calcium pantothenates.Preparation method provided by the invention, simple for process, the period is short, high income, good product quality, no coupling product, and no waste water and waste liquid belongs to environmentally friendly production technology.
Description
Technical field
The present invention relates to biotechnology and synthesis technical field more particularly to a kind of preparation methods of D-VB5 calcium.
Background technology
D-VB5 calcium (D- (+)-N- (2,4- dihydroxy -3,3- dimethyl butyryl)-Beta-alanine calcium) is the right side of pantothenic acid
Isomers calcium salt is revolved, is white powder, it is odorless, it is bitter, there is a slight moisture absorption, whens pH value 5.0~7.0 is most stable, is dissolved in sweet
Oil, insoluble in ethyl alcohol, chloroform and ether.One of B family vitamin is the raw materials such as a kind of important medicine, food, health products.
The method for preparing D-VB5 calcium at present, obtains D-VB5 including employing from fermentation culture, is carried by resin
The method taken obtains D-VB5, then the technique of calcium pantothenate is prepared by pantothenic acid, and this method fermentation period is long, and yield is low, operates
Journey is cumbersome, resin treatment complex process, and process has used a large amount of organic acid, and recycling and the discharge of waste water are very big,
It has a certain impact to environment；A large amount of noxious material aminopropionitrile is also used as starting material, using the processing of resin
Mode, entire building-up process high energy consumption, waste liquid yield is big, is unfavorable for energy-saving and environment-friendly idea of development；In addition, also have using micro-
The fractionation that biogenic D-pantoyl lactone hydrolase carries out DL- pantoic acid lactones obtains Pantothenic acid, then by Pantothenic acid
The method for generating D-pantoyl lactone that lactonizes is carried out, this method fractionation period is long, and enzyme dosage is big, and the process of lactonizing employs greatly
The use of sulfuric acid is measured, process is cumbersome, there are a large amount of inorganic salts to generate.
Invention content
It is long for the production cycle of the existing technology, the problems such as process is cumbersome, and waste water and waste liquid yield is big, and yield is low, this
Invention provides a kind of preparation method of D-VB5 calcium.
To achieve the above object of the invention, the embodiment of the present invention employs following technical solution：
A kind of preparation method of D-VB5 calcium, includes the following steps：
(1) L- pantoic acid lactone hydrolases are added in into DL- pantoic acid lactone aqueous solutions, is hydrolyzed, is contained
The feed liquid of D-pantoyl lactone；
(2) after the filtered processing of the feed liquid, extraction processing is carried out with esters solvent, takes organic phase, after washing, obtain
D-pantoyl lactone solution；
(3) by the D-pantoyl lactone solution after decolorization, dehydration, distillation and concentration processing is carried out, is obtained
To D-pantoyl lactone concentrate；
(4) alanine calcium is added in into the D-pantoyl lactone concentrate, after insulation reaction, D-VB5 is obtained by filtration
Calcium solution, crystallized processing, filtration treatment, drying process, obtains D-VB5 calcium.
Relative to the prior art, the preparation method of D-VB5 calcium provided by the invention, simple for process, the period is short, high income,
Good product quality, the L- pantoic acid ammonia generated in the process is recyclable, and water phase can be recycled by reverse-osmosis treated, process
No coupling product generates, and no waste water and waste liquid generates, and belongs to environmentally friendly production technology, convenient for industrialized production.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of preparation method of D-VB5 calcium.The preparation method of the D-VB5 calcium, including as follows
Step：
(1) L- pantoic acid lactone hydrolases are added in into DL- pantoic acid lactone aqueous solutions, is hydrolyzed, is contained
The feed liquid of D-pantoyl lactone；
(2) after the filtered processing of the feed liquid, extraction processing is carried out with esters solvent, takes organic phase, after washing, obtain
D-pantoyl lactone solution；
(3) by the D-pantoyl lactone solution after decolorization, dehydration, distillation and concentration processing is carried out, is obtained
To D-pantoyl lactone concentrate；
(4) alanine calcium is added in into the D-pantoyl lactone concentrate, after insulation reaction, D-VB5 is obtained by filtration
Calcium solution, crystallized processing, filtration treatment, drying process, obtains D-VB5 calcium.
Specifically, DL- pantoic acid lactones be DL- Alpha-hydroxy-β, beta-dimethyl-gamma-butyrolactone alpha-hydroxy-beta, be D-pantoyl lactone with
The racemic modification of L- pantoic acid lactones.
Specifically, in step (1), L- pantoic acid ammonia is further included in the feed liquid containing D-pantoyl lactone, L- pantoic acid ammonia can
Recycling uses.
Specifically, in step (4), the molar ratio of D-pantoyl lactone and alanine calcium is 1:1-1.5.
Preferably, the mass ratio of the L- pantoic acid lactone hydrolases and DL- pantoic acid lactones is (2-20):(5-50),
DL- pantoic acid lactones is made fully to be split, obtain D-pantoyl lactone.
Preferably, the L- pantoic acid lactone hydrolases be ionic dependent type glycosylase, be one kind with physics or change
Mode identifies the enzyme with removal modified base from sugared phosphoric acid DNA chain, L- pantoic acid lactones is only split in split process, most
Remaining D-pantoyl lactone afterwards.
Preferably, the DL- pantoic acid lactones aqueous solution adjusts pH to 5.5-7.5 with ammonium hydroxide, with obtained L- pantoic acid
L- pantoic acid ammonia is formed, convenient for subsequent separating-purifying.
Preferably, the washing times are 2-4 times, make thalline relic and impurity soluble in water, layering removal water phase.
Preferably, the decolorization is carried out by adding in the activated carbon of D-pantoyl lactone solution quality 0.5-1.5%
Decoloration.
Preferably, the dehydration is 80-85 DEG C of reflux 30-60min.
Preferably, the temperature of the insulation reaction is≤60 DEG C, and reaction time 0.5-5h makes D-pantoyl lactone and ammonia
Base calcium propionate fully reacts.
Preferably, the crystallization treatment is to add in the crystal seed of D-VB5 calcium solution quality 0.5-3%, and cooling is crystallized.
Preferably, it is described to be dried under vacuum condition, to be dried in 40-90 DEG C.
The preparation method of D-VB5 calcium provided in an embodiment of the present invention, simple for process, the period is short, high income, product quality
Good, the L- pantoic acid ammonia generated in the process is recyclable, and water phase can be recycled by reverse-osmosis treated, process no coupling product
It generates, no waste water and waste liquid generates, and belongs to environmentally friendly production technology, convenient for industrialized production.
In order to better illustrate the preparation method of D-VB5 calcium provided in an embodiment of the present invention, below by embodiment do into
The illustration of one step.
Embodiment 1
A kind of preparation method of D-VB5 calcium, includes the following steps：
(1) racemic DL- pantoic acid lactones 500kg is dissolved in water, is configured to the aqueous solution that content is 50%, adds in
Ammonium hydroxide adjusts pH in 5.5-7.5, and the L- pantoic acid lactone hydrolases of addition DL- pantoic acid lactone aqueous solutions quality 20% carry out
Hydrolysis process obtains the feed liquid containing D-pantoyl lactone and L- pantoic acid ammonia, after testing 246kg containing D-pantoyl lactone；
(2) after the filtered processing removal bacteria residue of the feed liquid, extraction processing is carried out with using 5 times of ethyl acetate solvent,
Organic phase 1230L is taken, the water for adding in 247L carries out circulated sprinkling 20min, organic layer is layered to obtain after standing, later again to organic
The water that 247L is added in layer carries out circulated sprinkling 20min, stands to obtain organic layer 1160L, obtains D-pantoyl lactone solution；
(3) activated carbon that D-pantoyl lactone quality 1.5% is added in into the D-pantoyl lactone solution is taken off
Color processing, the solution after filtering are warming up to 80-85 DEG C of reflux 30min dehydration, and distillation and concentration residual volume to 820L obtains
D-pantoyl lactone concentrate；
(4) alanine calcium 212kg is added in into the D-pantoyl lactone concentrate, the heat preservation of control temperature≤60 DEG C is anti-
After answering 0.5h, D-VB5 calcium solution is obtained by filtration, adds in the seeded crystallization of D-VB5 calcium solution quality 3%, after filtering, vacuum 45
DEG C be dried, obtain D-VB5 calcium 390kg.
Embodiment 2
A kind of preparation method of D-VB5 calcium, includes the following steps：
(1) racemic DL- pantoic acid lactones 500kg is dissolved in water, is configured to the aqueous solution that content is 30%, adds in
Ammonium hydroxide adjusts pH in 5.5-7.5, and the L- pantoic acid lactone hydrolases of addition DL- pantoic acid lactone aqueous solutions quality 5% carry out water
Solution processing, obtains the feed liquid containing D-pantoyl lactone and L- pantoic acid ammonia, after testing 242kg containing D-pantoyl lactone；
(2) after the filtered processing removal bacteria residue of the feed liquid, extraction processing is carried out with using 10 times of ethyl acetate solvent,
Organic phase 2420L is taken, the water for being separately added into 242L in three times carries out circulated sprinkling 20min, and organic layer is layered to obtain after standing
2280L obtains D-pantoyl lactone solution；
(3) activated carbon that D-pantoyl lactone quality 0.5% is added in into the D-pantoyl lactone solution is taken off
Color processing, the solution after filtering are warming up to 80-85 DEG C of reflux 60min dehydration, and distillation and concentration residual volume to 800L obtains
D-pantoyl lactone concentrate；
(4) alanine calcium 205kg is added in into the D-pantoyl lactone concentrate, the heat preservation of control temperature≤60 DEG C is anti-
After answering 2h, D-VB5 calcium solution is obtained by filtration, adds in the seeded crystallization of D-VB5 calcium solution quality 0.5%, after filtering, vacuum 80
DEG C be dried, obtain D-VB5 calcium 375kg.
As seen from the above embodiment, the preparation method of D-VB5 calcium provided in an embodiment of the present invention, simple for process, period
Short, high income, process no coupling product generates, and no waste water and waste liquid generates, and belongs to environmentally friendly production technology, convenient for industrial metaplasia
Production.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent replacement or improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of D-VB5 calcium, it is characterised in that：Include the following steps：
(1) L- pantoic acid lactone hydrolases are added in into DL- pantoic acid lactone aqueous solutions, are hydrolyzed, are obtained general containing D-
Solve the feed liquid of acid lactone；
(2) after the filtered processing of the feed liquid, extraction processing is carried out with esters solvent, takes organic phase, after washing, it is general to obtain D-
Solve acid lactone solution；
(3) by the D-pantoyl lactone solution after decolorization, dehydration, distillation and concentration processing is carried out, obtains D-
Pantoic acid lactone concentrate；
(4) alanine calcium is added in into the D-pantoyl lactone concentrate, after insulation reaction, it is molten that D-VB5 calcium is obtained by filtration
Liquid, crystallized processing, filtration treatment, drying process, obtains D-VB5 calcium.
2. the preparation method of D-VB5 calcium as described in claim 1, it is characterised in that：The L- pantoic acid lactone hydrolases with
The mass ratio of DL- pantoic acid lactones is (2-20):(5-50).
3. the preparation method of D-VB5 calcium as claimed in claim 2, it is characterised in that：The L- pantoic acid lactone hydrolases are
Ionic dependent type glycosylase.
4. the preparation method of D-VB5 calcium as described in claim 1, it is characterised in that：The DL- pantoic acid lactones aqueous solution
PH to 5.5-7.5 is adjusted with ammonium hydroxide.
5. the preparation method of D-VB5 calcium as described in claim 1, it is characterised in that：The washing times are 2-4 times.
6. the preparation method of D-VB5 calcium as described in claim 1, it is characterised in that：The decolorization is general by adding in D-
The activated carbon of solution acid lactone solution quality 0.5-1.5% decolourizes.
7. the preparation method of D-VB5 calcium as described in claim 1, it is characterised in that：The dehydration is returned for 80-85 DEG C
Flow 30-60min.
8. the preparation method of D-VB5 calcium as described in claim 1, it is characterised in that：The temperature of the insulation reaction is≤60
DEG C, reaction time 0.5-5h.
9. such as the preparation method of claim 1-8 any one of them D-VB5 calcium, it is characterised in that：The crystallization treatment is adds
Enter the crystal seed of D-VB5 calcium solution quality 0.5-3%, cooling is crystallized.
10. such as the preparation method of claim 1-8 any one of them D-VB5 calcium, it is characterised in that：The drying process is
Under vacuum condition, it is dried in 40-90 DEG C.
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| CN201810022854.8A CN108129345A (en) | 2018-01-10 | 2018-01-10 | A kind of preparation method of D-VB5 calcium |
| CN202310228550.8A CN116217427A (en) | 2018-01-10 | 2018-01-10 | Preparation method of D-calcium pantothenate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257464A (en) * | 2019-07-12 | 2019-09-20 | 抚顺顺特化工有限公司 | A kind of preparation method of D-VB5 calcium |
| CN111410614A (en) * | 2020-05-14 | 2020-07-14 | 吴江 | Full-synthesis environment-friendly process of D-calcium pantothenate |
| CN111518861A (en) * | 2020-05-14 | 2020-08-11 | 吴江 | Novel process for preparing D-calcium pantothenate |
| CN111748591A (en) * | 2019-03-29 | 2020-10-09 | 安徽华恒生物科技股份有限公司 | Production method of D-pantoic acid lactone |
| CN112409303A (en) * | 2020-12-09 | 2021-02-26 | 合肥工业大学 | Purification method of D-pantoic acid lactone |
| CN112457181A (en) * | 2020-12-11 | 2021-03-09 | 黄冈美丰化工科技有限公司 | Synthesis method of D-calcium pantothenate |
| CN113214046A (en) * | 2020-12-04 | 2021-08-06 | 安徽华恒生物科技股份有限公司 | Method for recycling D-calcium pantothenate mother liquor |
| CN115925573A (en) * | 2022-11-14 | 2023-04-07 | 浙江新和成股份有限公司 | Purification method of D-calcium pantothenate |
| CN116217428A (en) * | 2022-12-22 | 2023-06-06 | 黑龙江新和成生物科技有限公司 | Methanol hydrate crystal of D-calcium pantothenate and process for producing D-calcium pantothenate |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748591A (en) * | 2019-03-29 | 2020-10-09 | 安徽华恒生物科技股份有限公司 | Production method of D-pantoic acid lactone |
| CN111748591B (en) * | 2019-03-29 | 2022-04-01 | 安徽华恒生物科技股份有限公司 | Production method of D-pantoic acid lactone |
| CN110257464A (en) * | 2019-07-12 | 2019-09-20 | 抚顺顺特化工有限公司 | A kind of preparation method of D-VB5 calcium |
| CN111410614A (en) * | 2020-05-14 | 2020-07-14 | 吴江 | Full-synthesis environment-friendly process of D-calcium pantothenate |
| CN111518861A (en) * | 2020-05-14 | 2020-08-11 | 吴江 | Novel process for preparing D-calcium pantothenate |
| CN111518861B (en) * | 2020-05-14 | 2022-05-03 | 安徽泰格生物科技有限公司 | Novel process for preparing D-calcium pantothenate |
| CN113214046A (en) * | 2020-12-04 | 2021-08-06 | 安徽华恒生物科技股份有限公司 | Method for recycling D-calcium pantothenate mother liquor |
| CN113214046B (en) * | 2020-12-04 | 2023-07-28 | 安徽华恒生物科技股份有限公司 | Method for recycling D-calcium pantothenate mother liquor |
| CN112409303A (en) * | 2020-12-09 | 2021-02-26 | 合肥工业大学 | Purification method of D-pantoic acid lactone |
| CN112457181A (en) * | 2020-12-11 | 2021-03-09 | 黄冈美丰化工科技有限公司 | Synthesis method of D-calcium pantothenate |
| CN112457181B (en) * | 2020-12-11 | 2023-08-29 | 黄冈美丰化工科技有限公司 | Synthesis method of D-calcium pantothenate |
| CN115925573A (en) * | 2022-11-14 | 2023-04-07 | 浙江新和成股份有限公司 | Purification method of D-calcium pantothenate |
| CN115925573B (en) * | 2022-11-14 | 2024-06-04 | 浙江新和成股份有限公司 | Purification method of D-calcium pantothenate |
| CN116217428A (en) * | 2022-12-22 | 2023-06-06 | 黑龙江新和成生物科技有限公司 | Methanol hydrate crystal of D-calcium pantothenate and process for producing D-calcium pantothenate |
| CN116217428B (en) * | 2022-12-22 | 2024-04-02 | 黑龙江新和成生物科技有限公司 | Methanol hydrate crystal of D-calcium pantothenate and process for producing D-calcium pantothenate |
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| CN116217427A (en) | 2023-06-06 |
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Application publication date: 20180608 |