CN106220557A - A kind of separating and extracting process of food stage nicotinic acid - Google Patents
A kind of separating and extracting process of food stage nicotinic acid Download PDFInfo
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- CN106220557A CN106220557A CN201610579361.5A CN201610579361A CN106220557A CN 106220557 A CN106220557 A CN 106220557A CN 201610579361 A CN201610579361 A CN 201610579361A CN 106220557 A CN106220557 A CN 106220557A
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- nicotinic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom 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
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/79—Acids; Esters
- C07D213/80—Acids; Esters in position 3
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom 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
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/79—Acids; Esters
- C07D213/803—Processes of preparation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of food stage nicotinic acid separating and extracting process based on bioconversion, remove thalline including to conversional solution through ceramic membrane or plate-and-frame filtration, the nicotinic acid solution after process through macroporous resin adsorption, eluting, concentrate, crystallize, be dried, obtain nicotinic acid finished product.Primary crystallization mother solution need to reclaim to improve nicotinic acid yield.This technological operation is succinct, energy-conserving and environment-protective, and can realize producing continuously.Cigarette extracts total recovery and can reach more than 90%, and product quality meets national standard.
Description
Technical field
The invention belongs to biological chemical field, relate to one and prepare extraction, particularly relate to preparation from fermentation liquid and extract
The method of food stage nicotinic acid.
Background technology
Nicotinic acid (Nicotinic acid) chemical name is pyridine-3-carboxylic acid, is commonly called as nicotinic acid, vitamin PP or vitamin
B3, is one of 13 kinds of vitamin of needed by human, and its molecular formula is C6H5NO2, and molecular weight is 123.11, and fusing point 236 DEG C is readily soluble
In boiling water, boiling ethanol, alkali hydroxide and alkali carbonate solution, it is dissolved in propylene glycol, insoluble in ether, its structural formula such as Fig. 1.
The demand of nicotinic acid is every day by human body: adult 10～20mg, baby 4～11mg (Li Yanyun, Beijing petrochemical industry
Institute's journal, 2006,14:59-64).Necessary composition during nicotinic acid is also the animal diets such as pig, chicken simultaneously.Nicotinic acid can affect
Hematopoiesis, promotes ferrum to absorb and the generation of hemocyte；Nicotinic acid is the material that synthetic hormones is integral, can maintain health
Nervous system and normal brain function；The health of facilitating digestion system, alleviates gastrointestinal disorders；Treatment oral cavity, lip inflammation, prevent
Halitosis；Reduce cholesterol and triglyceride.In addition nicotinic acid can also improve the production performance of poultry, promotes feed conversion rate and product
Egg rate.Affect glycolysis, tricarboxylic acid cycle, respiratory chain and fatty acid biological synthesis during nicotinic acid deficiency, cause pellagra.
In view of these functions of nicotinic acid, being the most widely used at industry tools such as food, medicine and feedstuffs, (Zhu Bingchun etc., chemical industry is indulged
Horizontal stroke, 2004,18:1-4).
Up to now the production method of nicotinic acid includes chemical oxidization method and biotransformation method.Nicotinic acid preparation the earliest produces work
Before skill builds on 100 years, mainly used at that time potassium dichromate oxidation nicotine prepare nicotinic acid (Chuck R., Chimia,
2000,54:508-513).The existing industrial process of nicotinic acid includes potassium permanganate oxidation method, nitre potassium permanganate oxidation method, nitre
Nitric acid-sulfuric acid oxidizing process, ammonia oxidation etc. (Wang Liucheng etc., fine chemistry industry, 2004,21:133-136).But these existing methods
Needing to carry out under high pressure, hot conditions, corrosivity is big, high to equipment requirements, and production cost is high, and economic benefit is low, and the three wastes are dirty
Dye is serious.Compared to chemical method, utilizing biological enzyme synthesis nicotinic acid to have course of reaction simple, by-product is few, process conditions
Gentleness, the most progressively come into one's own (Gong JS, et al.Microb Cell Fact, 2012,11:142), bioconversion
Method is current prefered method, and its product extracts flow process and generally includes: the acidifying of microbe conversion liquid, ceramic membrane filter, ultrafiltration, activity
Carbon decoloring, crystallization.The method flow process complexity, extracting cycle length, acid adding waste water intractability are big, high to equipment investment cost, receipts
Rate is the most on the low side.The present invention uses macroporous resin D201 to separate nicotinic acid from conversional solution, and resins selective is good, can effectively remove filter
Inorganic salt in liquid, solubility foreign protein, pigment etc., product quality and yield are high, and production cost is low.Technique is a large amount of without using
Concentrated acid, concise in technology, discharge of wastewater, energy-conserving and environment-protective are greatly reduced, and can realize producing continuously.Cigarette extracts total recovery and can reach
More than 90%, product quality meets standard GB/T 14757-2010, food additive nicotinic acid.
Summary of the invention
The present invention uses a kind of physical method that bioconversion broth is carried out pretreatment, the solution after process again through hanging column, wash
Take off, concentrate, be dried, produce the purity of the nicotinic acid obtained more than 99.5%.The operation of the method more original method is easier, one-tenth
Basis is the lowest, also improve product yield, reduce highly polluted wastewater displacement；It is to country's accelerated development environmental protection processing skill
Providing powerful support for of art.
It is an object of the invention to provide a kind of convenient and swift, low cost, effective macroporous resin from bioconversion broth
The method of middle separation and Extraction nicotinic acid.
Therefore it is an object of the invention to provide a kind of from fermentation liquid extraction prepare the technical solution of nicotinic acid, specifically
Comprise the steps:
(1) conversional solution pretreatment: the conversional solution containing nicotinic acid is removed thalline through ceramic membrane or plate-and-frame filtration, obtains filtrate；
(2) resin regeneration: loaded by resin in resin column, is passed through 50% ethanol solution；It is passed through 5%NaOH solution, has led to
After, with pure water to pH8.0；It is passed through 5%HCl solution, after having led to, with pure water to pH3.5；
(3) hanging column absorption: the employing macroporous resin D201 containing nicotinic acid filtrate collected by step (1) is carried out upper prop absorption,
After absorption terminates, add pure water and wash post, add the hot water that temperature is 60-70 DEG C and resolve, obtain nicotinic acid desorbed solution；
(4) concentrate, be dried: desorbed solution pumps into membrane evaporator and is concentrated in vacuo, and temperature is 35-55 DEG C, is placed in by concentrated solution
In crystallizer, stirring, cool to 15-30 DEG C, temperature control crystallizes；Centrifugal collection crystal, and use purified water washing crystal, it is placed in
Far infrared drying oven is dried, it is thus achieved that nicotinic acid finished product；Meanwhile, crystalline mother solution need to reclaim, and hangs according to step 3
Post, wash post, parsing, and again carry out concentrating, crystallize, be dried, obtain finished product.
The present invention for the advantage of the method for nicotinic acid separation and Extraction is: operating procedure is simple, and separating step is few, production cost
Low, energy consumption is little, uses resin absorption desalination bleaching can effectively remove inorganic salt, soluble protein and the pigment in conversional solution
Deng, the product quality of results and yield are high, and production cost is low.Product quality meets standard GB/T 14757-2010, food additive
Add agent nicotinic acid.
Accompanying drawing explanation
Fig. 1 nicotinic acid structural formula
Detailed description of the invention
Below by embodiment, technical scheme is described in further detail.
Embodiment 1
After nicotinic acid bioconversion has reacted, taking nicotinic acid conversional solution 100L, conversion acid production rate is 150g/L, will convert liquid pump
Entering filter area is 1m2, the purpose ceramic-film filter of aperture 50nm filter, control temperature be 30 DEG C, enter film pressure and membrane
Pressure differential is 0.25MPa, and filtering velocity is 20L/h, is continuously added to purified water top when remaining feed liquid 25L and washes, and maintains liquid level 15L to continue
Filter, until Nicotinic Acid Content is less than stopping during below 1.5g/L filtering in dope, obtain nicotinic acid membrane filtration liquid 160L, content 93.7g/
L, the film yield of crossing of nicotinic acid is 99.5%.The punching adsorbent resin that 90L model is D201 is loaded the resin of φ 40cm × 150cm
In post, use 50% ethanol solution, flow velocity 40L/h, when being passed through 100L, soak 4h, then be passed through 60L stopping；It is passed through 5%NaOH
Solution, flow velocity 60L/h, after having led to, with pure water to pH8.0；It is passed through 5%HCl solution 200L, speed 60L/h, after having led to,
Stand-by to pH3.5 with pure water；Ceramic membrane filter gained filtrate 160L is carried out upper prop absorption, and flow velocity is 30L/h, absorption knot
Adding 140L pure water after bundle and wash post, flow velocity 30L/h, add the hot water that temperature is 60 DEG C and resolve, flow velocity is 15L/h, is solved
Analysis liquid 290L, Nicotinic Acid Content 49.52g/L, yield is 95.73%.Desorbed solution being pumped into membrane evaporator be concentrated in vacuo, temperature is
45 DEG C, it is concentrated into when volume is 20L and stops concentrating；Concentrated solution is placed in crystallizer, stirs, cool to 20 DEG C, temperature control
Crystallization；Centrifugal collection crystal, and use purified water washing crystal, it is placed in far infrared drying oven and is dried, it is thus achieved that nicotinic acid finished product；
Meanwhile, the centrifugal crystalline mother solution obtained of collecting need to reclaim simultaneously, again adsorbs macroporous resin, washes post, parsing, and again enters
Row concentrates, crystallizes, is dried, obtains finished product, obtains nicotinic acid solid, and conversional solution nicotinic acid disposably extracts and disposing mother liquor adds up to total receipts
Rate is 91.3%, and purity is 99.7% after testing.
Embodiment 2
After nicotinic acid bioconversion has reacted, taking nicotinic acid conversional solution 200L, conversion acid production rate is 150g/L, will convert liquid pump
Entering filter area is 2m2, the purpose ceramic-film filter of aperture 50nm filter, control temperature be 30 DEG C, enter film pressure and membrane
Pressure differential is 0.25MPa, and filtering velocity is 20L/h, is continuously added to purified water top when remaining feed liquid 25L and washes, and maintains liquid level 15L to continue
Filter, until Nicotinic Acid Content is less than stopping during below 1.5g/L filtering in dope, obtain nicotinic acid membrane filtration liquid 280L, content
106.4g/L, the film yield of crossing of nicotinic acid is 99.3%.Punching adsorbent resin that 140L model is D201 is loaded φ 40cm ×
In the resin column of 150cm, by resin regeneration, ceramic membrane filter gained filtrate 280L being carried out upper prop absorption, flow velocity is 30L/
H, absorption adds 200L pure water after terminating and washes post, flow velocity 30L/h, adds the hot water that temperature is 60 DEG C and resolves, and flow velocity is 15L/
H, obtains desorbed solution 460L, Nicotinic Acid Content 63.3g/L, and yield is 97.06%.Desorbed solution is pumped into membrane evaporator vacuum dense
Contracting, temperature is 50 DEG C, is concentrated into when volume is 30L and stops concentrating；Concentrated solution is placed in crystallizer, stir, cool to
20 DEG C, temperature control crystallizes；Centrifugal collection crystal, and use purified water washing crystal, it is placed in far infrared drying oven and is dried, it is thus achieved that
Nicotinic acid finished product；The centrifugal crystalline mother solution obtained of collecting need to reclaim simultaneously, again adsorbs macroporous resin, washes post, parsing, and again
Secondary carrying out concentrating, crystallize, be dried, obtain finished product, obtain nicotinic acid solid, conversional solution nicotinic acid disposably extracts and disposing mother liquor adds up to
Total recovery is 93.6%, and it is white powder that gained nicotinic acid observes its outward appearance under natural light, content ＞ 99.5%.
The invention is not restricted to these disclosed embodiments, the present invention is by the scope described by soverlay technique scheme, Yi Jiquan
The various deformation of profit claimed range and equivalence change, on the premise of without departing from the technical solution of the present invention, to the present invention
Any amendment, equivalent or the improvement that the those skilled in the art made easily realize, belongs to the present invention claimed
Scope.
Claims (5)
1. a food stage nicotinic acid separating and extracting process based on bioconversion, it is characterised in that described separating and extracting process bag
Include: bioconversion broth is removed thalline through ceramic membrane or plate-and-frame filtration, nicotinic acid solution macroporous resin adsorption again after process, wash
Take off, concentrate, be dried, produce and obtain purity nicotinic acid more than 99.5%.
2. the method for claim 1, it is characterised in that to the nicotinic acid solution pump through ceramic membrane or plate-and-frame filtration pretreatment
Enter and strong-base anion-exchange resin carries out upper prop absorption, then wash post by pure water, utilize the pyrohydrolysis that temperature is 60-70 DEG C
Analysis, obtains nicotinic acid desorbed solution.
3. the method for claim 1, it is characterised in that macroporous resin is after using 5-10 to criticize continuously, according to following step
Suddenly carry out resin regeneration: loaded by resin in resin column, be passed through 50% ethanol solution；It is passed through 5%NaOH solution, after having led to, uses
Pure water is to pH8.0；It is passed through 5%HCl solution, after having led to, with pure water to pH3.5.
4. the method for claim 1, it is characterised in that described concentration, dry concrete operations are: destaining solution pumps into thin
Film evaporator is concentrated in vacuo, and temperature is 35-55 DEG C；Concentrated solution is placed in crystallizer, stirs, cool to 15-30 DEG C, control
Temperature crystallization；Centrifugal collection crystal, and use purified water washing crystal, it is placed in far infrared drying oven and is dried, it is thus achieved that nicotinic acid becomes
Product.
5. method as claimed in claim 4, is characterized by, after the centrifugal collection of crystal, crystalline mother solution need to reclaim, according to power
Profit requires that step described in 2 carries out hanging column, washes post, parsing, and carry out concentrating according to step described in claim 4, crystallize, be dried,
Obtain finished product.
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| CN201610579361.5A CN106220557B (en) | 2016-07-22 | 2016-07-22 | A kind of separating and extracting process of food-grade niacin |
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| CN201610579361.5A CN106220557B (en) | 2016-07-22 | 2016-07-22 | A kind of separating and extracting process of food-grade niacin |
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| CN106220557A true CN106220557A (en) | 2016-12-14 |
| CN106220557B CN106220557B (en) | 2019-06-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108112855A (en) * | 2017-12-14 | 2018-06-05 | 成都新柯力化工科技有限公司 | A kind of method that wholefood antioxidant is extracted from areca leaf |
| CN110746351A (en) * | 2019-10-30 | 2020-02-04 | 南宁学院 | Method for extracting nicotinic acid from beef tripe |
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| CN102249994A (en) * | 2011-05-10 | 2011-11-23 | 浙江爱迪亚营养科技开发有限公司 | Preparation method of nicotinic acid |
| CN103060397A (en) * | 2012-12-13 | 2013-04-24 | 江南大学 | Method of immobilizing gibberella and using gibberella for biological transformation to prepare nicotinic acid |
-
2016
- 2016-07-22 CN CN201610579361.5A patent/CN106220557B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249994A (en) * | 2011-05-10 | 2011-11-23 | 浙江爱迪亚营养科技开发有限公司 | Preparation method of nicotinic acid |
| CN103060397A (en) * | 2012-12-13 | 2013-04-24 | 江南大学 | Method of immobilizing gibberella and using gibberella for biological transformation to prepare nicotinic acid |
Non-Patent Citations (2)
| Title |
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| 王大明: "烟酸的生物转化与提取工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108112855A (en) * | 2017-12-14 | 2018-06-05 | 成都新柯力化工科技有限公司 | A kind of method that wholefood antioxidant is extracted from areca leaf |
| CN110746351A (en) * | 2019-10-30 | 2020-02-04 | 南宁学院 | Method for extracting nicotinic acid from beef tripe |
| CN110746351B (en) * | 2019-10-30 | 2021-03-16 | 南宁学院 | Method for extracting nicotinic acid from beef tripe |
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| CN106220557B (en) | 2019-06-25 |
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