CN106220557B - A kind of separating and extracting process of food-grade niacin - Google Patents
A kind of separating and extracting process of food-grade niacin Download PDFInfo
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- CN106220557B CN106220557B CN201610579361.5A CN201610579361A CN106220557B CN 106220557 B CN106220557 B CN 106220557B CN 201610579361 A CN201610579361 A CN 201610579361A CN 106220557 B CN106220557 B CN 106220557B
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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
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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
- C07D213/803—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-grade niacin separating and extracting process based on bioconversion, including remove thallus through ceramic membrane or plate-frame filtering to conversion fluid, treated niacin solution obtain niacin finished product through macroporous resin adsorption, elution, concentration, crystallization, drying.Primary crystallization mother liquor need to be recycled to improve niacin yield.The technological operation is succinct, energy conservation and environmental protection, and can realize continuous production.Cigarette, which extracts total recovery, can reach 90% or more, and product quality meets national standard.
Description
Technical field
The invention belongs to biological chemical field, be related to it is a kind of prepare extraction, extracted more particularly to being prepared from fermentation liquid
The method of food-grade niacin.
Background technique
Niacin (Nicotinic acid) chemical name is pyridine-3-carboxylic acid, is commonly called as niacin, nicotinic acid or vitamin
B3, is one of 13 kinds of vitamin needed by human, molecular formula C6H5NO2, and molecular weight 123.11 is 236 DEG C of fusing point, readily soluble
In boiling water, boiling ethyl alcohol, alkali hydroxide and alkali carbonate solution, it is dissolved in propylene glycol, does not dissolve in ether, structural formula such as Fig. 1.
Human body is daily to the demand of niacin are as follows: adult 10~20mg, 4~11mg of baby (Li Yanyun, Beijing petrochemical industry
Institute's journal, 2006,14:59-64).Niacin is also necessary ingredient in the animal diets such as pig, chicken simultaneously.Niacin can influence
Hematopoiesis promotes iron to absorb the generation with haemocyte；Niacin is the integral substance of synthetic hormones, can maintain health
Nervous system and normal brain function；Promote the health of digestive system, mitigates gastrointestinal disorders；Oral cavity, lip inflammation are treated, is prevented
Halitosis；Reduce cholesterol and triglyceride.Furthermore niacin can also improve the production performance of livestock and poultry, promote feed conversion rate and production
Egg rate.Glycolysis, citrate cycle, respiratory chain and fatty acid biological synthesis are influenced when niacin deficiency, cause pellagra.
In view of these functions of niacin, in industries such as food, medicine and feeds, with being widely applied, (Zhu Bingchun etc., chemical industry are vertical at present
Cross, 2004,18:1-4).
Up to now the production method of niacin includes chemical oxidization method and biotransformation method.Earliest niacin preparation production work
Skill was built on before 100 years, mainly prepared at that time using potassium dichromate oxidation nicotine niacin (Chuck R., Chimia,
2000,54:508-513).The existing industrial process of niacin 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
It needs to carry out under high pressure, hot conditions, corrosivity is big, and the high requirements on the equipment, high production cost, economic benefit is low, and the three wastes are dirty
Dye is serious.Compared to chemical method, have reaction process simple using biological enzyme synthesis niacin, by-product is few, process conditions
Mildly, therefore be gradually taken seriously (Gong JS, et al.Microb Cell Fact, 2012,11:142), bioconversion
Method is current prefered method, and product extracts process and generally includes: the acidification of microbe conversion liquid, ceramic membrane filter, ultrafiltration, activity
Carbon decoloring, crystallization.This method process is complicated, extracting cycle is long, acid adding wastewater treatment difficulty is big, receipts high to equipment investment cost
Rate is relatively relatively low.The present invention separates niacin using macroreticular resin D201 from conversion fluid, and resins selective is good, can effectively remove filter
Inorganic salts, soluble foreign protein, pigment in liquid etc., product quality and high income, production cost are low.Technique is without using a large amount of
Concentrated acid, concise in technology are greatly reduced discharge of wastewater, energy conservation and environmental protection, and can realize continuous production.Cigarette extracts total recovery and can reach
90% or more, product quality meets standard GB/T 14757-2010, food additives niacin.
Summary of the invention
The present invention pre-processes bioconversion broth using a kind of physical method, treated solution again through hanging column, wash
De-, concentration, drying, produce the purity of the niacin of acquisition 99.5% or more.The operation is more convenient for the more original method of this method, at
Sheet is lower, also improves product yield, reduces highly polluted wastewater displacement；It is to the environmentally protective processing skill of national accelerated development
The strong support of art.
The purpose of the present invention is to provide a kind of convenient and efficient, at low cost, macroreticular resins that effect is good from bioconversion broth
The method of middle separation and Extraction niacin.
Therefore the purpose of the present invention is to provide a kind of from fermentation liquid, and extraction prepares the technical solution of niacin, specifically
Include the following steps:
(1) conversion fluid pre-processes: the conversion fluid containing niacin being removed thallus through ceramic membrane or plate-frame filtering, obtains filtrate；
(2) resin regeneration: resin is fitted into resin column, is passed through 50% ethanol solution；It is passed through 5%NaOH solution, has been led to
Afterwards, 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 adsorbs: filtrate containing niacin collected by step (1) is subjected to upper prop absorption using macroreticular resin D201,
After absorption, pure water is added and washes column, adds the hot water that temperature is 60-70 DEG C and parse, obtain niacin desorbed solution；
(4) be concentrated, be dry: desorbed solution is pumped into thin film evaporator vacuum concentration, and temperature is 35-55 DEG C, and concentrate is placed in
It in crystallizing tank, stirs, cool to 15-30 DEG C, temperature control crystallizes；Crystal is collected by centrifugation, and with water washing crystal is purified, is placed in
It is dried in far infrared drying oven, obtains niacin finished product；Meanwhile crystalline mother solution need to be recycled, and be hung according to step 3
Column washes column, parsing, and is concentrated again, crystallizes, dries, obtains finished product.
The present invention be used for niacin separation and Extraction method the advantages of be: operating procedure is simple, and separating step is few, production cost
Low, production energy consumption is small, and inorganic salts, soluble protein and pigment in conversion fluid can be effectively removed using resin adsorption desalination bleaching
Deng the product quality and high income of harvest, production cost is low.Product quality meets standard GB/T 14757-2010, food additive
Add agent niacin.
Detailed description of the invention
Fig. 1 niacin structural formula
Specific embodiment
Below by embodiment, technical scheme of the present invention will be described in further detail.
Embodiment 1
Niacin bioconversion after the reaction was completed, takes niacin conversion fluid 100L, and conversion acid production rate is 150g/L, will convert liquid pump
Entering filter area is 1m2, aperture 50nm purpose ceramic-film filter be filtered, controlled at 30 DEG C, into film pressure and membrane
Pressure difference is 0.25MPa, filtering velocity 20L/h, is continuously added to purified water top as remaining feed liquid 25L and washes, and liquid level 15L is maintained to continue
Filtering stops filtering when until Nicotinic Acid Content being lower than 1.5g/L or less in dope, obtains niacin membrane filtration liquid 160L, content 93.7g/
The film yield of crossing of L, niacin are 99.5%.By the resin of 90L model D201 beaten macroporous adsorbent resin and be packed into φ 40cm × 150cm
In column, using 50% ethanol solution, flow velocity 40L/h impregnates 4h when being passed through 100L, then is 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,
It is stand-by to pH3.5 with pure water；Filtrate 160L obtained by ceramic membrane filter is subjected to upper prop absorption, flow velocity 30L/h, absorption knot
140L pure water is added after beam and washes column, flow velocity 30L/h adds the hot water that temperature is 60 DEG C and parses, and flow velocity 15L/h is solved
Analyse liquid 290L, Nicotinic Acid Content 49.52g/L, yield 95.73%.Desorbed solution is pumped into thin film evaporator vacuum concentration, temperature is
It 45 DEG C, is concentrated into when volume is 20L and stops concentration；Concentrate is placed in crystallizing tank, stirs, cool to 20 DEG C, temperature control
Crystallization；Crystal is collected by centrifugation, and with water washing crystal is purified, is placed in far infrared drying oven and is dried, obtain niacin finished product；
Meanwhile while the crystalline mother solution that is collected by centrifugation need to be recycled, adsorb macroreticular resin again, wash column, parsing, and again into
Row concentration crystallizes, is dry, obtaining finished product to get niacin solid, and conversion fluid niacin disposably extracts and the total total receipts of disposing mother liquor
Rate is 91.3%, is 99.7% through detection purity.
Embodiment 2
Niacin bioconversion after the reaction was completed, takes niacin conversion fluid 200L, and conversion acid production rate is 150g/L, will convert liquid pump
Entering filter area is 2m2, aperture 50nm purpose ceramic-film filter be filtered, controlled at 30 DEG C, into film pressure and membrane
Pressure difference is 0.25MPa, filtering velocity 20L/h, is continuously added to purified water top as remaining feed liquid 25L and washes, and liquid level 15L is maintained to continue
Filtering stops filtering when until Nicotinic Acid Content being lower than 1.5g/L or less in dope, obtains niacin membrane filtration liquid 280L, content
The film yield of crossing of 106.4g/L, niacin are 99.3%.By 140L model D201 beat macroporous adsorbent resin be packed into φ 40cm ×
In the resin column of 150cm, by resin regeneration, filtrate 280L obtained by ceramic membrane filter is subjected to upper prop absorption, flow velocity 30L/
H is added 200L pure water and washes column after absorption, flow velocity 30L/h adds the hot water that temperature is 60 DEG C and parses, flow velocity 15L/
H obtains desorbed solution 460L, Nicotinic Acid Content 63.3g/L, yield 97.06%.It is dense that desorbed solution is pumped into thin film evaporator vacuum
Contracting, temperature are 50 DEG C, are concentrated into when volume is 30L and stop concentration；Concentrate is placed in crystallizing tank, stir, cool to
20 DEG C, temperature control crystallization；Crystal is collected by centrifugation, and with water washing crystal is purified, is placed in far infrared drying oven and is dried, obtain
Niacin finished product；The crystalline mother solution being collected by centrifugation simultaneously need to be recycled, and adsorbed macroreticular resin again, washed column, parsing, and again
Secondary to be concentrated, crystallized, dried, obtaining finished product to get niacin solid, conversion fluid niacin disposably extracts and disposing mother liquor is total
Total recovery is 93.6%, and it is white powder, content > 99.5% that gained niacin observes its appearance under natural light.
Disclosed embodiment that the present invention is not restricted to these, the present invention is by range described in soverlay technique scheme, Yi Jiquan
The various modifications and equivalence changes of sharp claimed range, under the premise of without departing from technical solution of the invention, to the present invention
It is claimed to belong to the present invention for made those skilled in the art any modification, equivalent replacement or improvement easy to accomplish
Range.
Claims (1)
1. a kind of food-grade niacin separating and extracting process based on bioconversion, which comprises the steps of:
(1) conversion fluid pre-processes: the conversion fluid containing niacin being removed thallus through ceramic membrane or plate-frame filtering, obtains filtrate；
(2) resin regeneration: resin is fitted into resin column, is passed through 50% ethanol solution；It is passed through 5%NaOH solution, after having led to, is used
Pure water is to pH8.0；It is passed through 5%HCl solution, after having led to, with pure water to pH3.5；
(3) hanging column adsorbs: filtrate containing niacin collected by step (1) is carried out upper prop absorption, absorption using macroreticular resin D201
After, pure water is added and washes column, adds the hot water that temperature is 60-70 DEG C and parses, obtain niacin desorbed solution；
(4) be concentrated, be dry: desorbed solution is pumped into thin film evaporator vacuum concentration, and temperature is 35-55 DEG C, and concentrate is placed in crystallization
It in tank, stirs, cool to 15-30 DEG C, temperature control crystallizes；Crystal is collected by centrifugation, and with water washing crystal is purified, is placed in remote red
It is dried in outer drying box, obtains niacin finished product；Meanwhile crystalline mother solution need to be recycled, and carried out hanging column according to step 3, washed
Column, parsing, and be concentrated again, crystallize, dry, 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 CN106220557A (en) | 2016-12-14 |
| CN106220557B true CN106220557B (en) | 2019-06-25 |
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| 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 |
| CN110746351B (en) * | 2019-10-30 | 2021-03-16 | 南宁学院 | Method for extracting nicotinic acid from beef tripe |
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 |
-
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 |
|---|
| 3-甲基吡啶化学制备工艺优化及分离新工艺研究;许晶;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20140115(第01期);第34页第11-12行，倒数第1行,第48页第2-5段 |
| 烟酸的生物转化与提取工艺研究;王大明;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20130315(第03期);第55页第4段,57页第1段,第71页倒数第1-7行和第72页第1-2行 |
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