CN108084185A - A kind of environment-friendly type folic acid process for purification - Google Patents
A kind of environment-friendly type folic acid process for purification Download PDFInfo
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- CN108084185A CN108084185A CN201711469517.5A CN201711469517A CN108084185A CN 108084185 A CN108084185 A CN 108084185A CN 201711469517 A CN201711469517 A CN 201711469517A CN 108084185 A CN108084185 A CN 108084185A
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- Prior art keywords
- folic acid
- filtrate
- crude product
- sulfuric acid
- add
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D475/00—Heterocyclic compounds containing pteridine ring systems
- C07D475/02—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4
- C07D475/04—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4 with a nitrogen atom directly attached in position 2
Abstract
The invention discloses a kind of methods that environment-friendly type folic acid refines, and by the way that folic acid crude product is dissolved in sulfuric acid solution, after adding water stirring that yellow solid is precipitated, filtering obtains folic acid highly finished product and filtrate；Active carbon adsorption filtering is added in filtrate；Filtrate after filtering further carries out nanofiltration processing；The concentrated sulfuric acid is finally added in filtrate, it is 40 45% to adjust concentration, for the refined of folic acid crude product, is repeated in above-mentioned steps, filtrate can be recycled 35 times.Folic acid is carried out using method provided by the invention to refine, concentrated sulfuric acid dosage saves more than 60%, and the folic acid purity after acid treating is up to more than 90%, and power consumption is small, extensive and automated production easy to implement.
Description
Technical field
It is particularly a kind of to be removed using active carbon adsorption and nanofiltration filtering technique the present invention relates to a kind of folic acid process for purification
Acid molten impurities in water during folic acid crude product refining, and recycle the effective ways of the molten water of acid.
Background technology
Folic acid is a kind of water-soluble B vitamin, as the coenzyme of one carbon unit transfer enzyme system in internal biochemical reaction, is risen
The effect of one carbon unit carrier, the synthesis of participation purine and thymidine and further synthetic DNA and RNA, participates in amino
Acid metabolic mutually converts process between glycine and serine, histidine and glutamic acid, homocysteine and methionine
In serve as the carrier of one carbon unit, participate in the synthesis of hemoglobin and methyl compound such as adrenaline, choline, creatine etc..Leaf
Acid plays an important role to the synthesis of protein, nucleic acid and the metabolism of various amino acid.
For folic acid as the essential nutriment of human body, social required quantity is big, is mainly used in feed, food, medicine
It can trigger the diseases such as megaloblastic anemia disease, neural tube malformation with fields, shortages such as health products.The existing folic acid synthesis in China
Technique is mainly conventional chemical methods, there are low yield, wastewater flow rate is big the shortcomings of, if dealt with improperly, can cause environmental pollution.
Our company obtains highly finished product, concrete technology by folic acid crude product made of chemical method, it is necessary to carry out isolation and purification
It is fully dissolved in for folic acid crude product in the molten water of acid (42% sulfuric acid solution), stirs and yellow solid is gradually precipitated, add suitable water, then
Stirring a period of time, suction filtration obtain the folid acid extract (folate content more than 90%) of yellow, and sour extract is obtained using alkali refining
To folic acid highly finished product.A large amount of strongly acid wastewaters (sulfuric acid concentration 7-8) are given birth to when folic acid crude product is with 42% sulfuric acid solution acid treating, in palm fibre
Color is darker, wherein containing the itrogenous organic substances such as dihydrofoilic acid, 5- chlorine folic acid, pteroic acid, different folic acid and a small amount of folic acid.Afterwards
Phase wastewater treatment difficulty is big, increases entire folic acid production cost.Thus, how above-mentioned organic matter and sulfuric acid are separated, sulfuric acid is molten
Liquid carries out circulating repetition utilization again, on the one hand reduces production cost, while reaches folic acid green syt, meets efficient, green, section
It can requirement.
The content of the invention
The present invention is after the molten water of acid separates purified folate highly finished product for the prior art, and filtrate impurity content is high, acid strong,
The feature that environmental pollution is big, processing cost is high provides a kind of method that environment-friendly type folic acid refines.
Above-mentioned technical problem is solved, the invention mainly comprises following steps：
(1) folic acid crude product is dissolved in sulfuric acid solution, add water stirring be precipitated yellow solid after, filtering obtain folic acid highly finished product and
Filtrate；
(2) active carbon adsorption filtering is added in the filtrate obtained in step (1)；
(3) nanofiltration processing is carried out to the filtrate that step (2) obtains；
(4) concentrated sulfuric acid is added to the filtrate that step (3) obtains, adjusting concentration is 40-45%, for the essence of folic acid crude product
System；
(5) repeat the above steps, filtrate can be recycled 3-5 times.
In step (1) plus water whipping process, water can first add, add afterwards or add while stirring.
To obtain better effects, the sulfuric acid solution concentration is 40-45%；NF membrane selection Tao Shi nf270.
The present invention can be realized by the following method：
(1) folic acid crude product (folate content about 70-75%) is dissolved in 40-45% sulfuric acid solutions, stirs and Huang is gradually precipitated
Color solid adds suitable water, is stirred for a period of time, and suction filtration obtains the folid acid extract (folate content more than 90%) of yellow,
And filtrate (the molten water of acid), filtrate brownish black CODcrContent is 3100-3400mg/L；
(2) active carbon adsorption is added in the molten water of acid obtained in step (1), after filtering, liquor C ODcrContent is 2800-
3100mg/L；
(3) the molten impurities in water that deacidifies is removed in nanofiltration, selects NF membrane Tao Shi nf270 (four cun of components), removes impurity, filtrate
CODcrContent≤50mg/L；
(4) filtrate after nanofiltration adds in a certain amount of concentrated sulfuric acid, and adjusting concentration is 40-45%, for folic acid crude product
Acid treating；
(5) repeat the above steps, the molten water of acid can recycle 3-5 times, the folic acid separation and Extraction rate in the molten water of acid
Up to more than 93%.
By method provided by the invention, following advantageous effect can be realized：
(1) using activated adoption and nanofiltration, the molten impurities in water removal rate of acid is up to more than 99%, and the time is very short, nothing
Pollution；
(2) using the molten water of acid is recycled, concentrated sulfuric acid dosage saves more than 60%, and the folic acid purity after acid treating is up to 90%
More than；(3) compared with other methods, power consumption is small, extensive and automated production easy to implement, so as to save resource, section
The about energy realizes green, energy-saving and environmental protection.
Specific embodiment
With reference to embodiment, the invention will be further described, but not limited to this, all systems can with equal proportion into
Row amplification.
Embodiment 1
120 milliliters of 40-45% sulfuric acid are added in beaker, 30-35 DEG C is added with stirring 80-120 grams of (folic acid of folic acid crude product
Content about 70-75%), for folic acid crude product all after dissolving, solution colour and soy sauce are similar, stir 10-20 minutes, gradually analyse
Go out yellow solid, when stirring 1-2 is small, add 600-800 milliliters of tap water, 30-35 DEG C is stirred for 30-60 minutes, and (workshop is just for suction filtration
It is plate frame), obtain folic acid highly finished product, content 93.8%；100 liters of filtrates are measured, add in 10-15 grams of activated carbon, room temperature is stirred
After mixing 15-30 minutes, further nanofiltration filtering adds in the appropriate concentrated sulfuric acid, regulating vitriol oil concentration 40-45%, liquor C ODcrContain
Amount≤50mg/L is refined available for thick folic acid in next step.
Embodiment 2
120 milliliter of 40% sulfuric acid is added in beaker, 30 DEG C are added with stirring 80 grams of folic acid crude product (folate content is about
70-75%), after folic acid crude product all dissolves, solution colour and soy sauce are similar, stir 10 minutes, yellow solid is gradually precipitated,
Stir 1 it is small when, add 600 milliliters of tap water, 30 DEG C are stirred for 30 minutes, filter (workshop is exactly plate frame), obtain folic acid and refine
Product, content 93.2%；100 liters of filtrates are measured, add in 10 grams of activated carbon, after being stirred at room temperature 15 minutes, further nanofiltration filtering,
Add in the appropriate concentrated sulfuric acid, regulating vitriol oil concentration 40-45%, liquor C ODcrContent≤50mg/L, available for thick folic acid in next step
It is refined.
Embodiment 3
120 milliliter of 45% sulfuric acid is added in beaker, 35 DEG C are added with stirring 120 grams of folic acid crude product (folate content is about
70-75%), after folic acid crude product all dissolves, solution colour and soy sauce are similar, stir 20 minutes, yellow solid is gradually precipitated,
Stir 2 it is small when, add 800 milliliters of tap water, 35 DEG C are stirred for 60 minutes, filter (workshop is exactly plate frame), obtain folic acid and refine
Product, content 94%；100 liters of filtrates are measured, add in 15 grams of activated carbon, after being stirred at room temperature 30 minutes, further nanofiltration filtering,
Add in the appropriate concentrated sulfuric acid, regulating vitriol oil concentration 40-45%, liquor C ODcrContent≤50mg/L, available for thick folic acid in next step
It is refined.
Embodiment 4
120 milliliter of 42% sulfuric acid is added in beaker, 32 DEG C are added with stirring 100 grams of folic acid crude product (folate content is about
70-75%), after folic acid crude product all dissolves, solution colour and soy sauce are similar, stir 15 minutes, yellow solid is gradually precipitated,
Stir 1 it is small when, add 666 milliliters of tap water, 32 DEG C are stirred for 45 minutes, filter (workshop is exactly plate frame), obtain folic acid and refine
Product, content 93%；100 liters of filtrates are measured, add in 12 grams of activated carbon, after being stirred at room temperature 25 minutes, further nanofiltration filtering adds
Enter the appropriate concentrated sulfuric acid, regulating vitriol oil concentration 40-45%, liquor C ODcrContent≤50mg/L, available for thick folic acid essence in next step
System.
Embodiment 5
120 milliliter of 45% sulfuric acid is added in beaker, 30 DEG C are added with stirring 100 grams of folic acid crude product (folate content is about
70-75%), after folic acid crude product all dissolves, solution colour and soy sauce are similar, stir 20 minutes, yellow solid is gradually precipitated,
Stir 2 it is small when, add 800 milliliters of tap water, 33 DEG C are stirred for 45 minutes, filter (workshop is exactly plate frame), obtain folic acid and refine
Product, content 94.5%；100 liters of filtrates are measured, add in 12 grams of activated carbon, after being stirred at room temperature 30 minutes, further nanofiltration filtering,
Add in the appropriate concentrated sulfuric acid, regulating vitriol oil concentration 40-45%, liquor C ODcrContent≤50mg/L, available for thick folic acid in next step
It is refined.
Claims (8)
1. a kind of environment-friendly type folic acid process for purification, feature are including the following steps：
(1) folic acid crude product is dissolved in sulfuric acid solution, and after adding water stirring that yellow solid is precipitated, filtering obtains folic acid highly finished product and filter
Liquid；
(2) active carbon adsorption filtering is added in the filtrate obtained in step (1)；
(3) nanofiltration processing is carried out to the filtrate that step (2) obtains；
(4) concentrated sulfuric acid is added to the filtrate that step (3) obtains, adjusting concentration is 40-45%, for the refined of folic acid crude product；
(5) repeat the above steps, filtrate can be recycled 3-5 times.
2. method described in claim 1, it is characterised in that the water can first add, add afterwards or add while stirring.
3. the method described in claim 2, it is characterised in that the sulfuric acid solution concentration is 40-45%.
4. the method described in Claims 2 or 3, it is characterised in that the NF membrane is Tao Shi nf270.
5. the method described in claim 4, it is characterised in that be as follows：
(1) folic acid crude product is dissolved in 40-45% sulfuric acid solutions, stirs and yellow solid is gradually precipitated, add suitable water, be stirred for one
Folic acid highly finished product and the filtrate of yellow is obtained by filtration in the section time；
(2) active carbon adsorption is added in the filtrate obtained in step (1), filtered；
(3) impurity in nanofiltration removal step (2) filtrate, NF membrane Tao Shi nf270 (four cun of components) are passed through；
(4) filtrate after nanofiltration measures liquor C ODcrDuring content≤50mg/L, a certain amount of concentrated sulfuric acid is added in, adjusts concentration
For 40-45%, for the refined of folic acid crude product；
(5) repeat the above steps, filtrate can recycle 3-5 times.
6. the method described in claim 5, it is characterised in that be filtered into suction filtration or plate-frame filtering in step (1).
7. the method described in claim 4, it is characterised in that specific method is as follows：120 milliliters of 40-45% sulfuric acid, 30-35 DEG C is stirred
Lower 80-120 grams of addition folic acid crude product is mixed, folic acid crude product all after dissolving, stirs 10-20 minutes, yellow solid is gradually precipitated, after
When continuous stirring 1-2 is small, add 600-800 milliliters of tap water, 30-35 DEG C is stirred for 30-60 minutes, and folic acid highly finished product are obtained by filtration；
100 liters of filtrates are measured, add in 10-15 grams of activated carbon, after being stirred at room temperature 15-30 minutes, further nanofiltration filtering adds in appropriate dense
Sulfuric acid, regulating vitriol oil concentration 40-45%, liquor C ODcr contents≤50mg/L, for the refined of next folic acid crude product.
8. the method described in claim 7, it is characterised in that specific method is as follows：120 milliliter of 40% sulfuric acid, 30 DEG C of stirrings are lower to be added
Enter 80 grams of folic acid crude product, folic acid crude product all after dissolving, stirs 10 minutes, yellow solid is gradually precipitated, continue stirring 1 it is small when,
Add 600 milliliters of tap water, 30 DEG C are stirred for 30 minutes, and folic acid highly finished product are obtained by filtration；100 liters of filtrates are measured, add in 10 grams of work
Property carbon, after being stirred at room temperature 15 minutes, further nanofiltration filtering adds in the appropriate concentrated sulfuric acid, regulating vitriol oil concentration 40-45%, filter
Liquid CODcrContent≤50mg/L, for the refined of next folic acid crude product.
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| CN201711469517.5A CN108084185A (en) | 2017-12-29 | 2017-12-29 | A kind of environment-friendly type folic acid process for purification |
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| CN201711469517.5A CN108084185A (en) | 2017-12-29 | 2017-12-29 | A kind of environment-friendly type folic acid process for purification |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323614A (en) * | 2008-07-29 | 2008-12-17 | 河北冀衡（集团）药业有限公司 | Acidum folicum production method without sewerage discharge |
| CN102432610A (en) * | 2011-09-29 | 2012-05-02 | 河北冀衡（集团）药业有限公司 | Folic acid production method for controlling content of technical pteroic acid |
| CN105541845A (en) * | 2016-01-14 | 2016-05-04 | 青岛琅琊台集团股份有限公司 | Folic-acid cleaning production technology |
| CN107312004A (en) * | 2017-06-14 | 2017-11-03 | 河北冀衡（集团）药业有限公司 | A kind of production method of folic acid |
-
2017
- 2017-12-29 CN CN201711469517.5A patent/CN108084185A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323614A (en) * | 2008-07-29 | 2008-12-17 | 河北冀衡（集团）药业有限公司 | Acidum folicum production method without sewerage discharge |
| CN102432610A (en) * | 2011-09-29 | 2012-05-02 | 河北冀衡（集团）药业有限公司 | Folic acid production method for controlling content of technical pteroic acid |
| CN105541845A (en) * | 2016-01-14 | 2016-05-04 | 青岛琅琊台集团股份有限公司 | Folic-acid cleaning production technology |
| CN107312004A (en) * | 2017-06-14 | 2017-11-03 | 河北冀衡（集团）药业有限公司 | A kind of production method of folic acid |
Non-Patent Citations (2)
| Title |
|---|
| 刘纯根: "《生物工艺（食品生物工艺专业）》", 31 December 2002, 高等教育出版社 * |
| 詹益兴: "《精细化工新产品（第1集）》", 30 June 2007, 科学技术文献出版社 * |
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Application publication date: 20180529 |