CN112500415A - Method for recovering folic acid from wastewater in folic acid dissolution and elutriation stage - Google Patents
Method for recovering folic acid from wastewater in folic acid dissolution and elutriation stage Download PDFInfo
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- C07D475/02—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4
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Abstract
The invention provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage. The method comprises the following steps: (1) adjusting the pH value of the wastewater in the folic acid dissolution and elutriation stage to be more than or equal to 7 by using a calcium-containing compound, converting folic acid in the wastewater into calcium folate precipitate, and performing solid-liquid separation to obtain a filter cake; (2) mixing the filter cake obtained in the step (1) with acid to dissolve calcium folate to obtain a solution, or carrying out solid-liquid separation to obtain a filtrate and a filter cake; (3) and (3) adjusting the pH value of the solution or the filtrate obtained in the step (2) to 3-5 to precipitate folic acid, and carrying out solid-liquid separation to obtain folic acid. The method provided by the invention is simple to operate and low in cost, reduces acidic substances in the wastewater while recycling folic acid, and is beneficial to comprehensive treatment of the wastewater.
Description
Technical Field
The invention belongs to the technical field of industrial wastewater treatment, and particularly relates to a method for recovering folic acid from wastewater in a folic acid dissolving and elutriating stage.
Background
Folic acid is a water-soluble vitamin with important nutritional and medicinal values, and is widely present in natural vegetables and fruits. Folic acid was first discovered in spinach to have an anti-anemia effect, and through the constant search and practice of researchers and experts over the years, the role of folic acid in disease treatment and daily dietary health care is more and more prominent.
The production process of folic acid mainly comprises three stages of crude product synthesis, acid dissolution and water precipitation and alkali dissolution and refining. In general, the folic acid crude product is prepared by the reaction of three main materials, namely N- (4-aminobenzoyl) -L-glutamic acid, trichloroacetone and 2,4, 5-triamino-6-hydroxypyrimidine sulfate, and is refined and purified through the subsequent steps of acid dissolution and water precipitation and alkali dissolution refining. Acid-soluble elutriation means that a folic acid crude product is dissolved by acid liquor in an acid-soluble elutriation tank, and then the dissolved crude product is elutriated and filtered to obtain an acid extract. A large amount of waste water is generated in the stage, and part of folic acid can be remained in the waste water and can not enter the next alkali-soluble refining step.
CN 107312004A discloses a folic acid production method, which adopts a carbon decoloration adsorption and ammonia neutralization method to treat the wastewater generated in the folic acid dissolution elutriation stage, and the treated wastewater enters an acid dissolution elutriation tank to be used as process water. However, this treatment method is expensive and cannot recover folic acid in the wastewater, resulting in waste of raw materials.
Therefore, there is a need in the art for a method of treating the wastewater produced in the folate elutriation stage to recover folic acid.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
(1) adjusting the pH value of the wastewater in the folic acid dissolution elutriation stage to be more than or equal to 7 (for example, 7, 7.2, 7.5, 7.8, 8, 8.2, 8.5, 8.8, 9, 9.5, 10, 10.5, 11, 11.5 or 12 and the like) by using a calcium-containing compound, converting folic acid in the wastewater into calcium folate for precipitation, and carrying out solid-liquid separation to obtain a filter cake;
(2) mixing the filter cake obtained in the step (1) with acid to dissolve calcium folate to obtain a solution, or carrying out solid-liquid separation to obtain a filtrate and a filter cake;
(3) adjusting the pH of the solution or filtrate obtained in step (2) to 3-5 (for example, 3, 3.2, 3.3, 3.5, 3.6, 3.8, 4, 4.2, 4.3, 4.5, 4.6, 4.8 or 5), precipitating folic acid, and performing solid-liquid separation to obtain folic acid.
In the present invention, the folic acid-soluble elutriation stage wastewater refers to wastewater generated in an acid-soluble elutriation stage when folic acid is prepared by a crude product synthesis method, an acid-soluble elutriation method, and an alkaline dissolution and purification method. The wastewater contains folic acid and other inorganic acids (such as hydrochloric acid or sulfuric acid).
According to the invention, the calcium-containing compound is adopted to treat the folic acid dissolution elutriation stage wastewater, folic acid is converted into calcium folate for precipitation, then the calcium folate is dissolved, and finally the proper pH is adjusted to precipitate folic acid, so that the folic acid residual in the folic acid dissolution elutriation stage wastewater is recovered. The method is simple to operate and low in cost, reduces acidic substances in the wastewater while recycling the folic acid, and is beneficial to comprehensive treatment of the wastewater.
In the step (1) of the present invention, at least all the acid in the wastewater needs to be neutralized so that folic acid is sufficiently converted into calcium folate to be precipitated. In the step (3), the pH value of the solution or the filtrate needs to be adjusted to 3-5 so as to fully separate out folic acid; when the pH is too low or too high, the solubility of folic acid is high, which is not favorable for precipitation.
In the invention, when the wastewater does not contain SO in the folic acid dissolution elutriation stage4 2-In the process, the filter cake obtained in the step (1) usually only contains calcium folate, and after the calcium folate is dissolved in the step (2), a uniform solution is obtained; when the wastewater contains SO in the folic acid dissolution and elutriation stage4 2-In the process, the filter cake obtained in the step (1) contains calcium folate and calcium sulfate, the calcium folate can be dissolved by acid in the step (2), and the calcium sulfate cannot be dissolved and can be removed and recovered through solid-liquid separation.
In one embodiment of the invention, the pH is adjusted to 7-8 in step (1).
In one embodiment of the present invention, the calcium-containing compound in step (1) is one or a combination of at least two selected from the group consisting of calcium hydroxide, calcium oxide, calcium bicarbonate and calcium carbonate, preferably calcium hydroxide.
In an embodiment of the present invention, the method further comprises: washing the filter cake obtained in the step (1) with water before the step (2).
In one embodiment of the present invention, the acid in step (2) is a strong inorganic acid.
In one embodiment of the present invention, the strong inorganic acid is hydrochloric acid and/or sulfuric acid, and hydrochloric acid is more preferable. Wherein, the mass fraction of the hydrochloric acid and the sulfuric acid is preferably 20-30%.
The amount of the acid used in step (2) is not particularly limited in the present invention, as long as complete dissolution of calcium folate is ensured. Empirically, the volume ratio of the acid used in step (2) to the wastewater in step (1) was 1: 6.
In one embodiment of the present invention, the reagent used for adjusting the pH in step (3) is sodium hydroxide and/or potassium hydroxide.
Among them, sodium hydroxide and potassium hydroxide may be added in the form of a solid or a solution, and if they are added in the form of a solution, the mass fraction thereof is preferably 30 to 35%.
In one embodiment of the invention, the pH is adjusted to 3.5-4 in step (3).
The pH value in the step (3) of the invention is most preferably adjusted to 3.5-4, which is helpful for further promoting the precipitation of folic acid and improving the purity of the recovered folic acid.
In an embodiment of the present invention, the method further comprises: after the solid-liquid separation in step (3), the obtained cake is washed with water.
In one embodiment of the present invention, the wastewater contains SO4 2-The method further comprises the following steps: and (3) washing the filter cake obtained in the step (2) with water, carrying out solid-liquid separation, and drying solid components to obtain calcium sulfate.
In one embodiment of the invention, the folic acid-dissolving elutriation stage wastewater is obtained by a method comprising the steps of:
(i) taking N- (p-aminobenzoyl) -L-glutamic acid, 2,4, 5-triamino-6-hydroxypyrimidine sulfate and trichloroacetone as raw materials, sodium pyrosulfite as an antioxidant, water as a solvent, performing cyclization reaction under the conditions that the pH is 3-3.5 and the temperature is 32-35 ℃, filtering after the reaction is finished, and collecting a filter cake;
(ii) and (e) dissolving the filter cake obtained in the step (i) with acid liquor, stirring, standing, and filtering to obtain filtrate, namely the folic acid dissolved water precipitation stage wastewater.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the calcium-containing compound is adopted to treat the folic acid dissolution elutriation stage wastewater, folic acid is converted into calcium folate for precipitation, then the calcium folate is dissolved, and finally the proper pH is adjusted to precipitate folic acid, so that the folic acid residual in the folic acid dissolution elutriation stage wastewater is recovered. The method is simple to operate and low in cost, reduces acidic substances in the wastewater while recycling the folic acid, and is beneficial to comprehensive treatment of the wastewater.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the specific embodiments are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The folic acid is prepared by the following method in the embodiment of the invention, and the folic acid is generated as the wastewater in the acid dissolution and water precipitation stage:
crude product synthesis: the raw materials are added in two batches, and the temperature is controlled to be 32-35 ℃. Adding 13.3g of N- (4-aminobenzoyl) -L-glutamic acid into 700mL of water in a first batch, stirring for 15 minutes, then adding 11.95g of 2,4, 5-triamino-6-hydroxypyrimidine sulfate, stirring for 15 minutes, then adding 4.75g of sodium metabisulfite, adding 12.8g of trichloroacetone for crystallization after the materials are uniformly stirred, stirring and mixing uniformly for about 40 minutes in common use, then adjusting the pH to 3.5 by using a sodium carbonate solution with the mass fraction of 10%, detecting the system by LC-MS, when the concentration of the N- (4-aminobenzoyl) -L-glutamic acid is reduced to 1/4 of the initial concentration, then sequentially adding 13.3g of N- (4-aminobenzoyl) -L-glutamic acid and 2 according to the adding method of the materials in the first batch, 11.95g of 4, 5-triamino-6-hydroxypyrimidine sulfate and 1.9g of sodium metabisulfite, uniformly stirring, adding 12.8g of trichloroacetone crystals, continuously adjusting the pH to 3.5 by using a sodium carbonate solution with the mass fraction of 10% after uniformly stirring, keeping the temperature of the system at 32-35 ℃, continuously reacting for 6 hours, detecting the conversion rate of the N- (4-aminobenzoyl) -L-glutamic acid to be 90% by LC-MS, cooling to 25 ℃, and performing suction filtration to obtain a filter cake, namely a folic acid crude product for the next step of acid dissolution.
Acid dissolution and water precipitation: 1/3 crude folic acid is taken and added with 35 percent of sulfuric acid aqueous solution until the crude folic acid is completely dissolved, then the residual crude folic acid is added, after stirring for 3-5 minutes, pure water (the volume of the added pure water is about 6 times of that of the sulfuric acid aqueous solution) is added, stirring is carried out for 5 minutes, after standing for 1 hour, solid is separated out, and suction filtration is carried out, wherein a filter cake is an acid extract, and the filtrate is waste water, which is used in the embodiment of the invention.
Example 1
The embodiment provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
step (1): taking 300mL of folic acid-dissolved water-out stage wastewater, slowly adding calcium hydroxide solid, detecting the change of pH value during the process, adjusting the pH value to 7.5, using the calcium hydroxide about 10g, carrying out suction filtration at normal pressure, and washing a filter cake twice by using pure water;
step (2): adding 50mL of industrial hydrochloric acid with the mass fraction of 30% into the filter cake obtained in the step (1), stirring, and performing suction filtration to obtain a filter cake and a filtrate;
and (3): adding 50mL of pure water into the filter cake obtained in the step (2), washing, and performing suction filtration to obtain white calcium sulfate; adding 250mL of pure water into the filtrate obtained in the step (2), adding 42mL of sodium hydroxide solution with the mass fraction of 30% to adjust the pH value to 3.5-4, performing suction filtration, washing twice during suction filtration to obtain recovered folic acid, drying, and detecting to obtain 3.22g of crude folic acid with the purity of 80.7%.
In the embodiment of the invention, the purity of the folic acid crude product is detected by liquid chromatography;
the preparation method of the mobile phase comprises the following steps: 19.64g of potassium dihydrogenphosphate and 9.68g of dipotassium hydrogenphosphate were weighed out and dissolved in water, 240mL of methanol was added, and a volume of 2000mL (pH: 6.4-6.7) was made with water.
A detection instrument: agilent Technologies 1220 Infinity LC.
Detecting the flow rate: 0.600 mL/min.
Detection wavelength: 280 nm.
A detection step: weighing 0.01g folic acid sample, placing in a 50mL volumetric flask, adding 0.9mL potassium hydroxide solution (0.1mol/L) and 10mL mobile phase for dissolution, adding the mobile phase to a constant volume to scale, shaking up, filtering with a 0.45 μm filter membrane, and taking a proper amount of folic acid sample to a sample introduction bottle for sample introduction and detection.
Example 2
The embodiment provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
step (1): taking 300mL of folic acid-dissolved water-out stage wastewater, slowly adding calcium hydroxide solid, detecting the change of pH value during the process, adjusting the pH value to 7.2, using the calcium hydroxide about 10g, carrying out suction filtration at normal pressure, and washing a filter cake twice by using pure water;
step (2): adding 50mL of industrial hydrochloric acid with the mass fraction of 30% into the filter cake obtained in the step (1), stirring, and performing suction filtration to obtain a filter cake and a filtrate;
and (3): adding 50mL of pure water into the filter cake obtained in the step (2), washing, and performing suction filtration to obtain white calcium sulfate; adding 250mL of pure water into the filtrate obtained in the step (2), adding 45mL of 30% sodium hydroxide solution by mass fraction to adjust the pH value to 4-4.5, performing suction filtration, washing twice during suction filtration to obtain recovered folic acid, and drying to obtain 2.98g of crude folic acid with the purity of 76.4%.
Example 3
The embodiment provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
step (1): taking 300mL of folic acid-dissolved water-out stage wastewater, slowly adding calcium hydroxide solid, detecting the change of pH value during the process, adjusting the pH value to 7.8, using the calcium hydroxide about 10g, carrying out suction filtration at normal pressure, and washing a filter cake twice by using pure water;
step (2): adding 50mL of industrial hydrochloric acid with the mass fraction of 30% into the filter cake obtained in the step (1), stirring, and performing suction filtration to obtain a filter cake and a filtrate;
and (3): adding 50mL of pure water into the filter cake obtained in the step (2), washing, and performing suction filtration to obtain white calcium sulfate; adding 250mL of pure water into the filtrate obtained in the step (2), adding 48mL of 30% sodium hydroxide solution by mass fraction to adjust the pH value to 4.5-5, performing suction filtration, washing twice during suction filtration to obtain recovered folic acid, and drying to obtain 2.40g of crude folic acid with the purity of 71.9%.
Example 4
The embodiment provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
step (1): taking 300mL of folic acid-dissolved water-out stage wastewater, slowly adding calcium hydroxide solid, detecting the change of pH value during the process, adjusting the pH value to 8, wherein the dosage of the calcium hydroxide is about 10g, carrying out suction filtration at normal pressure, and washing a filter cake twice by using pure water;
step (2): adding 50mL of sulfuric acid solution with the mass fraction of 20% into the filter cake obtained in the step (1), stirring, and performing suction filtration to obtain a filter cake and a filtrate;
and (3): adding 50mL of pure water into the filter cake obtained in the step (2), washing, and performing suction filtration to obtain white calcium sulfate; adding 250mL of pure water into the filtrate obtained in the step (2), adding 42mL of sodium hydroxide solution with the mass fraction of 30% to adjust the pH value to 3.5-4, performing suction filtration, washing twice during suction filtration to obtain recovered folic acid, and drying to obtain 2.47g of crude folic acid with the purity of 69.1%.
Example 5
The embodiment provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
step (1): taking 300mL of folic acid-dissolved water-out stage wastewater, slowly adding calcium carbonate solid, detecting the change of pH value during the process, adjusting the pH value to 7, carrying out suction filtration at normal pressure, and washing a filter cake twice by using pure water;
step (2): adding 50mL of industrial hydrochloric acid with the mass fraction of 30% into the filter cake obtained in the step (1), stirring, and performing suction filtration to obtain a filter cake and a filtrate;
and (3): adding 50mL of pure water into the filter cake obtained in the step (2), washing, and performing suction filtration to obtain white calcium sulfate; adding 250mL of pure water into the filtrate obtained in the step (2), adding 42mL of sodium hydroxide solution with the mass fraction of 30% to adjust the pH value to 3.5-4, performing suction filtration, washing twice during suction filtration to obtain recovered folic acid, and drying to obtain 2.75g of crude folic acid with the purity of 72.6%.
Example 6
The embodiment provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
step (1): taking 300mL of folic acid-dissolved water-out stage wastewater, slowly adding alkali mixed by calcium carbonate and calcium hydroxide according to the mass ratio of 4:1, detecting the change of pH value in the period, adjusting the pH value to 7.3, carrying out suction filtration at normal pressure, and washing a filter cake twice by using pure water;
step (2): adding 50mL of industrial hydrochloric acid with the mass fraction of 30% into the filter cake obtained in the step (1), stirring, and performing suction filtration to obtain a filter cake and a filtrate;
and (3): adding 50mL of pure water into the filter cake obtained in the step (2), washing, and performing suction filtration to obtain white calcium sulfate; adding 250mL of pure water into the filtrate obtained in the step (2), adding 42mL of sodium hydroxide solution with the mass fraction of 30% to adjust the pH value to 3.5-4, performing suction filtration, washing twice during suction filtration to obtain recovered folic acid, and drying to obtain 2.80g of crude folic acid with the purity of 74.6%.
Example 7
The embodiment provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
step (1): taking 300mL of folic acid-dissolved water-out stage wastewater, slowly adding alkali mixed by calcium carbonate and calcium hydroxide according to the mass ratio of 1:1, detecting the change of pH value in the period, adjusting the pH value to 7.6, carrying out suction filtration at normal pressure, and washing a filter cake twice by using pure water;
step (2): adding 50mL of industrial hydrochloric acid with the mass fraction of 30% into the filter cake obtained in the step (1), stirring, and performing suction filtration to obtain a filter cake and a filtrate;
and (3): adding 50mL of pure water into the filter cake obtained in the step (2), washing, and performing suction filtration to obtain white calcium sulfate; adding 250mL of pure water into the filtrate obtained in the step (2), adding 42mL of sodium hydroxide solution with the mass fraction of 30% to adjust the pH value to 3.5-4, performing suction filtration, washing twice during suction filtration to obtain recovered folic acid, and drying to obtain 2.96g of crude folic acid with the purity of 75.3%.
Example 8
The embodiment provides a method for recovering folic acid from wastewater in a folic acid dissolving elutriation stage, which comprises the following steps:
step (1): taking 300mL of folic acid-dissolved water-out stage wastewater, slowly adding calcium bicarbonate, detecting the change of pH value during the process, adjusting the pH value to 7, carrying out suction filtration at normal pressure, and washing a filter cake twice by using pure water;
step (2): adding 50mL of industrial hydrochloric acid with the mass fraction of 30% into the filter cake obtained in the step (1), stirring, and performing suction filtration to obtain a filter cake and a filtrate;
and (3): adding 50mL of pure water into the filter cake obtained in the step (2), washing, and performing suction filtration to obtain white calcium sulfate; adding 250mL of pure water into the filtrate obtained in the step (2), adding 40.5mL of sodium hydroxide solution with the mass fraction of 30% to adjust the pH value to 3-3.5, carrying out suction filtration, washing twice during suction filtration to obtain recovered folic acid, and drying to obtain 2.96g of crude folic acid with the purity of 75.1%.
Comparative example 1
There is provided a process for recovering folic acid from a waste water in a folic acid-dissolving elutriation stage, which is different from example 1 in that the pH is adjusted to 2.5 in step (3). 2.74g of crude folic acid with the purity of 71.9 percent is obtained.
Comparative example 2
There is provided a process for recovering folic acid from a waste water in a folic acid-dissolving elutriation stage, which is different from example 1 in that the pH is adjusted to 5.5 in step (3). 2.13g of crude folic acid with the purity of 66.5 percent is obtained.
As can be seen by comparing example 1 with comparative examples 1 to 2, when the pH adjusted in step (3) is out of the range of 3 to 5, the amount of folic acid recovered is small and the purity is low.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for recovering folic acid from wastewater in a folic acid dissolution elutriation stage, which is characterized by comprising the following steps of:
(1) adjusting the pH value of the wastewater in the folic acid dissolution and elutriation stage to be more than or equal to 7 by using a calcium-containing compound, converting folic acid in the wastewater into calcium folate precipitate, and performing solid-liquid separation to obtain a filter cake;
(2) mixing the filter cake obtained in the step (1) with acid to dissolve calcium folate to obtain a solution, or carrying out solid-liquid separation to obtain a filtrate and a filter cake;
(3) and (3) adjusting the pH value of the solution or the filtrate obtained in the step (2) to 3-5 to precipitate folic acid, and carrying out solid-liquid separation to obtain folic acid.
2. The method according to claim 1, wherein the pH is adjusted to 7 to 8 in step (1).
3. The method according to claim 1 or 2, wherein the calcium-containing compound in step (1) is selected from one or a combination of at least two of calcium hydroxide, calcium oxide, calcium bicarbonate and calcium carbonate, preferably calcium hydroxide.
4. The method according to any one of claims 1-3, further comprising: washing the filter cake obtained in the step (1) with water before the step (2).
5. The process according to any one of claims 1 to 4, wherein the acid in step (2) is a strong inorganic acid, preferably hydrochloric acid and/or sulfuric acid, further preferably hydrochloric acid.
6. The process according to any one of claims 1 to 5, wherein the agent used for adjusting the pH in step (3) is sodium hydroxide and/or potassium hydroxide.
7. The process according to any one of claims 1 to 6, wherein the pH is adjusted to 3.5 to 4 in step (3).
8. The method according to any one of claims 1-7, further comprising: after the solid-liquid separation in step (3), the obtained cake is washed with water.
9. The method according to any one of claims 1 to 8, wherein the wastewater contains SO4 2-The method further comprises the following steps: and (3) washing the filter cake obtained in the step (2) with water, carrying out solid-liquid separation, and drying solid components to obtain calcium sulfate.
10. A process according to any one of claims 1 to 9, wherein the folic acid-dissolving elutriation stage wastewater is obtained from a process comprising the steps of:
(i) taking N- (p-aminobenzoyl) -L-glutamic acid, 2,4, 5-triamino-6-hydroxypyrimidine sulfate and trichloroacetone as raw materials, sodium pyrosulfite as an antioxidant, water as a solvent, performing cyclization reaction under the conditions that the pH is 3-3.5 and the temperature is 32-35 ℃, filtering after the reaction is finished, and collecting a filter cake;
(ii) and (e) dissolving the filter cake obtained in the step (i) with acid liquor, stirring, standing, and filtering to obtain filtrate, namely the folic acid dissolved water precipitation stage wastewater.
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| QIAN ZHANG ET AL.: "Technology of foam fractionation coupled with crystallization for the enrichment and purification of folic acid", 《SEPARATION AND PURIFICATION TECHNOLOGY》 * |
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Application publication date: 20210316 |