CN111018814B - Method for recycling vitamin C secondary mother liquor - Google Patents
Method for recycling vitamin C secondary mother liquor Download PDFInfo
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- CN111018814B CN111018814B CN201911238710.7A CN201911238710A CN111018814B CN 111018814 B CN111018814 B CN 111018814B CN 201911238710 A CN201911238710 A CN 201911238710A CN 111018814 B CN111018814 B CN 111018814B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members 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
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
Abstract
A method for recycling a second vitamin C mother liquor comprises the steps of membrane decoloration, concentration, transesterification and the like, and active ingredients in the second vitamin C mother liquor are used for preparing sodium vitamin C, so that the second vitamin C mother liquor is recycled; methanol is added in the later stage of the concentration step for continuous concentration, the water content of the concentrated material is obviously reduced by the methanol with water, and the ester conversion yield is improved; the concentrated material is not added with sulfuric acid, but the original sulfuric acid and other mixed acids in the vitamin C secondary mother liquor are fully utilized for catalytic esterification reaction, so that the consumption of raw materials is saved; the sealed decolorizing membrane equipment is adopted for decolorizing, and two mother dry product centrifugal operations are cancelled, so that the working environment of the staff is obviously improved; the recovery rate of the effective components is improved, the loss of the effective components is reduced, and the pressure of environment-friendly treatment is also reduced; the transesterification reaction time is shortened, and the production efficiency is improved.
Description
Technical Field
The invention relates to a method for recycling vitamin C II mother liquor, belonging to the technical field of vitamin C production.
Background
Vitamin C, also known as L-ascorbic acid, is widely used as vitamin drugs, food additives and feed additives.
At present, the industrial production method of vitamin C mainly adopts a two-step fermentation method to prepare an intermediate 2-keto-L-gulonic acid of vitamin C, then the 2-keto-L-gulonic acid and methanol are subjected to esterification conversion reaction to obtain sodium vitamin C, and the sodium vitamin C is subjected to exchange, decoloration, concentration, crystallization and filtration to obtain the vitamin C. A second vitamin C mother liquor is generated in the production process of vitamin C, the second vitamin C mother liquor contains active ingredients such as vitamin C, 2-keto-L-gulonic acid methyl ester and the like, and impurities such as sulfuric acid, oxalic acid, pigments and the like, and has the problems of dark color, high viscosity, strong acidity and high recovery difficulty.
Many scholars have conducted extensive research on the recovery of vitamin C mother liquor.
CN101613332B, CN103254159A and CN1733747A all adopt a simulated moving bed system to separate gulonic acid from vitamin C in vitamin C mother liquor, and the separated liquid is returned to the original working procedures for esterification, conversion, crystallization and secondary utilization after being concentrated. The technical proposal disclosed in the three patent documents adopts complicated simulated moving bed equipment and has huge investment, and because the content of each component is reduced because the resolving agent is water, and a large amount of steam is consumed for concentration, the practical value is not great.
CN101555239B neutralizes, decolors, concentrates, crystallizes and filters the vitamin C mother liquor to obtain 2-keto-L-gulonic acid salt, then dissolves the 2-keto-L-gulonic acid salt in water, and then obtains the 2-keto-L-gulonic acid through exchange, concentration, crystallization and separation, and the vitamin C is obtained through exchange, concentration, crystallization and separation of the mother liquor after the 2-keto-L-gulonic acid salt is separated out. The method needs multiple times of concentration, crystallization and separation, has complex process, large consumption of acid, alkali and steam, high cost, large discharge amount of resin regeneration wastewater and increased environment-friendly treatment pressure.
CN102267962B concentrates the mother liquor of vitamin C to be viscous, adds methanol and concentrated sulfuric acid to carry out esterification reaction at 60-65 ℃, dehydrates methanol vapor with water generated in the esterification reaction process through a rectifying tower, then adds sodium bicarbonate to carry out conversion, cooling and centrifugation to obtain a crude product of vitamin C sodium. The method carries out concentration transesterification without decolorization, which causes the prepared crude vitamin C sodium product to have heavier color and poor quality, and because the concentration dehydration effect is poor, reaction rectification is adopted to continuously remove water in the esterification process and methanol is supplemented, the esterification time is as long as 5-7 hours, the operation complexity and the cost are increased, the conversion is carried out by sodium bicarbonate, the conversion time is as long as 5-7 hours, and the cost is high.
CN103102335A decolorizes vitamin C mother liquor by macroporous absorbent resin, concentrates decolorized solution, crystallizes and centrifuges to obtain a crude vitamin C mother liquor recycled product, the recycled product is crushed and dried by a micro powder dryer and then undergoes an esterification reaction with methanol for 4 hours, the esterification reaction temperature is controlled to be 68 ℃ in the first hour, 60 ℃ in the second hour, 55 ℃ in the third hour and 50 ℃ in the fourth hour; and then adding sodium bicarbonate to carry out conversion reaction to obtain an intermediate crude sodium ascorbate. Although the quality of the crude product of the sodium ascorbate is improved by the method, the decolorization is carried out by adopting the macroporous resin, the decolorized mother liquor is diluted, the steam consumption for concentration is inevitably increased, the resin regeneration not only has large acid and alkali consumption, but also generates a large amount of waste water, in addition, the esterification reaction time is long, the time-sharing control of the esterification temperature is complicated to operate, and the conversion and alkali addition adopt the sodium bicarbonate, so the cost reduction is not facilitated.
Disclosure of Invention
The invention aims to overcome the defects of the conventional vitamin C II mother liquor recovery process, and provides a method for recovering and utilizing vitamin C II mother liquor, which can reduce material consumption, improve production efficiency, improve product quality, improve operating environment and reduce environmental protection treatment pressure.
The purpose of the invention can be realized by the following technical scheme:
a method for recycling vitamin C secondary mother liquor comprises the following steps:
1. film decolorization
And (3) decolorizing membrane equipment: adopting a strong acid and high pressure resistant decolorizing membrane, namely acid and high pressure resistant decolorizing membrane equipment;
directly adding the vitamin C secondary mother liquor stock solution into acid-resistant and high-pressure-resistant decoloring membrane equipment, and circularly decoloring under the pressure of 20-60 bar to obtain clear liquid, wherein in the period, when the volume of the obtained clear liquid reaches 60-80% of the volume of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment, water with the volume 0.05-0.5 times of the volume of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment is added into the decoloring membrane equipment, diluting turbid liquid, continuously decoloring, stopping until the decoloring yield reaches more than 80%, and discharging the turbid liquid for environment-friendly treatment;
2. concentrating
Vacuum concentration is carried out on the clear liquid obtained in the step one, water with the volume of 30-70% of the feeding volume of the clear liquid is concentrated, then methanol with the volume of 0.2-1 time of the feeding volume of the clear liquid is added, and concentration is continued until liquid with the volume equal to that of the added methanol is concentrated;
3. transesterification
Adding methanol with the volume to the mass ratio L/kg of the concentrated material of 2-5 into the concentrated material, heating, carrying out esterification reaction for 1.5-2.5 hours under a reflux state, adding sodium carbonate after the esterification, carrying out conversion reaction for 2-4 hours at the temperature of 58-66 ℃, then cooling and filtering to obtain sodium ascorbate, wherein the ratio of the added sodium carbonate to the total amount of effective components in the concentrated material is 0.5-0.6, and the effective components in the concentrated material are vitamin C, 2-keto-L-gulonic acid and 2-keto-L-gulonic acid methyl ester.
The material of the second vitamin C mother liquor is viscous and strong in acidity, a common decolorizing membrane is not strong acid resistant and high pressure resistant, the operating pressure is generally not more than 20bar, and the second vitamin C mother liquor can not be used for decolorizing. The decolorizing membrane equipment adopted by the invention adopts a strong acid and high pressure resistant decolorizing membrane, the operating pressure of the membrane is more than 20bar, preferably 20-60 bar, the decolorizing effect on the vitamin C secondary mother liquor is good, the decolorizing yield can reach more than 80 percent, and the decolorizing yield is generally controlled at 80-90 percent.
The invention achieves the following beneficial effects:
1. adopts acid-resistant and high-pressure-resistant decolorizing membrane equipment, effectively removes pigment of the vitamin C mother liquor, and improves the quality of recovered products.
2. Methanol is added in the later stage of the concentration step for continuous concentration, the water content of the concentrated material is obviously reduced by the methanol with water, and the ester conversion yield is improved.
3. The concentrated material is not added with sulfuric acid, but the original sulfuric acid and other heteroacid in the vitamin C secondary mother liquor are fully utilized for catalytic esterification reaction, so that the consumption of raw materials is saved, and the production cost is reduced.
4. Because the closed decolorizing membrane equipment is adopted for decolorizing, and the two-mother dry product centrifugal operation commonly adopted in the prior art is cancelled, the field environment is improved, and the working environment of the staff is obviously improved.
5. The recovery rate of the effective components is improved, the loss of the effective components is reduced, and the pressure of environmental protection treatment is also reduced.
6. The transesterification reaction time is shortened, and the production efficiency is improved.
Detailed Description
In order to better illustrate the present invention, the following examples are given, but the scope of the present invention is not limited thereto, and the scope of the claims is set forth in the claims.
Example 1
A method for recycling a vitamin C secondary mother solution comprises the following steps:
1. film decolorization
And (3) decolorizing membrane equipment: adopting a strong acid and high pressure resistant decolorizing membrane, namely acid and high pressure resistant decolorizing membrane equipment;
directly adding the vitamin C secondary mother liquor stock solution (without diluting and adding water) into an acid-resistant and high-pressure-resistant decoloring membrane device, circularly decoloring under the pressure of 20bar to obtain clear liquid, adding water with the volume 0.05 times of the volume of the vitamin C secondary mother liquor stock solution added into the decoloring membrane device during the period when the volume of the obtained clear liquid reaches 60 percent of the volume of the vitamin C secondary mother liquor stock solution added into the decoloring membrane device, diluting turbid liquid, continuously decoloring until the decoloring yield reaches 83.71 percent, and discharging the turbid liquid for environment-friendly treatment;
2. concentrating
Carrying out vacuum concentration on the clear liquid obtained in the first step, firstly concentrating water with the volume of 30% of the feeding volume of the clear liquid, then adding methanol with the volume of 0.2 time of the feeding volume of the clear liquid, and continuing to concentrate until liquid with the volume equal to that of the added methanol is concentrated;
3. transesterification of esters
Adding methanol with the volume and the mass ratio L/kg of the concentrated material of 3 to the concentrated material, heating, carrying out esterification reaction for 1.5 hours in a reflux state, adding sodium carbonate after the esterification, carrying out conversion reaction for 3 hours at the temperature of 58 ℃, then cooling and filtering to obtain crude sodium ascorbate, wherein the ratio of the added sodium carbonate to the total amount of effective components in the concentrated material is 0.5.
The obtained crude sodium ascorbate product is yellow, the content of the product is 80.15 percent, and the total recovery rate of the effective components is 75.36 percent.
Example 2
A method for recycling vitamin C secondary mother liquor comprises the following steps:
1. film decolorization
And (3) decolorizing membrane equipment: a strong acid and high pressure resistant decolorizing membrane is adopted, and the equipment is acid and high pressure resistant decolorizing membrane equipment;
directly adding the vitamin C secondary mother liquor stock solution (without diluting and adding water) into acid-resistant and high-pressure-resistant decoloring membrane equipment, circularly decoloring under the pressure of 35bar to obtain clear liquid, adding water with the volume 0.2 times that of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment after the volume of the obtained clear liquid reaches 70% of that of the vitamin C secondary mother liquor added into the decoloring membrane equipment, diluting turbid liquid, continuously decoloring until the decoloring yield reaches 89.01%, and discharging the turbid liquid for environment-friendly treatment;
2. concentrating
Concentrating the clear liquid obtained in the step one in vacuum, concentrating to obtain water with the volume of 70% of the feed volume of the clear liquid, adding methanol with the volume equal to that of the feed volume of the clear liquid, and continuing to concentrate until liquid with the volume equal to that of the added methanol is concentrated;
3. transesterification
Adding methanol with the volume to the mass ratio L/kg of the concentrated material of 2.
The obtained crude sodium ascorbate product is yellow, the content of the product is 78.42 percent, and the total recovery rate of the effective components is 79.17 percent.
Example 3
A method for recycling vitamin C secondary mother liquor comprises the following steps:
1. film decolorization
And (3) decolorizing membrane equipment: adopting a strong acid and high pressure resistant decolorizing membrane, namely acid and high pressure resistant decolorizing membrane equipment;
directly adding the vitamin C secondary mother liquor stock solution (without diluting and adding water) into acid-resistant and high-pressure-resistant decoloring membrane equipment, circularly decoloring under the pressure of 50bar to obtain clear liquid, adding water with the volume 0.1 time that of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment after the volume of the obtained clear liquid reaches 80% of that of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment, diluting turbid liquid, continuously decoloring until the decoloring yield reaches 88.69%, and discharging the turbid liquid for environment-friendly treatment;
2. concentrating
Carrying out vacuum concentration on the clear liquid obtained in the first step, firstly concentrating water with the volume of 60% of the feeding volume of the clear liquid, then adding methanol with the volume of 0.5 time that of the feeding volume of the clear liquid, and continuing to concentrate until liquid with the volume equal to that of the added methanol is concentrated;
3. transesterification
Adding methanol with the volume to the mass ratio L/kg of the concentrated material of 4 to the concentrated material, then heating, carrying out esterification reaction for 2.5 hours under a reflux state, adding sodium carbonate after the esterification is finished, carrying out conversion reaction for 4 hours at the temperature of 62 ℃, then cooling and filtering to obtain crude sodium ascorbate, wherein the ratio of the added sodium carbonate to the total amount of effective components in the concentrated material is 0.54.
The obtained crude sodium ascorbate product is yellow, the content of the product is 82.76 percent, and the total recovery rate of the effective components is 81.22 percent.
Example 4
A method for recycling vitamin C secondary mother liquor comprises the following steps:
1. film decolorization
And (3) decolorizing membrane equipment: adopting a strong acid and high pressure resistant decolorizing membrane, namely acid and high pressure resistant decolorizing membrane equipment;
directly adding the vitamin C secondary mother liquor stock solution (without diluting and adding water) into acid-resistant and high-pressure-resistant decoloring membrane equipment, circularly decoloring under the pressure of 60bar to obtain clear liquid, adding water with the volume 0.5 times of the volume of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment after the volume of the obtained clear liquid reaches 80% of the volume of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment, diluting turbid liquid, continuously decoloring until the decoloring yield reaches 89.73%, and discharging the turbid liquid for environment-friendly treatment;
2. concentrating
Concentrating the clear liquid obtained in the step one in vacuum, concentrating to obtain water with the volume of 50% of the feeding volume of the clear liquid, adding methanol with the volume of 0.7 time that of the feeding volume of the clear liquid, and continuing to concentrate until liquid with the volume equal to that of the added methanol is obtained;
3. transesterification
Adding methanol with the volume to the mass ratio L/kg of the concentrated material of 5 to the concentrated material, heating, carrying out esterification reaction for 2.5 hours in a reflux state, adding sodium carbonate after the esterification is finished, carrying out conversion reaction for 4 hours at the temperature of 66 ℃, then cooling and filtering to obtain crude sodium ascorbate, wherein the ratio of the added sodium carbonate to the total amount of effective components in the concentrated material is 0.56.
The obtained crude sodium ascorbate product is yellow, the content of the product is 84.13 percent, and the total recovery rate of the effective components is 83.24 percent.
Claims (2)
1. A method for recycling vitamin C secondary mother liquor is characterized by comprising the following steps:
1. film decolorization
And (3) decolorizing membrane equipment: adopting a strong acid and high pressure resistant decolorizing membrane, namely acid and high pressure resistant decolorizing membrane equipment;
directly adding the vitamin C secondary mother liquor stock solution into acid-resistant and high-pressure-resistant decoloring membrane equipment, and circularly decoloring under the pressure of 20-60 bar to obtain clear liquid, wherein in the period, when the volume of the obtained clear liquid reaches 60-80% of the volume of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment, water with the volume 0.05-0.5 times of the volume of the vitamin C secondary mother liquor stock solution added into the decoloring membrane equipment is added into the decoloring membrane equipment, diluting turbid liquid, continuously decoloring, stopping until the decoloring yield reaches more than 80%, and discharging the turbid liquid for environment-friendly treatment;
2. concentrating
Carrying out vacuum concentration on the clear liquid obtained in the step one, firstly concentrating water with the volume of 30-70% of the feed volume of the clear liquid, then adding methanol with the volume of 0.2-1 time of the feed volume of the clear liquid, and continuing to concentrate until liquid with the volume equal to that of the added methanol is concentrated;
3. transesterification
Adding methanol with the volume to the mass ratio L/kg of the concentrated material of 2-5 into the concentrated material, heating, carrying out esterification reaction for 1.5-2.5 hours under a reflux state, adding sodium carbonate after the esterification, carrying out conversion reaction for 2-4 hours at the temperature of 58-66 ℃, then cooling and filtering to obtain sodium ascorbate, wherein the ratio of the added sodium carbonate to the total amount of effective components in the concentrated material is 0.5-0.6, and the effective components in the concentrated material are vitamin C, 2-keto-L-gulonic acid and 2-keto-L-gulonic acid methyl ester.
2. The method for recycling vitamin C secondary mother liquor according to claim 1, wherein the method comprises the following steps: and (5) decoloring the membrane until the decoloring yield reaches 80-90%.
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| CN112876437B (en) * | 2021-01-22 | 2023-10-24 | 无锡绿色分离应用技术研究所有限公司 | Method for extracting vitamin C by using macroporous chelate resin |
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