CN112414910B - Method for precisely controlling decoloring active carbon usage amount by quantitative analysis - Google Patents

Method for precisely controlling decoloring active carbon usage amount by quantitative analysis Download PDF

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CN112414910B
CN112414910B CN202011025833.5A CN202011025833A CN112414910B CN 112414910 B CN112414910 B CN 112414910B CN 202011025833 A CN202011025833 A CN 202011025833A CN 112414910 B CN112414910 B CN 112414910B
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activated carbon
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CN112414910A (en
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朱路晗
陈剑彬
许凯兵
吴文忠
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Heilongjiang Nuoshu Biotechnology Co ltd
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    • G01N21/29Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using visual detection
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention discloses a method for quantitatively analyzing and accurately controlling the using amount of decolored active carbon, which comprises the following steps: according to the detected color value of the Rovicone of the liquid to be decolorized, after the pH value of the liquid is regulated to 3.0-5.0, the adding amount of the corresponding activated carbon is calculated according to a formula, and the activated carbon is added into the liquid to be decolorized by the activated carbon for decolorization. The invention can reduce the consumption of active carbon and the input cost of raw materials while ensuring the decoloring target. Meanwhile, the production of waste activated carbon is reduced, and the treatment cost of the waste activated carbon is reduced. Ensuring that the primary decolorization reaches the target, preventing secondary decolorization, shortening the time consumption of the decolorization process in the production flow, improving the productivity and increasing the profit.

Description

Method for precisely controlling decoloring active carbon usage amount by quantitative analysis
Technical Field
The invention relates to the technical field of activated carbon decolorization, in particular to a method for quantitatively analyzing and accurately controlling the using amount of decolorized activated carbon.
Background
In the process of separating and purifying the solution of some soluble products, active carbon is required to be used for decoloring the solution in order to ensure the purity of the final product. According to the content mentioned in the prior art CN201711382980.6 method for producing amino acid by efficiently treating fermentation broth, 0.5% active carbon of the original fermentation broth is added during decolorization. Because different target products or the same products but different batches of solutions have different property states, the optimal activated carbon amount required for achieving the decoloring effect is different. Adding activated carbon in fixed amounts tends to result in two results:
1. the color of the final product can not reach the standard due to the insufficient addition amount of the activated carbon, or the production efficiency is reduced due to the need of secondary decolorization.
2. The excessive addition of the activated carbon can achieve the decoloring target, but the excessive addition of the activated carbon causes the increase of cost, and as the waste activated carbon is a dangerous solid product, the waste activated carbon is required to be additionally treated by a production enterprise, so that the treatment cost of the waste activated carbon can be increased.
In summary, in the decoloring process, the addition amount of the activated carbon is precisely controlled, and the minimum use amount of the activated carbon for achieving the decoloring target is pursued to have practical significance for production.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for quantitatively analyzing and accurately controlling the using amount of decolored active carbon.
The aim of the invention is achieved by the following technical scheme: a method for quantitatively analyzing and accurately controlling the use amount of decolored active carbon comprises the following steps:
(1) Determination of liquid colour by the Rovepone colour Scale before colour removal
The color of the liquid to be decolorized by active carbon is visually detected by using a rovider colorimeter, and the rovider unit value of red (R), yellow (Y), blue (B) and neutral gray (N) of the liquid to be decolorized is obtained.
(2) Regulating pH value of liquid to be decolorized
The pH of the liquid to be decolorized is adjusted to 3.0-5.0 using an acid.
The acid is dilute sulfuric acid, dilute hydrochloric acid or dilute nitric acid.
The dilute sulfuric acid is 10-30% of the mass fraction of dilute sulfuric acid.
The dilute hydrochloric acid is 10-20% of the mass fraction of the dilute hydrochloric acid.
The dilute nitric acid is 10-25% of the mass fraction of the dilute nitric acid.
(3) Adding activated carbon for decolorizing
Calculating the addition amount of the corresponding activated carbon according to a formula according to the detected chromaticity value of the rovided, and adding the activated carbon into the liquid to be decolorized for decolorization; wherein the addition amount of the activated carbon is the mass percent of the liquid to be decolorized (for example, 100kg of the liquid to be decolorized, 1% is added, namely, 1kg of the activated carbon is added). The specific addition amount is controlled according to the following table (taking target products of L-valine, L-arginine, L-glutamine and glutamine dipeptide as examples, and the concentration of the target products in the decolorized liquid of the activated carbon is 22-235 g/L).
(1) When the chromaticity value of the rovided is 3 colors of red (R), yellow (Y) and blue (B), calculating the addition amount of the corresponding activated carbon according to a formula I;
formula I: x= (0.98×a+0.63×b+11.7)/10000×100%
Wherein X is the mass percent (accurate to 0.01%) of the active carbon to be added, A is the detected yellow chromaticity value, and B is the sum of the detected red (R) and blue (B) chromaticity values.
(2) When the chromaticity value of the rovided is 1-2 of 3 colors of red (R), yellow (Y) and blue (B), calculating the corresponding addition amount of the activated carbon according to a formula II;
formula II: x= (24.98×a+1.51×b-7.0)/10000×100%
Wherein X is the mass percent (accurate to 0.01%) of the active carbon to be added, A is the detected gray (N) chromaticity value, B is the sum of 1 or 2 color chromaticity values detected in the 3 colors of red (R), yellow, (Y) and blue (B), namely when the Rovepone chromaticity value is 1 in the 3 colors of red (R), yellow, (Y) and blue (B), B is the 1 color chromaticity value detected in the 3 colors of red (R), yellow, (Y) and blue (B); when the chromaticity value of the rovapone is 2 of 3 colors of red (R), yellow, (Y) and blue (B), B is the sum of the chromaticity values of 2 colors detected from the 3 colors of red (R), yellow, (Y) and blue (B).
According to the property of target product in the liquid to be decolorized (10-90 ℃), selecting whether to raise the temperature. If the target product has strong medium and high temperature resistance, the temperature is increased to 40-60 ℃ during decoloring. If the target product is not high temperature resistant, the target product can be decolorized at a proper temperature, for example, the proper temperature for decolorizing L-arginine and L-valine is 60 ℃, the proper temperature for decolorizing L-glutamine is 40 ℃, and the proper temperature for decolorizing the proglutin is 35 ℃.
In the decoloring process, the liquid is required to be continuously stirred or gas (compressed air or nitrogen) is introduced (no bacteria is required) to be continuously mixed, the decoloring time is more than 30min, and if the temperature is not more than 40 ℃, the decoloring time is required to be prolonged by 5-10min on the basis of 30min.
(4) Determination of liquid colour by the colour scale of roviden after decolouration
The color of the decolorized liquid is visually detected by using a rovider colorimeter, and the unit values of the rovider, the yellow (Y), the blue (B) and the neutral gray of the liquid to be decolorized are obtained.
If the color reaches the target decoloring end point (for example, the color is required to be yellow or less than or equal to 0.4, red, blue and gray or less than or equal to 0.1, and for example, the color is required to be yellow or less than or equal to 1.0, and red, blue and gray or less than or equal to 0.1) for the L-arginine, L-valine and L-glutamine, the decoloring is finished.
After decolorization, the pH of the solution is adjusted back to the appropriate pH using calcium hydroxide or ammonia or sodium hydroxide.
The invention has the beneficial effects that:
(1) The method can ensure the decoloring target, simultaneously reduce the using amount of the activated carbon to the maximum extent and reduce the input cost of production raw materials. Meanwhile, the production of waste activated carbon is reduced, and the treatment cost of the waste activated carbon is reduced.
(2) Ensuring that the primary decolorization reaches the target, preventing secondary decolorization, shortening the time consumption of the decolorization process in the production flow, improving the productivity and increasing the profit.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
The starting materials used in the examples below are all the usual target product solutions obtained in production according to the prior art.
Example 1 (L-arginine)
The color of the solution with the target product L-arginine concentration of 120g/L was visually detected as yellow=29.0, red=11.8, blue=4.2 by using a rovider colorimeter before decolorization. Adding 18% dilute sulfuric acid to regulate pH to 4.0, adding active carbon 0.5% according to formula I, heating to 60deg.C, and decolorizing under stirring for 30min. After 30min, the color was visually checked using a rovider colorimeter to be yellow=0.1, red, blue, gray=0, and the decolorizing endpoint requirement was reached.
Example 2 (L-valine)
The color of the solution of the target product L-valine at 82g/L was visually checked as yellow=60.0, red=16.5, blue=6.5 using a rovider colorimeter before decolorization. Adding 18% dilute sulfuric acid to regulate pH to 4.0, adding active carbon 0.8% according to formula I, heating to 60deg.C, and stirring for decolorizing for 30min. After 30min, the color was visually checked using a rovider colorimeter to be yellow=0.2, red, blue=0, and gray=0.1, reaching the decoloration endpoint requirement.
Example 3 (L-valine)
The color of the solution of the target product L-valine at 62g/L was visually checked as yellow=15.0, red, blue=0, and gray=0.3 using a roviden colorimeter before decoloring. Adding 18% dilute sulfuric acid to regulate pH to 4.0, adding active carbon to 0.23% according to formula II, heating to 60deg.C, and stirring for decolorizing for 30min. After 30min, the color was visually checked using a rovider colorimeter to be yellow=0.1, red, blue, gray=0, and the decolorizing endpoint requirement was reached.
Example 4 (L-Glutamine)
The color of the solution with the concentration of the target product L-glutamine of 22g/L is visually detected to be yellow=15.0 by using a rovidence colorimeter before decoloring, red=7.0, blue=0, gray=0.2, 18 percent dilute sulfuric acid is added to adjust the pH value to 4.0, 0.31 percent of active carbon is added according to the formula II, the temperature is raised to 40 ℃, and the mixture is stirred and decolored for 30 minutes. After 30min, the color was visually checked using a rovider colorimeter to be yellow=0.1, red, blue, gray=0, and the decolorizing endpoint requirement was reached.
Example 5 (Provaladipeptide)
Before decoloring a solution with the target product of which the concentration of the proglutide is 235g/L, visually detecting that the color is yellow=7.0 by using a rovidence colorimeter, red=2.0, blue=0.5, adding 18% dilute sulfuric acid to adjust the pH value to 4.0, adding 0.2% of active carbon according to a formula I, heating to 35 ℃, and stirring for decoloring for 40min. After 40min, the color was visually checked with a rovider colorimeter to be yellow=0.1, red, blue, gray=0, and the decolorizing endpoint requirement was reached.
Comparative example 1 (L-arginine)
The color of the solution with the target product L-arginine concentration of 120g/L was visually detected as yellow=29.0, red=11.8, blue=4.2 by using a rovider colorimeter before decolorization. Adding 18% dilute sulfuric acid to regulate pH to 4.0, adding active carbon to 0.3%, heating to 60deg.C, and decolorizing under stirring for 30min. After 30min, the color was visually checked using a rovider colorimeter as yellow=0.5, red=0.1, blue=0, gray=0.1, and the decolorizing endpoint requirement was not reached.
Then, secondary activated carbon decolorization is needed, 0.2% of activated carbon is added, and stirring decolorization is carried out for 30min. After 30min, the color was visually checked to be yellow 0.1, red, blue, gray=0 using a rovider colorimeter, reaching the decolorization standard.
The total number of decolorization runs required per day was 4, calculated as the plant producing 7000 tons of L-arginine per year. In every 10 batches, 1 batch needs to be subjected to secondary decolorization due to insufficient addition of active carbon, and the production time of adding active carbon in the decolorization process, stirring and decolorizing and color measurement steps is prolonged by 1 hour, so that the yield of the batch needing secondary decolorization can only reach 96% of the original yield. The production of the product is reduced by 28 tons every year, and the profit loss is 112 ten thousand yuan.
Comparative example 2 (L-arginine)
The color of the solution with the target product L-arginine concentration of 120g/L was visually detected as yellow=29.0, red=11.8, blue=4.2 by using a rovider colorimeter before decolorization. Adding 18% dilute sulfuric acid to regulate pH to 4.0, adding active carbon to 0.7%, heating to 60deg.C, and decolorizing under stirring for 30min. After 30min, the color was visually checked using a rovider colorimeter to be yellow=0.1, red, blue, gray=0, and the decolorizing endpoint requirement was reached.
As 0.5% of activated carbon is calculated according to the formula I, the decolorization target can be achieved, and 0.7% of activated carbon is actually added, and 0.2% of activated carbon is added, and according to the annual L-arginine 7000 ton production factory, total 1200 tons of decolorized liquid are required for 4 batches per day, and more 0.6 ton of activated carbon is added for 1 batch in 10 batches, so that 1.2 tons of waste activated carbon is generated.
The price of the active carbon is 10000 yuan/ton, and the cost is increased by 72 ten thousand yuan.
144 tons of waste activated carbon are generated each year, the treatment cost of the waste activated carbon is 3000 yuan/ton, and the cost is increased by 57.6 ten thousand yuan.
Comparative example 3 (L-valine)
The color of the solution of the target product L-valine at 82g/L was visually checked as yellow=60.0, red=16.5, blue=6.5 using a rovider colorimeter before decolorization. Adding 18% dilute sulfuric acid to regulate pH to 4.0, adding active carbon to 0.5%, heating to 60deg.C, and decolorizing under stirring for 30min. After 30min, the color was visually checked using a rovider colorimeter as yellow=0.7, red=0.2, blue=0, gray=0.1, and the decolorizing endpoint requirement was not reached.
Then, secondary activated carbon decolorization is needed, 0.3% of activated carbon is added, and stirring decolorization is carried out for 30min. After 30min, the color was visually checked using a rovider colorimeter to be yellow=0.2, red, blue=0, and gray=0.1, reaching the decoloration standard.
The total amount of decolorization was 3 batches per day calculated in a plant producing 12000 tons of L-valine per year. In every 10 batches, 1 batch needs to be subjected to secondary decolorization due to insufficient addition of active carbon, and the production time of adding active carbon in the decolorization process, stirring and decolorizing and color measurement steps is prolonged by 1 hour, so that the yield of the batch needing secondary decolorization can only reach 96% of the original yield. The production of the product is reduced by 48 tons each year, and the profit loss is 120 ten thousand yuan.
Comparative example 4 (L-valine)
The color of the solution with the concentration of the target product L-valine of 82g/L was visually detected as yellow=60, red=16.5, blue=6.5 by using a rovider colorimeter before decolorization. Adding 18% dilute sulfuric acid to regulate pH to 4.0, adding active carbon to 1%, heating to 60 ℃, and stirring for decolorizing for 30min. After 30min, the color was visually checked using a rovider colorimeter to be yellow=0.2, red, blue=0, and gray=0.1, reaching the decoloration endpoint requirement.
As 0.8% of activated carbon can reach the decolorization target, and 1% of activated carbon is actually added, 0.2% of activated carbon is added, and 3 batches of decolorized liquid are required to be 900 tons per day according to the industrial calculation of 12000 tons of annual L-valine production, and 1 batch of activated carbon is added for 0.6 ton per 10 batches, so that 1.2 tons of waste activated carbon is generated.
The active carbon is used for 54 tons each year, the price of the active carbon is 10000 yuan/ton, and the cost is increased by 54 ten thousand yuan.
The waste activated carbon is produced for 108 tons each year, the treatment cost of the waste activated carbon is 3000 yuan/ton, and the cost is increased by 32.4 ten thousand yuan.
Many possible variations and modifications of the disclosed technology can be made by anyone skilled in the art without departing from the scope of the technology, or the technology can be modified to be equivalent. Therefore, any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention shall still fall within the scope of the technical solution of the present invention.

Claims (10)

1. The method for quantitatively analyzing and accurately controlling the using amount of the decolored active carbon is characterized by comprising the following steps of:
according to the detected color value of the Rovinone of the liquid to be decolorized, after the pH value of the liquid is regulated to 3.0-5.0, calculating the corresponding usage amount of the active carbon according to a formula, adding the active carbon into the liquid to be decolorized, and decolorizing; the mass percentage of the used amount of the activated carbon is that the used amount of the activated carbon accounts for the mass percentage of the liquid to be decolorized;
when the chromaticity value of the rovided is 3 colors of red, yellow and blue, calculating the corresponding using amount of the activated carbon according to a formula I;
formula I: x= (0.98×a+0.63×b+11.7)/10000×100%
Wherein X is the mass percent of the usage amount of the activated carbon, A is the detected yellow chromaticity value, and B is the sum of the detected red and blue chromaticity values;
when the chromaticity value of the rovided is 1-2 of 3 colors of red, yellow and blue, calculating the corresponding using amount of the activated carbon according to a formula II;
formula II: x= (24.98×a+1.51×b-7.0)/10000×100%
Wherein X is the mass percent of the usage amount of the activated carbon, A is the detected gray shade value, and B is the sum of 1 color shade value or 2 color shade values detected in 3 colors of red, yellow and blue.
2. The method for quantitatively analyzing and precisely controlling the use amount of decolorizing active carbon according to claim 1, wherein the reagent used for adjusting the pH of the liquid to 3.0 to 5.0 is an acid.
3. The method for quantitatively analyzing and precisely controlling the use amount of decolorized activated carbon according to claim 2, wherein the acid is dilute sulfuric acid, dilute hydrochloric acid or dilute nitric acid.
4. The method for quantitatively analyzing and precisely controlling the use amount of decolored activated carbon according to claim 3, wherein the dilute sulfuric acid is 10-30% by mass; the dilute hydrochloric acid is 10-20% of the dilute hydrochloric acid by mass fraction; the dilute nitric acid is 10-25% of the mass fraction of the dilute nitric acid.
5. The method for quantitatively analyzing and precisely controlling the use amount of decolorizing active carbon according to claim 1, wherein the target product in the liquid to be decolorized is L-valine, L-arginine, L-glutamine or glutamine dipeptide.
6. The method for quantitatively analyzing and precisely controlling the use amount of the decolored activated carbon according to claim 1, wherein the decoloring time is more than 30 minutes.
7. The method for quantitatively analyzing and precisely controlling the use amount of decolorized activated carbon according to claim 1, wherein the decolorization temperature is 10 to 90 ℃.
8. The method for precisely controlling the use amount of the decolorized activated carbon by quantitative analysis according to claim 7, wherein the decolorization time is 35 to 40 minutes when the decolorization temperature is lower than 40 ℃.
9. The method for quantitatively analyzing and precisely controlling the use amount of the decolorized activated carbon according to claim 1, wherein the decolorization process is performed under stirring or by introducing a gas.
10. The method for quantitatively analyzing and precisely controlling the use amount of decolorized activated carbon according to claim 1, wherein the pH of the decolorized solution is adjusted by using calcium hydroxide or ammonia or sodium hydroxide.
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