CN112414910A - Method for quantitatively analyzing and accurately controlling usage amount of decolorized activated carbon - Google Patents

Method for quantitatively analyzing and accurately controlling usage amount of decolorized activated carbon Download PDF

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CN112414910A
CN112414910A CN202011025833.5A CN202011025833A CN112414910A CN 112414910 A CN112414910 A CN 112414910A CN 202011025833 A CN202011025833 A CN 202011025833A CN 112414910 A CN112414910 A CN 112414910A
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activated carbon
decolorized
decolorization
amount
active carbon
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CN112414910B (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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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/0866Sorption

Abstract

The invention discloses a method for quantitatively analyzing and accurately controlling the use amount of decolorized activated carbon, which comprises the following steps: and (3) according to the detected Lovibond chroma value of the liquid to be decolorized, after the pH value of the liquid is adjusted to be 3.0-5.0, calculating the corresponding addition amount of the activated carbon according to a formula, and adding the activated carbon into the liquid to be decolorized by the activated carbon for decolorization. The method ensures the target of decolorization, simultaneously reduces the use amount of the active carbon to the maximum extent, and reduces the input cost of production raw materials. Meanwhile, the generation of waste active carbon is reduced, and the treatment cost of the waste active carbon is reduced. The method ensures that the primary decolorization reaches the target, prevents the secondary decolorization, shortens the time consumption of the decolorization process in the production flow, improves the productivity and improves the profit.

Description

Method for quantitatively analyzing and accurately controlling usage amount of decolorized activated carbon
Technical Field
The invention relates to the technical field of activated carbon decolorization, in particular to a method for accurately controlling the use amount of decolorized activated carbon through quantitative analysis.
Background
In the process of separating and purifying the solution of some soluble products, in order to ensure the color of the final product to be pure, activated carbon is required to be used for carrying out solution decolorization treatment. According to the content mentioned in the prior art "method for producing amino acid by efficiently processing fermentation liquor" CN201711382980.6, the analysis of "adding 0.5% of active carbon into original fermentation liquor" is carried out during decolorization. Because different target products or the same product but different batches of solutions have different property states, the optimal active carbon amount required for achieving the decoloring effect is different. Adding activated carbon in fixed amounts tends to cause two results:
1. the addition amount of the active carbon is insufficient, the aim of decolorization cannot be achieved, the color of a final product cannot reach the standard, or secondary decolorization is required, and the production efficiency is reduced.
2. The excessive addition of the activated carbon can achieve the decolorization target, but the excessive addition of the activated carbon causes cost increase, and the production enterprises need to additionally treat the waste activated carbon because the waste activated carbon is a dangerous solid product, so that the treatment cost of the waste activated carbon can be increased.
In conclusion, in the decoloring process, the adding amount of the activated carbon is accurately controlled, and the minimum using amount of the activated carbon for achieving the decoloring target is required, so that the practical significance is realized on 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 use amount of decolorized activated carbon.
The purpose of the invention is realized by the following technical scheme: a method for quantitatively analyzing and accurately controlling the use amount of decolorized activated carbon comprises the following steps:
(1) determination of liquid colour on Lovibond colour scale before decolouration
Visually detecting the color of the liquid to be decolorized by the activated carbon by using a Lovibond colorimeter to obtain the Lovibond unit values of red (R), yellow (Y), blue (B) and neutral gray (N) of the liquid to be decolorized.
(2) Adjusting the pH value of the solution to be decolorized
Using acid to adjust the pH value of the liquid to be decolorized to 3.0-5.0.
The acid is dilute sulfuric acid, dilute hydrochloric acid or dilute nitric acid.
The dilute sulfuric acid is 10-30% by mass.
The dilute hydrochloric acid is 10-20% by mass.
The dilute nitric acid is 10-25% by mass.
(3) Adding active carbon for decolorizing
According to the detected chromatic value of the Lovibond, calculating the corresponding addition amount of activated carbon according to a formula, and adding the activated carbon into the liquid to be decolorized for decolorization; wherein the adding amount of the activated carbon is the mass percent of the liquid to be decolorized (for example, 1 percent of the activated carbon is added when 100kg of the liquid to be decolorized is added). The specific addition amount is controlled according to the following table (taking target products L-valine, L-arginine, L-glutamine and glutamine dipeptide as examples, the concentration of the target product in the liquid to be decolorized by the activated carbon is 22-235 g/L).
When the chromatic values of the Lovibond are red (R), yellow (Y) and blue (B)3 colors, calculating the corresponding addition amount of the activated carbon according to a formula I;
formula I: x ═ (0.98 a + 0.63B + 11.7)/10000%
Wherein X is the mass percentage (accurate to 0.01%) of the activated carbon to be added, A is the detected yellow colorimetric value, and B is the sum of the detected red (R) colorimetric values and blue (B) colorimetric values.
Secondly, when the chromatic values of the Lovibond are 1-2 of 3 colors of red (R), yellow (Y) and blue (B), calculating the addition amount of the corresponding active carbon according to a formula II;
formula II: x ═ (24.98A + 1.51B-7.0)/10000%
Wherein X is the mass percentage (accurate to 0.01%) of the activated carbon to be added, A is the detected chroma value of gray (N), B is the sum of chroma values of 1 color or 2 colors detected in 3 colors of red (R), yellow, (Y) and blue (B), namely when the chroma value of Lovibond is 1 color of 3 colors of red (R), yellow (Y) and blue (B), B is the detected chroma value of 1 color in 3 colors of red (R), yellow (Y) and blue (B); when the chroma value of the Lovibond is 2 chroma values in 3 colors of red (R), yellow, (Y) and blue (B), B is the sum of the detected chroma values of 2 colors in 3 colors of red (R), yellow, (Y) and blue (B).
According to the property of the target product in the liquid (10-90 ℃) to be decolorized, whether temperature rise is carried out or not is selected. If the medium-high temperature resistance of the target product is stronger, the temperature is increased to 40-60 ℃ during decolorization. If the target product is not resistant to high temperature, the target product can be decolorized at a proper temperature, such as 60 ℃ for L-arginine and L-valine, 40 ℃ for L-glutamine and 35 ℃ for glutamine dipeptide.
In the decolorizing process, continuously stirring the liquid or introducing gas (compressed air or nitrogen) (without aseptic) for continuously mixing, decolorizing for more than 30min, and if the temperature is not higher than 40 deg.C, prolonging the decolorizing time by 5-10min on the basis of 30 min.
(4) Determination of liquid color on Lovibond color Scale after decolorization
Visually detecting the color of the decolorized liquid by using a Lovibond colorimeter to obtain red (R), yellow (Y), blue (B) and neutral gray Lovibond unit values of the liquid to be decolorized.
If the color reaches the target decolorizing end point (taking L-arginine, L-valine and L-glutamine as examples, the color needs to reach yellow less than or equal to 0.4 and red, blue and gray less than or equal to 0.1, taking glutamine dipeptide as examples, the color needs to reach yellow less than or equal to 1.0 and red, blue and gray less than or equal to 0.1), the decolorizing 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 decolorization target is ensured, and simultaneously, the use amount of the active carbon is reduced to the maximum extent, and the input cost of production raw materials is reduced. Meanwhile, the generation of waste active carbon is reduced, and the treatment cost of the waste active carbon is reduced.
(2) The method ensures that the primary decolorization reaches the target, prevents the secondary decolorization, shortens the time consumption of the decolorization process in the production flow, improves the productivity and improves the profit.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
The starting materials used in the following examples are in general the target product solutions obtained in production according to the prior art.
Example 1 (L-arginine)
The color of the target product L-arginine solution with the concentration of 120g/L is 29.0 parts by visual inspection using a Lovibond colorimeter, 11.8 parts by red and 4.2 parts by blue before decolorization. Adding 18% dilute sulfuric acid to adjust pH to 4.0, adding 0.5% active carbon according to formula I, heating to 60 deg.C, stirring, and decolorizing for 30 min. After 30min, the color is visually detected to be yellow 0.1 and red, blue and gray 0 by using a Lovibond colorimeter, and the requirement of the decoloration end point is met.
Example 2 (L-valine)
The color of the target product L-valine solution with the concentration of 82g/L is 60.0 percent of yellow, 16.5 percent of red and 6.5 percent of blue visually detected by a Lovibond colorimeter before decolorization. Adding 18% dilute sulfuric acid to adjust pH to 4.0, adding activated carbon 0.8% according to formula I, heating to 60 deg.C, stirring, and decolorizing for 30 min. After 30min, the color is visually detected to be yellow 0.2, red and blue 0 and gray 0.1 by using a Lovibond colorimeter, and the requirement of the decoloration end point is met.
Example 3 (L-valine)
The color of the target product L-valine solution with the concentration of 62g/L is 15.0 percent of yellow, 0 percent of red and blue and 0.3 percent of gray which are visually detected by a Lovibond colorimeter before decolorization. Adding 18% dilute sulfuric acid to adjust pH to 4.0, adding activated carbon 0.23% according to formula II, heating to 60 deg.C, stirring, and decolorizing for 30 min. After 30min, the color is visually detected to be yellow 0.1 and red, blue and gray 0 by using a Lovibond colorimeter, and the requirement of the decoloration end point is met.
Example 4 (L-Glutamine)
The color of a solution of a target product L-glutamine with the concentration of 22g/L is detected to be 15.0 percent yellow, 7.0 percent red, 0 percent blue and 0.2 percent gray by visual inspection by using a Lovibond colorimeter before decolorization, 18 percent dilute sulfuric acid is added to adjust the pH value of the solution to be 4.0, 0.31 percent activated carbon is added according to the formula II, the temperature is raised to 40 ℃, and the solution is stirred and decolorized for 30 min. After 30min, the color is visually detected to be yellow 0.1 and red, blue and gray 0 by using a Lovibond colorimeter, and the requirement of the decoloration end point is met.
Example 5 (Glutamine)
Before decoloring the solution with the concentration of the target product glutamine dipeptide 235g/L, visually detecting the color of yellow-7.0, red-2.0 and blue-0.5 by using a Lovibond colorimeter, adding 18 percent of dilute sulfuric acid to adjust the pH value of the solution to be 4.0, adding 0.2 percent of activated carbon according to the formula I, heating to 35 ℃, and stirring and decoloring for 40 min. After 40min, the color is visually detected to be yellow 0.1 and red, blue and gray 0 by using a Lovibond colorimeter, and the requirement of the decoloration end point is met.
COMPARATIVE EXAMPLE 1 (L-arginine)
The color of the target product L-arginine solution with the concentration of 120g/L is 29.0 parts by visual inspection using a Lovibond colorimeter, 11.8 parts by red and 4.2 parts by blue before decolorization. Adding 18% dilute sulfuric acid to adjust pH to 4.0, adding active carbon to 0.3%, heating to 60 deg.C, stirring, and decolorizing for 30 min. After 30min, the color is visually detected to be yellow 0.5, red 0.1, blue 0 and gray 0.1 by using a Lovibond colorimeter, and the requirement of the decoloration end point is not met.
Then, secondary activated carbon decolorization is needed, 0.2 percent of activated carbon is added, and stirring is carried out for 30 min. After 30min, the color is yellow 0.1 by visual detection by using a Lovibond colorimeter, and the color is red, blue and gray 0, so that the standard of decolorization is reached.
According to the calculation of a factory producing 7000 tons of L-arginine per year, 4 batches of decolorization are needed daily. In 1 batch of 10 batches, secondary decolorization is required due to insufficient addition of the active carbon, the production time of 1 hour is prolonged by adding the active carbon in the decolorization process, stirring the decolorization and measuring the color, and the capacity of the batch requiring the secondary decolorization can only reach 96 percent of the original capacity. The product production 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 target product L-arginine solution with the concentration of 120g/L is 29.0 parts by visual inspection using a Lovibond colorimeter, 11.8 parts by red and 4.2 parts by blue before decolorization. Adding 18% dilute sulfuric acid to adjust pH to 4.0, adding active carbon to 0.7%, heating to 60 deg.C, stirring, and decolorizing for 30 min. After 30min, the color is visually detected to be yellow 0.1 and red, blue and gray 0 by using a Lovibond colorimeter, and the requirement of the decoloration end point is met.
Because 0.5 percent of activated carbon is calculated according to the formula I to achieve the decolorization target, 0.7 percent of the activated carbon is actually added, 0.2 percent of the activated carbon is added, 4 batches of decolorized liquid are needed to be 1200 tons every day according to the factory calculation of 7000 tons of L-arginine produced every year, 0.6 ton of the activated carbon is added in 1 batch of the decolorized liquid every 10 batches, and 1.2 tons of waste activated carbon is produced.
The activated carbon is used for 72 tons each year, the price of the activated carbon is 10000 yuan/ton, and the cost is increased by 72 ten thousand yuan.
144 tons of waste active carbon are generated every year, the treatment cost of the waste active 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 target product L-valine solution with the concentration of 82g/L is 60.0 percent of yellow, 16.5 percent of red and 6.5 percent of blue visually detected by a Lovibond colorimeter before decolorization. Adding 18% dilute sulfuric acid to adjust pH to 4.0, adding active carbon to 0.5%, heating to 60 deg.C, stirring, and decolorizing for 30 min. After 30min, the color is visually detected to be yellow 0.7, red 0.2, blue 0 and gray 0.1 by using a Lovibond colorimeter, and the requirement of the decoloration end point is not met.
Then, secondary activated carbon decolorization is needed, 0.3 percent of activated carbon is added, and stirring is carried out for 30 min. After 30min, the color is visually detected to be yellow 0.2, red and blue 0 and gray 0.1 by using a Lovibond colorimeter, and the decolorization standard is reached.
The decolorization was carried out for 3 batches per day, calculated in 12000 tons of L-valine produced per year. In 1 batch of 10 batches, secondary decolorization is required due to insufficient addition of the active carbon, the production time of 1 hour is prolonged by adding the active carbon in the decolorization process, stirring the decolorization and measuring the color, and the capacity of the batch requiring the secondary decolorization can only reach 96 percent of the original capacity. The product production is reduced by 48 tons every year, and the profit loss is 120 ten thousand yuan.
Comparative example 4 (L-valine)
The color of the target product L-valine solution with the concentration of 82g/L is 60 percent yellow, 16.5 percent red and 6.5 percent blue by visual inspection by using a Lovibond colorimeter before decolorization. Adding 18% dilute sulfuric acid to adjust pH to 4.0, adding activated carbon 1%, heating to 60 deg.C, stirring, and decolorizing for 30 min. After 30min, the color is visually detected to be yellow 0.2, red and blue 0 and gray 0.1 by using a Lovibond colorimeter, and the requirement of the decoloration end point is met.
As 0.8 percent of activated carbon can reach the decoloration target, 1 percent of the activated carbon is actually added, 0.2 percent of the activated carbon is added, according to the factory calculation of 12000 tons of L-valine produced annually, 900 tons of decoloration liquid are needed for 3 batches each day, 0.6 ton of activated carbon is added for 1 batch in each 10 batches, and 1.2 tons of waste activated carbon is produced.
54 tons of activated carbon are used each year, the price of the activated carbon is 10000 yuan/ton, and the cost is increased by 54 ten thousand yuan.
108 tons of waste active carbon are generated every year, the treatment cost of the waste active carbon is 3000 yuan/ton, and the cost is increased by 32.4 ten thousand yuan.
It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.

Claims (10)

1. A method for quantitatively analyzing and accurately controlling the use amount of decolorized activated carbon is characterized by comprising the following steps:
according to the detected Lovibond chroma value of the liquid to be decolorized, after the pH value of the liquid is adjusted to be 3.0-5.0, the corresponding active carbon addition amount is calculated according to a formula, and the active carbon is added into the liquid to be decolorized by the active carbon for decolorization; the adding amount of the active carbon is the mass percentage of the liquid to be decolorized;
when the chromatic values of the Lovibond are 3 colors of red, yellow and blue, calculating the corresponding addition amount of the activated carbon according to a formula I;
formula I: x ═ (0.98 a + 0.63B + 11.7)/10000%
Wherein X is the mass percentage of the active carbon to be added, A is the detected yellow colorimetric value, and B is the sum of the detected red and blue colorimetric values;
when the chromatic value of the Lovibond is 1-2 of 3 colors of red, yellow and blue, calculating the addition amount of the corresponding active carbon according to a formula II;
formula II: x ═ (24.98A + 1.51B-7.0)/10000%
Wherein X is the mass percentage of the active carbon to be added, A is the detected gray colorimetric value, and B is the sum of 1 color colorimetric values or 2 color colorimetric values detected in 3 colors of red, yellow and blue.
2. The method for quantitatively and accurately controlling the amount of decolorized activated carbon used 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 and precisely controlling the amount of decolorized activated carbon to be used according to claim 2, wherein the acid is dilute sulfuric acid, dilute hydrochloric acid, or dilute nitric acid.
4. The method for quantitatively and accurately controlling the use amount of the discolored activated carbon according to claim 3, wherein the dilute sulfuric acid is 10-30% by mass; the dilute hydrochloric acid is 10-20% by mass; the dilute nitric acid is 10-25% by mass.
5. The method for quantitatively and accurately controlling the use amount of decolorizing active carbon according to claim 1, characterized in that the target product in the liquid to be decolorized by active carbon is L-valine, L-arginine, L-glutamine or glutamine dipeptide.
6. The method for quantitatively and accurately controlling the amount of decolorized activated carbon used according to claim 1, wherein the time for decolorization is 30min or more.
7. The method for quantitatively and precisely controlling the amount of decolorized activated carbon used according to claim 1, wherein the temperature of decolorization is 10 to 90 ℃.
8. The method for quantitatively and precisely controlling the amount of decolorized activated carbon used according to claim 7, wherein the time for decolorization is 35 to 40min when the temperature for decolorization is lower than 40 ℃.
9. The method for quantitatively and accurately controlling the amount of decolorized activated carbon used according to claim 1, wherein the decolorization process is performed under stirring or by introducing a gas.
10. The method for quantitatively and precisely controlling the amount of decolorized activated carbon used according to claim 1, wherein the pH of the solution after decolorization is adjusted using calcium hydroxide, ammonia water, or sodium hydroxide.
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CN114235803A (en) * 2021-12-14 2022-03-25 安图实验仪器(郑州)有限公司 Decolorization determination method used after microbial staining
CN114235803B (en) * 2021-12-14 2024-05-14 安图实验仪器(郑州)有限公司 Decoloring judgment method for microorganism after dyeing

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