CN111233953B - Method for recycling activated carbon after gentamycin sulfate decoloration - Google Patents
Method for recycling activated carbon after gentamycin sulfate decoloration Download PDFInfo
- Publication number
- CN111233953B CN111233953B CN202010160280.8A CN202010160280A CN111233953B CN 111233953 B CN111233953 B CN 111233953B CN 202010160280 A CN202010160280 A CN 202010160280A CN 111233953 B CN111233953 B CN 111233953B
- Authority
- CN
- China
- Prior art keywords
- activated carbon
- washing
- filtrate
- heating
- filter cake
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/22—Cyclohexane rings, substituted by nitrogen atoms
- C07H15/222—Cyclohexane rings substituted by at least two nitrogen atoms
- C07H15/226—Cyclohexane rings substituted by at least two nitrogen atoms with at least two saccharide radicals directly attached to the cyclohexane rings
- C07H15/234—Cyclohexane rings substituted by at least two nitrogen atoms with at least two saccharide radicals directly attached to the cyclohexane rings attached to non-adjacent ring carbon atoms of the cyclohexane rings, e.g. kanamycins, tobramycin, nebramycin, gentamicin A2
- C07H15/236—Cyclohexane rings substituted by at least two nitrogen atoms with at least two saccharide radicals directly attached to the cyclohexane rings attached to non-adjacent ring carbon atoms of the cyclohexane rings, e.g. kanamycins, tobramycin, nebramycin, gentamicin A2 a saccharide radical being substituted by an alkylamino radical in position 3 and by two substituents different from hydrogen in position 4, e.g. gentamicin complex, sisomicin, verdamycin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for recycling activated carbon after gentamycin sulfate decoloration, which comprises the following process flows of: activated carbon after decolorization → heating alkaline washing → hot filtering → washing drying → heating acid washing → hot filtering → washing drying → gentamicin sulfate powder and regenerated activated carbon, which can not only reduce gentamicin sulfate loss caused by the decolorization step, but also obtain regenerated activated carbon for reuse in the carbon removal treatment of gentamicin sulfate. The invention has the following advantages: the cycle is short, and the productivity is high; the yield of gentamicin sulfate is improved, and the production cost is reduced; the activated carbon is reused, the production cost is reduced, and the environment is protected. The treated active carbon can be reused after being dried, so that the production cost is reduced; the waste discharge is reduced, and the environment is protected; the investment reconstruction is small, the operation is simple, and the efficiency is high; the invention has the advantages of small investment modification, simple operation and high efficiency, and is suitable for industrial production.
Description
Technical Field
The invention relates to an active carbon recycling method, in particular to a method for recycling active carbon after gentamicin sulfate decoloration. Belongs to the technical field of pharmacy.
Background
Gentamicin sulfate is a broad-spectrum aminoglycoside antibiotic, and has antibacterial and bactericidal effects on various gram-negative bacteria and gram-positive bacteria. Has strong effects on gram-negative bacteria such as pseudomonas aeruginosa, aerobacter, pneumobacillus, salmonella, escherichia coli, proteus, staphylococcus aureus and the like. The action mechanism of gentamicin sulfate is to bind firmly with specific proteins on bacterial ribosomal subunits, interfere with ribosomal functions, prevent protein synthesis, and cause errors in the code on translated messenger ribonucleic acid (mRNA) to synthesize non-functional proteins. The traditional Chinese medicine composition is clinically used for treating septicemia, respiratory tract infection, biliary tract infection, purulent peritonitis, intracranial infection, urinary tract infection, bacillary dysentery and other diseases caused by staphylococcus aureus, pseudomonas aeruginosa, escherichia coli, dysentery bacillus, klebsiella, proteus and other sensitive bacteria.
The traditional production process of gentamicin sulfate is as follows: gentamycin fermentation liquid → acidification and inactivation → resin adsorption → shaking sieve separation → ammonia water analysis → nanofiltration membrane filtration → film evaporator concentration → salification → carbon desorption → gentamycin sulfate finished product liquid. The traditional process is characterized in that the activated carbon used in the step of carbon removal is discarded after being treated according to medical waste, so that the treatment process is complicated, the workload is high, the period is long, the personnel allocation is large, the cost is high, and the environment is polluted after the activated carbon is discarded; this treatment method is in need of improvement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for recycling activated carbon after the gentamicin sulfate is decolorized, so that the yield of the gentamicin sulfate is improved, the recycling of the activated carbon is realized, the production cost is reduced, and the hidden danger of environmental protection is eliminated.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for recycling the active carbon after the gentamycin sulfate is decolorized comprises the following specific steps:
(1) firstly, heating and alkali washing waste activated carbon decolorized by gentamicin sulfate at 80-85 ℃, filtering while hot, feeding the obtained filtrate I into an acid-base neutralization tank, washing and drying the obtained filter cake I, and then feeding into the step (2);
(2) heating and acid washing at 60-65 ℃, filtering while hot, and allowing the obtained filtrate II to enter the step (4) and the obtained filter cake II to enter the step (3);
(3) heating and acid washing at 60-65 ℃, filtering while hot, washing and drying the obtained filter cake III to obtain regenerated activated carbon, and allowing the obtained filtrate III to enter the step (4);
(4) and combining the filtrate II and the filtrate III, and concentrating, decoloring and spraying to obtain gentamicin sulfate powder.
Preferably, in the step (1), the specific method for washing and drying is as follows: and (3) leaching with hot water of 80-85 ℃ for three times, wherein the weight of the hot water used in each leaching is the same as that of the waste activated carbon, and blowing the waste activated carbon with air after the three leaching is completed.
Preferably, in the step (1), the specific method for heating and washing with alkali is as follows: stirring and mixing the waste activated carbon, water and sodium hydroxide, heating and stirring for 3 hours, and maintaining the pH value to be 13-14; wherein the mass ratio of the waste activated carbon to the water to the sodium hydroxide is 10: 20: 1.
preferably, in the step (2), the specific method for heating and pickling is as follows: stirring and mixing the filter cake I with water and concentrated sulfuric acid with the mass concentration of 98%, heating and stirring for 1 hour, and maintaining the pH value to be 1-2; wherein the mass ratio of the waste activated carbon to the water to the concentrated sulfuric acid is 250: 250: 3.
preferably, in the step (3), the specific method for heating and pickling is as follows: stirring and mixing the filter cake II with water and concentrated sulfuric acid with the mass concentration of 98%, stirring and heating for 1 hour, and maintaining the pH value to be 2-3; wherein the mass ratio of the waste activated carbon to the water to the concentrated sulfuric acid is 125: 375: 3.
preferably, in the step (3), the specific method of the washing and drying treatment is as follows: leaching the filter cake III with hot water of 60-65 ℃ twice, wherein the weight of the hot water used in each leaching is the same as that of the waste activated carbon, blowing the filter cake III with air after the leaching of the two times is completed, transferring the filter cake III into an oven, and drying the filter cake III for 6 hours at 100-105 ℃ to obtain the regenerated activated carbon.
Preferably, the specific method of step (4) is as follows:
(4-1) concentration: combining the filtrate II and the filtrate III, and concentrating to obtain gentamicin sulfate concentrated solution;
(4-2) decoloring: decolorizing with active carbon to obtain gentamycin sulfate finished product liquid;
(4-3) powder spraying: and finally, carrying out spray drying on the gentamicin sulfate finished product liquid to obtain a gentamicin sulfate finished product.
Further preferably, the specific method of step (4-1) is: and combining the filtrate II and the filtrate III, concentrating the mixture by using a film concentrator to 1/100 of the original volume to obtain a gentamicin sulfate concentrated solution.
Further preferably, the specific method of step (4-2) is: adding 0.1 weight of activated carbon into the concentrated solution, heating to 60-65 ℃, stirring for 4 hours, filtering to obtain a filtrate IV and a filter cake IV, washing the filter cake IV with 2 weight times of purified water of the activated carbon to obtain a washing solution, and combining the filtrate IV and the washing solution to obtain a finished product gentamicin sulfate solution.
Further preferably, in the step (4-3), the spray drying process conditions are as follows: the air inlet temperature is 130 ℃, the air outlet temperature is 85 ℃, and the spraying speed is 100L/h.
The invention has the beneficial effects that:
the invention provides a method for recycling activated carbon after gentamycin sulfate decoloration, which comprises the following process flows of: activated carbon after decolorization → heating alkaline washing → hot filtering → washing drying → heating acid washing → hot filtering → washing drying → gentamicin sulfate powder and regenerated activated carbon, thereby not only being capable of recovering gentamicin sulfate in the waste activated carbon, but also being capable of obtaining regenerated activated carbon for being reused in gentamicin sulfate carbon removal treatment. The invention has the following advantages:
1. short cycle and high productivity.
2. The yield of gentamicin sulfate is improved, and the production cost is reduced. The acid washing filtrate is concentrated, decolored and sprayed to obtain finished powder, so that the yield is improved, and the production cost is reduced.
3. The activated carbon is reused, the production cost is reduced, and the environment is protected. The treated active carbon can be reused after being dried, so that the production cost is reduced; reduce waste discharge and protect environment.
4. The investment transformation is small, the operation is simple, and the efficiency is high. The invention has the advantages of small investment modification, simple operation and high efficiency, and is suitable for industrial production.
5. The treatment steps of the method are very critical, and the steps of firstly carrying out alkali washing and then carrying out acid washing cannot be randomly reversed. If acid washing is performed before alkali washing, the recovered gentamicin sulfate is high in impurity, the pH value of the regenerated active carbon is high, the ash content is high, and the quality of both the gentamicin sulfate and the regenerated active carbon is not qualified.
Detailed Description
The present invention will be further illustrated by the following examples, which are intended to be merely illustrative and not limitative.
Example 1:
the method for recycling the active carbon after the gentamycin sulfate is decolorized comprises the following specific steps:
1 heating alkaline washing
1.1 putting 500kg of wet activated carbon into a 5 ton enamel reactor, adding 1000L of water and 50kg of sodium hydroxide, stirring and heating to 80 ℃ with steam, and keeping the temperature for 3 hours while maintaining the pH at 14.
1.2 discharging the feed liquid to a filter pressing box for hot filtration, and feeding the filtrate into an acid-base neutralization pond.
1.3 washing the filter cake with 500kg of hot water at 80 ℃ for three times, feeding the filtrate into an acid-base neutralization tank, and drying the washed filter cake by air to obtain the activated carbon after alkali washing.
2 heating and acid pickling
2.1 adding the activated carbon after alkali washing into a 5000L reaction kettle, adding 500L water, adding 6kg of concentrated sulfuric acid with the mass concentration of 98%, stirring, heating to 65 ℃, stirring, keeping the temperature for 1 hour, and keeping the pH value to 1.
2.2, performing thermal filtration, uniformly placing the pickling solution into a filter pressing box, starting the filter pressing box to stir vacuum seasonings for 5min, performing back flushing stirring uniformly, closing vacuum, standing and soaking for 15min, performing filter pressing, placing the filtrate into a receiving tank for storage, wherein the volume of the filtrate is 476L, and sampling the filtrate to detect that the concentration of the gentamicin is 3584 u/ml; adding the filtered activated carbon filter cake into a 5000L reaction kettle, adding 12kg of water and concentrated sulfuric acid with the mass concentration of 98% into the reaction kettle, stirring and heating to 65 ℃, stirring and preserving heat for 1 hour, maintaining the pH value to be 2, uniformly putting the pickling solution into a filter pressing box for filter pressing, putting the filtrate into a receiving tank for storage, and sampling the filtrate to detect that the concentration of the gentamicin is 2561u/ml, wherein the filtrate is 1457L.
2.3 adding 1000L of purified water into a 5000L reaction kettle, heating to 65 ℃, washing the filter cake twice with 500L of purified water at 65 ℃, respectively, placing the filtrate into a receiving tank for storage, filtering to obtain 959L of filtrate, sampling the filtrate to detect that the concentration of the gentamicin is 2016u/ml, and drying the filter cake with air.
2.4 putting the filter cake into an oven, drying for 6 hours at 100 ℃ to obtain the regenerated active carbon.
2.5 the data of the regenerative activated carbon test are shown in Table 1.
TABLE 1 test data for regenerative activated carbon
The regenerated active carbon meets the medicinal carbon standard of 2015 edition of Chinese pharmacopoeia.
3 recovering gentamicin sulfate in the filtrate
3.1, concentrating, combining the acid washing filtrates, concentrating by a film concentrator, combining the acid washing filtrates, and obtaining the gentamicin sulfate concentrated solution 74.39 hundred million u, wherein the sample detection gentamicin concentration is 2590u/ml, the concentration is 29L, and the sample detection gentamicin concentration is 256500 u/ml.
3.2, decoloring, adding active carbon into the concentrated solution, wherein the adding amount of the active carbon is 2.9kg, heating to 65 ℃, stirring for 4 hours, filtering, adding 5.8L of purified water to wash filter cakes, wherein the volume of the filtrate is 29.5L, and sampling to detect that the concentration of the gentamicin is 224600u/ml to obtain 66.26 hundred million u of finished gentamicin sulfate solution.
3.3 spraying powder, and performing spray drying on the gentamicin sulfate finished product liquid through a spray tower under the conditions of air inlet temperature of 130 ℃, air outlet temperature of 85 ℃ and spray speed of 100L/h to obtain the gentamicin sulfate finished product. 3.4 assay data for the recovered gentamicin sulfate end product are shown in Table 2.
TABLE 2 assay data for recovered gentamicin sulfate finished products
The recovered finished product of the gentamicin sulfate completely meets the standard of gentamicin sulfate in the 'Chinese pharmacopoeia' of 2015 edition.
Example 2:
the method for recycling the active carbon after the gentamycin sulfate is decolorized comprises the following specific steps:
1 heating alkaline washing
1.1 putting 500kg of wet activated carbon into a 5 ton enamel reactor, adding 1000L of water and 50kg of sodium hydroxide, stirring and heating to 85 ℃ with steam, and keeping the temperature for 3 hours while maintaining the pH value at 13.
1.2 discharging the feed liquid to a filter pressing box for hot filtration, and feeding the filtrate into an acid-base neutralization pond.
1.3 washing the filter cake with 500kg of 85 ℃ hot water for three times, feeding the filtrate into an acid-base neutralization tank, and drying the washed filter cake with air to obtain the alkali-washed active carbon.
2 heating and acid pickling
2.1 adding the activated carbon after alkali washing into a 5000L reaction kettle, adding 500L water, adding 6kg of concentrated sulfuric acid with the mass concentration of 98%, stirring, heating to 60 ℃, stirring, keeping the temperature for 1 hour, and maintaining the pH value to be 2.
2.2, performing thermal filtration, uniformly placing the pickling solution into a filter pressing box, starting the filter pressing box to stir vacuum seasonings for 5min, performing back flushing stirring uniformly, closing vacuum, standing and soaking for 15min, performing filter pressing, placing the filtrate into a receiving tank for storage, wherein the volume of the filtrate is 465L, and sampling the filtrate to detect that the concentration of the gentamicin is 3843 u/ml; adding the filtered activated carbon filter cake into a 5000L reaction kettle, adding 12kg of water and concentrated sulfuric acid with the mass concentration of 98% into the reaction kettle, stirring and heating to 60 ℃, stirring and preserving heat for 1 hour, maintaining the pH value to be 3, uniformly putting the pickling solution into a filter pressing box for filter pressing, putting the filtrate into a receiving tank for storage, filtering the filtrate into 1472L, and sampling the filtrate to detect the concentration of the gentamicin to be 2637 u/ml.
2.3 adding 1000L of purified water into a 5000L reaction kettle, heating to 60 ℃, washing the filter cake twice with 500L of purified water at 60 ℃, respectively, placing the filtrate into a receiving tank for storage, filtering to obtain 964L of filtrate, sampling the filtrate to detect that the concentration of the gentamicin is 2109u/ml, and drying the filter cake with air.
2.4 putting the filter cake into an oven, drying for 6 hours at 105 ℃ to obtain the regenerated active carbon.
2.5 the data of the regenerative activated carbon test are shown in Table 3.
TABLE 3 regenerative Activity charring test data
The regenerated active carbon meets the medicinal carbon standard of 2015 edition of Chinese pharmacopoeia.
3 recovering gentamicin sulfate in the filtrate
3.1, concentrating, combining the acid washing filtrates, concentrating by a film concentrator, combining the acid washing filtrates, and obtaining the gentamicin sulfate concentrated solution 76.47 hundred million u, wherein the concentration of the gentamicin is 2652u/ml by sampling detection and is concentrated to 29L, and the concentration of the gentamicin is 263700u/ml by sampling detection.
3.2, decoloring, adding active carbon into the concentrated solution, wherein the adding amount of the active carbon is 2.9kg, heating to 60 ℃, stirring for 4 hours, filtering, adding 5.8L of purified water to wash filter cakes, wherein the total volume of the filtrate is 30.2L, and sampling to detect the concentration of the gentamicin to be 233900u/ml to obtain 70.64 hundred million u of finished gentamicin sulfate solution.
3.3 spraying powder, and performing spray drying on the gentamicin sulfate finished product liquid through a spray tower under the conditions of air inlet temperature of 130 ℃, air outlet temperature of 85 ℃ and spray speed of 100L/h to obtain the gentamicin sulfate finished product.
3.4 assay data for the recovered gentamicin sulfate end product are shown in Table 4.
TABLE 4 assay data for recovered gentamicin sulfate finished products
The recovered finished product of the gentamicin sulfate completely meets the standard of gentamicin sulfate in the 'Chinese pharmacopoeia' of 2015 edition.
Example 3:
the method for recycling the active carbon after the gentamycin sulfate is decolorized comprises the following specific steps:
1 heating alkaline washing
1.1 putting 500kg of wet activated carbon into a 5 ton enamel reactor, adding 1000L of water and 50kg of sodium hydroxide, stirring, heating to 83 ℃ with steam, and keeping the temperature for 3 hours while maintaining the pH value at 13.5.
1.2 discharging the feed liquid to a filter pressing box for hot filtration, and feeding the filtrate into an acid-base neutralization pond.
1.3 washing the filter cake with 500kg of 83 ℃ hot water for three times, feeding the filtrate into an acid-base neutralization tank, and drying the washed filter cake with air to obtain the alkali-washed active carbon.
2 heating and acid pickling
2.1 adding the activated carbon after alkali washing into a 5000L reaction kettle, adding 500L water, adding 6kg of concentrated sulfuric acid with the mass concentration of 98%, stirring, heating to 64 ℃, stirring, keeping the temperature for 1 hour, and maintaining the pH value to be 1.5.
2.2, performing thermal filtration, uniformly placing the pickling solution into a filter pressing box, starting the filter pressing box to stir vacuum seasonings for 5min, performing back flushing stirring uniformly, closing vacuum, standing and soaking for 15min, performing filter pressing, placing the filtrate into a receiving tank for storage, wherein the volume of the filtrate is 481L, and sampling the filtrate to detect that the concentration of the gentamicin is 3579 u/ml; adding the filtered activated carbon filter cake into a 5000L reaction kettle, adding 12kg of water and concentrated sulfuric acid with the mass concentration of 98% into the reaction kettle, stirring and heating to 64 ℃, stirring and preserving heat for 1 hour, maintaining the pH value to be 2.5, uniformly putting the pickling solution into a filter pressing box for filter pressing, putting the filtrate into a receiving tank for storage, and sampling the filtrate to detect that the concentration of the gentamicin is 2551 u/ml.
2.3 adding 1000L of purified water into a 5000L reaction kettle, heating to 64 ℃, washing the filter cake twice with 500L of 64 ℃ purified water respectively, placing the filtrate into a receiving tank for storage, filtering to obtain 961L of filtrate, sampling the filtrate to detect that the concentration of the gentamicin is 2085u/ml, and drying the filter cake by air.
2.4 putting the filter cake into an oven, drying for 6 hours at 102 ℃ to obtain the regenerated active carbon.
2.5 the data of the regenerative activated carbon test are shown in Table 5.
TABLE 5 regenerated activated char assay data
The regenerated active carbon meets the medicinal carbon standard of 2015 edition of Chinese pharmacopoeia.
3 recovering gentamicin sulfate in the filtrate
3.1, concentrating, combining the acid washing filtrates, concentrating by a thin film concentrator, combining the acid washing filtrates, wherein the volume is 2910L, the concentration of the gentamicin by sampling detection is 2621u/ml, concentrating to 29L, and the concentration of the gentamicin by sampling detection is 265500u/ml to obtain the gentamicin sulfate concentrated solution 76.51 hundred million u.
3.2, decoloring, adding active carbon into the concentrated solution, wherein the adding amount of the active carbon is 2.9kg, heating to 64 ℃, stirring for 4 hours, filtering, adding 5.8L of purified water to wash filter cakes, wherein the volume of the filtrate is 29.5L, and sampling to detect that the concentration of the gentamicin is 231600u/ml to obtain 66.36 hundred million u of finished gentamicin sulfate solution.
3.3 spraying powder, and performing spray drying on the gentamicin sulfate finished product liquid through a spray tower under the conditions of air inlet temperature of 130 ℃, air outlet temperature of 85 ℃ and spray speed of 100L/h to obtain the gentamicin sulfate finished product.
3.4 assay data for the recovered gentamicin sulfate end product are shown in Table 6.
TABLE 6 test data for recovered gentamicin sulfate finished product
The recovered finished product of the gentamicin sulfate completely meets the standard of gentamicin sulfate in the 'Chinese pharmacopoeia' of 2015 edition.
Comparative example 1
The method for recycling the active carbon after the gentamycin sulfate is decolorized comprises the following specific steps:
1 heating and acid pickling
1.1 adding 500kg of wet activated carbon into a 5000L reaction kettle, adding 500L of water, adding 6kg of concentrated sulfuric acid with the mass concentration of 98%, stirring, heating to 65 ℃, stirring, keeping the temperature for 1 hour, and maintaining the pH value to be 1.
1.2, performing hot filtration, uniformly placing the pickling solution into a filter pressing box, starting the filter pressing box to stir vacuum seasonings for 5min, backflushing and uniformly stirring, closing vacuum, standing and soaking for 15min, performing filter pressing, and placing filtrate into a receiving tank for storage. Washing the filter cake twice with 500L of 65 ℃ purified water, and drying the filter cake with air to obtain the acid-washed active carbon.
2 heating alkaline washing
2.1 putting the activated carbon after acid washing into a 5 ton enamel reactor, adding 1000L water and 50kg sodium hydroxide, stirring, heating to 80 ℃ with steam, and keeping the temperature for 3 hours, wherein the pH value is 14.
2.2 discharging the feed liquid to a filter pressing box for hot filtration, and feeding the filtrate into an acid-base neutralization pond.
2.3 washing the filter cake with 500kg of hot water at 80 ℃ for three times, feeding the filtrate into an acid-base neutralization tank, and drying the washed filter cake with air to obtain the alkali-washed active carbon.
3 heating and pickling
3.1 adding the alkali-washed activated carbon into a 5000L reaction kettle, adding 1500L water and 12kg of concentrated sulfuric acid with the mass concentration of 98%, stirring and heating to 65 ℃, stirring and preserving heat for 1 hour, maintaining the pH value to be 2, uniformly putting the pickling solution into a filter pressing box for filter pressing, and putting the filtrate into a receiving tank for storage.
3.2 adding 1000L of purified water into a 5000L reaction kettle, heating to 65 ℃, respectively washing the filter cake twice with 500L of purified water at 65 ℃, placing the filtrate into a receiving tank for storage, and drying the filter cake by air.
3.3 the filter cake is put into an oven and dried for 6 hours at 100 ℃ to obtain the regenerated active carbon.
4 recovering gentamicin sulfate in the filtrate
4.1 concentration, the acid wash filtrates are combined, concentrated by a membrane concentrator and concentrated to 1/10 of the original volume.
And 4.2, decoloring, namely adding active carbon into the concentrated solution, wherein the adding amount of the active carbon is 2.9kg, heating to 65 ℃, stirring for 4 hours, filtering, and adding 5.8L of purified water to wash the filter cake.
4.3 spraying powder, and performing spray drying on the gentamicin sulfate finished product liquid through a spray tower under the conditions of air inlet temperature of 130 ℃, air outlet temperature of 85 ℃ and spray speed of 100L/h to obtain the gentamicin sulfate finished product.
Comparative example 2
The method for recycling the active carbon after the gentamycin sulfate is decolorized comprises the following specific steps:
1 heating and acid pickling
1.1 adding 500kg of wet activated carbon into a 5000L reaction kettle, adding 500L of water, adding 6kg of concentrated sulfuric acid with the mass concentration of 98%, stirring, heating to 65 ℃, stirring, keeping the temperature for 1 hour, and maintaining the pH value to be 1.
1.2, performing thermal filtration, uniformly placing the pickle liquor into a filter pressing box, starting the filter pressing box to stir vacuum seasonings for 5min, backflushing and uniformly stirring, turning off vacuum, standing and soaking for 15min, performing filter pressing, and placing the filtrate into a receiving tank for storage; adding the filtered activated carbon filter cake into a 5000L reaction kettle, adding 12kg of 1500L water and 98% concentrated sulfuric acid, stirring, heating to 65 ℃, stirring, keeping the temperature for 1 hour, keeping the pH value at 2, uniformly putting the pickling solution into a filter pressing box, performing filter pressing, and putting the filtrate into a receiving tank for storage.
1.3 adding 1000L of purified water into a 5000L reaction kettle, heating to 65 ℃, respectively washing a filter cake twice with 500L of purified water at 65 ℃, placing the filtrate into a receiving tank for storage, and drying the filter cake by air.
1.4 the filter cake is put into an oven and dried for 6 hours at 100 ℃ to obtain the acid-washed active carbon.
2 heating alkaline washing
2.1 putting the activated carbon after acid washing into a 5 ton enamel reactor, adding 1000L water and 50kg sodium hydroxide, stirring, heating to 80 ℃ with steam, and keeping the temperature for 3 hours, wherein the pH value is 14.
2.2 discharging the feed liquid to a filter pressing box for hot filtration, and feeding the filtrate into an acid-base neutralization pond.
2.3 washing the filter cake with 500kg of hot water at 80 ℃ for three times, feeding the filtrate into an acid-base neutralization tank, and drying the washed filter cake by air to obtain the regenerated activated carbon.
3 recovering gentamicin sulfate in the filtrate
3.1 concentration, combining the acid washing filtrates, concentrating by a membrane concentrator, and concentrating to 1/10 of the original volume.
3.2, decoloring, adding active carbon into the concentrated solution, wherein the adding amount of the active carbon is 2.9kg, heating to 65 ℃, stirring for 4 hours, filtering, adding 5.8L of purified water, and washing the filter cake.
3.3 spraying powder, and performing spray drying on the gentamicin sulfate finished product liquid through a spray tower under the conditions of air inlet temperature of 130 ℃, air outlet temperature of 85 ℃ and spray speed of 100L/h to obtain the gentamicin sulfate finished product.
Test examples
The test data of the regenerated activated carbon obtained in example 1, the regenerated activated carbon obtained in comparative example 1 and the regenerated activated carbon obtained in comparative example 2 are compared with the test data of the finished product of gentamicin sulfate, and the test data are shown in tables 7 and 8.
TABLE 7 regenerated activated char assay data
TABLE 8 Gentamicin sulfate assay data
The treatment steps of example 1 are alkali washing → acid washing, the treatment steps of comparative example 1 are acid washing → alkali washing → acid washing, and the treatment steps of comparative example 2 are acid washing → alkali washing, and it can be seen from tables 7 and 8 that gentamicin sulfate recovered in comparative example 1 and comparative example 2 has high impurity content and is unqualified, and the recovered activated carbon has high pH value and high ash content and is unqualified compared with example 1.
Although the present invention has been described with reference to the specific embodiments, it is not intended to limit the scope of the present invention, and various modifications and variations can be made by those skilled in the art without inventive changes based on the technical solution of the present invention.
Claims (8)
1. The method for recycling the activated carbon after the gentamicin sulfate is decolorized is characterized by comprising the following specific steps of:
(1) firstly, heating and alkali washing waste activated carbon decolorized by gentamicin sulfate at 80-85 ℃, filtering while hot, feeding the obtained filtrate I into an acid-base neutralization tank, washing and drying the obtained filter cake I, and then feeding into the step (2);
(2) heating and acid washing at 60-65 ℃, filtering while hot, and allowing the obtained filtrate II to enter the step (4) and the obtained filter cake II to enter the step (3);
(3) heating and acid washing at 60-65 ℃, filtering while hot, washing and drying the obtained filter cake III to obtain regenerated activated carbon, and allowing the obtained filtrate III to enter the step (4);
(4) mixing the filtrate II and the filtrate III, and concentrating, decolorizing and spraying to obtain gentamicin sulfate powder;
in the step (1), the specific method for heating and alkali washing comprises the following steps: stirring and mixing the waste activated carbon, water and sodium hydroxide, heating and stirring for 3 hours, and maintaining the pH value to be 13-14; wherein the mass ratio of the waste activated carbon to the water to the sodium hydroxide is 10: 20: 1;
in the step (2), the specific method for heating and pickling comprises the following steps: stirring and mixing the filter cake I with water and concentrated sulfuric acid with the mass concentration of 98%, heating and stirring for 1 hour, and maintaining the pH value to be 1-2; wherein the mass ratio of the waste activated carbon to the water to the concentrated sulfuric acid is 250: 250: 3.
2. the method according to claim 1, wherein in the step (1), the specific method for washing and drying is as follows: and (3) leaching with hot water of 80-85 ℃ for three times, wherein the weight of the hot water used in each leaching is the same as that of the waste activated carbon, and blowing the waste activated carbon with air after the three leaching is completed.
3. The method according to claim 1, wherein in the step (3), the specific method for heating and pickling is as follows: stirring and mixing the filter cake II with water and concentrated sulfuric acid with the mass concentration of 98%, stirring and heating for 1 hour, and maintaining the pH value to be 2-3; wherein the mass ratio of the waste activated carbon to the water to the concentrated sulfuric acid is 125: 375: 3.
4. the method according to claim 1, wherein in the step (3), the specific method of the washing and drying treatment is as follows: leaching the filter cake III with hot water of 60-65 ℃ twice, wherein the weight of the hot water used in each leaching is the same as that of the waste activated carbon, blowing the filter cake III with air after the leaching of the two times is completed, transferring the filter cake III into an oven, and drying the filter cake III for 6 hours at 100-105 ℃ to obtain the regenerated activated carbon.
5. The method of claim 1, wherein the specific method of step (4) is as follows:
(4-1) concentration: combining the filtrate II and the filtrate III, and concentrating to obtain gentamicin sulfate concentrated solution;
(4-2) decoloring: decolorizing with active carbon to obtain gentamycin sulfate finished product liquid;
(4-3) powder spraying: and finally, carrying out spray drying on the gentamicin sulfate finished product liquid to obtain a gentamicin sulfate finished product.
6. The method according to claim 5, wherein the specific method of step (4-1) is: and combining the filtrate II and the filtrate III, concentrating the mixture by using a film concentrator to 1/100 of the original volume to obtain a gentamicin sulfate concentrated solution.
7. The method according to claim 5, wherein the specific method of step (4-2) is: adding 0.1 weight of activated carbon into the concentrated solution, heating to 60-65 ℃, stirring for 4 hours, filtering to obtain a filtrate IV and a filter cake IV, washing the filter cake IV with 2 weight times of purified water of the activated carbon to obtain a washing solution, and combining the filtrate IV and the washing solution to obtain a finished product gentamicin sulfate solution.
8. The method according to claim 5, wherein in the step (4-3), the spray drying process conditions are as follows: the air inlet temperature is 130 ℃, the air outlet temperature is 85 ℃, and the spraying speed is 100L/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010160280.8A CN111233953B (en) | 2020-03-10 | 2020-03-10 | Method for recycling activated carbon after gentamycin sulfate decoloration |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010160280.8A CN111233953B (en) | 2020-03-10 | 2020-03-10 | Method for recycling activated carbon after gentamycin sulfate decoloration |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111233953A CN111233953A (en) | 2020-06-05 |
| CN111233953B true CN111233953B (en) | 2021-04-20 |
Family
ID=70877012
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010160280.8A Active CN111233953B (en) | 2020-03-10 | 2020-03-10 | Method for recycling activated carbon after gentamycin sulfate decoloration |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111233953B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648982A (en) * | 2009-09-22 | 2010-02-17 | 南阳普康药业有限公司 | Method for recycling gentamicin from waste active carbon generated by discoloring gentamycin sulfate |
| CN101659684A (en) * | 2009-09-22 | 2010-03-03 | 南阳普康药业有限公司 | Method for recovering lincomycin from waste active carbon decolorized by lincomycin |
| CN102241712A (en) * | 2011-05-23 | 2011-11-16 | 南阳普康药业有限公司 | Decolorizing method for gentamicin sulfate production |
| CN106807342A (en) * | 2017-03-15 | 2017-06-09 | 广州同胜环保科技有限公司 | Regenerating active carbon system and method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0278697A (en) * | 1988-09-12 | 1990-03-19 | Agency Of Ind Science & Technol | Regeneration of oxidation type coenzyme |
-
2020
- 2020-03-10 CN CN202010160280.8A patent/CN111233953B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648982A (en) * | 2009-09-22 | 2010-02-17 | 南阳普康药业有限公司 | Method for recycling gentamicin from waste active carbon generated by discoloring gentamycin sulfate |
| CN101659684A (en) * | 2009-09-22 | 2010-03-03 | 南阳普康药业有限公司 | Method for recovering lincomycin from waste active carbon decolorized by lincomycin |
| CN102241712A (en) * | 2011-05-23 | 2011-11-16 | 南阳普康药业有限公司 | Decolorizing method for gentamicin sulfate production |
| CN106807342A (en) * | 2017-03-15 | 2017-06-09 | 广州同胜环保科技有限公司 | Regenerating active carbon system and method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111233953A (en) | 2020-06-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11555049B2 (en) | Method for separation and purification of n-acetylglucosamine | |
| CN106831895B (en) | A method of purifying N-acetylglucosamine | |
| CN109593034B (en) | Method for preparing shikimic acid from ginkgo leaf extraction waste liquid | |
| CN107513030B (en) | Method for separating and purifying L-hydroxyproline from L-hydroxyproline fermentation liquor | |
| CN106366136A (en) | Sialic acid, and preparation method and application thereof | |
| CN101486637A (en) | Method for extracting amber acid from fermentation liquor | |
| CN106631852A (en) | Method for extracting L-ornithine hydrochloride from L-ornithine fermentation broth | |
| CN106831894B (en) | A kind of method of deacetylation Coupling Adsorption separation D-Glucosamine Hydrochloride | |
| US20230167474A1 (en) | Methods for enzymatic production of glucosamine salts and the purification methods thereof | |
| CN101781190B (en) | Method for extracting refined citric acid from citric acid fermentation liquid | |
| CN110846368B (en) | Clean extraction process for producing chondroitin and co-producing high-quality type II collagen from pig and ox nasal bones | |
| CN103087126A (en) | Preparation method of zhongshengmycin bulk drug | |
| CN101701069B (en) | Method for extracting epsilon-polylysine and salt thereof | |
| CN111233953B (en) | Method for recycling activated carbon after gentamycin sulfate decoloration | |
| CN106928288B (en) | A kind of preparation method of dihydrostreptomycin sulfate | |
| CN103420826A (en) | Method for extracting succinic acid from fermentation broth | |
| CN101942039A (en) | Parnaparin production method | |
| CN102618610A (en) | Preparation method of sericin compound amino acid | |
| CN112409426B (en) | Preparation method of sisomicin sulfate | |
| CN104610385A (en) | Refining method of D-glucosamine hydrochloride | |
| CN112662714B (en) | Production process for preparing ornithine | |
| CN103626838A (en) | Removal method of endotoxin in N-(2)-L-alanyl-L-glutamine active pharmaceutical ingredient | |
| CN102250220B (en) | Preparation method of colistin sulphate | |
| CN112390806A (en) | Method for improving extraction yield of spectinomycin | |
| CN113045610A (en) | Method for extracting glucosamine from N-acetylglucosamine fermentation liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |