CN112794536A - Penicillin waste acid water treatment method and recycling method thereof - Google Patents
Penicillin waste acid water treatment method and recycling method thereof Download PDFInfo
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- CN112794536A CN112794536A CN202011521273.2A CN202011521273A CN112794536A CN 112794536 A CN112794536 A CN 112794536A CN 202011521273 A CN202011521273 A CN 202011521273A CN 112794536 A CN112794536 A CN 112794536A
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- acid water
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002253 acid Substances 0.000 title claims abstract description 56
- 239000002699 waste material Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 40
- 229930182555 Penicillin Natural products 0.000 title claims abstract description 31
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 title claims abstract description 31
- 229940049954 penicillin Drugs 0.000 title claims abstract description 31
- 238000004064 recycling Methods 0.000 title claims abstract description 11
- 239000012528 membrane Substances 0.000 claims abstract description 46
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 44
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 claims abstract description 23
- 238000000502 dialysis Methods 0.000 claims abstract description 19
- 150000003839 salts Chemical class 0.000 claims abstract description 17
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 238000011033 desalting Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims description 18
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 9
- 235000011152 sodium sulphate Nutrition 0.000 claims description 9
- 238000000855 fermentation Methods 0.000 claims description 6
- 230000004151 fermentation Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical group CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000012466 permeate Substances 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 11
- 238000004065 wastewater treatment Methods 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- -1 i.e. Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/041—Treatment of water, waste water, or sewage by heating by distillation or evaporation by means of vapour compression
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- C02F1/02—Treatment of water, waste water, or sewage by heating
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- C02F1/048—Purification of waste water by evaporation
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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Abstract
The invention belongs to the technical field of pharmaceutical wastewater treatment, and particularly relates to a penicillin waste acid water treatment method and a recycling method thereof. Aiming at the problem that the treatment of the waste acid water in the penicillin production process is difficult in the prior art, the invention provides a penicillin waste acid water treatment method, which comprises the following steps: (1) sending into an ultrafiltration membrane group for treatment, concentrating by at least 8-12 times to obtain concentrated solution and dialysate, and sending the concentrated solution into a biochemical system for treatment; (2) feeding the dialysate into a reverse osmosis membrane group, and concentrating by 3-5 times to obtain reverse osmosis membrane concentrated solution and reverse osmosis dialysis water; (3) evaporating and desalting the reverse osmosis membrane concentrated solution by adopting MVR; (4) the reverse osmosis dialysis water is recycled as the water for the production process. The invention also provides salt and reverse osmosis dialysis water obtained in the treatment process. The invention can reduce the pressure of the biochemical system for treating the wastewater, recover a large amount of process water and salt, effectively reduce the production cost of the penicillin and has high application value.
Description
Technical Field
The invention belongs to the technical field of pharmaceutical wastewater treatment, and particularly relates to a penicillin waste acid water treatment method and a recycling method thereof.
Background
In the prior art, the production of natural penicillin usually adopts a method of strain fermentation and then extraction. In the extraction process of penicillin, the pH of the filtrate of the fermentation broth needs to be adjusted to 2-2.5 for extraction, and the raffinate of the extracted fermentation broth is the waste acid water. In the production of penicillin, a large amount of waste acid water is generated, and the waste acid water contains a large amount of acid, salt and organic matters, wherein the organic matters are treated by oxidation treatment in a biochemical system (such as an anaerobic tank and the like).
The biochemical system is a sewage treatment method which mixes and contacts the waste water or solid waste with microorganisms, decomposes organic matters and certain inorganic poisons (such as cyanides, sulfides and the like) in the waste water by utilizing the biochemical action in the microorganisms and converts unstable organic matters and inorganic poisons into nontoxic substances. The process of the method is dependent on the microorganisms in the system. If the treatment capacity of the wastewater is large and the differences between the pH value, the salt content and the like of the wastewater and the biochemical system are large, the microbial activity is reduced, the biochemical system is abnormal, and the burden of the biochemical system is increased. Thereby causing low wastewater treatment efficiency of a biochemical system or weakening the effect of reducing COD of the wastewater.
There is currently little research into how the waste acid water produced in penicillin production can be better handled. Chinese patent CN1696102A discloses a method and equipment for separating butyl acetate from waste acid water of penicillin fermentation liquor raffinate waste water. However, the problem of high acid and salt content in the wastewater is not solved after the treatment by the method. The waste acid water can not be avoided to burden the biochemical system.
Disclosure of Invention
Aiming at the problem that the treatment of the waste acid water in the penicillin production process is difficult in the prior art, the invention provides a penicillin waste acid water treatment method and salt and reverse osmosis dialysis water obtained in the treatment process, and the invention aims to: a large amount of water and salt which can be recycled in the production process are separated from the waste acid water, so that the amount of wastewater entering a biochemical system for treatment is greatly reduced, the treatment burden of the biochemical system is reduced, and the production cost is reduced.
A method for treating penicillin waste acid water comprises the following steps:
(1) sending the waste acid water with the solvent removed or without the solvent removed into an ultrafiltration membrane group for treatment, wherein the solvent is butyl ester, the cut-off molecular weight of an ultrafiltration membrane in the ultrafiltration membrane group is 5000-10000 Dalton, and the concentration is 8-12 times to obtain concentrated solution and dialysate, and the concentrated solution is sent into a biochemical system for treatment;
(2) feeding the dialysate into a reverse osmosis membrane group, and concentrating by 3-5 times to obtain reverse osmosis membrane concentrated solution and reverse osmosis dialysis water;
(3) evaporating and desalting the reverse osmosis membrane concentrated solution obtained in the step (2) by adopting MVR (mechanical vapor recompression) to obtain a mixture of salt and water;
(4) and (3) recycling the reverse osmosis dialysis water obtained in the step (2) as water for the production process and/or clean water.
Preferably, the waste acid water without solvent removal is raffinate obtained by extracting a filtrate of a fermentation broth in a production process of natural penicillin after adjusting the pH to 2-2.5;
and/or, the waste acid water after solvent removal is obtained by the following method: adjusting the pH value to 4.5-5.5 with alkali liquor, and distilling the waste acid water without solvent;
and/or the indexes of the waste acid water after solvent removal are as follows: the conductance is more than or equal to 15000us/cm, the COD is more than or equal to 10000mg/L, and the pH is 4.5-5.5;
preferably, the operating pressure of the ultrafiltration membrane module in step (1) is 10-30bar, preferably 15-20bar, and further preferably 20 bar;
and/or the reverse osmosis membrane module in the step (2) is operated at the pressure of 70-120bar, preferably 90 bar.
Preferably, the ultrafiltration membranes in the ultrafiltration membrane module in step (1) have a molecular weight cut-off of 8000 dalton.
Preferably, the temperature of the ultrafiltration membrane group in the step (1) is 20-40 ℃, and preferably 30 ℃;
and/or the temperature of the reverse osmosis membrane group in the step (2) is 20-40 ℃, and preferably 30 ℃.
Preferably, the MVR in step (3) is evaporated to remove salt to obtain a mixture of sodium sulfate and water, and the sodium sulfate in the mixture is recycled.
The invention also provides the salt obtained in the step (3) in the penicillin waste acid water treatment method.
Preferably, the salt is sodium sulfate.
Preferably, the reverse osmosis dialysis water is obtained by a penicillin waste acid water treatment method.
Preferably, the index satisfies the following condition: the conductivity is less than 500 us/cm; COD is less than 400 mg/L; the chloride ion is less than 20 mg/L; the ammonia nitrogen is less than 300 mg/L; sulfate is less than 300 mg/L; the pH value is 4.5-5.5;
and/or the reverse osmosis dialysis water is used for preparing acid and alkali, washing a tower or used as clean water.
By adopting the technical scheme of the invention, 60-70% of water in the penicillin waste acid water can be recycled into production process water, and part of inorganic salt can be recycled; the water entering the biochemical system for treatment is not more than 10 percent, the treatment capacity of the wastewater can be obviously reduced, the treatment pressure of the biochemical system is reduced, and the production cost is reduced. The invention is economical and environment-friendly, and has strong practical application value.
In addition, the present invention prefers the molecular weight cut-off of the ultrafiltration membrane module. In the experimental process, the trapped protein with the trapped molecular weight higher than 10000 Dalton is too little, and the membrane system in the subsequent process is polluted. If the molecular weight cut-off of 5000 daltons is selected to improve the water quality, the investment cost is increased. The limited range of the invention can effectively cut off the molecular weight to meet the requirement of process water and meet the production requirement and reduce the production cost.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 is a comparison of water before and after treatment according to an embodiment of the present invention, in which waste acid water before treatment, reverse osmosis dialyzed water after treatment, and a concentrated solution after ultrafiltration are sequentially provided from left to right.
Detailed Description
Example 1
The treatment procedure of the waste acid water generated in penicillin production in this example is as follows:
1. distilling the waste acid water to remove a solvent; the solvent is butyl ester.
2. Feeding waste acid water into an ultrafiltration membrane group for treatment, wherein the operating pressure of the ultrafiltration membrane group is 20bar, the temperature is 40 ℃, the cut-off molecular weight of an ultrafiltration membrane in the ultrafiltration membrane group is 8000 daltons, concentrating by at least 8-12 times to obtain concentrated solution and dialysate, and feeding the concentrated solution into a biochemical system for treatment;
3. feeding the dialysate into a reverse osmosis membrane group, wherein the operating pressure of the reverse osmosis membrane group is 90bar, the temperature is 40 ℃, and the concentration is 3-5 times to obtain reverse osmosis membrane concentrated solution and reverse osmosis dialysis water;
4. the reverse osmosis membrane concentrated solution obtained in the step 3 is desalted by MVR evaporation, and the obtained sodium sulfate can be recycled;
5. and 3, recycling the reverse osmosis dialysis water obtained in the step 3 as production process water.
FIG. 1 is a graph showing a comparison of three groups of sample water, i.e., waste acid water before treatment, reverse osmosis dialyzed water after treatment and concentrated solution after ultrafiltration, and it can be seen that the reverse osmosis dialyzed water after treatment is clear and transparent, and the concentrated solution is darker in color than the waste acid water before treatment.
The following table shows the test results of various indexes before and after the treatment of the waste acid water generated in the penicillin production of three batches of raw materials:
TABLE 1 indexes before and after treatment of three batches of waste acid water
As can be seen from the above table, the concentrated solution obtained by ultrafiltration has higher indexes relative to the waste acid water; and all indexes of the treated reverse osmosis dialysis water are obviously reduced, and the treated reverse osmosis dialysis water reaches the recycling standard. Therefore, the method of the invention can concentrate the organic matters, salts and the like to be treated in the concentrated solution for further treatment, and the volume of the concentrated solution is greatly reduced compared with the volume of the waste acid water, so that the pressure generated to a biochemical system in the biochemical treatment process can be obviously reduced.
Example 2
The treatment procedure of the waste acid water generated in penicillin production in this example is as follows:
1. distilling the waste acid water to remove a solvent; the solvent is butyl ester.
2. Feeding waste acid water into an ultrafiltration membrane group for treatment, wherein the operating pressure of the ultrafiltration membrane group is 40bar, the temperature is 40 ℃, the cut-off molecular weight of an ultrafiltration membrane in the ultrafiltration membrane group is 10000 daltons, concentrating by at least 8-12 times to obtain concentrated solution and dialysate, and feeding the concentrated solution into a biochemical system for treatment;
3. feeding the dialysate into a reverse osmosis membrane group, wherein the operating pressure of the reverse osmosis membrane group is 60bar, the temperature is 40 ℃, and the concentration is 3-5 times to obtain reverse osmosis membrane concentrated solution and reverse osmosis dialysis water;
4. the reverse osmosis membrane concentrated solution obtained in the step 3 is desalted by MVR evaporation, and the obtained sodium sulfate can be recycled;
5. and 3, recycling the reverse osmosis dialysis water obtained in the step 3 as production process water.
From the examples 1-2, it can be seen that the technical scheme provided by the invention can effectively reduce the amount of wastewater (concentrated solution) sent to a biochemical system for treatment, and each index of a large amount of treated reverse osmosis dialysis water can reach the standard of recycling process water, and in addition, inorganic salts such as sodium sulfate and the like can be recovered for utilization. The scheme of this application has reduced waste water treatment's pressure, has practiced thrift the cost of production, has very high application potential.
Claims (10)
1. A penicillin waste acid water treatment method is characterized by comprising the following steps:
(1) sending the waste acid water with the solvent removed or without the solvent removed into an ultrafiltration membrane group for treatment, wherein the solvent is butyl ester, the cut-off molecular weight of an ultrafiltration membrane in the ultrafiltration membrane group is 5000-10000 Dalton, and the concentration is 8-12 times to obtain concentrated solution and dialysate, and the concentrated solution is sent into a biochemical system for treatment;
(2) feeding the dialysate into a reverse osmosis membrane group, and concentrating by 3-5 times to obtain reverse osmosis membrane concentrated solution and reverse osmosis dialysis water;
(3) evaporating and desalting the reverse osmosis membrane concentrated solution obtained in the step (2) by adopting MVR (mechanical vapor recompression) to obtain a mixture of salt and water;
(4) and (3) recycling the reverse osmosis dialysis water obtained in the step (2) as water for the production process and/or clean water.
2. The method for treating penicillin waste acid water as claimed in claim 1, wherein:
the waste acid water without solvent removal is raffinate obtained by extracting filtrate of fermentation liquor in the production process of natural penicillin after adjusting the pH to 2-2.5;
and/or, the waste acid water after solvent removal is obtained by the following method: adjusting the pH value to 4.5-5.5 with alkali liquor, and distilling the waste acid water without solvent;
and/or the indexes of the waste acid water after solvent removal are as follows: the conductance is more than or equal to 15000us/cm, the COD is more than or equal to 10000mg/L, and the pH is 4.5-5.5.
3. The method for treating penicillin waste acid water as claimed in claim 1, wherein: the operating pressure of the ultrafiltration membrane module in the step (1) is 10-30bar, preferably 15-20bar, and further preferably 20 bar;
and/or the reverse osmosis membrane module in the step (2) is operated at the pressure of 70-120bar, preferably 90 bar.
4. The method for treating penicillin waste acid water as claimed in claim 1, wherein: the molecular weight cut-off of the ultrafiltration membrane in the ultrafiltration membrane group in the step (1) is 8000 daltons.
5. The method for treating penicillin waste acid water as claimed in claim 1, wherein: the temperature of the ultrafiltration membrane group in the step (1) is 20-40 ℃, and preferably 30 ℃;
and/or the temperature of the reverse osmosis membrane group in the step (2) is 20-40 ℃, and preferably 30 ℃.
6. The method for treating penicillin waste acid water as claimed in claim 1, wherein: and (4) evaporating and desalting the MVR in the step (3) to obtain a mixture of sodium sulfate and water, and recycling the sodium sulfate in the mixture.
7. The salt obtained in step (3) of the acid water treatment method for penicillin waste acid as claimed in any one of claims 1 to 6.
8. The salt of claim 7, wherein: the salt is sodium sulfate.
9. A reverse osmosis permeate obtained from the process for the acid water treatment of penicillin waste acid as claimed in any one of claims 1 to 6.
10. A reverse osmosis dialysis water according to claim 9 wherein: the indexes meet the following conditions: the conductivity is less than 500 us/cm; COD is less than 400 mg/L; the chloride ion is less than 20 mg/L; the ammonia nitrogen is less than 300 mg/L; sulfate is less than 300 mg/L; the pH value is 4.5-5.5;
and/or the reverse osmosis dialysis water is used for preparing acid and alkali, washing a tower or used as clean water.
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