CN112429867B - Treatment method of sulbactam acid wastewater - Google Patents
Treatment method of sulbactam acid wastewater Download PDFInfo
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- CN112429867B CN112429867B CN202011165360.9A CN202011165360A CN112429867B CN 112429867 B CN112429867 B CN 112429867B CN 202011165360 A CN202011165360 A CN 202011165360A CN 112429867 B CN112429867 B CN 112429867B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/09—Bromine; Hydrogen bromide
- C01B7/096—Bromine
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- C—CHEMISTRY; METALLURGY
- 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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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The invention particularly relates to a treatment method of sulbactam acid wastewater, belonging to the technical field of pharmaceutical wastewater treatment. The invention comprises the following steps: (1) heating the reaction wastewater for synthesizing 6-bromopenicillanic acid, dropwise adding concentrated sulfuric acid, removing the generated gas to a falling film absorber for absorption treatment, adjusting the pH value of the residual mother liquor to be 7, and concentrating to obtain sodium sulfate; (2) adding potassium permanganate into the reaction wastewater for synthesizing the 6-bromopenicillanic sulfone acid, adjusting the pH value to 7 after the reaction is finished, filtering to obtain manganese dioxide, concentrating the residual mother liquor under reduced pressure, precipitating potassium sulfate, centrifuging, and continuously concentrating the residual mother liquor under reduced pressure to obtain sodium sulfate; (3) and (3) dropwise adding hydrogen peroxide into the sulbactam acid synthesis reaction wastewater, simultaneously heating and introducing nitrogen, condensing to obtain liquid bromine, reacting for synthesizing 6-bromopenicillanic acid, cooling and filtering the residual mother liquor to obtain zinc hydroxide solid. The method is simple and easy to implement, reduces the sewage treatment pressure, reduces the sewage treatment cost, and has better environmental protection benefit.
Description
Technical Field
The invention particularly relates to a treatment method of sulbactam acid wastewater, belonging to the technical field of pharmaceutical wastewater treatment.
Background
Sulbactam acid (sulbactam), the chemical name of which is (2S, 5R) -3, 3-dimethyl-7-oxo-4-thiabicyclo [3,2,0] heptane-2-2 carboxylic acid-4, 4-dioxide compound, is a white-like or light yellow crystalline powder which is easily soluble in water, alcohol and ester and is difficult to dissolve in ether.
Sulbactam acid is a semisynthetic broad-spectrum competitive irreversible beta-lactamase inhibitor, because of long-term use of a large amount of cephalosporins and penicillins, the beta-lactamase generates antibiotic resistance, and the sulbactam acid is combined with beta-lactam antibiotic medicines such as penicillins or cephalosporins, so that the problem of antibiotic resistance is solved, an excellent synergistic effect is embodied, the antibacterial activity of the two is greatly improved, the antibacterial spectrum is expanded, and the sulbactam acid is widely applied to medicines in recent years.
The traditional synthesis process of sulbactam acid usually takes 6-aminopenicillanic acid as a starting material, and the sulbactam acid is prepared by diazotization reaction with sodium nitrite under an acidic condition, then dibromination reaction with bromine to synthesize 6-bromine penicillanic acid, oxidation with potassium permanganate to synthesize 6-bromine penicillanic sulfone acid, and finally reduction with metal powder zinc powder. A large amount of strong acid wastewater and high salt wastewater are generated in the sulbactam acid production, the wastewater treatment cost is high, the treatment difficulty is high, the environmental protection pressure is high, the wastewater is combined in the production, and then the activated sludge method is adopted for water treatment. The activated sludge method needs to continuously culture the activated sludge, and the load of the organic matters in the inlet water is not too high; in order to achieve a certain decontamination capability, the aeration tank needs to have large volume, occupy more land and have high capital construction cost; the aerobic rate varies along the length of the tank, and the oxygen supply rate is difficult to match with the aerobic rate, thereby affecting the treatment effect.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, provides a sulbactam acid wastewater treatment method, is simple and easy to implement, reduces the wastewater treatment pressure, reduces the wastewater treatment cost, and has better environmental protection benefit.
The treatment method of sulbactam acid wastewater comprises the following steps:
(1) heating the reaction wastewater for synthesizing 6-bromopenicillanic acid to 45-50 ℃, dropwise adding 98 wt% concentrated sulfuric acid, removing the generated gas to a falling film absorber for absorption treatment, wherein liquid alkali is added into the water phase of the falling film absorber for absorption treatment, adding sodium hydroxide into the residual mother liquor to adjust the pH value to 7, then concentrating to obtain pure sodium sulfate, and evaporating a water jacket for the next production;
(2) adding potassium permanganate into the reaction wastewater for synthesizing the 6-bromopenicillanic sulfone acid, after the reaction is finished, adding sodium hydroxide to adjust the pH value to be 7, filtering to obtain manganese dioxide, concentrating the residual mother liquor under reduced pressure, precipitating potassium sulfate, centrifuging, continuously concentrating the residual mother liquor under reduced pressure to obtain sodium sulfate, and steaming out a water jacket for the next production;
(3) dropwise adding hydrogen peroxide into the sulbactam acid synthesis reaction wastewater, simultaneously heating to 60-65 ℃, introducing nitrogen, taking out generated bromine, condensing to obtain liquid bromine, reacting to synthesize 6-bromopenicillanic acid, cooling the residual mother liquor to 5-10 ℃, filtering to obtain zinc hydroxide solid, and treating the residual low-salt wastewater with sewage.
The reaction wastewater for synthesizing 6-bromopenicillanic acid contains water, sodium sulfate, sodium nitrite and sulfuric acid.
In the step (1), the generated gas is nitric oxide and nitrogen dioxide.
The reaction waste water for synthesizing 6-bromine penicillanic sulfone acid contains sodium sulfate, manganese sulfate, potassium sulfate, water and sulfuric acid.
In the step (2), the pressure of the reduced pressure concentration is-0.09 MPa to-0.095 MPa, and the temperature of the reduced pressure concentration is 45 ℃ to 50 ℃.
The waste water from the sulbactam acid synthesis reaction contains zinc bromide, water and a small amount of 6-bromine penicillanic sulfone acid.
In the step (3), the mass concentration of the hydrogen peroxide is 25%.
In the step (3), the residual low-salt wastewater contains water, a small amount of zinc hydroxide and a small amount of 6-bromine penicillanic sulfone acid.
Compared with the prior art, the invention has the following beneficial effects:
(1) the mixed salt in the reaction wastewater for synthesizing the 6-bromopenicillanic acid is changed into single salt to obtain pure sodium sulfate, and the distilled water jacket is used for the next batch of production, so that the wastewater discharge amount is reduced, and the environmental protection pressure is relieved;
(2) mixed salt in the reaction wastewater for synthesizing the 6-bromopenicillanic sulfone acid is respectively extracted, so that the benefit maximization of a byproduct is realized, and the evaporation water jacket is used for the next batch of production, so that the wastewater discharge is reduced, and the environmental protection pressure is relieved;
(3) salt in the sulbactam acid synthesis reaction wastewater is extracted, and the residual low-salt wastewater is subjected to sewage treatment, so that the sewage treatment pressure is reduced, and the sewage treatment cost is reduced (according to the current production scale, about 500 plus 600 ten thousand yuan is saved in one year);
(4) the liquid bromine separated from the sulbactam acid synthesis reaction wastewater is used for synthesizing 6-bromopenicillanic acid, so that the liquid bromine is recycled, the production investment cost is reduced (about 450 yuan is saved by 500 ten thousand yuan per year according to the current annual consumption of bromine), and the method has better economic benefit and environmental protection benefit.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
656g of synthetic 6-bromopenicillanic acid reaction wastewater (containing 550g of water, 65g of sodium sulfate, 5g of sodium nitrite and 36g of sulfuric acid) is heated to 50 ℃, 3.7g of 98% concentrated sulfuric acid is added dropwise, generated gas is absorbed by a falling film absorber, 29.4g of sodium hydroxide is added into the residual mother liquor to adjust the pH value to be 7, then the mixture is concentrated to obtain 122.2g of sodium sulfate, and 563g of water is evaporated.
1763g of reaction wastewater for synthesizing 6-bromine penicillanic sulfone acid (containing 40g of sodium sulfate, 146g of manganese sulfate, 84g of potassium sulfate, 1464g of water and 29g of sulfuric acid) is taken, 101.9g of potassium permanganate is added, 75.2g of sodium hydroxide is added after the reaction is finished to adjust the pH value to be 7, the manganese dioxide is obtained by filtration, the residual mother liquor is concentrated under reduced pressure (-0.095MPa), the temperature is controlled at 45 ℃, 140g of potassium sulfate is separated out firstly, the residual mother liquor is continuously concentrated under reduced pressure after centrifugation, 173.4g of sodium sulfate is obtained, and 1486g of water is evaporated.
2206g of synthetic sulbactam acid reaction wastewater (containing 191g of zinc bromide, 1986g of water and 29g of 6-bromopenicillanic sulphone acid) is taken, 115.4g of 25% hydrogen peroxide is added dropwise, the temperature is raised to 65 ℃, nitrogen is introduced, generated bromine is taken out, 135.8g of liquid bromine is obtained by condensation and used for synthesizing 6-bromopenicillanic acid reaction, the residual mother liquor is cooled to 5 ℃ and filtered to obtain 84g of zinc hydroxide solid, and the residual low-salt wastewater is subjected to sewage treatment.
Example 2
656g of synthetic 6-bromopenicillanic acid reaction wastewater (containing 550g of water, 65g of sodium sulfate, 5g of sodium nitrite and 36g of sulfuric acid) is heated to 45 ℃, 3.7g of 98% concentrated sulfuric acid is added dropwise, generated gas is absorbed by a falling film absorber, 29.4g of sodium hydroxide is added into the residual mother liquor to adjust the pH value to be 7, then the mixture is concentrated to obtain 122g of sodium sulfate, and 561g of water is evaporated.
1763g of reaction wastewater for synthesizing 6-bromine penicillanic sulfone acid (containing 40g of sodium sulfate, 146g of manganese sulfate, 84g of potassium sulfate, 1464g of water and 29g of sulfuric acid) is taken, 101.8g of potassium permanganate is added, after the reaction is finished, 75.1g of sodium hydroxide is added to adjust the pH value to be 7, the mixture is filtered to obtain 140g of manganese dioxide, the residual mother liquor is concentrated under reduced pressure (-0.09MPa), the temperature is controlled to be 50 ℃, 139g of potassium sulfate is separated out, after centrifugation, the residual mother liquor is continuously concentrated under reduced pressure to obtain 174g of sodium sulfate, and 1484g of water is evaporated.
2206g of synthetic sulbactam acid reaction wastewater (containing 191g of zinc bromide, 1986g of water and 29g of 6-bromine penicillanic sulfone acid) is taken, 115.8g of 25% hydrogen peroxide is added dropwise, the temperature is raised to 60 ℃, nitrogen is introduced, generated bromine is taken out, 135.5g of liquid bromine is obtained by condensation and used for synthesizing 6-bromine penicillanic acid reaction, the residual mother liquor is cooled to 10 ℃ and filtered to obtain 83g of zinc hydroxide solid, and the residual low-salt wastewater is subjected to sewage treatment.
Example 3
656g of synthetic 6-bromopenicillanic acid reaction wastewater (containing 550g of water, 65g of sodium sulfate, 5g of sodium nitrite and 36g of sulfuric acid) is heated to 48 ℃, 3.8g of 98% concentrated sulfuric acid is added dropwise, generated gas is absorbed by a falling film absorber, 29.6g of sodium hydroxide is added into the residual mother liquor to adjust the pH value to be 7, then the mixture is concentrated to obtain 123g of sodium sulfate, and 560g of water is distilled out.
1763g of reaction wastewater for synthesizing 6-bromine penicillanic sulfone acid (containing 40g of sodium sulfate, 146g of manganese sulfate, 84g of potassium sulfate, 1464g of water and 29g of sulfuric acid) is taken, 101.9g of potassium permanganate is added, 75.5g of sodium hydroxide is added after the reaction is finished to adjust the pH value to be 7, the manganese dioxide is obtained by filtration, the residual mother liquor is concentrated under reduced pressure (-0.092MPa), the temperature is controlled at 47 ℃, 139.70g of potassium sulfate is firstly separated out, the residual mother liquor is continuously concentrated under reduced pressure after centrifugation to obtain 174g of sodium sulfate, and 1480g of water is evaporated.
2206g of synthetic sulbactam acid reaction wastewater (containing 191g of zinc bromide, 1986g of water and 29g of 6-bromine penicillanic sulfone acid) is taken, 115.1g of 25% hydrogen peroxide is added dropwise, the temperature is raised to 64 ℃, nitrogen is introduced, generated bromine is taken out, 135g of liquid bromine is obtained by condensation and is used for synthesizing 6-bromine penicillanic acid for reaction, the residual mother liquor is cooled to 5 ℃ and filtered to obtain 83g of zinc hydroxide solid, and the residual low-salt wastewater is subjected to sewage treatment.
Comparative example 1
656g of synthetic 6-bromopenicillanic acid reaction wastewater (containing 550g of water, 65g of sodium sulfate, 5g of sodium nitrite and 36g of sulfuric acid) is taken, 3.7g of 98% concentrated sulfuric acid is dropwise added at room temperature, only a small amount of gas is generated, the generated gas is absorbed by a falling film absorber, the pH value of the residual mother liquor is adjusted to 7 by adding 32.2g of sodium hydroxide, and then the mixed salt is concentrated to obtain 126.6g of mixed salt, wherein 121.8g of sodium sulfate and 4.8g of sodium nitrite do not obtain single salt, the effect of purifying the salt is not achieved, and the experimental result is not ideal.
1763g of reaction wastewater (containing 40g of sodium sulfate, 146g of manganese sulfate, 84g of potassium sulfate, 1464g of water and 29g of sulfuric acid) for synthesizing 6-bromine penicillanic sulfone acid is added with 132g of 25 percent hydrogen peroxide, and solid manganese dioxide can not be generated under the acidic condition. 1763g of wastewater is taken, sodium hydroxide is added to adjust the pH value to 7, concentration is carried out under reduced pressure (-0.095MPa), the temperature is controlled at 45 ℃, 83.8g of potassium sulfate is separated out, the residual mother liquor is continuously concentrated under reduced pressure after centrifugation, 228g of mixed salt is obtained, 82g of sodium sulfate and 146g of manganese sulfate are not separated into single salt, and the experimental result is not ideal.
2206g of reaction wastewater for synthesizing sulbactam acid (containing 191g of zinc bromide, 1986g of water and 29g of 6-bromopenicillanic sulfone acid) is taken, 70g of chlorine gas is introduced, after the reaction is finished, nitrogen gas is introduced at room temperature to take out generated bromine, the bromine taking-out speed is too slow, the whole experiment time is prolonged, and the residual chlorine gas in the reaction needs to be subjected to post-treatment. The remaining mother liquor was concentrated under reduced pressure (-0.095MPa) to give 144.4g of a mixture, of which 115.4g of zinc chloride and 29g of organic matter failed to give a single zinc chloride, and the experimental results were not satisfactory.
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.
Claims (10)
1. A treatment method of sulbactam acid wastewater is characterized by comprising the following steps: the method comprises the following steps:
(1) heating the reaction wastewater for synthesizing 6-bromopenicillanic acid, dropwise adding 98 wt% concentrated sulfuric acid, removing the generated gas to a falling film absorber for absorption treatment, adding sodium hydroxide into the residual mother liquor to adjust the pH to 7, then concentrating to obtain pure sodium sulfate, and steaming out a water jacket for the next production;
(2) adding potassium permanganate into the reaction wastewater for synthesizing the 6-bromopenicillanic sulfone acid, after the reaction is finished, adding sodium hydroxide to adjust the pH value to be 7, filtering to obtain manganese dioxide, concentrating the residual mother liquor under reduced pressure, precipitating potassium sulfate, centrifuging, continuously concentrating the residual mother liquor under reduced pressure to obtain sodium sulfate, and steaming out a water jacket for the next production;
(3) dropwise adding hydrogen peroxide into the sulbactam acid synthesis reaction wastewater, simultaneously heating and introducing nitrogen, taking out generated bromine, condensing to obtain liquid bromine for synthesizing 6-bromopenicillanic acid, cooling and filtering the residual mother liquor to obtain zinc hydroxide solid, and treating the residual low-salt wastewater with sewage.
2. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: the reaction waste water for synthesizing 6-bromopenicillanic acid contains water, sodium sulfate, sodium nitrite and sulfuric acid.
3. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: in the step (1), the temperature is increased to 45-50 ℃.
4. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: the reaction waste water for synthesizing 6-bromine penicillanic sulfone acid contains sodium sulfate, manganese sulfate, potassium sulfate, water and sulfuric acid.
5. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: in the step (2), the pressure of the reduced pressure concentration is-0.09 MPa to-0.095 MPa, and the temperature of the reduced pressure concentration is 45 ℃ to 50 ℃.
6. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: the waste water from the sulbactam acid synthesis reaction contains zinc bromide, water and 6-bromine penicillanic sulfone acid.
7. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: in the step (3), the mass concentration of the hydrogen peroxide is 25%.
8. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: in the step (3), the temperature is raised to 60-65 ℃.
9. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: in the step (3), the temperature of the residual mother liquor is reduced to 5-10 ℃.
10. A method for treating sulbactam acid wastewater as claimed in claim 1, characterized in that: in the step (3), the residual low-salt wastewater contains water, zinc hydroxide and 6-bromine penicillanic sulfone acid.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525195A (en) * | 2009-03-24 | 2009-09-09 | 吴秀玲 | Method for treating profenofos synthetic wastewater by using hydrogen peroxide |
| CN102532164A (en) * | 2011-12-27 | 2012-07-04 | 山东鑫泉医药有限公司 | Synthesis method for sulbactam |
| US10773969B1 (en) * | 2016-12-12 | 2020-09-15 | Veolia Water Technologies, Inc. | Method for producing potassium sulfate and sodium chloride from wastewater |
| CN111808122A (en) * | 2020-07-20 | 2020-10-23 | 青岛科技大学 | Method for synthesizing sulbactam acid |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525195A (en) * | 2009-03-24 | 2009-09-09 | 吴秀玲 | Method for treating profenofos synthetic wastewater by using hydrogen peroxide |
| CN102532164A (en) * | 2011-12-27 | 2012-07-04 | 山东鑫泉医药有限公司 | Synthesis method for sulbactam |
| US10773969B1 (en) * | 2016-12-12 | 2020-09-15 | Veolia Water Technologies, Inc. | Method for producing potassium sulfate and sodium chloride from wastewater |
| CN111808122A (en) * | 2020-07-20 | 2020-10-23 | 青岛科技大学 | Method for synthesizing sulbactam acid |
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