CN111925062A - Combined treatment process for pharmaceutical intermediate production wastewater - Google Patents
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- C02F9/00—Multistage treatment of water, waste water or sewage
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C02F1/722—Oxidation by peroxides
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- 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
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
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- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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- C02F2209/10—Solids, e.g. total solids [TS], total suspended solids [TSS] or volatile solids [VS]
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
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- C02F3/28—Anaerobic digestion processes
- C02F3/2846—Anaerobic digestion processes using upflow anaerobic sludge blanket [UASB] reactors
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
Abstract
The invention discloses a combined treatment process of pharmaceutical intermediate production wastewater, which comprises the following steps: adding the wastewater produced in the pharmaceutical process into a Fenton reaction device, adjusting the pH, and adding Fe2+The solution is added with H after the temperature is stabilized2O2Adding the mixture into an iron-carbon micro-electrolysis reactor to carry out iron-carbon micro-electrolysis; B. hydrolysis and acidification: diluting the wastewater, adding the diluted wastewater into a hydrolysis acidification reactor, and controlling the inflow, the reflux and the ascending flow rate of a main reactor; C. UASB anaerobic treatment; D. inoculating and domesticating activated sludge in the SBR reactor; E. after the reaction is finished, the reactor is connected to a UASB reactor and then is connected in series for continuous operation. An aeration adjusting tank is additionally arranged between the SBR reactor and the UASB reactor, and water is discharged. The COD concentration is reduced by Fenton oxidation/iron carbon micro-electrolysis, hydrolytic acidification and UASB and SBR combined process, each part of the combined process is simpler and has deeper understanding on each part at present, the pretreatment raw material is easy to obtain and has low price,is more economical compared with other treatment methods.
Description
Technical Field
The invention belongs to the field of wastewater treatment, and particularly relates to a combined treatment process for medical intermediate production wastewater.
Background
With the rapid development of the pharmaceutical industry in China, the pollution and treatment of pharmaceutical wastewater have attracted great attention and concern of people. The pharmaceutical industry is one of 12 industries which are important to be treated by national environmental protection planning. According to statistics, the pharmaceutical industry accounts for 1.7% of the total value of the national industry, and the sewage discharge accounts for 2%. Pharmaceutical industry wastewaters in generalHas the advantages of complex composition, multiple organic pollutants, high concentration, COD and BOD5High value of NH4 +high-N concentration, deep chromaticity, high toxicity, high SS concentration of suspended solids and the like, wherein the suspended solids are difficult to degrade or have inhibiting effect on microorganisms, can be remained in the environment for a long time, especially comprise 'three-cause' organic pollutants which have great harm to human health, even if the concentration of the suspended solids in water is less than 10-9g/L, still has great harm to human health.
At present, for the treatment of pharmaceutical wastewater, no economic method which can be widely popularized is available at home and abroad. The developed countries mostly adopt a stable but high-cost mixed dilution aerobic treatment process, and the research on the treatment of pharmaceutical wastewater in China starts late, and an economical, effective and feasible treatment measure is not found yet.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a combined treatment process of medical intermediate production wastewater so as to reduce adverse effects on the environment.
In order to solve the technical problems, the technical scheme of the invention is as follows: a combined treatment process of medical intermediate production wastewater comprises the following steps:
A. pretreatment: adding the wastewater produced in the pharmaceutical process into a Fenton reaction device, adjusting the pH, and adding Fe2+The solution is added with H after the temperature is stabilized2O2Stirring and reacting for 2h, and adjusting the pH value again; adding 1L of effluent of a Fenton reaction device into an iron-carbon micro-electrolysis reactor, uniformly adding scrap iron and activated carbon into an iron-carbon micro-electrolysis reaction container, and performing iron-carbon micro-electrolysis for 2 h;
B. hydrolysis and acidification: diluting the pretreated wastewater in the step A, adding the diluted wastewater into a hydrolysis acidification reactor, controlling the inflow, the reflux and the rising flow velocity of the hydrolysis acidification reactor, and starting a hydrolysis acidification experimental device;
C. UASB anaerobic treatment: b, diluting the wastewater in the step B, inoculating dewatered sludge, performing medium-temperature anaerobic fermentation, and controlling the conditions of a UASB reactor; starting the UASB reactor, increasing the load after the operation is stable, and increasing the load when the treatment efficiency reaches more than 85%;
D. inoculating and domesticating activated sludge of the SBR: aerating the returned sludge, standing for 30min for precipitation, inoculating 2L of the precipitated sludge into an SBR reactor, diluting wastewater subjected to UASB anaerobic treatment by 50 times, placing 3-5L of the wastewater into the SBR reactor, adjusting the pH value to be neutral, adding a nutrient solution, and carrying out aeration; operating the SBR reactor after 3-5 days, increasing the wastewater produced in the pharmaceutical process to be treated gradually when the COD removal rate is 70%, controlling the conditions of the reactor, and performing sludge domestication and culture; after 20d, finishing the process after all indexes in the reactor meet the requirements;
E. the operation of the SBR reactor: and D, after the step D is finished, connecting the reactor to a UASB reactor, and then connecting the reactor in series for continuous operation, wherein an aeration adjusting tank is additionally arranged between the SBR reactor and the UASB reactor, and discharging water.
In the step A, the pH is adjusted by using 18mol/L sulfuric acid for coarse adjustment and using 0.5mol/L sulfuric acid for fine adjustment, and Fe2+Volume 4mL, molar concentration 0.1mol/L, H2O2The volume is 3mL, the mass fraction is 30%, the pH values of Fenton oxidation and iron-carbon micro-electrolysis are both regulated to 5.0, and the mass ratio of scrap iron to active carbon is 1: 2.
and in the step B, 3.6L of diluted wastewater is added into the hydrolysis acidification reactor, the water inlet flow is 0.35L/h, the reflux flow is 3.24L/h, and the rising flow rate of the hydrolysis acidification reactor is 1.8 m/h.
In the step C, in the inoculation and starting processes, the COD of the inlet water is diluted to 5000mg/L, the inoculation sludge amount is 20g/L, the mass concentration ratio of C/N/P in the reactor (350-500) is controlled to be 5:1, the temperature is 30-35 ℃, the pH value is 6.5-7.5, the reflux ratio is 6, and the hydraulic retention time is 20 hours; the volume load is increased by 0.5 kgCOD/(m)3∙ d) and the running time is 10-15 d, the requirement of the reactor is that the hydraulic retention time is shortened from 20h to 12h, and the volume load of the preliminarily designed reactor is 10 kgCOD/(m)3∙d)。
In the step D, the operation mode of the SBR reactor is discharge ratio 1/4, the period is 2 cycles per day and 12 hours per cycle, and water inlet time, aeration time and precipitation time are 30min, precipitation time and water discharge time are 30min in the operation period. The medicine to be treatedThe increasing proportion of the wastewater produced in the process is 5 percent; controlling the pH value of the reactor to be 7-8, the DO value to be 2-4 mg/L and the SV value30More than 30 percent, SVI of 120 and MLSS of more than 2000 mg/L; the sludge domestication and culture indexes are that the sludge is yellow brown, and the coccid, rotifer, roaming insect, branchionus, oligotrichia and a large amount of zoogloea can be observed by microscopic examination.
In the step E, the SBR reactor is operated according to a discharge ratio of 1/4 after the aeration tank is additionally arranged, and the operation is carried out in a mode of 2 cycles per day and 12 hours per cycle.
The invention has the beneficial effects that: the COD concentration is reduced by the Fenton oxidation/iron-carbon micro-electrolysis, hydrolysis acidification and UASB and SBR combined process, each part of the combined process is simpler, all parts are deeply known at present, the pretreatment raw materials are easy to obtain, the price is low, and the method is more economic compared with other treatment methods.
Drawings
FIG. 1 is a process flow diagram of the combined treatment process of the pharmaceutical intermediate production wastewater of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
Examples
As shown in the figure, wastewater produced by a certain pharmaceutical company in Tianjin is taken for testing. The raw water quality and the discharge standard thereof are shown in table 1: it can be seen that the raw water has higher COD and lower biodegradability.
TABLE 1 Water quality and effluent discharge Standard of wastewater from pharmaceutical company of Tianjin City
A. Pretreatment: adding wastewater from pharmaceutical processThe mixture was put into a Fenton reaction apparatus, adjusted to pH 5.0 with 18mol/L sulfuric acid (coarse adjustment) and 0.5mol/L sulfuric acid (fine adjustment), and 4.0mL (0.1 mol/L molar concentration) of Fe was added2+The solution, after temperature stabilization, was added 3mL (30% mass fraction) of H2O2And degrading for 2 hours after stirring. And then taking 1L of effluent of the Fenton reaction device, adjusting the pH value to 5.0, adding iron chips and activated carbon into an iron-carbon micro-electrolysis reaction container according to the mass ratio of 1:2, carrying out iron-carbon micro-electrolysis, and degrading for 2 h.
B. Hydrolysis and acidification: 3.6L of diluted wastewater is added into the hydrolysis acidification reactor, the inflow is controlled to be 0.35L/h, the reflux flow is controlled to be 3.24L/h, the ascending flow velocity of the main reactor is 1.8m/h, and the hydrolysis acidification experimental device is started.
C. UASB anaerobic treatment: diluting the COD of the inlet water to 5000mg/L, inoculating 20g/L of dewatered sludge in an anaerobic reaction tank of a certain Tianjin sewage plant, adopting medium-temperature anaerobic fermentation, controlling the mass concentration ratio of C/N/P in a reactor to be (350-500): 5:1, the temperature to be 30-35 ℃, the pH value to be 6.5-7.5, and the reflux ratio to be 6. The initial hydraulic retention time of the start-up is 20 h. When the system is started, no gas is generated, gas production starts in 16 days but the gas production rate is low, when 28 days, the COD of the effluent is 2360mg/L, the removal rate reaches 56%, the pH of the effluent is 7.2, the gas production rate is 910mL/d, and the system is switched to normal operation.
The volume load is gradually increased by 0.5 kgCOD/(m)3∙ d), when the operation is stable (COD removing rate is stable or improved, and abnormal phenomena such as acidification and the like do not occur), the load is increased. When the processing efficiency reaches more than 85 percent, the load is increased.
D. Inoculating and domesticating activated sludge of the SBR: and (3) aerating return sludge in a secondary sedimentation tank taken from a certain Tianjin sewage plant, standing and precipitating for 30min, and inoculating 2L of precipitated sludge into the SBR reactor. Diluting the wastewater subjected to UASB anaerobic treatment by 50 times, placing 3-5L of the wastewater in an SBR reactor, adjusting the pH value to be neutral, adding a nutrient solution, and carrying out aeration. After 3-5 days, the SBR reactor is operated in a mode of discharging ratio 1/4, 2 cycles per day and 12 hours per cycle. The operation period comprises water inlet for 30min, aeration for 10h, sedimentation for 1h and water drainage for 30 min. When the COD removal rate is 70%, the original industrial wastewater is gradually increased by 5 percentIncreasing the wastewater load for acclimatization culture. Controlling the pH value to be 7-8, the DO value to be 2-4 mg/L and the SV value in the reactor30The SVI value is 120, the MLSS is 2000mg/L, and the SVI value is more than 30%. After 20 days of sludge acclimation and culture, measuring that MLSS in the SBR reactor is 3745mg/L and SV3041 percent, 109 percent of SVI, 0.32kgCOD/(kgMLSS ∙ d) of organic load, 7.2 of pH, yellow brown sludge, and the trypanosome, rotifer, roaming insect, mullet, oligochaete and a large amount of zoogloea observed by microscopic examination to finish the acclimatization and culture of the sludge.
E. The operation of the SBR reactor: the SBR reactor is connected to the UASB reactor after being domesticated and cultured by sludge and then is connected in series for continuous operation. An aeration adjusting tank is additionally arranged between the SBR reactor and the UASB reactor. The operation is carried out according to the discharge ratio 1/4 in a mode of 2 cycles per day and 12h per cycle, and water is discharged.
According to the embodiment, after Fenton oxidation/iron carbon micro-electrolysis pretreatment, the COD removal rate reaches 30%, and the COD removal rate of the hydrolysis acidification reactor is 5%. The removal rate of COD by the UASB treatment process is 30-55%. The removal rate of COD by SBR is 35-60%, considering the discharge standard and improving the treatment efficiency, the operation period of SBR should be increased to more than 24h, and the load can be increased, and proper fillers are installed.
In summary, the disclosure of the present invention is not limited to the embodiments described, and various changes, modifications, substitutions and alterations can be made by persons skilled in the art without departing from the principle and spirit of the invention.
Claims (6)
1. A combined treatment process for medical intermediate production wastewater is characterized by comprising the following steps:
A. pretreatment: adding the wastewater produced in the pharmaceutical process into a Fenton reaction device, adjusting the pH, and adding Fe2+The solution is added with H after the temperature is stabilized2O2Stirring and reacting for 2h, and adjusting the pH value again; adding 1L of effluent of a Fenton reaction device into an iron-carbon micro-electrolysis reactor, uniformly adding scrap iron and activated carbon into an iron-carbon micro-electrolysis reaction container, and performing iron-carbon micro-electrolysis for 2 h;
B. hydrolysis and acidification: diluting the pretreated wastewater in the step A, adding the diluted wastewater into a hydrolysis acidification reactor, controlling the inflow, the reflux and the rising flow velocity of the hydrolysis acidification reactor, and starting a hydrolysis acidification experimental device;
C. UASB anaerobic treatment: b, diluting the wastewater in the step B, inoculating dewatered sludge, performing medium-temperature anaerobic fermentation, and controlling the conditions of a UASB reactor; starting the UASB reactor, increasing the load after the operation is stable, and increasing the load when the treatment efficiency reaches more than 85%;
D. inoculating and domesticating activated sludge of the SBR: aerating the returned sludge, standing for 30min for precipitation, inoculating 2L of the precipitated sludge into an SBR reactor, diluting wastewater subjected to UASB anaerobic treatment by 50 times, placing 3-5L of the wastewater into the SBR reactor, adjusting the pH value to be neutral, adding a nutrient solution, and carrying out aeration; operating the SBR reactor after 3-5 days, increasing the wastewater produced in the pharmaceutical process to be treated gradually when the COD removal rate is 70%, controlling the conditions of the reactor, and performing sludge domestication and culture; after 20d, finishing the process after all indexes in the reactor meet the requirements;
E. the operation of the SBR reactor: and D, after the step D is finished, connecting the reactor to a UASB reactor, and then connecting the reactor in series for continuous operation, wherein an aeration adjusting tank is additionally arranged between the SBR reactor and the UASB reactor, and discharging water.
2. The combined treatment process for wastewater from pharmaceutical intermediate production according to claim 1, wherein in step A, pH adjustment is carried out by using 18mol/L sulfuric acid for coarse adjustment and using 0.5mol/L sulfuric acid for fine adjustment, and Fe2+Volume 4mL, molar concentration 0.1mol/L, H2O2The volume is 3mL, the mass fraction is 30%, the pH values of Fenton oxidation and iron-carbon micro-electrolysis are both regulated to 5.0, and the mass ratio of scrap iron to active carbon is 1: 2.
3. the combined treatment process of medical intermediate production wastewater according to claim 1, wherein in the step B, 3.6L of diluted wastewater is added into the hydrolysis acidification reactor, the water inlet flow is 0.35L/h, the reflux flow is 3.24L/h, and the rising flow rate of the hydrolysis acidification reactor is 1.8 m/h.
4. The combined treatment process of the medical intermediate production wastewater according to claim 1, wherein in the step C, in the inoculation and starting processes, the inflow COD is diluted to 5000mg/L, the inoculation sludge amount is 20g/L, the mass concentration ratio of C/N/P in the reactor (350-500) is controlled to be 5:1, the temperature is 30-35 ℃, the pH value is 6.5-7.5, the reflux ratio is 6, and the hydraulic retention time is 20 hours; the volume load is increased by 0.5 kgCOD/(m)3∙ d) and the running time is 10-15 d, the requirement of the reactor is that the hydraulic retention time is shortened from 20h to 12h, and the volume load of the preliminarily designed reactor is 10 kgCOD/(m)3∙d)。
5. The combined treatment process of medical intermediate production wastewater according to claim 1, wherein in the step D, the SBR reactor is operated in a discharge ratio of 1/4, 2 cycles per day and 12 hours per cycle, and water is fed for 30min, aerated for 10h, precipitated for 1h and drained for 30min in the operation cycle. The increasing proportion of the wastewater produced in the pharmaceutical process to be treated is 5 percent; controlling the pH value of the reactor to be 7-8, the DO value to be 2-4 mg/L and the SV value30More than 30 percent, SVI of 120 and MLSS of more than 2000 mg/L; the sludge domestication and culture indexes are that the sludge is yellow brown, and the coccid, rotifer, roaming insect, branchionus, oligotrichia and a large amount of zoogloea can be observed by microscopic examination.
6. The combined treatment process of medical intermediate production wastewater according to claim 1, wherein in the step E, the SBR reactor is operated according to a discharge ratio of 1/4 after the aeration tank is added, and the operation is carried out for 2 cycles per day and 12 hours per cycle.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115124190A (en) * | 2022-06-24 | 2022-09-30 | 苏州苏沃特环境科技有限公司 | Di-tert-butyl dicarbonate wastewater standard treatment device and method |
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2020
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| CN103359876A (en) * | 2013-05-13 | 2013-10-23 | 苏州有色金属研究院有限公司 | Harmless dimethylacetamide wastewater treatment method |
| US20160257582A1 (en) * | 2013-09-26 | 2016-09-08 | Nanjing University | Method for Sludge-Reduced Electrocatalytic Reduction-Oxidation Pretreatment of Nitrotoluene Production Wastewater |
| CN103739142A (en) * | 2013-11-15 | 2014-04-23 | 安徽省绿巨人环境技术有限公司 | Chinese patent medicine production wastewater treatment technology |
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