CN112225402A - Method for treating wastewater from solvent recovery in chemical synthesis of pharmacy - Google Patents
Method for treating wastewater from solvent recovery in chemical synthesis of pharmacy Download PDFInfo
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- CN112225402A CN112225402A CN202011086782.7A CN202011086782A CN112225402A CN 112225402 A CN112225402 A CN 112225402A CN 202011086782 A CN202011086782 A CN 202011086782A CN 112225402 A CN112225402 A CN 112225402A
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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
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/465—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electroflotation
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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
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/30—Aerobic and anaerobic processes
Abstract
The invention relates to the field of wastewater treatment, and discloses a method for treating wastewater from solvent recovery in chemical synthesis pharmacy, which comprises the following steps: step I: performing physicochemical treatment, namely pretreating the wastewater by adopting an electrolytic air flotation pretreatment system; step II: solvent recovery, including concentration stage, rectification stage and dehydration stage, the purity of the treated solvent is greater than 98%; step III: and (3) biochemical treatment, namely treating the wastewater after the solvent is recovered by using a UASB reactor, a secondary series aerobic-anaerobic system and an MBR reactor in sequence. The invention can realize the recovery of the solvent in the chemical synthesis pharmaceutical wastewater and the sufficient degradation of impurities.
Description
Technical Field
The invention relates to the field of wastewater treatment, in particular to a method for treating solvent recovery wastewater of chemical synthesis pharmacy.
Background
The chemical synthesis pharmaceutical wastewater is wastewater with complex components and strong biological toxicity, contains complex organic matters, inorganic matters, catalysts, raw materials, reaction intermediates and the like, and generally has the characteristics of high chemical oxygen demand and low biodegradability. Due to the characteristics of the chemical synthesis pharmaceutical wastewater, microorganisms are difficult to grow, so that great difficulty is brought to a biochemical treatment mode adopted by the traditional wastewater treatment.
The water treatment mode adopted by the chemical pharmaceutical wastewater at present is generally as follows: the physicochemical treatment is combined with the biochemical treatment, and although the treatment mode can neutralize and degrade the wastewater, the solvents such as methanol, ethanol, acetone, isopropanol, ethyl acetate, dimethyl sulfoxide and the like contained in the wastewater cannot be well recycled, so that the problem of resource waste exists.
Disclosure of Invention
The invention aims to provide a method for treating chemical synthesis pharmaceutical solvent recovery wastewater, which aims to solve the problem of resource waste in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals comprises the following steps:
step I: performing physicochemical treatment, namely pretreating the wastewater by adopting an electrolytic air flotation pretreatment system;
step II: solvent recovery, including concentration stage, rectification stage and dehydration stage, the purity of the treated solvent is greater than 98%;
step III: and (3) biochemical treatment, namely treating the wastewater after the solvent is recovered by using a UASB reactor, a secondary series aerobic-anaerobic system and an MBR reactor in sequence.
The principle and the advantages of the scheme are as follows: in practical application, in the technical scheme, when the chemical synthesis pharmaceutical wastewater is treated, firstly, the wastewater is aerated and suspended by the electrolytic air flotation pretreatment system in a physicochemical treatment mode, and the use of a flocculating agent is combined, so that colloidal substances and suspended substances in the wastewater can be removed, and in addition, more than 60 percent of COD and BOD in the wastewater can be removed at the stage; after physicochemical treatment and before biochemical treatment, solvents such as methanol, ethanol, acetone, isopropanol, ethyl acetate and the like in the wastewater are recovered, and the pretreated wastewater is concentrated by a concentration step so as to facilitate later rectification classification and downstream wastewater treatment. After the wastewater is preliminarily concentrated, the wastewater is classified through a rectification stage to obtain solvents with different components, and the rectification stage can also synchronously reduce the water content in the solvents so as to facilitate later dehydration treatment; in the dehydration stage, the solvent is further dehydrated to improve the purity of the solvent, so that the purity of the treated solvent is more than 98 percent. When the wastewater with the solvent recovered is subjected to biochemical treatment, most organic pollutants in the wastewater can be degraded by anaerobic fermentation by using the UASB reactor, COD and BOD in the wastewater can be further removed by using a secondary series aerobic-anaerobic system, and nitrogen compounds in the wastewater can be effectively removed; the MBR reactor can realize the separation and filtration of the wastewater, and the clarity of the wastewater is ensured.
The beneficial effects of this technical scheme lie in: the wastewater treatment method of the technical scheme can not only realize the degradation of organic matters in the wastewater, the removal of colloidal substances and suspended matters and the clarification of the wastewater, but also realize the recovery of the recyclable solvent in the wastewater, thereby avoiding the problem of resource waste to a certain extent.
Preferably, as an improvement, in the step I, the electrolytic air flotation pretreatment system comprises a magnet fluidized bed, a micro-electrolysis reactor, a fenton reactor and a reaction sedimentation tank which are arranged in sequence, and a pipeline is connected between adjacent devices.
In the technical scheme, when the wastewater is subjected to physicochemical treatment, the wastewater is firstly aerated and suspended through the fluidized bed, then COD and BOD are preliminarily removed by utilizing the micro-electrolysis reactor and the Fenton reactor, organic compounds in the wastewater are oxidized into inorganic state, and flocculation and precipitation are realized by combining a flocculating agent, so that the preliminary treatment on the wastewater is realized.
Preferably, as an improvement, in the step I, the magnet fluidized bed is divided into three stages, including an aeration section, a reaction section and a separation section, wherein the Hydraulic Retention Time (HRT) of the aeration section is 20-24h, and the hydraulic retention time of the separation section is 3-4 h.
In the technical scheme, when the magnet fluidized bed is used for treating the wastewater, the wastewater sequentially passes through the aeration section, the reaction section and the separation section, and the HRT of each stage is the better time verified by experiments.
Preferably, as an improvement, in the step I, the micro-electrolysis reactor is in an aeration state, the hydraulic retention time of the Fenton reactor is 5-6h, and the hydraulic retention time of the reaction sedimentation tank is 4-5 h.
In the technical scheme, when the micro-electrolysis reactor is used for treating wastewater, the micro-electrolysis reactor is set to be in an aeration state, the treatment effect can be enhanced, and the HRT of the wastewater in each reactor is the better time length verified by experiments.
Preferably, as an improvement, in step II, the solvent-containing pharmaceutical wastewater is evaporated by an evaporator and then introduced into a degassing tower for degassing separation in the concentration stage, so as to obtain a solvent primary concentrated solution.
In the technical scheme, when the chemical synthesis pharmaceutical wastewater containing the solvent is treated, firstly, the wastewater is evaporated through an evaporator, then the wastewater is introduced into a degassing tower for degassing, and the primary concentration of the solvent in the wastewater is realized after the evaporation and degassing treatment; in addition, evaporation and degasification treatment can also realize TDS (total dissolved solids) primary classification in the waste water, and later stage rectification classification and downstream waste water treatment are facilitated.
Preferably, as an improvement, in step II, the rectification stage utilizes a rectification system to rectify and classify the primary concentrated solution of the solvent, the rectification system includes a mother liquor storage tank, a preheater, a falling film tower kettle and a rectification tower, pipelines are communicated between the mother liquor storage tank, the preheater, the falling film tower kettle and the rectification tower, and the water content of the solvent after rectification and classification is less than 12 wt%.
In the technical scheme, in the process of rectifying the pharmaceutical wastewater containing the solvent, the primary concentrated solution of the solvent obtained by evaporation enters a mother solution storage tank, is pumped into a preheater by a pump to be preheated, enters a falling film tower kettle after being preheated, enters a rectifying tower after falling film evaporation to be rectified and classified, finally solvents with different fractions are obtained, and the classification treatment of the solvents is realized.
Preferably, as an improvement, the rectifying tower is of a multi-section structure and comprises a steam section, a cold water section and a low-temperature water section from bottom to top.
In the technical scheme, the rectifying tower is arranged into a multi-section structure, and different rectifying temperatures are arranged in different rectifying sections, so that the directional rectifying and classifying of the solvent can be realized, and the solvents with different temperature fractions can be obtained.
Preferably, as an improvement, in step II, the membrane separation system is used in the dehydration stage to perform dehydration, and the membrane separation system includes a superheater, an evaporator, a membrane separation assembly, a finished product cooler, and a finished product dehydration part, and adjacent devices are communicated with each other through a pipeline.
In the technical scheme, when the solvent is subjected to membrane separation treatment, raw materials meeting the requirement of membrane feeding enter a superheater and an evaporator through a raw material pump, enter a membrane separation assembly after preheating, water and a small amount of organic matters in the raw materials permeate to the downstream side of a membrane from the upstream side of the membrane through the membrane separation assembly, and the raw materials at the upstream side of the membrane are cooled and dehydrated to obtain a solvent recovery finished product.
Preferably, as an improvement, in step III, the UASB reactor is further communicated at its front end with a water diversion box for controlling water inflow parameters.
In the technical scheme, the water distribution box is additionally arranged at the front end of the UASB reactor, so that the water inlet parameter can be ensured to meet the requirement of the UASB reactor, and the problems of equipment failure and the like are avoided.
Preferably, as an improvement, the feed water parameters of the UASB reactor are: pH6.8-7.5, and the water inlet temperature is 35 ℃.
In the technical scheme, the water inlet parameter is within a proper parameter range, and the water inlet temperature is controlled to be 35 ℃, so that the UASB reactor is in a medium-temperature reaction state after water inlet, and the reaction is favorably carried out.
Drawings
FIG. 1 is a plan view of a wastewater treatment apparatus for solvent recovery according to a first embodiment of the present invention.
FIG. 2 is a plan view of a wastewater treatment apparatus for solvent recovery in the second embodiment of the present invention.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: the device comprises a triple-effect evaporator 1, a degassing tower 2, a mother liquor storage tank 3, a preheater 4, a falling film tower kettle 5, a rectifying tower 6, a steam section 7, a cold water section 8, a low-temperature water section 9, a superheater 10, an evaporator 11, a membrane separation assembly 12, a finished product cooler 13, a centrifugal pump 14, a vacuum unit 15, a condenser 16, a permeate pump 17, a hot water tank 18 and a circulating vacuum pump 19.
Example one
A method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals comprises the following steps:
step I: performing physicochemical treatment, namely pretreating the wastewater by adopting an electrolytic air flotation pretreatment system, wherein the electrolytic air flotation pretreatment system comprises a magnet fluidized bed, a micro-electrolysis reactor, a Fenton reactor and a reaction sedimentation tank which are sequentially arranged, and a pipeline is connected between adjacent equipment; the magnetic fluidized bed is divided into three stages, including an aeration section, a reaction section and a separation section, wherein the Hydraulic Retention Time (HRT) of the aeration section is 24h, and the HRT of the separation section is 4 h; the micro-electrolysis reactor is in an aeration state, the HRT of the Fenton reactor is 6h, and the HRT of the reaction sedimentation tank is 5 h;
step II: solvent recovery, including a concentration stage, a rectification stage and a dehydration stage, as shown in figure 1,
and (3) a concentration stage: introducing the chemically synthesized pharmaceutical wastewater subjected to physicochemical treatment into a triple-effect evaporator 1, evaporating by the triple-effect evaporator 1, introducing into a degassing tower 2, degassing and separating to obtain a primary solvent concentrate; compared with single-effect evaporation, the three-effect evaporation has high energy utilization efficiency, and the steam required by the evaporation of the wastewater of unit volume can be reduced by more than half;
a rectification stage: a rectification system is utilized to carry out rectification classification on the primary solvent concentrated solution, the rectification system comprises a mother solution storage tank 3, a preheater 4, a falling film tower kettle 5 and a rectification tower 6, pipelines are also communicated among the mother solution storage tank 3, the preheater 4, the falling film tower kettle 5 and the rectification tower 6, and the mother solution storage tank 3 is connected with the degassing tower 2 through a pipeline; the top end of the falling film tower kettle 5 in the embodiment is provided with a steam port, and the bottom end is provided with a hot water port; the rectifying tower 6 is of a multi-section structure and comprises a steam section 7, a cold water section 8 and a low-temperature water section 9 from bottom to top; during rectification, the primary solvent concentrated solution is introduced into a solvent mother solution storage tank 3, pumped into a preheater 4 through a pump, preheated and then enters a falling film evaporator 11, and after falling film evaporation, the primary solvent concentrated solution enters a rectifying tower 6 for rectification and classification to obtain solvents with different fractions, wherein the water content of the rectified and classified solvents is less than 12 wt%;
and (3) a dehydration stage: the solvent-containing pharmaceutical wastewater is dehydrated by adopting a membrane separation system, the membrane separation system comprises a superheater 10, an evaporator 11, a membrane separation assembly 12, a finished product cooler 13 and a finished product dehydration part, the dehydration part in the embodiment is a centrifugal pump 14, and adjacent equipment is communicated through a pipeline. The membrane separation component 12 is formed by connecting a plurality of membrane components in series, and the membrane components in the embodiment are all provided with molecular sieve membranes; during dehydration, raw materials meeting the requirement of entering a membrane are guided into a superheater 10 and an evaporator 11 through a raw material pump, enter a membrane module in a steam form after reaching a certain temperature, moisture and a small amount of organic matters in the raw materials permeate to the downstream side of the membrane from the upstream side of the membrane through the membrane module, and the raw materials on the upstream side of the membrane are subjected to preliminary dehydration, are cooled by a finished product cooler 13 and then are discharged under the action of a centrifugal pump 14; the penetrating fluid steam on the downstream side of the membrane firstly enters the condenser 16 under the suction action of the vacuum unit 15, is cooled into a liquid state by the condenser 16 and then is discharged under the action of the penetrating fluid pump 17, and the purity of the treated solvent is more than 98 percent through detection;
step III: performing biochemical treatment, namely treating the wastewater after solvent recovery by using a UASB reactor, a secondary series aerobic-anaerobic system and an MBR reactor in sequence; the front end of the UASB reactor is also communicated with a water distribution box for controlling water inlet parameters, and the water inlet parameters are controlled as follows: pH6.8-7.5, and the water inlet temperature is 35 ℃. The pharmaceutical wastewater treated by the embodiment meets the requirements of the discharge standard GB21904-2008 of chemical synthesis pharmaceutical industry water pollutants.
Example two
As shown in fig. 2, the present embodiment is different from the first embodiment in that: in this embodiment, the hot water port is connected to a hot water tank 18 and a water circulation vacuum pump 19. In this embodiment, the steam in the falling film tower kettle 5 is condensed into liquid (hot water) after heat exchange, and is discharged along the hot water port, and the temporary storage and later-stage recycling of the part of hot water can be realized through the hot water tank 18 and the water circulation vacuum pump 19.
The foregoing is merely an example of the present invention and common general knowledge in the art of designing and/or characterizing particular aspects and/or features is not described in any greater detail herein. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. A method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals is characterized by comprising the following steps:
step I: performing physicochemical treatment, namely pretreating the wastewater by adopting an electrolytic air flotation pretreatment system;
step II: solvent recovery, including concentration stage, rectification stage and dehydration stage, the purity of the treated solvent is greater than 98%;
step III: and (3) biochemical treatment, namely treating the wastewater after the solvent is recovered by using a UASB reactor, a secondary series aerobic-anaerobic system and an MBR reactor in sequence.
2. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 1, wherein the method comprises the following steps: in the step I, the electrolysis air flotation pretreatment system comprises a magnet fluidized bed, a micro-electrolysis reactor, a Fenton reactor and a reaction sedimentation tank which are arranged in sequence, and a pipeline is connected between adjacent devices.
3. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 2, wherein the method comprises the following steps: in the step I, the magnet fluidized bed is divided into three stages, including an aeration section, a reaction section and a separation section, wherein the hydraulic retention time of the aeration section is 20-24h, and the hydraulic retention time of the separation section is 3-4 h.
4. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 3, wherein the method comprises the following steps: in the step I, the micro-electrolysis reactor is in an aeration state, the hydraulic retention time of the Fenton reactor is 5-6h, and the hydraulic retention time of the reaction sedimentation tank is 4-5 h.
5. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 4, wherein the method comprises the following steps: in the step II, in the concentration stage, the pharmaceutical wastewater containing the solvent is evaporated by an evaporator and then is introduced into a degassing tower for degassing and separation to obtain a solvent primary concentrated solution.
6. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 5, wherein the method comprises the following steps: in the step II, in the rectification stage, a rectification system is used for rectifying and classifying the primary concentrated solution of the solvent, the rectification system comprises a mother liquor storage tank, a preheater, a falling film tower kettle and a rectification tower, pipelines are communicated among the mother liquor storage tank, the preheater, the falling film tower kettle and the rectification tower, and the water content of the solvent after rectification and classification is less than 12 wt%.
7. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 6, wherein the method comprises the following steps: the rectifying tower is of a multi-section structure and comprises a steam section, a cold water section and a low-temperature water section from bottom to top.
8. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 7, wherein the method comprises the following steps: and in the step II, a membrane separation system is adopted for dehydration in the dehydration stage, the membrane separation system comprises a superheater, an evaporator, a membrane separation assembly, a finished product cooler and a finished product dehydration part, and adjacent equipment are communicated through a pipeline.
9. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 8, wherein the method comprises the following steps: in the step III, the front end of the UASB reactor is also communicated with a water distribution box for controlling water inlet parameters.
10. The method for treating wastewater from solvent recovery in chemical synthesis of pharmaceuticals according to claim 9, wherein the method comprises the following steps: the water inlet parameters of the UASB reactor are as follows: pH6.8-7.5, and the water inlet temperature is 35 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113559536A (en) * | 2021-08-08 | 2021-10-29 | 建德建业资源再生技术有限公司 | System and method for recycling methanol from waste organic solvent |
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Application publication date: 20210115 |