CN103880235A - Treatment method for dimetronidazole production wastewater - Google Patents

Treatment method for dimetronidazole production wastewater Download PDF

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Publication number
CN103880235A
CN103880235A CN201410152222.5A CN201410152222A CN103880235A CN 103880235 A CN103880235 A CN 103880235A CN 201410152222 A CN201410152222 A CN 201410152222A CN 103880235 A CN103880235 A CN 103880235A
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China
Prior art keywords
wastewater
waste water
filtrate
dimetridazole
treatment method
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CN201410152222.5A
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Chinese (zh)
Inventor
方耀
徐双喜
周拥军
肖涛
邓支华
晏浩哲
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HUBEI HONGYUAN PHARMACEUTICAL CO Ltd
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HUBEI HONGYUAN PHARMACEUTICAL CO Ltd
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Priority to CN201410152222.5A priority Critical patent/CN103880235A/en
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Abstract

The invention discloses a treatment method for dimetronidazole production wastewater. The treatment method for dimetronidazole production wastewater comprises the following steps: step 1, collecting the wastewater; step 2, performing reduced pressure concentration so as to reduce the volume of the wastewater to 1/3-2/3 of the original volume, filtering the concentrated wastewater at 35-55 DEG C, recovering solids and collecting the filtrate; step 3, carrying out low-temperature crystallization and centrifugal spin filter on the filtrate obtained in the step 2 at 5-10 DEG C, recovering solids and collecting the filtrate. The wastewater treatment method disclosed by the invention is mainly used for removing organic matters and a part of inorganic salt in the wastewater by means of reduced pressure concentration and low-temperature crystallization, few in the added chemical agents, simple in wastewater treatment process and low in cost; according to the wastewater treatment method disclosed by the invention, the discharge of organic matters is reduced, environmental pollution is reduced, and a part of raw materials is recovered, thus contributing to reduction for production cost.

Description

The treatment process of Dimetridazole factory effluent
Technical field
The present invention relates to technical field of waste water processing, be specifically related to a kind for the treatment of process of Dimetridazole factory effluent.
Background technology
Along with the development of medicine industry, the waste water producing in pharmaceutical industry has become serious source of pollution.Because need to use a large amount of industrial chemicals in medicine production, complex manufacturing in addition, water-quality COD is high, and the water yield is large, forms the problems such as complicated, causes the waste water of medication chemistry industry to be difficult to process.The antibiotics pharmacy waste water that wherein contains multiple toxin, hard-degraded substance is difficult to process especially.
Dimetridazole, also referred to as 1,2-dimethyl-5-nitroimidazole, large U.S. element, an imidazoles, dimetridazole, it is a kind of antibiotics bulk drug in pharmaceutical industry, in production process, experience cyclization, the chemical reaction such as nitrated, made multiple Organic Chemicals after chemical reaction obtain medicine intermediate and synthesis material medicine.All kinds of organic raw material of a large amount of use in its production process, through polystep reaction, complex process.The raw material that contains multiple not complete reaction in Dimetridazole factory effluent and reaction product, comprise the raw materials such as 2-methyl-5-nitroimidazole, and the pollutent such as other organism, salt (as the ammonium sulfate producing in production technique).If the organism in waste water directly discharges, easily cause the eutrophication of water body, decomposite multiple obnoxious flavour, not only cause the serious water pollution also can polluted air; In waste water, a large amount of inorganic salt can make water body pH value change, destroy its natural shock absorption, elimination or anti-bacteria and microbial growth, hinder self-purification of waters, can greatly increase water hardness simultaneously, cause salting of soil, all bring disadvantageous effect to industry and life.
But these organism and inorganic salts also have important utility value simultaneously.For example, in waste water, contained organic itrated compound can be used as and produces medical material intermediate, returns to the operation that methylates as raw material; Ammonium sulfate is widely used in the fields such as chemical alkaline, composting; Therefore, if the direct discharge that contains a large amount of organic itrated compounds and inorganic salt is not only caused to environmental pollution, or a kind of very large waste.
Summary of the invention
The object of the invention is to, for above-mentioned defect of the prior art, propose a kind for the treatment of process of Dimetridazole factory effluent the high technical problem of organic content in Dimetridazole factory effluent in solution prior art.
Technical scheme of the present invention comprises a kind for the treatment of process of Dimetridazole factory effluent, comprising:
Step 1: collect waste water;
Step 2: by concentrating under reduced pressure, the volume of described waste water is reduced to originally 1/3~2/3, the waste water after concentrated is filtered at 35~55 ℃, reclaim solid and also collect filtrate;
Step 3: step 2 gained filtrate is carried out to low temperature crystallization at 5~10 ℃, and centrifugal rejection filter, reclaims solid and collect filtrate.
Preferably, described step 1 also comprises described waste water is carried out to centrifugal step.
Preferably, described step 2 also comprises the described filtrate pH value to 5.0 of adjusting, and then the step of filtering.
Preferably, after step 3, also comprise the steps:
The pH value to 7.0 of regulating step 3 gained filtrates.
Compared with prior art, beneficial effect of the present invention comprises: method of wastewater treatment of the present invention mainly adopts the mode of concentrating under reduced pressure and low temperature crystallization that the organism in waste water and part inorganic salt are removed, add chemical agent few, waste water treatment process is simple, and cost is low; Method of wastewater treatment of the present invention has reduced organic discharge, reduces environmental pollution, has reclaimed part material simultaneously, contributes to reduce production costs.
Accompanying drawing explanation
Fig. 1 is the schema of the treatment process of Dimetridazole factory effluent of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
The raw material that contains multiple not complete reaction in Dimetridazole factory effluent and reaction product, comprise the raw materials such as 2-methyl-5-nitroimidazole, and the pollutent such as other organism, salt (as the ammonium sulfate producing in production technique).The present invention is directed to that above-mentioned waste water contains the multiple organism with high pollution and salt, directly discharge causes the pollution to environment, and multiple useful matter does not obtain the problem of effective recycling, a kind for the treatment of process of waste water is provided, significantly reduce the organism of contaminative and the content of inorganic salts in above-mentioned waste water, make waste water after treatment reach discharging standards, can be to environment, and can reclaim the useful organism such as itrated compound, ammonium sulfate and inorganics, economize in raw materials, reduce production costs, and treatment process is simple, easy to operate.
Please refer to shown in Fig. 1, the invention provides a kind for the treatment of process of Dimetridazole factory effluent, comprise the steps:
Step S1, collects waste water;
Step S2: by concentrating under reduced pressure, the volume of described waste water is reduced to originally 1/3~2/3, the waste water after concentrated is filtered at 35~55 ℃, reclaim solid and also collect filtrate;
Step S3: step S2 gained filtrate is carried out to low temperature crystallization at 5~10 ℃, and centrifugal rejection filter, reclaims solid and collect filtrate.
In described step S2, after concentrating under reduced pressure, when temperature is adjusted to 35~55 ℃, raw materials for production 2-methyl-5-nitroimidazole that the crystal of separating out is Dimetridazole, reclaims rear recycle, continues as the medicine intermediate raw material of producing Dimetridazole.In described step S3, at 5~10 ℃, carry out crystallization, the solid of separating out is ammonium sulfate.
In described step 2, being filtered into physical filtering, can be that normal pressure filters or pressure filtration, and the pressure of described pressure filtration is 0.5 to 2Mpa, and its filtration medium adopting can be a kind of or combination in filter core, filter membrane.
Described step S1 also comprises described waste water is carried out to centrifugal step.
Described step S2 also comprises the described filtrate pH value to 5.0 of adjusting, and then the step of filtering, and the object of inferior step is to make part itrated compound solid to separate out, and reduces the content of itrated compound in waste water.
After step S3, also comprise the steps: step S4, the pH value to 7.0 of regulating step S3 gained filtrate.
Above-mentioned adjusting pH acid used is sulfuric acid, and the object of step S4 is waste water to be adjusted to neutrality, meets emission standard.
Method of wastewater treatment of the present invention mainly adopts the mode of concentrating under reduced pressure and low temperature crystallization that the organism in waste water and part inorganic salt are removed, then with sour, wastewater pH is adjusted to neutrality, adds chemical agent few, and waste water treatment process is simple, and cost is low; Method of wastewater treatment of the present invention has reduced organic discharge, reduces environmental pollution, has reclaimed part material simultaneously, contributes to reduce production costs.
embodiment 1:
Embodiments of the invention 1 provide a kind for the treatment of process of Dimetridazole factory effluent, get the synthetic middle secondary centrifuging waste water 1200ml of Dimetridazole crude product, put in 2L flask, be evaporated to residue 400ml solution, heat filtering at 55 ℃ of temperature, filter to obtain 2-methyl-5-nitroimidazole, dry to obtain 106.3g; Above-mentioned filtrate regulates pH=5 to separate out itrated compound 9g with sulfuric acid, stirs filtering drying under room temperature; Then filtrate is lowered the temperature again, and holding temperature is 10 ℃ of left and right, crystallization 1 hour, and rejection filter, reclaims and obtains ammonium sulfate 130g (content is 98%).
Finally waste water is adjusted to neutrality with ammonia soln, discharges.
embodiment 2:
Embodiments of the invention 2 provide a kind for the treatment of process of Dimetridazole factory effluent, get the synthetic middle secondary centrifuging waste water 1200ml of Dimetridazole crude product, put in 2L flask, be evaporated to residue 450ml solution, heat filtering at 55 ℃ of temperature, filter to obtain 2-methyl-5-nitroimidazole, dry to obtain 105.3g; Above-mentioned filtrate regulates pH=5 to separate out itrated compound 9.3g with sulfuric acid, stirs filtering drying under room temperature; Then filtrate is lowered the temperature again, and holding temperature is 10 ℃ of left and right, crystallization 1 hour, and rejection filter, reclaims and obtains ammonium sulfate 129g (content is 98%).
Finally waste water is adjusted to neutrality with ammonia soln, discharges.
embodiment 3:
Embodiments of the invention 3 provide a kind for the treatment of process of Dimetridazole factory effluent, get the useless 1200ml of the synthetic middle secondary centrifuging of Dimetridazole crude product, put in 2L flask, be evaporated to residue 390ml solution, heat filtering at 55 ℃ of temperature, filter to obtain 2-methyl-5-nitroimidazole, dry to obtain 107.3g; Above-mentioned filtrate regulates pH=5 to separate out itrated compound 9.2g with sulfuric acid, stirs filtering drying under room temperature; Then filtrate is lowered the temperature again, and holding temperature is 10 ℃ of left and right, crystallization 1 hour, and rejection filter, reclaims and obtains ammonium sulfate 133g (content is 98%).
Finally waste water is adjusted to neutrality with ammonia soln, discharges.
embodiment 4:
Embodiments of the invention 4 provide a kind for the treatment of process of Dimetridazole factory effluent, get the useless 1200ml of the synthetic middle secondary centrifuging of Dimetridazole crude product, put in 2L flask, be evaporated to residue 500ml solution, heat filtering at 55 ℃ of temperature, filter to obtain 2-methyl-5-nitroimidazole, dry to obtain 103.3g; Above-mentioned filtrate regulates pH=5 to separate out itrated compound 9.3g with sulfuric acid, stirs filtering drying under room temperature; Then filtrate is lowered the temperature again, and holding temperature is 10 ℃ of left and right, crystallization 1 hour, and rejection filter, reclaims and obtains ammonium sulfate 135g (content is 98%).
Finally waste water is adjusted to neutrality with ammonia soln, discharges.
embodiment 5:
Embodiments of the invention 5 provide a kind for the treatment of process of Dimetridazole factory effluent, get the useless 1200ml of the synthetic middle secondary centrifuging of Dimetridazole crude product, put in 2L flask, be evaporated to residue 800ml solution, heat filtering at 35 ℃ of temperature, filter to obtain 2-methyl-5-nitroimidazole, dry to obtain 103.3g; Above-mentioned filtrate regulates pH=5 to separate out itrated compound 9.3g with sulfuric acid, stirs filtering drying under room temperature; Then filtrate is lowered the temperature again, and holding temperature is 5 ℃ of left and right, crystallization 1 hour, and rejection filter, reclaims and obtains ammonium sulfate 135g (content is 98%).
Finally waste water is adjusted to neutrality with ammonia soln, discharges.
embodiment 6:
Embodiments of the invention 6 provide a kind for the treatment of process of Dimetridazole factory effluent, get the useless 1200ml of the synthetic middle secondary centrifuging of Dimetridazole crude product, put in 2L flask, be evaporated to residue 500ml solution, heat filtering at 50 ℃ of temperature, filter to obtain 2-methyl-5-nitroimidazole, dry to obtain 103.3g; Above-mentioned filtrate regulates pH=5 to separate out itrated compound 9.3g with sulfuric acid, stirs filtering drying under room temperature; Then filtrate is lowered the temperature again, and holding temperature is 8 ℃ of left and right, crystallization 1 hour, and rejection filter, reclaims and obtains ammonium sulfate 135g (content is 98%).
Finally waste water is adjusted to neutrality with ammonia soln, discharges.
The above the specific embodiment of the present invention, does not form limiting the scope of the present invention.Various other corresponding changes and distortion that any technical conceive according to the present invention is made, all should be included in the protection domain of the claims in the present invention.

Claims (4)

1. a treatment process for Dimetridazole factory effluent, is characterized in that, comprising:
Step 1: collect waste water;
Step 2: by concentrating under reduced pressure, the volume of described waste water is reduced to originally 1/3~2/3, the waste water after concentrated is filtered at 35~55 ℃, reclaim solid and also collect filtrate;
Step 3: step 2 gained filtrate is carried out to low temperature crystallization at 5~10 ℃, and centrifugal rejection filter, reclaims solid and collect filtrate.
2. the treatment process of Dimetridazole factory effluent according to claim 1, is characterized in that, described step 1 also comprises carries out centrifugal step to described waste water.
3. the treatment process of Dimetridazole factory effluent according to claim 1, is characterized in that, described step 2 also comprises the described filtrate pH value to 5.0 of adjusting, and then the step of filtering.
4. the treatment process of Dimetridazole factory effluent according to claim 1, is characterized in that, after step 3, also comprises the steps:
The pH value to 7.0 of regulating step 3 gained filtrates.
CN201410152222.5A 2014-04-16 2014-04-16 Treatment method for dimetronidazole production wastewater Pending CN103880235A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105753236A (en) * 2016-03-24 2016-07-13 湖北省宏源药业科技股份有限公司 Treatment method of double-effect condensate water in metronidazole wastewater
CN117263296A (en) * 2023-11-21 2023-12-22 山东戴克生物科技有限公司 Dimethoimidazole production wastewater storage device and method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0072919A1 (en) * 1981-08-13 1983-03-02 BASF Aktiengesellschaft Process for the preparation of 1,2-dimethyl-5-nitroimidazole of high purity
CN86105875A (en) * 1986-08-29 1988-03-09 贵州省化工研究所 The new process of production of high-quality bariumchloride
CN101914062A (en) * 2010-09-01 2010-12-15 中南民族大学 Method for recovering metronidazole finished product from industrial waste residue of metronidazole
CN102344220A (en) * 2011-07-19 2012-02-08 湖北省宏源药业有限公司 Method for treating metronidazole waste water

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0072919A1 (en) * 1981-08-13 1983-03-02 BASF Aktiengesellschaft Process for the preparation of 1,2-dimethyl-5-nitroimidazole of high purity
CN86105875A (en) * 1986-08-29 1988-03-09 贵州省化工研究所 The new process of production of high-quality bariumchloride
CN101914062A (en) * 2010-09-01 2010-12-15 中南民族大学 Method for recovering metronidazole finished product from industrial waste residue of metronidazole
CN102344220A (en) * 2011-07-19 2012-02-08 湖北省宏源药业有限公司 Method for treating metronidazole waste water

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105753236A (en) * 2016-03-24 2016-07-13 湖北省宏源药业科技股份有限公司 Treatment method of double-effect condensate water in metronidazole wastewater
CN105753236B (en) * 2016-03-24 2019-03-08 湖北省宏源药业科技股份有限公司 The processing method of economic benefits and social benefits condensed water in a kind of metronidazole waste water
CN117263296A (en) * 2023-11-21 2023-12-22 山东戴克生物科技有限公司 Dimethoimidazole production wastewater storage device and method
CN117263296B (en) * 2023-11-21 2024-02-02 山东戴克生物科技有限公司 Dimethoimidazole production wastewater storage device and method

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Address after: 438600 Fengshan City, Huanggang province Luotian County, north of the town of water Yi Road, No. 428

Applicant after: HUBEI HONGYUAN PHARMACEUTICAL TECHNOLOGY CO., LTD.

Address before: 438600 Fengshan City, Huanggang province Luotian County, north of the town of water Yi Road, No. 428

Applicant before: Hubei Hongyuan Pharmaceutical Co., Ltd.

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Application publication date: 20140625