CN103449654A - Treatment method of Omeprazole intermediate production wastewater - Google Patents
Treatment method of Omeprazole intermediate production wastewater Download PDFInfo
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- CN103449654A CN103449654A CN2013104197349A CN201310419734A CN103449654A CN 103449654 A CN103449654 A CN 103449654A CN 2013104197349 A CN2013104197349 A CN 2013104197349A CN 201310419734 A CN201310419734 A CN 201310419734A CN 103449654 A CN103449654 A CN 103449654A
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- waste water
- saltcake
- sodium sulfate
- sulfate anhydrous
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Abstract
The invention discloses a treatment method of Omeprazole intermediate production wastewater. The method comprises the following steps: adding an industrial concentrated sulfuric acid for precipitating wastewater, firing filter residues, cooling and crystallizing filter liquor, and evaporating by using a multi-effect evaporator, The method can be used for treating wastewater containing various inorganic substances to obtain anhydrous sodium sulphate and reusable cooling water. According to the wastewater treatment method disclosed by the invention, because a problem of high wastewater treatment cost in the prior art is solved, the wastewater treatment cost is saved, and the economic benefit is high.
Description
Technical field
The invention belongs to Pollution abatement and resource and reclaim field, be specifically related to a kind for the treatment of process of the waste water that produces in intermediate of omeprazole 2-sulfydryl-5-methoxyl group benzo imidazoles intermediate production process.
Background technology
Omeprazole is a kind of effectively proton pump inhibitor of gastric acid secretion inhibiting, the trade name of circulation comprises peace stomach piperazine azoles, Omeprazole, inferior maple imidazoles, Losec, OMEPRAZOLE, Omeprazole, Losec on the market, belong to and press down the acids medicine, the common acids medicine that presses down also comprises pantoprazole, rabeprazole, esomeprazole.The domestic method for preparing omeprazole is mainly by 2-sulfydryl-5-methoxyl group benzo imidazoles and 2-chloromethyl-3 at present, 5-dimethyl-4-methoxypyridine condensation obtains 2-[2-(4-methoxyl group-3, the 5-dimethyl) picolyl sulphur]-4-methoxyl group benzo imidazoles, finally with the metachloroperbenzoic acid oxidation, obtain the final product omeprazole.Wherein as the production of the 2-sulfydryl of intermediate important in the omeprazole production process-5-methoxyl group benzo imidazoles (CAS:37052-78-1), usually take 2-nitro-4-anisidine (purplish red base GP) is raw material, add sodium persulfide and dithiocarbonic anhydride, in the aqueous solution, react, gained solution, through neutralization, suction filtration, recrystallization, obtains target product.Wherein this dithiocarbonic anhydride reduction method, with respect to traditional two-step approach, has technique simple, has avoided producing easily oxidized intermediate product 4-methoxyl group O-Phenylene Diamine, solvent toxicity is little, raw material is cheap and be easy to get, and the advantage such as be conducive to reduce production costs, have better market outlook.
Although the method has plurality of advantages on synthesis technique, the method can produce a large amount of purplish red waste water (product per ton approximately produces 5 ~ 6 tons of waste water), pH=11.5 ~ 12.5, and component in solution mainly comprises NaHS, Na
2s
2, Na
2s
2o
3and Na
2s etc., and there is obvious H
2the S stink, the meeting serious environment pollution, and also in waste water, contained inorganics has important utility value.But inorganics complicated component in waste water, classification is reclaimed can cost be higher, therefore studies a kind of simple and Pollution abatement of the waste water that cost is low and the method that resource reclaims and has great significance, and produces certain economic benefit.
Summary of the invention
The object of the present invention is to provide a kind of administer the simply and easily waste water produced in omeprazole synthetic intermediate 2-sulfydryl-5-methoxyl group benzo imidazoles production process and the method that reclaims resource in waste water.
The technical solution that realizes the object of the invention is:
A kind for the treatment of process of intermediate of omeprazole factory effluent, in described waste water solution, main component comprises NaHS, Na
2s
2, Na
2s
2o
3and Na
2s the treating method comprises following steps:
Step 1, to the industrial sulphuric acid that adds 98wt% in waste water solution, regulating pH value is 6.0 ~ 7.5, tail gas absorption H
2s gas, stirring reaction;
Step 2, after reaction finishes, waste water, through centrifugation or press filtration, obtains respectively filter residue and filtrate; Filtrate is cooled to 0 ~ 8 ℃ and standing 12 ~ 48h, separates out saltcake, and saltcake is separated with supernatant liquid; Filter residue, through 500 ~ 600 ℃ of calcinations, obtains Sodium sulfate anhydrous.min(99);
Step 3, the saltcake obtained in step 2 is dried, and obtains Sodium sulfate anhydrous.min(99);
Step 4, the supernatant liquid obtained in step 2 evaporates through multiple-effect evaporator, obtains respectively water of condensation and the Sodium sulfate anhydrous.min(99) that can reuse.
Wherein, in step 1, the dosage of industrial sulphuric acid is that every square meter waste water adds 120 ~ 220kg; Churning time is 30 ~ 120min.
Multiple-effect evaporator described in step 4 uses 2 ~ 3 effects, uses the cross-flow flow process.
Compared with prior art, its remarkable advantage is in the present invention: (1) has proposed a kind of Pollution abatement and its recovery method as resource of the waste water that produces in a set of intermediate of omeprazole 2-sulfydryl-5-methoxyl group benzo imidazoles production process first.(2) treatment process is easy, and equipment is simple, and the reagent of interpolation only has industrial sulphuric acid, and institute's with medicament is cheap and be easy to get.(3) in water, the refuse clearance is high, and water can reuse.
Embodiment
The following examples can make the present invention of those skilled in the art comprehend.
Embodiment 1
Wastewater source is in the auspicious mattress chemical industry of Yancheng lattice company limited, dark brown red.Main containing NaHS, Na
2s
2, NaS
2o
3and Na
2s, pH=11.6, solid content=29%
(1) to the industrial sulphuric acid that adds 98wt% in waste water solution, dosage is that every square meter waste water adds 120kg, and regulating pH value is 7.5, tail gas absorption H
2s gas, stir the 30min reaction;
(2), after reaction finishes, waste water leaves the heart through 5000 to be separated, and obtains respectively 45kg filter residue and 0.8m
3filtrate; Filtrate is cooled to 8 ℃ and standing 18h, separates out the 300kg saltcake, and saltcake is separated with supernatant liquid; Filter residue, through 500 ℃ of calcinations, obtains Sodium sulfate anhydrous.min(99) 4.15kg, and rate of weight loss is 90.8%;
(3) saltcake obtained in step (2) is dried, and obtains Sodium sulfate anhydrous.min(99);
(4) supernatant liquid obtained in step (2) evaporates through multiple-effect evaporator, and multiple-effect evaporator uses 3 effects, uses the cross-flow flow process, obtains respectively the water of condensation 0.6m that can reuse
3with Sodium sulfate anhydrous.min(99) 117kg.
Embodiment 2
Wastewater source is in the auspicious mattress chemical industry of Yancheng lattice company limited, dark brown red.Main containing NaHS, Na
2s
2, Na
2s
2o
3and Na
2s, pH=12.0, solid content=33%
(1) to the industrial sulphuric acid that adds 98wt% in waste water solution, dosage is that every square meter waste water adds 160kg, and regulating pH value is 6.9, tail gas absorption H
2s gas, stir the 120min reaction;
(2), after reaction finishes, waste water leaves the heart through 5000 to be separated, and obtains respectively 70kg filter residue and 0.8m
3filtrate; Filtrate is cooled to 0 ℃ and standing 48h, separates out the 357kg saltcake, and saltcake is separated with supernatant liquid; Filter residue, through 600 ℃ of calcinations, obtains Sodium sulfate anhydrous.min(99) 5.6kg, and rate of weight loss is 92%;
(3) saltcake obtained in step (2) is dried, and obtains Sodium sulfate anhydrous.min(99) 157.5kg;
(4) supernatant liquid obtained in step (2) evaporates through multiple-effect evaporator, and multiple-effect evaporator uses 3 effects, uses the cross-flow flow process, obtains respectively the water of condensation 0.6m that can reuse
3with Sodium sulfate anhydrous.min(99) 125kg.
Embodiment 3
Wastewater source is in the auspicious mattress chemical industry of Yancheng lattice company limited, dark brown red.Main containing NaHS, Na
2s
2, Na
2s
2o
3and Na
2s, pH=12.2, solid content=31.5%
(1) to the industrial sulphuric acid that adds 98wt% in waste water solution, dosage is that every square meter waste water adds 220kg, and regulating pH value is 6.0, tail gas absorption H
2s gas, stir the 120min reaction;
(2), after reaction finishes, waste water leaves the heart through 6000 to be separated, and obtains respectively 70kg filter residue and 0.8m
3filtrate; Filtrate is cooled to 2 ℃ and standing 24h, separates out the 384kg saltcake, and saltcake is separated with supernatant liquid; Filter residue, through 600 ℃ of calcinations, obtains Sodium sulfate anhydrous.min(99) 6kg, and rate of weight loss is 91.4%;
(3) saltcake obtained in step (2) is dried, and obtains Sodium sulfate anhydrous.min(99) 147kg;
(4) supernatant liquid obtained in step (2) evaporates through multiple-effect evaporator, and multiple-effect evaporator uses 3 effects, uses the cross-flow flow process, obtains respectively the water of condensation 0.6m that can reuse
3with Sodium sulfate anhydrous.min(99) 122kg.
Embodiment 4
Wastewater source is in the auspicious mattress chemical industry of Yancheng lattice company limited, dark brown red.Main containing NaHS, Na
2s
2, Na
2s
2o
3and Na
2s, pH=11.6, solid content=29%
(1) to the industrial sulphuric acid that adds 98wt% in waste water solution, dosage is that every square meter waste water adds 130kg, and regulating pH value is 7.5, tail gas absorption H
2s gas, stir the 90min reaction;
(2) after reaction finishes, waste water separates through press filtration, obtains respectively 50kg filter residue and 0.8m
3filtrate; Filtrate is cooled to 5 ℃ and standing 12h, separates out the 300kg saltcake, and saltcake is separated with supernatant liquid; Filter residue, through 500 ℃ of calcinations, obtains Sodium sulfate anhydrous.min(99) 4kg, and rate of weight loss is 92%;
(3) saltcake obtained in step (2) is dried, and obtains Sodium sulfate anhydrous.min(99) 132kg;
(4) supernatant liquid obtained in step (2) evaporates through multiple-effect evaporator, and multiple-effect evaporator uses 2 effects, uses the cross-flow flow process, obtains respectively the water of condensation 0.6m that can reuse
3with Sodium sulfate anhydrous.min(99) 109kg.
Embodiment 5
Wastewater source is in the auspicious mattress chemical industry of Yancheng lattice company limited, dark brown red.Main containing NaHS, Na
2s
2, Na
2s
2o
3and Na
2s, pH=11.6, solid content=29%
(1) to the industrial sulphuric acid that adds 98wt% in waste water solution, dosage is that every square meter waste water adds 130kg, and regulating pH value is 6.5, tail gas absorption H
2s gas, stir the 100min reaction;
(2) after reaction finishes, waste water separates through press filtration, obtains respectively 55kg filter residue and 0.8m
3filtrate; Filtrate is cooled to 5 ℃ and standing 24h, separates out the 301kg saltcake, and saltcake is separated with supernatant liquid; Filter residue, through 500 ℃ of calcinations, obtains Sodium sulfate anhydrous.min(99) 4.3kg, and rate of weight loss is 92.2%;
(3) saltcake obtained in step (2) is dried, and obtains Sodium sulfate anhydrous.min(99) 132kg;
(4) supernatant liquid obtained in step (2) evaporates through multiple-effect evaporator, and multiple-effect evaporator uses 3 effects, uses the cross-flow flow process, obtains respectively the water of condensation 0.6m that can reuse
3with Sodium sulfate anhydrous.min(99) 109kg.
Claims (3)
1. a kind for the treatment of process of intermediate of omeprazole factory effluent, is characterized in that in described waste water solution, main component comprises NaHS, Na
2s
2, Na
2s
2o
3and Na
2s the treating method comprises following steps:
Step 1, to the industrial sulphuric acid that adds 98wt% in waste water solution, regulating pH value is 6.0 ~ 7.5, tail gas absorption H
2s gas, stirring reaction;
Step 2, after reaction finishes, waste water, through centrifugation or press filtration, obtains respectively filter residue and filtrate; Filtrate is cooled to 0 ~ 8 ℃ and standing 12 ~ 48h, separates out saltcake, and saltcake is separated with supernatant liquid; Filter residue, through 500 ~ 600 ℃ of calcinations, obtains Sodium sulfate anhydrous.min(99);
Step 3, the saltcake obtained in step 2 is dried, and obtains Sodium sulfate anhydrous.min(99);
Step 4, the supernatant liquid obtained in step 2 evaporates through multiple-effect evaporator, obtains respectively water of condensation and the Sodium sulfate anhydrous.min(99) that can reuse.
2. treatment process according to claim 1, it is characterized in that: in step 1, the dosage of industrial sulphuric acid is that every square meter waste water adds 120 ~ 220kg; Churning time is 30 ~ 120min.
3. treatment process according to claim 1, is characterized in that: multiple-effect evaporator use 2 ~ 3 effects described in step 4, use cross-flow flow process.
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|---|---|---|---|
| CN201310419734.9A CN103449654B (en) | 2013-09-16 | 2013-09-16 | Treatment method of Omeprazole intermediate production wastewater |
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|---|---|---|---|
| CN201310419734.9A CN103449654B (en) | 2013-09-16 | 2013-09-16 | Treatment method of Omeprazole intermediate production wastewater |
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Citations (1)
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|---|---|---|---|---|
| CN102887534A (en) * | 2012-11-07 | 2013-01-23 | 广东光华科技股份有限公司 | Method for recovering reagent level anhydrous sodium sulfate from raffinate obtained in process of extracting nickel from nickel sulfate solution |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887534A (en) * | 2012-11-07 | 2013-01-23 | 广东光华科技股份有限公司 | Method for recovering reagent level anhydrous sodium sulfate from raffinate obtained in process of extracting nickel from nickel sulfate solution |
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Effective date of registration: 20161014 Address after: 210094 Xiaolingwei, Jiangsu, No. 200, Patentee after: Nanjing University of Science and Technology Patentee after: Yancheng Green Chemicals Co., Ltd. Address before: 210094 Xiaolingwei, Jiangsu, No. 200, Patentee before: Nanjing University of Science and Technology |
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Granted publication date: 20150311 Termination date: 20200916 |