CN103833180B - The treatment process of Yi Zhong oxazole method synthesise vitamins B6 waste water - Google Patents
The treatment process of Yi Zhong oxazole method synthesise vitamins B6 waste water Download PDFInfo
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- CN103833180B CN103833180B CN201310576862.4A CN201310576862A CN103833180B CN 103833180 B CN103833180 B CN 103833180B CN 201310576862 A CN201310576862 A CN 201310576862A CN 103833180 B CN103833180 B CN 103833180B
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Abstract
The treatment process of Yi Zhong oxazole method synthesise vitamins B6 waste water, is characterized in that: is Jiang the separately process of each operation waste water of oxazole method synthesise vitamins B6.By high for 4-methyl-5-Yi Yang Ji oxazole operation cyclization workshop section COD concentration, color and luster is dark, containing the waste water individual curing of high concentration phosphorus hydrochlorate, add calcium chloride wherein, generate calcium phosphate precipitation, solid-liquid separation, after the liquid obtained adds sulfuric acid tune pH value, add ferrous sulfate and hydrogen peroxide stirring, after hydro-oxidation sodium adjusts pH value, merge other operation waste water and enter biochemistry pool process, qualified discharge.Present method has reformed traditional high investment, high cost, the vitamin B6 method of wastewater treatment that step is numerous and diverse, solve that vitamin B6 wastewater treatment capacity is large, difficulty is high, the difficult problem up to standard of processed waste water, and energy-conserving and environment-protective, simple, with low cost, the vitamin B6 waste water after process reaches " chemosynthesis class pharmaceutical industry pollution discharge standard " (GB1904-2008).
Description
Technical field
The present invention relates to a kind of method of wastewater treatment, relate to the treatment process of oxazole method synthesise vitamins B6 waste water especially.
Background technology
Vitamin B6 is one of VITAMIN of needed by human, is body fat and glycometabolic required material, is the moiety of some coenzyme in human body, participates in multiple metabolic reaction, be widely used in medicine, food, fodder additives and cosmetic industry field.At present, general Cai is by Xian Jin oxazole (4-methyl-5-Yi Yang Ji oxazole) method technology generations for old road line pyridone method both at home and abroad, makes vitamin B6 production technique reach new height.Its main processes is divided into three operations: esterification prepares N-ethoxy oxalyl alanine ethyl ester; Ring-closure reaction prepares 4-methyl-5-Yi Yang Ji oxazole; The preparation of vitamin B6 crude product is with refining.
N-ethoxy oxalyl alanine ethyl ester and vitamin B6 crude product prepare the waste water that the waste water produced with refining two operations is mainly Distillation recovery, easily process.And 4-methyl-5-Yi Yang Ji oxazole carries out ring-closure reaction by N-ethoxy oxalyl alanine ethyl ester and phosphorus oxychloride, triethylamine, toluene, after extracting and demixing, alkaline hydrolysis, acidifying, decarboxylation obtain.Produce a large amount of waste water containing organic pigment, impurity and high density salinity in this step operation cyclization workshop section production process, wastewater treatment difficulty is large, be produce in vitamin B6 each procedure technology factory effluent the most reluctant.
The factory effluent of the non-individual curing 4-methyl of conventional vitamin B6 wastewater treatment-5-Yi Yang Ji oxazole operation cyclization workshop section, but adopt concentrated each operation waste water, electrolytic process used in combination, biochemical process or combined method process, other operations can be processed by simply dealt a large amount of waste water together with not tractable 4-methyl-5-second oxygen base oxazole operation cyclization workshop section factory effluent, cause process the water yield large, difficulty is high, costly, treatment process very complicated, the waste water after process is difficult to the situation reaching emission standard.
Summary of the invention
The object of the present invention is to provide the treatment process of Yi Zhong oxazole method synthesise vitamins B6 waste water.The technique of the method Zhen Dui oxazole method synthesise vitamins B6 and each operation produce the feature of waste water, after 4-methyl-5-Yi Yang Ji oxazole operation cyclization workshop section factory effluent individual curing, He Bing oxazole method synthesise vitamins B6 produces other workshop sections and operation easily processes waste water again, after proceeding to biochemistry pool process, qualified discharge.Present method looks for another way, reform the numerous and diverse and treatment process of high cost, high investment of traditional step, Xie Jue oxazole method synthesise vitamins B6 production wastewater treatment amount is large, difficulty is high, waste water after process is difficult to the common problem reaching emission standard, and high-efficiency environment friendly, save energy, step is simple, easy handling, with low cost, the vitamin B6 waste water after process reaches " chemosynthesis class pharmaceutical industry pollution discharge standard " (GB1904-2008).
The treatment process that the invention provides Yi Zhong oxazole method synthesise vitamins B6 waste water is as follows: 4-methyl-5-Yi Yang Ji oxazole operation cyclization workshop section produces the mother liquor produced, after adding sodium hydroxide and dissociate and isolating triethylamine, obtain containing high concentration phosphorus hydrochlorate waste water, COD concentration is: 4.0 × 10
4~ 5.0 × 10
4mg/L, phosphate content is 4.0 ~ 5.0%(mass percent concentration), color and luster is dark, and intractability is large.Calcium chloride is added in waste water, it is made to transfer calcium phosphate precipitation to, adopt conventional separation method, as: centrifuge or board and frame machine press filtration or pressure filter press filtration, make solid-liquid separation, liquid adds sulfuric acid again and regulates pH value to be 3.0 ~ 5.0, preferably 3.5, add the ferrous sulfate that mass percent is the treatment solution scale of construction 0.1 ~ 5.0% subsequently, preferably 0.2 ~ 3.0%, add the 30%(mass percent concentration that mass percent is the treatment solution scale of construction 0.5 ~ 10.0% again) the aqueous solution of hydrogen peroxide, preferably 3.0 ~ 5.0%, mix and blend is after 12 ~ 15 hours, adding sodium hydroxide regulates pH value to be 8.0 ~ 9.0, obtain light yellow after process, COD concentration is: 3000 ~ 3300 mg/L, phosphate content is≤1.0%(mass percent concentration) liquid, merge other operation waste water and proceed to biochemistry pool process, qualified discharge after process.
Embodiment
Embodiment one
One ton of 4-methyl-5-Yi Yang Ji oxazole preparation section cyclization workshop section produces the processed waste water isolating triethylamine produced, and dark red, COD concentration is 4.25 × 10
4mg/L, phosphate content is 4.17%(mass percent concentration), add 75kg calcium chloride and carry out neutralization reaction, time controling 2 hours, temperature of reaction controls at 50 ~ 65 DEG C, be 7.0 to pH value, centrifuge is adopted to carry out solid-liquid separation, after being separated, liquid keeps 25 ~ 30 DEG C, adding sulfuric acid under whipped state regulates pH value to be 3.5, continue maintenance 25 ~ 30 DEG C subsequently, add 2kg ferrous sulfate, stir after 30 minutes, add 30%(mass percent concentration) the aqueous solution 35kg of hydrogen peroxide, keep 25 ~ 30 DEG C of mix and blends after 12 hours, adding sodium hydroxide regulates pH value to be 8.0, obtain light yellow, COD concentration is 3200 mg/L, phosphate content is 0.85%(mass percent concentration) liquid, merge other operation waste water and proceed to biochemistry pool, water colorless clarification after process, COD concentration is 95 mg/L, phosphate content is 0.45%(mass percent concentration), qualified discharge.
Embodiment two
Two tons of 4-methyl-5-Yi Yang Ji oxazole preparation section cyclization workshop sections produce the processed waste water isolating triethylamine produced, and dark red, COD concentration is 4.85 × 10
4mg/L, phosphate content is 4.52%(mass percent concentration), add 160kg calcium chloride and carry out neutralization reaction, time controling 2 hours, temperature of reaction controls at 50 ~ 65 DEG C, be 7.2 to pH value, board and frame machine press filtration is adopted to carry out solid-liquid separation, after being separated, liquid keeps 25 ~ 30 DEG C, adding sulfuric acid under whipped state regulates pH value to be 3.5, continue maintenance 25 ~ 30 DEG C subsequently, add 20kg ferrous sulfate, stir after 30 minutes, add 30%(mass percent concentration) the aqueous solution 76kg of hydrogen peroxide, keep 25 ~ 30 DEG C of mix and blends after 13 hours, adding sodium hydroxide regulates pH value to be 8.5, , obtain light yellow, COD concentration is 3100 mg/L, phosphate content is 0.75%(mass percent concentration) liquid, merge other operation waste water and proceed to biochemistry pool, water colorless clarification after process, COD concentration is 90 mg/L, phosphate content is 0.40%(mass percent concentration), qualified discharge.
Embodiment three
Five tons of 4-methyl-5-Yi Yang Ji oxazole preparation section cyclization workshop sections produce the processed waste water isolating triethylamine produced, and dark red, COD concentration is 4.60 × 10
4mg/L, phosphate content is 4.20%(mass percent concentration), add 370kg calcium chloride and carry out neutralization reaction, time controling 2 hours, temperature of reaction controls at 50 ~ 65 DEG C, be 7.2 to PH, pressure filter press filtration is adopted to carry out solid-liquid separation, after being separated, liquid keeps 25 ~ 30 DEG C, adding sulfuric acid under whipped state regulates pH value to be 3.8, continue maintenance 25 ~ 30 DEG C subsequently, add 75kg ferrous sulfate, stir after 30 minutes, add 30%(mass percent concentration) the aqueous solution 200kg of hydrogen peroxide, keep 25 ~ 30 DEG C of mix and blends after 15 hours, adding sodium hydroxide regulates pH value to be 9.0, obtain light yellow, COD concentration is 3200 mg/L, phosphate content is 0.80%(mass percent concentration) liquid, merge other operation waste water and proceed to biochemistry pool, water colorless clarification after process, COD concentration is 90 mg/L, phosphate content is 0.42%(mass percent concentration), qualified discharge.
Claims (2)
1. oxazole method synthesise vitamins B6 is produced the separately process of each master operation waste water by the treatment process: of Yi Zhong oxazole method synthesise vitamins B6 waste water, oxazole method synthesise vitamins B6 prepares the waste water of 4-methyl-5-Yi Yang Ji oxazole operation cyclization workshop section in producing, its COD concentration is high, color and luster is dark, containing high salt concentration, in the mother liquor of 4-methyl-5-Yi Yang Ji oxazole operation cyclization workshop section, add sodium hydroxide to dissociate and after isolating triethylamine, obtain the waste water containing high concentration phosphorus hydrochlorate, add calcium chloride, it is made to transfer calcium phosphate precipitation to, adopt conventional separation methods, carry out solid-liquid separation, after the liquid that separation obtains adds sulfuric acid adjustment pH value, add ferrous sulfate and hydrogen peroxide successively, after mix and blend, after adding sodium hydroxide adjustment pH value again, merge other operations and workshop section easily to process waste water and proceed to biochemistry pool, qualified discharge after process.
2. the method for claim 1, it is characterized in that making it be converted into calcium phosphate precipitation adding calcium chloride, time controling 2 hours, temperature of reaction controls, at 50 ~ 65 DEG C, to reach 7.0 ~ 7.2 judge reaction end with pH value.
3. the method for claim 1, is characterized in that the conventional separation methods that separation calcium phosphate precipitation adopts is centrifuge or pressure filter press filtration.
4. the method for claim 1, the liquid obtained after it is characterized in that being separated calcium phosphate precipitation adds sulfuric acid and regulates pH value to be 3.0 ~ 5.0 under whipped state, and temperature is 25 ~ 30 DEG C.
5. the method for claim 1, it is characterized in that adding sulfuric acid regulates pH value to be after 3.0 ~ 5.0, keep temperature 25 ~ 30 DEG C, add the ferrous sulfate that mass percent is the treatment solution scale of construction 0.1 ~ 5.0%, stir after 30 minutes, to add mass percent be the mass percent concentration of the treatment solution scale of construction 0.5 ~ 10.0% is the aqueous solution of the hydrogen peroxide of 30%, mix and blend 12 hours ~ 15 hours.
6. the method for claim 1, is characterized in that the liquid of mix and blend after 12 ~ 15 hours, adds sodium hydroxide and regulates pH value to be after 8.0 ~ 9.0, merges other workshop sections and operation and easily processes waste water and proceed to biochemistry pool, qualified discharge after process.
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| CN106832223B (en) * | 2016-12-29 | 2018-11-06 | 武汉工程大学 | The black paste generated in vitamin B6 industrial processes is in anticorrosive paint as the application of curing agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329048A (en) * | 2011-08-11 | 2012-01-25 | 湖北惠生药业有限公司 | Method for treating wastewater produced during chemical synthesis of vitamin B6 |
| CN102583867A (en) * | 2012-03-20 | 2012-07-18 | 石家庄杰克化工有限公司 | Method for treating waste water in chloro pyrimidine combining process |
| CN103011481A (en) * | 2012-11-30 | 2013-04-03 | 华中药业股份有限公司 | Method for treating production waste liquid of vitamin B1 and obtaining byproducts |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329048A (en) * | 2011-08-11 | 2012-01-25 | 湖北惠生药业有限公司 | Method for treating wastewater produced during chemical synthesis of vitamin B6 |
| CN102583867A (en) * | 2012-03-20 | 2012-07-18 | 石家庄杰克化工有限公司 | Method for treating waste water in chloro pyrimidine combining process |
| CN103011481A (en) * | 2012-11-30 | 2013-04-03 | 华中药业股份有限公司 | Method for treating production waste liquid of vitamin B1 and obtaining byproducts |
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