CN104402804A - Method for recycling pyridine from pharmaceutical waste liquid - Google Patents
Method for recycling pyridine from pharmaceutical waste liquid Download PDFInfo
- Publication number
- CN104402804A CN104402804A CN201410530287.9A CN201410530287A CN104402804A CN 104402804 A CN104402804 A CN 104402804A CN 201410530287 A CN201410530287 A CN 201410530287A CN 104402804 A CN104402804 A CN 104402804A
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- China
- Prior art keywords
- pyridine
- pharmaceutical waste
- waste liquor
- recycling
- waste liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/127—Preparation from compounds containing pyridine rings
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention relates to a method for recycling pyridine from a pharmaceutical waste liquid and belongs to the field of recycling method of wastes. The method for recycling pyridine from the pharmaceutical waste liquid comprises following steps: (1) filtering and pre-treating the pharmaceutical waste liquid; (2) mixing a potassium fluoride solution having a certain concentration with the pre-treated pharmaceutical waste liquid according to a certain mass proportion to obtain a mixture; (3) feeding the mixture to a layering device and allowing the mixture to stand for three hours for layering; (4) feeding a water-enriched phase after layering to an evaporator with steam at 140 DEG C being fed; and (5) recycling concentrated strong salt water back to the layering device for recycling. In the method recycling pyridine from a pharmaceutical waste liquid, the pyridine can be recycled from the pharmaceutical waste liquid through common rectification and a salt-adding phase-separating method are employed. When a mass ratio of the potassium fluoride solution being 60% in concentration and a material composed of 50% of the pyridine and 50% of water is 2.0, purity of the pyridine in an organic phase can reach 92.60%. A separation performance of a potassium fluoride weak solution in the water phase is not influenced after being recycled through the evaporator. The method is simple in process, is convenient to operate and is low in cost.
Description
Technical field
The present invention relates to a kind of method reclaiming pyridine from pharmaceutical waste liquor, belong to recovery and reuse of waste method field.
Background technology
In recent years, successfully develop a kind of novel agrochemical thiodicarb both at home and abroad, due to features such as its good disinsection effect, pesticide residue lack, day by day come into one's own.But this agricultural chemicals must adopt pyridine solvent just can produce up-to-standard thiodicarb product in building-up process, therefore unavoidably will produce pyridine waste water in production process.Pharmacy corporation adopts pyridine solvent, and in production process, every day produces about 8m3 containing pyridine l0%(massfraction) waste water.Because the recovery problem of pyridine in waste water does not solve, cause the pyridine of annual waste nearly ten million yuan, also need to pay very high effluent charge simultaneously.Because pyridine and water form azeotrope system, its azeotropic consists of pyridine: water=57.0:43.0(massfraction), bring very large difficulty to the separation of pyridine-aqueous systems.Domestic existing sodium hydroxide method process pyridine waste water, produces secondary pollution.
Therefore, study a kind of method reclaiming pyridine from pharmaceutical waste liquor that technique is simple, easy to operate, cost is low and there is certain ecnomics and enviroment benefit.
Summary of the invention
The present invention aims to provide a kind of method reclaiming pyridine from pharmaceutical waste liquor that technique is simple, easy to operate, cost is low.
The method reclaiming pyridine from pharmaceutical waste liquor of the present invention, comprises the following steps:
First pharmaceutical waste liquor carried out filtering and carry out pre-treatment, then after certain density potassium fluoride solution being mixed with pretreated pharmaceutical waste liquor by certain mass ratio, introduce in quantizer and leave standstill 3h layering, the later water enrichment phase of layering enters vaporizer and leads to strong brine that 140 DEG C of steam are condensed into and return quantizer and recycle, and the pyridine enrichment phase from quantizer then enters the pyridine solvent that finished pot is used further in pharmacy procedure.
Preferably, potassium fluoride solution concentration of the present invention is mass percent is 60%.
Preferred, the mass ratio of potassium fluoride solution of the present invention and pretreated pharmaceutical waste liquor is 2.0.
Preferred further, the pretreatment process of pharmaceutical waste liquor of the present invention is the pyridine solution obtaining containing 50% pyridine/50% water with conventional distillation from pharmaceutical waste liquor.
The method reclaiming pyridine from pharmaceutical waste liquor of the present invention, when Potassium monofluoride being added pyridine-aqueous systems, due to the salting-out effect of Potassium monofluoride, containing a small amount of water and minute quantity salt in making in formed two-phase pyridine mutually, substantially not containing pyridine in salt aqueous phase, most of water is sloughed in salt aqueous phase, obtains very high separation factor.
Be separated pyridine-aqueous systems with Potassium monofluoride, its objective is the salt containing a small amount of water and minute quantity in making pyridine mutually, the pyridine containing minute quantity in aqueous phase.Our experiments show that, the pyridine under higher Potassium monofluoride concentration in aqueous phase does not detect in chromatogram, pyridine mutually in salt adopt quantitative organism is dried after measure, salts contg is 10
-4magnitude, therefore non-pyridine in aqueous phase in the Liquid-liquid equilibrium data sheet of Pyridine-Water-KF System, salt-free in organic phase, thus the separation reached pyridine in pyridine-aqueous systems and recovery.
In method of the present invention, not easily reclaim due to solid salt in industrial production and recycle, therefore selecting that to be easy to reclaim be that salting-out agent are separated pyridine-aqueous systems with the strong brine recycled.The 60% KF aqueous solution is mixed by certain mass ratio with the material of 50% pyridine/50% water, is divided into two-phase very soon, leave standstill and to measure its two phase composites 25 DEG C time after 3h.Result shows, along with mass ratio increases, the dehydration rate of Potassium monofluoride increases, when mass ratio is increased to 2.5 by 2.0, salt water consumption adds 25%, but the dehydration rate of Potassium monofluoride merely add 1.43 %, therefore mass ratio=2.0 are proper, and under this condition, Potassium monofluoride dehydration rate is 92.01%.This is bright, and in organic phase, the purity of pyridine can reach 92.60%, and in aqueous phase, Potassium monofluoride dilute solution reclaims Posterior circle use through vaporizer does not affect separation performance.
Economic benefit is estimated, every year by the waste liquid containing pyridine 10% producing 300d, every day 8m3, the pyridine rate of recovery is by 95%, and pyridine price is by 50,000 yuan, and the pyridine of recyclable 1,055 ten thousand yuan every year, economic benefit is very considerable.
The method reclaiming pyridine from pharmaceutical waste liquor of the present invention, adopt conventional distillation and phase separation with salt technology can reclaim pyridine from pharmaceutical waste liquor, when the mass ratio of the material of 60% Potassium monofluoride strong solution and 50% pyridine/50% water is 2.0, in organic phase, the purity of pyridine can reach 92.60 %, and in aqueous phase, Potassium monofluoride dilute solution reclaims Posterior circle use through vaporizer does not affect separation performance.The method has the features such as technique is simple, easy to operate, cost is low, opens a new way for pharmaceutical industry reclaims pyridine from pharmaceutical waste liquor.
Embodiment
Embodiment one:
Pharmaceutical waste liquor is filtered, and obtains carrying out pre-treatment containing the pyridine solution of 50% pyridine/50% water from pharmaceutical waste liquor with conventional distillation.
Then by concentration be 60% potassium fluoride solution and pretreated pharmaceutical waste liquor be in mass ratio 2.0 mix after, introduce in quantizer and leave standstill 3h layering, the later water enrichment phase of layering enter vaporizer lead to concentration that 140 DEG C of steam are condensed into be 60% strong brine (potassium fluoride solution) return quantizer and recycle, the pyridine enrichment phase from quantizer then enters the pyridine solvent that finished pot is used further in pharmacy procedure.
Embodiment two: recovering effect
Use the method reclaiming pyridine from pharmaceutical waste liquor of the present invention, recovery pyridine is carried out to the pharmaceutical waste liquor containing 10% pyridine, first from pharmaceutical waste liquor, obtain the pyridine solution containing 50% pyridine/50% water with conventional distillation, reclaim by different mass ratioes from 50% pyridine/50% water by 60% Potassium monofluoride strong solution, recovering effect as shown in Table-1 again.
Table-1 recovering effect
Claims (4)
1. from pharmaceutical waste liquor, reclaim the method for pyridine, comprise the following steps:
First pharmaceutical waste liquor carried out filtering and carry out pre-treatment, then after certain density potassium fluoride solution being mixed with pretreated pharmaceutical waste liquor by certain mass ratio, introduce in quantizer and leave standstill 3h layering, the later water enrichment phase of layering enters vaporizer and leads to strong brine that 140 DEG C of steam are condensed into and return quantizer and recycle, and the pyridine enrichment phase from quantizer then enters the pyridine solvent that finished pot is used further in pharmacy procedure.
2. from pharmaceutical waste liquor, reclaim as claimed in claim 1 the method for pyridine, it is characterized in that described potassium fluoride solution concentration be mass percent is 60%.
3. from pharmaceutical waste liquor, reclaim the method for pyridine as claimed in claim 1, it is characterized in that the mass ratio of described potassium fluoride solution and pretreated pharmaceutical waste liquor is 2.0.
4. from pharmaceutical waste liquor, reclaim the method for pyridine as claimed in claim 1, it is characterized in that the pretreatment process of described pharmaceutical waste liquor is the pyridine solution obtaining containing 50% pyridine/50% water with conventional distillation from pharmaceutical waste liquor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410530287.9A CN104402804A (en) | 2014-10-10 | 2014-10-10 | Method for recycling pyridine from pharmaceutical waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410530287.9A CN104402804A (en) | 2014-10-10 | 2014-10-10 | Method for recycling pyridine from pharmaceutical waste liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104402804A true CN104402804A (en) | 2015-03-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410530287.9A Pending CN104402804A (en) | 2014-10-10 | 2014-10-10 | Method for recycling pyridine from pharmaceutical waste liquid |
Country Status (1)
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| CN (1) | CN104402804A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382831A (en) * | 2017-09-22 | 2017-11-24 | 湖北竹溪人福药业有限责任公司 | A kind of processing method for reclaiming pyridine |
| CN107474010A (en) * | 2016-06-08 | 2017-12-15 | 苏州长征－欣凯制药有限公司 | pyridine waste liquid treatment process |
| CN116332836A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Method for recovering pyridine waste solvent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5100514A (en) * | 1991-03-01 | 1992-03-31 | Lloyd Berg | Separation of pyridine from water by extractive distillation |
| CN101074211A (en) * | 2007-06-18 | 2007-11-21 | 浙江工业大学 | Process for treating high-purity pyridine solution |
| CN103992264A (en) * | 2014-04-25 | 2014-08-20 | 上海新华联制药有限公司 | Method for recovering pyridine from aqueous solution |
-
2014
- 2014-10-10 CN CN201410530287.9A patent/CN104402804A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5100514A (en) * | 1991-03-01 | 1992-03-31 | Lloyd Berg | Separation of pyridine from water by extractive distillation |
| CN101074211A (en) * | 2007-06-18 | 2007-11-21 | 浙江工业大学 | Process for treating high-purity pyridine solution |
| CN103992264A (en) * | 2014-04-25 | 2014-08-20 | 上海新华联制药有限公司 | Method for recovering pyridine from aqueous solution |
Non-Patent Citations (1)
| Title |
|---|
| 许文友 等: "用氟化钾水溶液从制药废液中回收吡啶", 《环境科学与技术》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107474010A (en) * | 2016-06-08 | 2017-12-15 | 苏州长征－欣凯制药有限公司 | pyridine waste liquid treatment process |
| CN107474010B (en) * | 2016-06-08 | 2022-05-13 | 苏州长征－欣凯制药有限公司 | Pyridine waste liquid treatment process |
| CN107382831A (en) * | 2017-09-22 | 2017-11-24 | 湖北竹溪人福药业有限责任公司 | A kind of processing method for reclaiming pyridine |
| CN116332836A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Method for recovering pyridine waste solvent |
| CN116332836B (en) * | 2022-07-28 | 2024-03-26 | 四川熔增环保科技有限公司 | Method for recovering pyridine waste solvent |
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Application publication date: 20150311 |
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