CN104230851A - Method for recovering N-methylmorpholine from valnemulin hydrochloride synthesis wastewater - Google Patents
Method for recovering N-methylmorpholine from valnemulin hydrochloride synthesis wastewater Download PDFInfo
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- CN104230851A CN104230851A CN201410455849.8A CN201410455849A CN104230851A CN 104230851 A CN104230851 A CN 104230851A CN 201410455849 A CN201410455849 A CN 201410455849A CN 104230851 A CN104230851 A CN 104230851A
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- methylmorpholine
- valnemulin hydrochloride
- synthetic wastewater
- valnemulin
- hydrochloride synthetic
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
- C07D295/027—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements containing only one hetero ring
- C07D295/03—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements containing only one hetero ring with the ring nitrogen atoms directly attached to acyclic carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
- C07D295/023—Preparation; Separation; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for recovering N-methylmorpholine from a valnemulin hydrochloride synthesis wastewater. The method is characterized by comprising the following steps: firstly, adjusting pH of valnemulin hydrochloride reaction quenching wastewater to 9-11, and then extracting by using an organic solvent; separating liquid and collecting an organic phase; drying the obtained organic phase by using a drying agent; and finally heating up, rectifying, and collecting fraction with the temperature of 115-116 DEG C. According to the method for recovering the N-methylmorpholine from the valnemulin hydrochloride synthesis wastewater disclosed by the invention, a relatively simple method is adopted to recycle N-methylmorpholine, and waste is changed into treasures, so that the cost of raw materials is reduced, meanwhile, the content of pollutants in sewage discharged is reduced, the environmental pollution is reduced, the method is beneficial to sustainable development of production, the content of the recycled N-methylmorpholine is greater than 98.0% and the recovery rate is higher than 95%.
Description
Technical field
The invention belongs to pharmaceutical chemistry technical field, be specifically related to a kind of method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater.
Background technology
Valnemulin (Valnemulin) is the novel animal specific microbiotic of the semi-synthetic wide spectrum of a kind of pleuromulins, for the disease such as chronic respiratory tract infection of prevention and therapy Streptococcus suis, porcine enzootic pneumonia, swine dysentery, hog middle spirochetosis and porcine proliferative enteronitis, chicken.The building-up process of valnemulin take pleuromutilin as raw material; first pleuromutilin is converted into sulfonation pleurin; again sulfonation pleurin and diethylin Mercaptamine are reacted obtained intermediate A; D-Val and methyl acetoacetate react obtained intermediate B; intermediate B and Vinyl chloroformate effect are reacted with intermediate A again, then through going protection to obtain valnemulin.When end reaction synthesis valnemulin, used N-methylmorpholine, its Main Function is acid binding agent, impels reaction forward to carry out, and with hydrogenchloride acid-base neutralisation in reaction, agent structure does not change, and discharges after reaction with waste water.Increase wastewater treatment difficulty like this, discharged valuable industrial chemicals N-methylmorpholine simultaneously, if N-methylmorpholine can be reclaimed, not only can the content of the dirty water pollutant of emissions reduction, reduce environmental pollution and wastewater treatment difficulty, obtain social influence, simultaneously can be cost-saving, obtain certain economic benefit.
Summary of the invention
Object of the present invention is just to provide a kind of method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater.The method achieve the recycling of valnemulin synthesis material, and decrease the content of pollutent in sewage effluent, while reducing environmental pollution, save production cost.
For achieving the above object, the technical scheme adopted is:
A kind of method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater, it is characterized in that: first valnemulin hydrochloride is reacted cancellation waste water and adjust pH9 ~ 11, then extract with organic solvent, separatory collects organic phase, the organic phase of gained is used desiccant dryness, finally heat up rectifying, collects the cut of collection 115 DEG C ~ 116 DEG C.
During described tune pH, material used is sodium hydroxide, potassium hydroxide or ammoniacal liquor.
Described organic solvent is methyl tertiary butyl ether, benzene or toluene.
Described organic solvent is methyl tertiary butyl ether.
Described extraction 1 ~ 3 time, extraction liquid consumption is respectively 1/8 ~ 1/4 of waste water cumulative volume.
Described siccative is anhydrous sodium sulphate, Calcium Chloride Powder Anhydrous or anhydrous magnesium sulfate, and consumption is 5% of solvent for use volume.
During described intensification rectifying, adopt Webster rectifying column or glass filler rectifying column.The N-methylmorpholine content reclaiming acquisition through the present invention is greater than 98.0%, and the rate of recovery is higher than 95%.
The method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater of the present invention, have employed comparatively simple method and recycling is carried out to N-methylmorpholine, turn waste into wealth, reduce raw materials cost, decrease the content of pollutent in sewage effluent simultaneously, reduce environmental pollution, to producing the meaning with Sustainable development.
Embodiment
Be explained the present invention with example below, it should be understood that example is for illustration of the present invention instead of limitation of the present invention.Scope of the present invention and core content are determined according to claims.
Waste water described in following instance reacts the waste water that cancellation produces in valnemulin hydrochloride synthesis.
Embodiment 1
Get valnemulin hydrochloride reaction cancellation waste water 200mL, adjust pH to 11 with 20% sodium hydroxide, use benzene to extract, extraction times is three times, and each benzene consumption is respectively 50mL, 25mL, 25mL.Extracted rear combined benzene phase, carried out drying with anhydrous magnesium sulfate, consumption is 5g.Cross and filter siccative, benzene heats up mutually, uses Webster distillation column to carry out rectifying, collects capital 115 ~ 116 DEG C of cuts.Finally reclaim N-methylmorpholine 10.65mL (charging capacity 11.10mL), the rate of recovery 96.0%, content 98.6%.
Embodiment 2
Get valnemulin hydrochloride reaction cancellation waste water 300mL, adjust pH to 10 with strong aqua, use toluene to extract, extraction times is three times, and each benzene consumption is respectively 70mL, 40mL, 40mL.Extracted rear combining methylbenzene phase, carried out drying with anhydrous magnesium sulfate, consumption is 7.5g.Cross and filter siccative, toluene heats up mutually, uses glass filler rectifying column to carry out rectifying, collects capital 115 ~ 116 DEG C of cuts.Finally reclaim N-methylmorpholine 15.84mL (charging capacity 16.64mL), the rate of recovery 95.2%, content 98.1%.
Embodiment 3
Get valnemulin hydrochloride reaction cancellation waste water 500mL, adjust pH to 11 with 20% sodium hydroxide, use methyl tertiary butyl ether to extract, extraction times is three times, and each methyl tertiary butyl ether consumption is respectively 125mL, 65mL, 65mL.Extracted rear combined ether phase, carried out drying by anhydrous sodium sulphate, consumption is 13g.Cross and filter siccative, ether heats up mutually, uses Webster distillation column to carry out rectifying, collects capital 115 ~ 116 DEG C of cuts.Finally reclaim N-methylmorpholine 26.84mL (charging capacity 27.73mL), the rate of recovery 96.8%, content 98.9%.
Embodiment 4
Get valnemulin hydrochloride reaction cancellation waste water 500mL, adjust pH to 10.5 with 20% potassium hydroxide, use methyl tertiary butyl ether to extract, extraction times is three times, and each methyl tertiary butyl ether consumption is respectively 125mL, 65mL, 65mL.Extracted rear combined ether phase, carried out drying with Calcium Chloride Powder Anhydrous, consumption is 13g.Cross and filter siccative, ether heats up mutually, uses glass filler rectifying column to carry out rectifying, collects capital 115 ~ 116 DEG C of cuts.Finally reclaim N-methylmorpholine 26.92mL (charging capacity 27.73mL), the rate of recovery 97.1%, content 98.8%.
Claims (7)
1. one kind is reclaimed the method for N-methylmorpholine from valnemulin hydrochloride synthetic wastewater, it is characterized in that: first valnemulin hydrochloride is reacted cancellation waste water and adjust pH9 ~ 11, then extract with organic solvent, separatory collects organic phase, the organic phase of gained is used desiccant dryness, finally heat up rectifying, collects the cut of collection 115 DEG C ~ 116 DEG C.
2., according to the method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater according to claim 1, when it is characterized in that described tune pH, material used is sodium hydroxide, potassium hydroxide or ammoniacal liquor.
3., according to the method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater according to claim 1, it is characterized in that described organic solvent is methyl tertiary butyl ether, benzene or toluene.
4., according to the method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater described in claim 1 or 3, it is characterized in that described organic solvent is methyl tertiary butyl ether.
5., according to the method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater according to claim 1, it is characterized in that described extraction 1 ~ 3 time, extraction liquid consumption is respectively 1/8 ~ 1/4 of waste water cumulative volume.
6., according to the method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater according to claim 1, it is characterized in that described siccative is anhydrous sodium sulphate, Calcium Chloride Powder Anhydrous or anhydrous magnesium sulfate, consumption is 5% of solvent for use volume.
7., according to the method reclaiming N-methylmorpholine from valnemulin hydrochloride synthetic wastewater according to claim 1, when it is characterized in that described intensification rectifying, adopt Webster rectifying column or glass filler rectifying column.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410455849.8A CN104230851A (en) | 2014-09-10 | 2014-09-10 | Method for recovering N-methylmorpholine from valnemulin hydrochloride synthesis wastewater |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410455849.8A CN104230851A (en) | 2014-09-10 | 2014-09-10 | Method for recovering N-methylmorpholine from valnemulin hydrochloride synthesis wastewater |
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| CN104230851A true CN104230851A (en) | 2014-12-24 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030089591A1 (en) * | 2001-10-30 | 2003-05-15 | Andreas Wolfert | Process for fractionating water-containing crude amine mixtures from amine synthesis |
| CN101735123A (en) * | 2009-12-22 | 2010-06-16 | 山东胜利股份有限公司 | Method for synthesizing valnemulin hydrochloride |
| CN101993400A (en) * | 2009-08-17 | 2011-03-30 | 北京中牧科技服务有限责任公司 | Valnemulin synthesis method |
| CN102532060A (en) * | 2011-07-28 | 2012-07-04 | 吉林化工学院化工分离技术开发中心 | Novel process for recovering N-methyl morpholine and N-ethyl morpholine |
| CN103382172A (en) * | 2013-06-20 | 2013-11-06 | 中国农业科学院兰州畜牧与兽药研究所 | Synthesis method for valnemulin hydrochloride |
-
2014
- 2014-09-10 CN CN201410455849.8A patent/CN104230851A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030089591A1 (en) * | 2001-10-30 | 2003-05-15 | Andreas Wolfert | Process for fractionating water-containing crude amine mixtures from amine synthesis |
| CN101993400A (en) * | 2009-08-17 | 2011-03-30 | 北京中牧科技服务有限责任公司 | Valnemulin synthesis method |
| CN101735123A (en) * | 2009-12-22 | 2010-06-16 | 山东胜利股份有限公司 | Method for synthesizing valnemulin hydrochloride |
| CN102532060A (en) * | 2011-07-28 | 2012-07-04 | 吉林化工学院化工分离技术开发中心 | Novel process for recovering N-methyl morpholine and N-ethyl morpholine |
| CN103382172A (en) * | 2013-06-20 | 2013-11-06 | 中国农业科学院兰州畜牧与兽药研究所 | Synthesis method for valnemulin hydrochloride |
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Application publication date: 20141224 |