CN104193642B - A kind of spectrasolv DMDA vacuum distilling takes off method and the system thereof of amine - Google Patents
A kind of spectrasolv DMDA vacuum distilling takes off method and the system thereof of amine Download PDFInfo
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- CN104193642B CN104193642B CN201410421964.3A CN201410421964A CN104193642B CN 104193642 B CN104193642 B CN 104193642B CN 201410421964 A CN201410421964 A CN 201410421964A CN 104193642 B CN104193642 B CN 104193642B
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Abstract
The invention provides a kind of N, N dimethyldecamide vacuum distilling and take off method and the system thereof of amine, comprise the following steps: by vacuum pump by the N containing dimethylamine, N dimethyldecamide inspiration distillating still；Under vacuum, ON cycle product pump, material in distillating still is carried out decompression distillation, and by spray column, the fraction of distillating still is carried out Sprayer Circulation；The one-tenth distilled by distillating still is switched to dimethylamine absorption plant, absorbs dimethylamine；Sample analysis, until sample, without dimethylamine, is cooled to room temperature, blowing, obtains the N without dimethylamine, N dimethyldecamide product.The present invention under vacuum, utilizes distillating still that the N containing dimethylamine, N dimethyldecamide material carries out decompression distillation, and use spray column Sprayer Circulation, ensure that the vacuum of the de-amine device of distillation, it is possible to effectively remove the dimethylamine in N, N dimethyldecamide.The method of the present invention is rationally effective, low cost, and de-amine is effective.
Description
Technical field
The invention belongs to chemical technology field, take off method and the system for use in carrying thereof of amine particularly to a kind of spectrasolv DMDA vacuum distilling.
Background technology
Spectrasolv DMDA, colourless transparent liquid, purposes: surfactant；Organic synthesis solvent is in order to medicine, veterinary drug, pesticide, cosmetics etc..
After spectrasolv DMDA typically uses capric acid and dimethylamine to react prepared spectrasolv DMDA crude product, obtain purity after rectification under vacuum and be not less than the spectrasolv DMDA product of 99%.But, owing to wherein containing the dimethylamine of trace, have obvious amine taste, the easy its colour changed into yellow color and the time lengthens, quality variation.
Colourless to the slightly yellow transparency liquid of quality criteria requirements of spectrasolv DMDA finished product, without amine taste.
Summary of the invention
It is an object of the invention to provide a kind of method that spectrasolv DMDA vacuum distilling takes off amine, to solve present in prior art in spectrasolv DMDA product containing dimethylamine, its colour changed into yellow caused, quality variation problem.
For achieving the above object, the present invention is by the following technical solutions:
A kind of method that spectrasolv DMDA vacuum distilling takes off amine, comprises the following steps:
A. by vacuum pump by the spectrasolv DMDA inspiration distillating still containing dimethylamine；
The most under vacuum, ON cycle product pump, material in distillating still is carried out decompression distillation, and by spray column, the fraction of distillating still is carried out Sprayer Circulation；
C. the one-tenth that distillating still distills is switched to dimethylamine absorption plant, absorbs dimethylamine；
D. sample analysis, until sample, without dimethylamine, is cooled to room temperature, blowing, obtains the spectrasolv DMDA product without dimethylamine.
Preferably, in described step b, vacuum distillation temperature controls less than or equal to 50 DEG C.
Preferably, in described step b, vacuum degree control is more than or equal to-0.09Mpa.
Present invention also offers the spectrasolv DMDA vacuum distilling for said method and take off amine system, technical scheme is as follows:
A kind of N for above-mentioned method, N-dimethyldecamide vacuum distilling takes off amine system, it is made up of vacuum pump, vacuum buffer tank, distillating still, recycle stock pump, spray column, the bottom of described distillating still is provided with baiting valve, the top of described distillating still arranges spray column, the bottom of distillating still connects recycle stock pump by pipeline, recycle stock pump is connected with spray column by pipeline, spray column, vacuum buffer tank, vacuum pump pass sequentially through pipeline and connect, and vacuum pump connects dimethylamine absorption plant by pipeline；Described recycle stock pump is provided with probe tube on the connecting line of spray column.
Preferably, described vacuum pump is oilless vertical vacuum pump.
Preferably, described recycle stock pump is magnetic drive pump.
The invention has the beneficial effects as follows: the present invention is under vacuum, utilize distillating still to the N containing dimethylamine, N-dimethyldecamide material carries out decompression distillation, and use spray column Sprayer Circulation, ensure that the vacuum of the de-amine device of distillation, can effectively remove N, dimethylamine in N-dimethyldecamide, obtain meeting the finished product N of quality standard, N-dimethyldecamide, and distillating still is distilled mainly contain dimethylamine and a small amount of water become to be switched to dimethylamine absorption plant, absorb dimethylamine.The method of the present invention is rationally effective, low cost, and de-amine is effective.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention.
In figure, 1-vacuum pump, 2-vacuum buffer tank 2,3-distillating still, 4-spray column, 5-recycle stock pump, 6-vacuum meter, 7-air bleeding valve, 8-baiting valve, 9-Pressure gauge, 10-probe tube, 11-samples valve, and 12-regulates valve.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment
1
N, N-dimethyldecamide product is carried out de-amine.
By vacuum pump by the spectrasolv DMDA inspiration distillating still containing dimethylamine；Under vacuum, ON cycle product pump, material in distillating still is carried out decompression distillation, and by spray column, the fraction of distillating still is carried out Sprayer Circulation, vacuum distillation temperature controls at 50 DEG C, and vacuum degree control is at-0.09Mpa；The one-tenth distilled by distillating still is switched to dimethylamine absorption plant, absorbs dimethylamine；Sample analysis, until sample, without dimethylamine, is cooled to room temperature, blowing, obtains the spectrasolv DMDA product without dimethylamine.
Embodiment
2
N, N-dimethyldecamide product is carried out de-amine.
By vacuum pump by the spectrasolv DMDA inspiration distillating still containing dimethylamine；Under vacuum, ON cycle product pump, material in distillating still is carried out decompression distillation, and by spray column, the fraction of distillating still is carried out Sprayer Circulation, vacuum distillation temperature controls at 30 DEG C, and vacuum degree control is at-0.20Mpa；The one-tenth distilled by distillating still is switched to dimethylamine absorption plant, absorbs dimethylamine；Sample analysis, until sample, without dimethylamine, is cooled to room temperature, blowing, obtains the spectrasolv DMDA product without dimethylamine.
Embodiment
3
N, N-dimethyldecamide product is carried out de-amine.
By vacuum pump by the spectrasolv DMDA inspiration distillating still containing dimethylamine；Under vacuum, ON cycle product pump, material in distillating still is carried out decompression distillation, and by spray column, the fraction of distillating still is carried out Sprayer Circulation, vacuum distillation temperature controls at 40 DEG C, and vacuum degree control is at-0.10Mpa；The one-tenth distilled by distillating still is switched to dimethylamine absorption plant, absorbs dimethylamine；Sample analysis, until sample, without dimethylamine, is cooled to room temperature, blowing, obtains the spectrasolv DMDA product without dimethylamine.
Embodiment
4
For above-described embodiment spectrasolv DMDA vacuum distilling take off amine system.
As shown in Figure 1, this system is formed by by vacuum pump 1, vacuum buffer tank 2, distillating still 3, recycle stock pump 5, spray column 4, the bottom of distillating still 3 is provided with baiting valve 8, the top of described distillating still 3 arranges spray column 4, the bottom of distillating still 3 connects recycle stock pump 5 by pipeline, recycle stock pump 5 is connected with spray column 4 by pipeline, and spray column 4, vacuum buffer tank 2, vacuum pump 1 pass sequentially through pipeline and connect, and vacuum pump 1 connects dimethylamine absorption plant by pipeline；It is provided with probe tube 10 on recycle stock pump 5 and the connecting line of spray column 4, and is provided with sampling valve 11.
Being provided with vacuum meter 6 on vacuum buffer tank 2, the bottom of vacuum buffer tank 2 is provided with air bleeding valve 7.Vacuum buffer tank 2 plays buffering and the effect of gas-liquid separation.
Recycle stock pump 5 is provided with Pressure gauge 9 on the connecting line of spray column 4, for monitoring the pressure on pipeline, prevents exception.
The preferred oilless vertical vacuum pump of vacuum pump 1.Oilless vertical vacuum pump be without any oil make lubrication can the oil-sealed rotary pump of operation, there is the advantages such as simple in construction, processing ease, easy to maintenance, ruggedness good, does not pollutes the environment.
The preferred magnetic drive pump of recycle stock pump 5.Magnetic drive pump realizes the transmission of contactless moment by magnetic drives thus replaces movable sealing with static seal, makes pump reach entirely without leakage.Owing to pump shaft, interior magnet rotor are completely enclosed by the pump housing, separation sleeve, thus thoroughly solve " run, drip, leak " problem, eliminate the potential safety hazard that inflammable, explosive, poisonous, hazardous medium is leaked by pump seal.
It is provided with regulation valve 12, for regulating the uninterrupted in pipeline on distillating still 3 and the connecting line of recycle stock pump 5.
Claims (1)
1. the method that a spectrasolv DMDA vacuum distilling takes off amine, it is characterised in that: comprise the following steps:
A. by vacuum pump by the spectrasolv DMDA inspiration distillating still containing dimethylamine；
The most under vacuum, ON cycle product pump, material in distillating still is carried out decompression distillation, and passes through spray column
The fraction of distillating still is carried out Sprayer Circulation, and vacuum distillation temperature controls less than or equal to 50 DEG C, and vacuum degree control is greatly
In equal to-0.09Mpa；
C. the one-tenth that distillating still distills is switched to dimethylamine absorption plant, absorbs dimethylamine；
D. sample analysis, until sample, without dimethylamine, is cooled to room temperature, blowing, obtains the N without dimethylamine, N-dimethyl
Decyl amide product.
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| CN201410421964.3A CN104193642B (en) | 2014-08-26 | 2014-08-26 | A kind of spectrasolv DMDA vacuum distilling takes off method and the system thereof of amine |
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| CN104193642B true CN104193642B (en) | 2016-08-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104998432A (en) * | 2015-06-30 | 2015-10-28 | 中复神鹰碳纤维有限责任公司 | Method and device for recovery of low concentration waste oil agent for chemical fibers |
| CN116239488A (en) * | 2021-12-08 | 2023-06-09 | 江苏万年长药业有限公司 | Method for recycling N, N-dimethyl capramide byproducts |
| CN115837260B (en) * | 2023-02-23 | 2023-05-30 | 大庆华理生物技术股份有限公司 | Oleic acid amidation deamination recovery device |
Citations (5)
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| US4568428A (en) * | 1983-07-05 | 1986-02-04 | General Signal Corporation | Method and apparatus for vacuum distillation |
| CN101139302A (en) * | 2007-08-20 | 2008-03-12 | 烟台东洁环保机械工程有限公司 | Method for treating waste gas from dimethylamine recovery by synthetic leather dimethyl formamide |
| CN201295543Y (en) * | 2008-10-28 | 2009-08-26 | 常州工程职业技术学院 | Atmospheric or vacuum rectification training device |
| CN202315373U (en) * | 2011-10-27 | 2012-07-11 | 东营市冠森绝缘制品有限公司 | Novel continuous dimethylacetylamide rectifying device |
| CN103381359A (en) * | 2013-07-29 | 2013-11-06 | 张家港市大伟助剂有限公司 | Preparation method for catalyst for N,N-dimethyl-caprylamide/decanamide |
-
2014
- 2014-08-26 CN CN201410421964.3A patent/CN104193642B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4568428A (en) * | 1983-07-05 | 1986-02-04 | General Signal Corporation | Method and apparatus for vacuum distillation |
| CN101139302A (en) * | 2007-08-20 | 2008-03-12 | 烟台东洁环保机械工程有限公司 | Method for treating waste gas from dimethylamine recovery by synthetic leather dimethyl formamide |
| CN201295543Y (en) * | 2008-10-28 | 2009-08-26 | 常州工程职业技术学院 | Atmospheric or vacuum rectification training device |
| CN202315373U (en) * | 2011-10-27 | 2012-07-11 | 东营市冠森绝缘制品有限公司 | Novel continuous dimethylacetylamide rectifying device |
| CN103381359A (en) * | 2013-07-29 | 2013-11-06 | 张家港市大伟助剂有限公司 | Preparation method for catalyst for N,N-dimethyl-caprylamide/decanamide |
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Denomination of invention: A Method and System for Vacuum Distillation Deamination of N, N-Dimethyldecanamide Effective date of registration: 20230831 Granted publication date: 20160824 Pledgee: Rudong sub branch of Bank of China Ltd. Pledgor: NANTONG WANNIANCHANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2023980054664 |
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