CN103183618A - Method for recovering dimethylamine from dimethylamine hydrochloride - Google Patents
Method for recovering dimethylamine from dimethylamine hydrochloride Download PDFInfo
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- CN103183618A CN103183618A CN2012105027641A CN201210502764A CN103183618A CN 103183618 A CN103183618 A CN 103183618A CN 2012105027641 A CN2012105027641 A CN 2012105027641A CN 201210502764 A CN201210502764 A CN 201210502764A CN 103183618 A CN103183618 A CN 103183618A
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- dimethylamine
- dimethylamine hydrochloride
- reclaims
- hydrochloride
- sodium hydroxide
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Abstract
The invention discloses a method for recovering dimethylamine from dimethylamine hydrochloride, which comprises the following steps: the dimethylamine hydrochloride and sodium hydroxide aqueous solution are reacted through taking toluene as solvent; and dimethylamine is recovered and obtained through heating, rectification, and arefaction with solid sodium hydroxide. The recovering method provided by the invention has high efficiency, is convenient for operation, solves the problem of recovering and reusing the dimethylamine from the dimethylamine hydrochloride, can be used for effectively recovering high purity dimethylamine from the dimethylamine hydrochloride, solves the problem of environment protection in waste treatment as obtained waste sodium chloride can be easily treated, and is suitable for large scale industrial production.
Description
Technical field
The present invention relates to the recovery method of a kind of chemical industry and medical material, particularly relate to a kind of method that reclaims dimethylamine from dimethylamine hydrochloride.
Background technology
Dimethylamine at room temperature is gas, the smell that similar ammonia is arranged, main as thiofide, leather depilitant, medicine, agricultural chemicals, textile industry solvent, dyestuff, explosive, propelling agent and dimethylhydrazine, N, the raw material of organic intermediates such as dinethylformamide.Dimethylamine is the important intermediate of agricultural chemicals, can prepare sterilant thiram, urbacide, ziram, Sankel, Asomat, Tuzet, dimethirimol; Sterilant Aphox, disosultap, desinsection list, kill snout moth's larva but, C-9140; Weedicide chlorotoluron, isoproturon, hexazinone, fluometuron etc.
Dimethylamine hydrochloride is mainly used in making catalyzer when acetylize is analyzed, and also is used for organic synthesis.
Because dimethylamine is of many uses, and the dimethylamine hydrochloride purposes is less, reclaiming dimethylamine in the dimethylamine hydrochloride that produces from industrial production becomes the important means that obtains the high purity dimethylamine.But because the dimethylamine hydrochloride that produces in the industrial production is impure more, be more difficult to get the high purity dimethylamine after the processing, cost recovery is higher, and waste is more difficult, and causing dimethylamine hydrochloride to reclaim dimethylamine can not scale operation.
The existing dimethylamine that reclaims from dimethylamine hydrochloride adopts calcium oxide solid and dimethylamine hydrochloride solid reacting by heating to reclaim the method for dimethylamine more, but because this method severe reaction conditions, the operation easier height, and the waste that produces is more difficult, has limited industrialized extensive popularization.
For from dimethylamine hydrochloride, reclaiming highly purified dimethylamine, and low cost, low risk, easy-operating method, do not see other reports.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of method that from dimethylamine hydrochloride, reclaims dimethylamine, be applicable to and from dimethylamine hydrochloride, reclaim highly purified dimethylamine, technological operation is simple and easy, reclaims the quality height, the effect height, cost is low.
The technical solution adopted in the present invention is:
Reclaim the method for dimethylamine from dimethylamine hydrochloride, dimethylamine hydrochloride and aqueous sodium hydroxide solution are that solvent reacts with toluene, reclaim and obtain dimethylamine through adding thermal rectification, and the use solid sodium hydroxide carry out drying and obtain dimethylamine.
The sodium chloride aqueous solution that described reaction produces is concentrated through distilling, and filters to obtain solid sodium chloride.
The concentration of described dimethylamine hydrochloride solution is 50% ~ 75%.
The concentration of described aqueous sodium hydroxide solution is 30% ~ 42%.
Described temperature of reaction is 60 ~ 65 ℃.
The mass ratio of described reaction solvent toluene and dimethylamine hydrochloride is 1:1.
Described heating rectification temperature is 65 ~ 78 ℃.
Described rectifying tower top temperature is 8 ~ 50 ℃.
Described drying is 1:8 with solid sodium hydroxide and dimethylamine hydrochloride mass ratio.
The distillation temperature of described sodium chloride aqueous solution is 95 ~ 110 ℃
Described sodium-chlor filtration temperature is 30 ~ 35 ℃.
It is that reaction solvent reacts with toluene that the present invention adopts dimethylamine hydrochloride and aqueous sodium hydroxide solution, reclaims and to obtain dimethylamine through adding thermal rectification, and use solid sodium hydroxide to carry out drying to obtain moisture＜0.5% dimethylamine.Recovery method efficient height of the present invention, easy to operate, processing cost is lower and be easy to industrialization, and used sodium hydroxide solution is general industry level raw material, be simple and easy to; Organic solvent toluene can reuse through behind the standing demix, has solved the recycling problem that reclaims dimethylamine from dimethylamine hydrochloride.Present method not only can effectively reclaim the high purity dimethylamine from dimethylamine hydrochloride, and can obtain more tractable waste sodium-chlor, has solved the environmental issue of offal treatment, is suitable for large-scale industrialization production.
Embodiment
Example 1
In a 500ml four-hole bottle that mechanical stirring, thermometer, reflux exchanger, distiller condenser and receiving bottle be housed, add 80g(50%) dimethylamine hydrochloride solution, 30g toluene drips 47g(42% down at 60 ~ 65 ℃) sodium hydroxide solution.Reflux exchanger feeds recirculated water, and fill with the 5g solid sodium hydroxide reflux exchanger inside, and distiller condenser feeds the heat-eliminating medium below-10 ℃, and receiving bottle is lowered the temperature with the heat-eliminating medium below-5 ℃.Be warming up to 78 ℃ after open stirring, and 78 ℃ of insulations till do not have dimethylamine and flow out, reaction finishes.Collect the about 20g of dimethylamine, moisture＜0.2%, yield about 90%.Lower aqueous layer distills out 56g water after the reaction solution layering under 95 ~ 110 ℃, is cooled to 30 ~ 35 ℃ of filtrations, obtains 15g solid sodium chloride waste.
The above; only be the preferable embodiment of the present invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to replacement or change according to technical scheme of the present invention and inventive concept thereof, all should be encompassed within protection scope of the present invention.
Claims (9)
1. from dimethylamine hydrochloride, reclaim the method for dimethylamine, it is characterized in that: dimethylamine hydrochloride and aqueous sodium hydroxide solution are that solvent reacts with toluene, reclaim and to obtain dimethylamine through adding thermal rectification, and use solid sodium hydroxide to carry out drying to obtain dimethylamine.
2. the method that reclaims dimethylamine from dimethylamine hydrochloride according to claim 1 is characterized in that
The sodium chloride aqueous solution that described reaction produces is concentrated through distilling, and filters to obtain solid sodium chloride.
3. the method that reclaims dimethylamine from dimethylamine hydrochloride according to claim 1, the concentration that it is characterized in that described dimethylamine hydrochloride solution is 50% ~ 75%.
4. the method that reclaims dimethylamine from dimethylamine hydrochloride according to claim 1, the concentration that it is characterized in that described aqueous sodium hydroxide solution is 30% ~ 42%.
5. the method that reclaims dimethylamine from dimethylamine hydrochloride according to claim 1 is characterized in that described temperature of reaction is 60 ~ 65 ℃.
6. the method that from dimethylamine hydrochloride, reclaims dimethylamine according to claim 1, the mass ratio that it is characterized in that described reaction solvent toluene and dimethylamine hydrochloride is 1:1,
The method that reclaims dimethylamine from dimethylamine hydrochloride according to claim 1 is characterized in that described heating rectification temperature is 65 ~ 78 ℃.
7. the method that reclaims dimethylamine from dimethylamine hydrochloride according to claim 1 is characterized in that described drying is 1:8 with solid sodium hydroxide and dimethylamine hydrochloride mass ratio.
8. the method that reclaims dimethylamine from dimethylamine hydrochloride according to claim 1, the distillation temperature that it is characterized in that described sodium chloride aqueous solution is 95 ~ 110 ℃.
9. the method that reclaims dimethylamine from dimethylamine hydrochloride according to claim 1 is characterized in that described sodium-chlor filtration temperature is 30 ~ 35 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105027641A CN103183618A (en) | 2012-11-30 | 2012-11-30 | Method for recovering dimethylamine from dimethylamine hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012105027641A CN103183618A (en) | 2012-11-30 | 2012-11-30 | Method for recovering dimethylamine from dimethylamine hydrochloride |
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| CN103183618A true CN103183618A (en) | 2013-07-03 |
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| CN2012105027641A Pending CN103183618A (en) | 2012-11-30 | 2012-11-30 | Method for recovering dimethylamine from dimethylamine hydrochloride |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965054A (en) * | 2013-01-30 | 2014-08-06 | 上海宏锐新材料科技有限公司 | Method and device for preparing high-purity waterless dimethylamine |
| CN104402734A (en) * | 2014-12-02 | 2015-03-11 | 安徽科立华化工有限公司 | Method for recovering dimethylamine from nicosulfuron waste water |
| CN104910020A (en) * | 2015-05-20 | 2015-09-16 | 盐城捷康三氯蔗糖制造有限公司 | Method for recovering dimethylamine from sucralose production wastewater |
| CN106278955A (en) * | 2015-06-25 | 2017-01-04 | 北大方正集团有限公司 | A kind of dimethylamine waste water recovery and treatment method |
| CN110590595A (en) * | 2019-09-26 | 2019-12-20 | 河北合佳医药科技集团股份有限公司 | Green and efficient methyl hydrazine crude product solution rectification method |
| CN111004131A (en) * | 2019-12-23 | 2020-04-14 | 南通市常海食品添加剂有限公司 | Method for recovering sucralose by-product salt |
| CN111018762A (en) * | 2019-12-13 | 2020-04-17 | 焦宏典 | Production process of dimethylamino sulfonyl chloride |
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| CN1237573A (en) * | 1998-06-01 | 1999-12-08 | 贵州群星科学技术经济合作公司 | Refining method of dimethyl allylamine and its salt |
| CN102079712A (en) * | 2010-12-31 | 2011-06-01 | 大连联化化学有限公司 | Method for recycling anhydrous organic amine from organic amine salt |
| CN102350220A (en) * | 2011-07-04 | 2012-02-15 | 天津凯铂能膜工程技术有限公司 | Stable gas membrane and method used for removing, recovering, and gathering ammonia or organic amine from dosage liquor or wastewater |
| US20120157676A1 (en) * | 2009-03-30 | 2012-06-21 | Tate & Lyle Technology Ltd. | Process for removing dimethylamine |
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2012
- 2012-11-30 CN CN2012105027641A patent/CN103183618A/en active Pending
Patent Citations (4)
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| CN1237573A (en) * | 1998-06-01 | 1999-12-08 | 贵州群星科学技术经济合作公司 | Refining method of dimethyl allylamine and its salt |
| US20120157676A1 (en) * | 2009-03-30 | 2012-06-21 | Tate & Lyle Technology Ltd. | Process for removing dimethylamine |
| CN102079712A (en) * | 2010-12-31 | 2011-06-01 | 大连联化化学有限公司 | Method for recycling anhydrous organic amine from organic amine salt |
| CN102350220A (en) * | 2011-07-04 | 2012-02-15 | 天津凯铂能膜工程技术有限公司 | Stable gas membrane and method used for removing, recovering, and gathering ammonia or organic amine from dosage liquor or wastewater |
Non-Patent Citations (1)
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| 张志萍等: "二甲基烯丙胺及其盐酸盐合成新工艺", 《化学研究与应用》, vol. 10, no. 02, 25 April 1998 (1998-04-25) * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965054A (en) * | 2013-01-30 | 2014-08-06 | 上海宏锐新材料科技有限公司 | Method and device for preparing high-purity waterless dimethylamine |
| CN103965054B (en) * | 2013-01-30 | 2015-06-24 | 上海宏锐新材料科技有限公司 | Method and device for preparing high-purity waterless dimethylamine |
| CN104402734A (en) * | 2014-12-02 | 2015-03-11 | 安徽科立华化工有限公司 | Method for recovering dimethylamine from nicosulfuron waste water |
| CN104910020A (en) * | 2015-05-20 | 2015-09-16 | 盐城捷康三氯蔗糖制造有限公司 | Method for recovering dimethylamine from sucralose production wastewater |
| CN106278955A (en) * | 2015-06-25 | 2017-01-04 | 北大方正集团有限公司 | A kind of dimethylamine waste water recovery and treatment method |
| CN110590595A (en) * | 2019-09-26 | 2019-12-20 | 河北合佳医药科技集团股份有限公司 | Green and efficient methyl hydrazine crude product solution rectification method |
| CN111018762A (en) * | 2019-12-13 | 2020-04-17 | 焦宏典 | Production process of dimethylamino sulfonyl chloride |
| CN111004131A (en) * | 2019-12-23 | 2020-04-14 | 南通市常海食品添加剂有限公司 | Method for recovering sucralose by-product salt |
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Application publication date: 20130703 |