CN109053464A - A method of dimethylamine is recycled from dimethylamine hydrochloride - Google Patents
A method of dimethylamine is recycled from dimethylamine hydrochloride Download PDFInfo
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- CN109053464A CN109053464A CN201810814274.2A CN201810814274A CN109053464A CN 109053464 A CN109053464 A CN 109053464A CN 201810814274 A CN201810814274 A CN 201810814274A CN 109053464 A CN109053464 A CN 109053464A
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- dimethylamine
- recycling
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- heating kettle
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The present invention provides a kind of method from dimethylamine hydrochloride recycling dimethylamine, it is related to Sewage treatment field, the following steps are included: the entrance of the gas outlet connection exhaust-gas treatment pipeline of heating kettle, the outlet of exhaust-gas treatment pipeline is communicated with outside, add waste water into heating kettle, after heating stirring, heat preservation, the leakage fluid dram of heating kettle is connected to the entrance of filtering ponds, waste liquid is drained into filtering ponds by heating kettle and carries out heat filtering, after staying liquid to remove slag, obtain mixed liquor, the outlet of filtering ponds is connected to the entrance of stirred tank, the outlet of stirred tank is connected to the entrance of rectifying column, mixed liquor is imported into stirred tank, after triethylamine solution is added, while heating stirring, condense rectifying recycling, obtain recycling dimethylamine.
Description
Technical field
The present invention relates to Sewage treatment fields, and in particular to a method of dimethylamine is recycled from dimethylamine hydrochloride.
Background technique
Dimethylamine is gaseous state at room temperature, while with the smell for having similar ammonia, and dimethylamine is mainly used for making rubber
Glue vulcanization accelerator, medicinal antibiosis element or pesticide herbicide etc., have a wide range of applications space in daily life.
Dimethylamine hydrochloride is a kind of compound, it is in life mainly in certain chemical reactions as the shape of catalyst
Formula exists, meanwhile, it can also be applied to organic synthesis, in process of factory production, a large amount of dimethylamine salt often contained in waste liquid
Hydrochlorate, since it is dissolved in waste liquid, cost for purification is high, is unfavorable for recycling, and in the prior art, rarely have about how from
The technique study of dimethylamine is recycled in dimethylamine hydrochloride, and is relied primarily on ammonia and methanol and acted on system in the environment of high temperature and pressure
, therefore in the waste water treatment process containing dimethylamine hydrochloride, need a kind of method and process that can extract high-purity wherein
Dimethylamine.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides it is a kind of from dimethylamine hydrochloride recycling dimethylamine method,
While handling the waste water containing dimethylamine hydrochloride, the cost for preparing dimethylamine is further decreased.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A method of dimethylamine is recycled from dimethylamine hydrochloride, comprising the following steps:
(1) entrance of the gas outlet connection exhaust-gas treatment pipeline of heating kettle, the outlet of exhaust-gas treatment pipeline are communicated with outside,
It adds waste water into heating kettle and keeps the temperature 40-50min after heating stirring to T；
(2) leakage fluid dram of heating kettle is connected to the entrance of filtering ponds, and waste liquid is drained into filtering ponds by heating kettle and carries out hot mistake
Filter, after staying liquid to remove slag, obtains mixed liquor；
(3) outlet of filtering ponds is connected to the entrance of stirred tank, and the outlet of stirred tank is connected to the entrance of rectifying column, will be mixed
It closes liquid and imports stirred tank, after triethylamine solution is added, while heating is stirred, condensation rectifying recycling obtains recycling dimethylamine.
Preferably, multi-stage absorption carbon-coating is equipped in exhaust-gas treatment pipeline described in step (1).
Preferably, T described in step (1) is 170-180 DEG C.
Preferably, filtering ponds described in step (2) are equipped with 16 meshes.
Preferably, heat filtering described in step (2) is to be filtered at 165-170 DEG C.
Preferably, heating described in step (3), which refers to, increases temperature to 40-50 DEG C, the temperature of the condensation be -8 DEG C to -
5℃。
Preferably, the triethylamine solution described in step (3) is the 50-60% aqueous solution of triethylamine, the triethylamine
The mass ratio of solution and the mixed liquor is 1-4:50.
(3) beneficial effect
The present invention provides a kind of methods from dimethylamine hydrochloride recycling dimethylamine, have the advantages that
Firstly, raw material is the industrial wastewater containing dimethylamine hydrochloride, the emission problem of industrial wastewater is always that environmental protection can
Important topic on sustainable development road, the recycling method provided through the invention are not only able to solve to contain dimethylamine hydrochloric acid
The processing emission problem of salt industrial waste water, and beneficiating ingredient dimethylamine is therefrom extracted, it realizes waste utilization, turns waste into wealth.
Secondly, on specific recovery method, using the impurity in the rough discharge waste liquid of first high-temperature heating, then high temperature mistake
Filter, further increases the content of dimethylamine hydrochloride in industrial wastewater, finally, triethylamine, which is added, carries out rectifying recycling, reaches back
Receive the purpose of high-purity dimethylamine.
Finally, recycling method provided by the invention, clean and environmental protection, the exhaust gas generated in removal process is after adsorption treatment
It just launches into air, further achievees the purpose that protect environment, prevents pollutant emission.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A method of dimethylamine is recycled from dimethylamine hydrochloride, comprising the following steps:
(1) entrance of the gas outlet connection exhaust-gas treatment pipeline of heating kettle, exhaust-gas treatment pipeline (are set in exhaust-gas treatment pipeline
Have multi-stage absorption carbon-coating) outlet communicated with outside, add waste water into heating kettle, heating stirring keeps the temperature 40min to after 180 DEG C；
(2) leakage fluid dram of heating kettle is connected to the entrance of filtering ponds, and waste liquid is drained into filtering ponds at 165 DEG C by heating kettle
At a temperature of carry out heat filtering (filter screen be 16 meshes), after staying liquid to remove slag, obtain mixed liquor；
(3) outlet of filtering ponds is connected to the entrance of stirred tank, and the outlet of stirred tank is connected to the entrance of rectifying column, will be mixed
It closes liquid and imports stirred tank, after triethylamine solution (60% aqueous solution of triethylamine) is added, triethylamine solution is added and is mixed with described
The mass ratio of liquid is 1:50, is warming up to 50 DEG C, while stirring, rectifying recycling is condensed at -8 DEG C, obtains recycling dimethylamine.
Embodiment 2:
A method of dimethylamine is recycled from dimethylamine hydrochloride, comprising the following steps:
(1) entrance of the gas outlet connection exhaust-gas treatment pipeline of heating kettle, exhaust-gas treatment pipeline (are set in exhaust-gas treatment pipeline
Have multi-stage absorption carbon-coating) outlet communicated with outside, add waste water into heating kettle, heating stirring keeps the temperature 50min to after 170 DEG C；
(2) leakage fluid dram of heating kettle is connected to the entrance of filtering ponds, and waste liquid is drained into filtering ponds at 170 DEG C by heating kettle
At a temperature of carry out heat filtering (filter screen be 16 meshes), after staying liquid to remove slag, obtain mixed liquor；
(3) outlet of filtering ponds is connected to the entrance of stirred tank, and the outlet of stirred tank is connected to the entrance of rectifying column, will be mixed
It closes liquid and imports stirred tank, after triethylamine solution (50% aqueous solution of triethylamine) is added, triethylamine solution is added and is mixed with described
The mass ratio of liquid is 2:25, is warming up to 40 DEG C, while stirring, rectifying recycling is condensed at -5 DEG C, obtains recycling dimethylamine.
Embodiment 3:
A method of dimethylamine is recycled from dimethylamine hydrochloride, comprising the following steps:
(1) entrance of the gas outlet connection exhaust-gas treatment pipeline of heating kettle, exhaust-gas treatment pipeline (are set in exhaust-gas treatment pipeline
Have multi-stage absorption carbon-coating) outlet communicated with outside, add waste water into heating kettle, heating stirring keeps the temperature 46min to after 174 DEG C；
(2) leakage fluid dram of heating kettle is connected to the entrance of filtering ponds, and waste liquid is drained into filtering ponds at 167 DEG C by heating kettle
At a temperature of carry out heat filtering (filter screen be 16 meshes), after staying liquid to remove slag, obtain mixed liquor；
(3) outlet of filtering ponds is connected to the entrance of stirred tank, and the outlet of stirred tank is connected to the entrance of rectifying column, will be mixed
It closes liquid and imports stirred tank, after triethylamine solution (55% aqueous solution of triethylamine) is added, triethylamine solution is added and is mixed with described
The mass ratio of liquid is 1:25, is warming up to 47 DEG C, while stirring, rectifying recycling is condensed at -7 DEG C, obtains recycling dimethylamine.
Embodiment 4:
A method of dimethylamine is recycled from dimethylamine hydrochloride, comprising the following steps:
(1) entrance of the gas outlet connection exhaust-gas treatment pipeline of heating kettle, exhaust-gas treatment pipeline (are set in exhaust-gas treatment pipeline
Have multi-stage absorption carbon-coating) outlet communicated with outside, add waste water into heating kettle, heating stirring keeps the temperature 44min to after 177 DEG C；
(2) leakage fluid dram of heating kettle is connected to the entrance of filtering ponds, and waste liquid is drained into filtering ponds at 167 DEG C by heating kettle
At a temperature of carry out heat filtering (filter screen be 16 meshes), after staying liquid to remove slag, obtain mixed liquor；
(3) outlet of filtering ponds is connected to the entrance of stirred tank, and the outlet of stirred tank is connected to the entrance of rectifying column, will be mixed
It closes liquid and imports stirred tank, after triethylamine solution (58% aqueous solution of triethylamine) is added, triethylamine solution is added and is mixed with described
The mass ratio of liquid is 3:50, is warming up to 45 DEG C, while stirring, rectifying recycling is condensed at -6 DEG C, obtains recycling dimethylamine.
Embodiment 5:
A method of dimethylamine is recycled from dimethylamine hydrochloride, comprising the following steps:
(1) entrance of the gas outlet connection exhaust-gas treatment pipeline of heating kettle, exhaust-gas treatment pipeline (are set in exhaust-gas treatment pipeline
Have multi-stage absorption carbon-coating) outlet communicated with outside, add waste water into heating kettle, heating stirring keeps the temperature 49min to after 176 DEG C；
(2) leakage fluid dram of heating kettle is connected to the entrance of filtering ponds, and waste liquid is drained into filtering ponds at 168 DEG C by heating kettle
At a temperature of carry out heat filtering (filter screen be 16 meshes), after staying liquid to remove slag, obtain mixed liquor；
(3) outlet of filtering ponds is connected to the entrance of stirred tank, and the outlet of stirred tank is connected to the entrance of rectifying column, will be mixed
It closes liquid and imports stirred tank, after triethylamine solution (57% aqueous solution of triethylamine) is added, triethylamine solution is added and is mixed with described
The mass ratio of liquid is 1:50, is warming up to 47 DEG C, while stirring, rectifying recycling is condensed at -8 DEG C, obtains recycling dimethylamine.
Beneficial effect in order to further illustrate the present invention selects slave dimethylamine salt described in 1-5 of the embodiment of the present invention
The method that hydrochlorate recycles dimethylamine carries out purity experiment test for the dimethylamine of recycling, and experimental result is recorded in following table
It is interior.
| Ingredient | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Dimethylamine | 89.49% | 91.32% | 91.12% | 91.99% | 89.73% |
| It is other | BaL | BaL | BaL | BaL | BaL |
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, including the element that sentence "including a ..." limits, it is not excluded that
There is also other identical elements in the process, method, article or apparatus that includes the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations, although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (7)
1. a kind of method from dimethylamine hydrochloride recycling dimethylamine, which comprises the following steps:
(1) entrance of the gas outlet connection exhaust-gas treatment pipeline of heating kettle, the outlet of exhaust-gas treatment pipeline is communicated with outside, will be given up
Water is added heating kettle and keeps the temperature 40-50min after heating stirring to T；
(2) leakage fluid dram of heating kettle is connected to the entrance of filtering ponds, and waste liquid is drained into filtering ponds by heating kettle and carries out heat filtering, is stayed
After liquid removes slag, mixed liquor is obtained；
(3) outlet of filtering ponds is connected to the entrance of stirred tank, and the outlet of stirred tank is connected to the entrance of rectifying column, by mixed liquor
Stirred tank is imported, after triethylamine solution is added, while heating is stirred, condensation rectifying recycling obtains recycling dimethylamine.
2. as described in claim 1 from the method for dimethylamine hydrochloride recycling dimethylamine, which is characterized in that institute in step (1)
It states and is equipped with multi-stage absorption carbon-coating in exhaust-gas treatment pipeline.
3. as described in claim 1 from the method for dimethylamine hydrochloride recycling dimethylamine, which is characterized in that institute in step (1)
Stating T is 170-180 DEG C.
4. as described in claim 1 from the method for dimethylamine hydrochloride recycling dimethylamine, which is characterized in that institute in step (2)
Filtering ponds are stated equipped with 16 meshes.
5. as described in claim 1 from the method for dimethylamine hydrochloride recycling dimethylamine, which is characterized in that institute in step (2)
Stating heat filtering is to be filtered at 165-170 DEG C.
6. as described in claim 1 from the method for dimethylamine hydrochloride recycling dimethylamine, which is characterized in that institute in step (3)
It states heating and refers to raising temperature to 40-50 DEG C, the temperature of the condensation is -8 DEG C to -5 DEG C.
7. as described in claim 1 from the method for dimethylamine hydrochloride recycling dimethylamine, which is characterized in that institute in step (3)
The 50-60% aqueous solution that the triethylamine solution is triethylamine is stated, the mass ratio of the triethylamine solution and the mixed liquor is
1-4:50。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810814274.2A CN109053464A (en) | 2018-07-23 | 2018-07-23 | A method of dimethylamine is recycled from dimethylamine hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810814274.2A CN109053464A (en) | 2018-07-23 | 2018-07-23 | A method of dimethylamine is recycled from dimethylamine hydrochloride |
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| CN109053464A true CN109053464A (en) | 2018-12-21 |
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| CN201810814274.2A Pending CN109053464A (en) | 2018-07-23 | 2018-07-23 | A method of dimethylamine is recycled from dimethylamine hydrochloride |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| WO2016187878A1 (en) * | 2015-05-28 | 2016-12-01 | 鹤山市新科达企业有限公司 | Treatment technology for synthetic leather production wastewater |
| CN108047053A (en) * | 2017-12-18 | 2018-05-18 | 江南大学 | Amine substance isolates and purifies recovery method in a kind of Sucralose waste water |
-
2018
- 2018-07-23 CN CN201810814274.2A patent/CN109053464A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| WO2016187878A1 (en) * | 2015-05-28 | 2016-12-01 | 鹤山市新科达企业有限公司 | Treatment technology for synthetic leather production wastewater |
| CN108047053A (en) * | 2017-12-18 | 2018-05-18 | 江南大学 | Amine substance isolates and purifies recovery method in a kind of Sucralose waste water |
Non-Patent Citations (3)
| Title |
|---|
| KOHEI OSAWA等: "Synthesis of Sequence-Specific Polymers with Amide Side Chains via Regio-/Stereoselective Ring-Opening Metathesis Polymerization of 3-Substituted cis-Cyclooctene", 《MACROMOLECULES》 * |
| 陈均志等: "合成革厂DMF蒸馏废水中回收二甲胺的新工艺研究 ", 《工业安全与环保》 * |
| 黄玉媛等: "《精细化工配方常用原料手册》", 31 March 1998 * |
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Application publication date: 20181221 |