CN108329227A - Method of purification containing Dimethylformamide Residue - Google Patents
Method of purification containing Dimethylformamide Residue Download PDFInfo
- Publication number
- CN108329227A CN108329227A CN201810205129.4A CN201810205129A CN108329227A CN 108329227 A CN108329227 A CN 108329227A CN 201810205129 A CN201810205129 A CN 201810205129A CN 108329227 A CN108329227 A CN 108329227A
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- Prior art keywords
- dimethylformamide
- residue
- dmf
- temperature
- dimethylformamide residue
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Hydrogenated Pyridines (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of methods of purification containing Dimethylformamide Residue, which is characterized in that includes the following steps：A, Dimethylformamide Residue enters heating in rectifying column；B, lateral line discharging recycles dimethylformamide product.Method of purification provided by the invention containing Dimethylformamide Residue, can purify dimethylformamide, DMF contents in final products>99.9%；Basic species total amount<100ppm.
Description
Technical field
The present invention relates to solvent purifications field, more particularly to a kind of method of purification containing Dimethylformamide Residue.
Background technology
Containing alkaline matters such as piperidines in pharmaceutical industry dimethylformamide (DMF) waste liquid, make DMF products that certain alkali be presented
Property.DMF remanufacture processes simultaneously, DMF are also made DMF products that certain alkalinity be presented by released dimethylamine is thermally decomposed.And
The limited provisioning request of alkali content in DMF solvent.For this purpose, in solvent recovery production, before DMF polishings, often to preliminary purification
DMF materials in the acidic materials such as a small amount of sulfuric acid, hydrochloric acid are added, to neutralize contained alkaline matter in DMF crude products, regulate and control final production
The basicity of product, to meet technological requirement.But acid adding modulates method, may only reduce the alkaline matters such as contained micro piperidines in DMF
Influence to final products basicity.But it carries out in DMF subtractive processes after modulation, because DMF is by the released diformazan of thermal decomposition
Amine can also be such that final DMF alkali contents increase.
Invention content
Purpose of the invention is to overcome the shortcomings in the prior art, provides a kind of carrying containing Dimethylformamide Residue
Pure method.
In order to achieve the above object, the invention is realized by the following technical scheme：
Method of purification containing Dimethylformamide Residue, which is characterized in that include the following steps：
A. Dimethylformamide Residue enters heating in rectifying column；
B. lateral line discharging recycles dimethylformamide product.
According to one embodiment of present invention, in step a, rectifying tower pressure interior force is 15-25kpa.
According to one embodiment of present invention, 100 DEG C -110 DEG C of bottom temperature.
According to one embodiment of present invention, tower top temperature is 75 DEG C -80 DEG C；Side stream temperature is 95 DEG C -105 DEG C.
According to one embodiment of present invention, 103 DEG C -105 DEG C of bottom temperature；Tower top temperature is 75 DEG C -78 DEG C；Side line temperature
Degree is 100 DEG C -102 DEG C.
Method of purification provided by the invention containing Dimethylformamide Residue, can purify dimethylformamide, final products
Middle DMF contents>99.9%；Basic species total amount<100ppm.
Description of the drawings
Fig. 1 is that the present invention uses process flow diagram.
Specific implementation mode
The present invention is described in detail with reference to embodiment：
Embodiment 1
Method of purification containing Dimethylformamide Residue, as shown in Figure 1, including the following steps：
A. Dimethylformamide Residue enters heating in rectifying column；Rectifying tower pressure interior force is 15kpa；103 DEG C of bottom temperature；
Tower top temperature is 76 DEG C.
B. lateral line discharging recycles dimethylformamide product, and side stream temperature is 101 DEG C.
It feeds in Dimethylformamide Residue, DMF:>99.8%, the alkaline matters such as piperidines<1000ppm.In final products
DMF contents>99.9%；Basic species total amount<100ppm.
Embodiment 2
Method of purification containing Dimethylformamide Residue, as shown in Figure 1, including the following steps：
A. Dimethylformamide Residue enters heating in rectifying column 100；Rectifying tower pressure interior force is 20kpa；Bottom temperature 103
℃；Tower top temperature is 76 DEG C.
B. lateral line discharging recycles dimethylformamide product, and side stream temperature is 101 DEG C.
It feeds in Dimethylformamide Residue, DMF:>99.8%, the alkaline matters such as piperidines<1000ppm.In final products
DMF contents>99.9%；Basic species total amount<100ppm.
Embodiment 3
Method of purification containing Dimethylformamide Residue, as shown in Figure 1, including the following steps：
A. Dimethylformamide Residue enters heating in rectifying column 100；Rectifying tower pressure interior force is 20kpa；Bottom temperature 102
℃；Tower top temperature is 75 DEG C.
B. lateral line discharging recycles dimethylformamide product, and side stream temperature is 100 DEG C.
It feeds in Dimethylformamide Residue, DMF:>99.8%, the alkaline matters such as piperidines<1000ppm.In final products
DMF contents>99.9%；Basic species total amount<100ppm.
Embodiment 4
Method of purification containing Dimethylformamide Residue, as shown in Figure 1, including the following steps：
A. Dimethylformamide Residue enters heating in rectifying column 100；Rectifying tower pressure interior force is 18kpa；Bottom temperature 104
℃；Tower top temperature is 78 DEG C.
B. lateral line discharging recycles dimethylformamide product, and side stream temperature is 100 DEG C.
It feeds in Dimethylformamide Residue, DMF:>99.8%, the alkaline matters such as piperidines<1000ppm.In final products
DMF contents>99.9%；Basic species total amount<100ppm.
Embodiment 5
Method of purification containing Dimethylformamide Residue, as shown in Figure 1, including the following steps：
A. Dimethylformamide Residue enters heating in rectifying column 100；Rectifying tower pressure interior force is 22kpa；Bottom temperature 105
℃；Tower top temperature is 80 DEG C.
B. lateral line discharging recycles dimethylformamide product, and side stream temperature is 102 DEG C.
It feeds in Dimethylformamide Residue, DMF:>99.8%, the alkaline matters such as piperidines<1000ppm.In final products
DMF contents>99.9%；Basic species total amount<100ppm.
Embodiment 6
Method of purification containing Dimethylformamide Residue, as shown in Figure 1, including the following steps：
A. Dimethylformamide Residue enters heating in rectifying column 100；Rectifying tower pressure interior force is 25kpa；Bottom temperature 108
℃；Tower top temperature is 75 DEG C.
B. lateral line discharging recycles dimethylformamide product, and side stream temperature is 103 DEG C.
It feeds in Dimethylformamide Residue, DMF:>99.8%, the alkaline matters such as piperidines<1000ppm.In final products
DMF contents>99.9%；Basic species total amount<100ppm.
Embodiment in the present invention is only used for that the present invention will be described, and is not construed as limiting the scope of claims limitation,
Other substantially equivalent replacements that those skilled in that art are contemplated that, all fall in the scope of protection of the present invention.
Claims (5)
1. the method for purification containing Dimethylformamide Residue, which is characterized in that include the following steps：
A. Dimethylformamide Residue enters heating in rectifying column；
B. lateral line discharging recycles dimethylformamide product.
2. the method for purification according to claim 1 containing Dimethylformamide Residue, which is characterized in that in step a, rectifying
Tower pressure interior force is 15-25kpa.
3. the method for purification according to claim 1 containing Dimethylformamide Residue, which is characterized in that bottom temperature 100
℃-110℃。
4. the method for purification according to claim 1 or 3 containing Dimethylformamide Residue, which is characterized in that tower top temperature
It is 75 DEG C -80 DEG C；Side stream temperature is 95 DEG C -105 DEG C.
5. the method for purification according to claim 4 containing Dimethylformamide Residue, which is characterized in that bottom temperature 103
℃-105℃；Tower top temperature is 75 DEG C -78 DEG C；Side stream temperature is 100 DEG C -102 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810205129.4A CN108329227B (en) | 2018-03-13 | 2018-03-13 | Method for purifying waste liquid containing dimethyl formamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810205129.4A CN108329227B (en) | 2018-03-13 | 2018-03-13 | Method for purifying waste liquid containing dimethyl formamide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108329227A true CN108329227A (en) | 2018-07-27 |
| CN108329227B CN108329227B (en) | 2021-03-09 |
Family
ID=62930732
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810205129.4A Active CN108329227B (en) | 2018-03-13 | 2018-03-13 | Method for purifying waste liquid containing dimethyl formamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108329227B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588828A (en) * | 2015-10-14 | 2017-04-26 | 中国石化仪征化纤有限责任公司 | Separation and purification method of THF (tetrahydrofuran) distillation waste liquid |
| CN106745421A (en) * | 2016-12-16 | 2017-05-31 | 常州大学 | A kind of multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of band |
-
2018
- 2018-03-13 CN CN201810205129.4A patent/CN108329227B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588828A (en) * | 2015-10-14 | 2017-04-26 | 中国石化仪征化纤有限责任公司 | Separation and purification method of THF (tetrahydrofuran) distillation waste liquid |
| CN106745421A (en) * | 2016-12-16 | 2017-05-31 | 常州大学 | A kind of multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of band |
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| Publication number | Publication date |
|---|---|
| CN108329227B (en) | 2021-03-09 |
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