CN110759832A - DMAC (dimethylacetamide) residual liquid recycling device and method - Google Patents
DMAC (dimethylacetamide) residual liquid recycling device and method Download PDFInfo
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- CN110759832A CN110759832A CN201911123225.5A CN201911123225A CN110759832A CN 110759832 A CN110759832 A CN 110759832A CN 201911123225 A CN201911123225 A CN 201911123225A CN 110759832 A CN110759832 A CN 110759832A
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- dmac
- tank
- residual liquid
- rectifying tower
- liquid
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- 239000007788 liquid Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 10
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 title claims description 47
- 238000004064 recycling Methods 0.000 title description 2
- 238000010992 reflux Methods 0.000 claims abstract description 30
- 238000011084 recovery Methods 0.000 claims abstract description 16
- 239000000446 fuel Substances 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 abstract 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 6
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- AVQQQNCBBIEMEU-UHFFFAOYSA-N 1,1,3,3-tetramethylurea Chemical compound CN(C)C(=O)N(C)C AVQQQNCBBIEMEU-UHFFFAOYSA-N 0.000 description 1
- 239000004376 Sucralose Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BAQAVOSOZGMPRM-QBMZZYIRSA-N sucralose Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](CO)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 BAQAVOSOZGMPRM-QBMZZYIRSA-N 0.000 description 1
- 235000019408 sucralose Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
-
- 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
Abstract
The invention relates to a DMAC residual liquid recovery device and a method, which are characterized in that: (1) starting a vacuum pump, and controlling the pressure in the rectifying tower to be-88 to-96 KPa; (2) the residual DMAC liquid is fed into a rectifying tower for vacuum rectification, the temperature is controlled to be 100-110 ℃, and the pressure is controlled to be-88 to-96 KPa; (3) and condensing the gas phase into liquid, flowing the liquid into a reflux tank, opening a pipeline flowing to a rectifying tower at the bottom of the reflux tank when the liquid level is 30-40% in volume in the reflux tank, controlling the reflux of the liquid with the volume of 30-40% in the reflux tank, finishing the rectification when the DMAC content extracted from the top of the tower is more than 80% and the DMAC content extracted from the bottom of the tower is less than 40%, and treating the bottom residual liquid to a final residual liquid tank as fuel. The invention has the advantages that: the equipment investment cost is low, the process is simple, and the operation is convenient; 80% of DMAC can be extracted, which accounts for about 50-70% of the total weight, so that the quality and yield of DMAC are improved; the DMAC residual liquid is generated about 150 square each month in production, and after recovery, the final residual liquid is about 60-70 square, and 70-80 square of DMAC can be recovered.
Description
Technical Field
The invention belongs to the technical field of wastewater recovery, and relates to a DMAC (dimethylacetamide) residual liquid recovery device and a DMAC residual liquid recovery method.
Background
In the production of sucralose, residual acidic DMF in the liquid purified and recovered by a DMF recovery working section is difficult to treat, in order to save energy, protect environment and develop an acidic DMF recovery working section, DMF in acidic DMF is firstly extracted preliminarily, then DMAC is generated by reaction of dimethylamine and acetic acid in acidic DMF, then DMF in acidic DMF is further extracted completely, and finally DMAC is rectified.
Disclosure of Invention
The present invention is directed to solving the above problems and to providing a DMAC raffinate recovery apparatus and a DMAC raffinate recovery method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the DMAC residual liquid recovery device is characterized by comprising the following devices: a residual liquid transfer tank, a rectifying tower (containing a reboiler), a condenser, a reflux tank, a buffer tank, a vacuum pump, a final residual liquid tank and a recovered residual liquid tank;
the residual liquid transfer tank is connected with an inlet at the top of a rectifying tower (containing a reboiler), an outlet at the top of the rectifying tower is sequentially connected with a condenser, a reflux tank, a buffer tank and a vacuum pump, and an outlet at the bottom of the rectifying tower is connected to a final residual liquid tank through a pipeline; the bottom of the reflux tank is respectively connected to an inlet at the top of the rectifying tower and a recovered residue tank through pipelines.
A DMAC residual liquid recovery method is characterized by comprising the following steps:
(1) after the valve is checked, a vacuum pump is started, air in the rectifying tower passes through a condenser, a reflux tank and a buffer tank and then is pumped to a tail gas system by the vacuum pump, and the pressure in the rectifying tower is controlled to be-88 to-96 KPa;
(2) the DMAC residual liquid (from an acidic DMF working section) in the residual liquid transfer tank is fed into a rectifying tower for vacuum rectification and concentration, and the temperature in the rectifying tower is controlled to be 100-110 ℃ and the pressure is controlled to be-88 to-96 KPa;
(3) gas phase (DMAC, tetramethylurea, acetic acid) from the top of the rectifying tower is condensed into liquid through a condenser (30-50 ℃) and flows into a reflux tank, when the liquid level is 30-40% of the volume in the reflux tank, a pipeline flowing to the rectifying tower at the bottom of the reflux tank is opened, the reflux of 30-40% of liquid in the reflux tank is controlled, the content of DMAC extracted from the top of the rectifying tower is above 80%, the rectification is finished when the content of DMAC extracted from the bottom of the rectifying tower is below 40%, and bottom residual liquid is extracted to a final residual liquid tank and is treated as fuel.
The DMAC residual liquid to be recovered is subjected to distillation and rectification treatment (the DMAC and various impurities are mainly utilized to achieve the separation effect of the DMAC and the residual liquid), so that the content of the DMAC in the residual liquid at the bottom of the tower is reduced, the waste liquid is increased (the DMAC cannot be further recovered and can only be treated as fuel), the content of the DMAC recovered at the top of the tower can reach more than 80%, and the material recovered at the top of the tower is returned to the previous working section to be further concentrated into pure DMAC.
The invention has the advantages that: 1. the equipment investment cost is low, the process is simple, the operation is convenient, and the labor force is saved; 2. the DMAC in the DMAC residual liquid can be effectively recovered, 80% of DMAC can be extracted, and the DMAC accounts for 50-70% of the total proportion, so that the quality and the yield of DMAC are improved, the DMAC can reach the high-quality standard of products in the chemical industry, and the DMAC can be directly sold; 3. the energy consumption and the equipment abrasion are reduced, the cost is saved, the residual liquid amount is reduced, and the environment is protected; 4. in the normal production process, the DMAC residual liquid can generate about 150 parts per month, after the DMAC residual liquid is recovered, the final residual liquid is about 60-70 parts, 80% of DMAC is recoverable, and the pressure for treating the residual liquid is greatly relieved.
Drawings
FIG. 1 is a schematic diagram of a DMAC raffinate recovery unit.
Detailed Description
The invention is further illustrated with reference to fig. 1:
a DMAC raffinate recovery device comprises the following equipment: the residual liquid transfer tank is connected with an inlet at the top of a rectifying tower (containing a reboiler), an outlet at the top of the rectifying tower is sequentially connected with a condenser, a reflux tank, a buffer tank and a vacuum pump, and an outlet at the bottom of the rectifying tower is connected to a final residual liquid tank through a pipeline; the bottom of the reflux tank is respectively connected to an inlet at the top of the rectifying tower and a recovered residue tank through pipelines.
A DMAC residual liquid recovery method comprises the following specific implementation steps:
(1) after the valve is checked, starting a vacuum pump, and pumping air in the rectifying tower to a tail gas system through a condenser, a reflux tank and a buffer tank and then through the vacuum pump to control the pressure in the rectifying tower to be-92 KPa;
(2) the DMAC residual liquid (from an acid DMF working section) in a residual liquid transfer tank is pumped into a rectifying tower (60 to 80 percent of the residual liquid is in the rectifying tower) for carrying out reduced pressure rectification and concentration, and the temperature in the rectifying tower is controlled to be 115 ℃ and the pressure is controlled to be-90 KPa;
(3) gas phase (crude product DMAC) from the top of the rectifying tower is condensed into liquid through a condenser (25-30 ℃) and flows into a reflux tank, when the reflux tank contains liquid level with the volume of 30-40%, a pipeline of which the bottom flows to the rectifying tower is opened, the reflux of 20% of liquid amount in the reflux tank is controlled, when the content of DMAC extracted from the top of the rectifying tower is more than 80%, the rectification is finished when the content of DMAC extracted from the bottom of the rectifying tower is less than 40%, and the bottom residual liquid is extracted to a final residual liquid tank and is treated as fuel.
Claims (2)
1. The DMAC residual liquid recovery device is characterized by comprising the following devices: a residual liquid transfer tank, a rectifying tower, a condenser, a reflux tank, a buffer tank, a vacuum pump, a final residual liquid tank and a recovered residual liquid tank;
the residual liquid transfer tank is connected with an inlet at the top of the rectifying tower, an outlet at the top of the rectifying tower is sequentially connected with a condenser, a reflux tank, a buffer tank and a vacuum pump, and an outlet at the bottom of the rectifying tower is connected to a final residual liquid tank through a pipeline; the bottom of the reflux tank is respectively connected to an inlet at the top of the rectifying tower and a recovered residue tank through pipelines.
2. A DMAC residual liquid recovery method is characterized by comprising the following steps:
(1) after the valve is checked, a vacuum pump is started, air in the rectifying tower passes through a condenser, a reflux tank and a buffer tank and then is pumped to a tail gas system by the vacuum pump, and the pressure in the rectifying tower is controlled to be-88 to-96 KPa;
(2) the DMAC residual liquid in the residual liquid transfer tank is fed into a rectifying tower for vacuum rectification and concentration, and the temperature in the rectifying tower is controlled to be 100-110 ℃ and the pressure is controlled to be-88 to-96 KPa;
(3) gas phase coming out of the top of the rectifying tower is condensed into liquid through a condenser and flows into a reflux tank, when the reflux tank contains liquid level of 30-40% of volume, a pipeline flowing to the rectifying tower at the bottom of the reflux tank is opened, reflux of 30-40% of the liquid in the reflux tank is controlled, when the content of DMAC (dimethylacetamide) extracted from the top of the rectifying tower is above 80%, rectification is finished when the content of DMAC extracted from the bottom of the rectifying tower is below 40%, and bottom residual liquid is extracted to a final residual liquid tank and is treated as fuel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911123225.5A CN110759832A (en) | 2019-11-16 | 2019-11-16 | DMAC (dimethylacetamide) residual liquid recycling device and method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911123225.5A CN110759832A (en) | 2019-11-16 | 2019-11-16 | DMAC (dimethylacetamide) residual liquid recycling device and method |
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| CN110759832A true CN110759832A (en) | 2020-02-07 |
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| CN201911123225.5A Pending CN110759832A (en) | 2019-11-16 | 2019-11-16 | DMAC (dimethylacetamide) residual liquid recycling device and method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111574394A (en) * | 2020-05-22 | 2020-08-25 | 安徽金禾实业股份有限公司 | Method for treating carboxylic acid-containing DMF (dimethyl formamide) in sucralose production |
| CN111592469A (en) * | 2020-05-22 | 2020-08-28 | 安徽金禾实业股份有限公司 | Method for recovering DMAC (dimethylacetamide) residual liquid in sucralose production |
| CN112742042A (en) * | 2020-11-30 | 2021-05-04 | 安徽金禾实业股份有限公司 | Acidic DMF single-effect evaporation treatment device and method |
| CN113185424A (en) * | 2021-05-21 | 2021-07-30 | 安徽金禾实业股份有限公司 | Method for removing trace DMAc in DMF (dimethyl formamide) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6193147A (en) * | 1984-10-15 | 1986-05-12 | Daicel Chem Ind Ltd | Method of purifying n-dimethylacetamide |
| DE10315214A1 (en) * | 2003-04-03 | 2004-10-14 | Basf Ag | Process for the purification of dimethylacetamide (DMAC) |
| CN203355328U (en) * | 2013-06-07 | 2013-12-25 | 河南骏化发展股份有限公司 | Dimethyl acetamide rectification system |
| CN106220537A (en) * | 2016-08-31 | 2016-12-14 | 烟台国邦化工机械科技有限公司 | A kind of by separate to rectifying section and stripping section rectification process |
| CN205990356U (en) * | 2016-08-31 | 2017-03-01 | 烟台国邦化工机械科技有限公司 | A kind of novel distillation system |
-
2019
- 2019-11-16 CN CN201911123225.5A patent/CN110759832A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6193147A (en) * | 1984-10-15 | 1986-05-12 | Daicel Chem Ind Ltd | Method of purifying n-dimethylacetamide |
| DE10315214A1 (en) * | 2003-04-03 | 2004-10-14 | Basf Ag | Process for the purification of dimethylacetamide (DMAC) |
| CN203355328U (en) * | 2013-06-07 | 2013-12-25 | 河南骏化发展股份有限公司 | Dimethyl acetamide rectification system |
| CN106220537A (en) * | 2016-08-31 | 2016-12-14 | 烟台国邦化工机械科技有限公司 | A kind of by separate to rectifying section and stripping section rectification process |
| CN205990356U (en) * | 2016-08-31 | 2017-03-01 | 烟台国邦化工机械科技有限公司 | A kind of novel distillation system |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111574394A (en) * | 2020-05-22 | 2020-08-25 | 安徽金禾实业股份有限公司 | Method for treating carboxylic acid-containing DMF (dimethyl formamide) in sucralose production |
| CN111592469A (en) * | 2020-05-22 | 2020-08-28 | 安徽金禾实业股份有限公司 | Method for recovering DMAC (dimethylacetamide) residual liquid in sucralose production |
| CN112742042A (en) * | 2020-11-30 | 2021-05-04 | 安徽金禾实业股份有限公司 | Acidic DMF single-effect evaporation treatment device and method |
| CN113185424A (en) * | 2021-05-21 | 2021-07-30 | 安徽金禾实业股份有限公司 | Method for removing trace DMAc in DMF (dimethyl formamide) |
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Application publication date: 20200207 |
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