CN1803764A - N, N-dimethylformamide regeneration method after C5 extraction desorption - Google Patents
N, N-dimethylformamide regeneration method after C5 extraction desorption Download PDFInfo
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- CN1803764A CN1803764A CN 200510131163 CN200510131163A CN1803764A CN 1803764 A CN1803764 A CN 1803764A CN 200510131163 CN200510131163 CN 200510131163 CN 200510131163 A CN200510131163 A CN 200510131163A CN 1803764 A CN1803764 A CN 1803764A
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- extraction
- regeneration
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- 238000011069 regeneration method Methods 0.000 title claims abstract description 20
- 238000000605 extraction Methods 0.000 title claims description 10
- 238000003795 desorption Methods 0.000 title claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 title 3
- 230000008929 regeneration Effects 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000007670 refining Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 238000009418 renovation Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000001172 regenerating effect Effects 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 10
- 238000001816 cooling Methods 0.000 abstract description 8
- 229920000642 polymer Polymers 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 6
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 4
- 239000000539 dimer Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010009866 Cold sweat Diseases 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- -1 m-pentadiene Chemical compound 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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Abstract
The disclosed recovery and regeneration method for N, N-DMF comprises: leading the material from stripper into the regeneration tower at some pressure and temperature to let most polymers and tar fall into the regeneration tower; cooling the material from regeneration tower to enter into the DMF recovery refining column and obtain the DMF with purification more than 95% at given pressure and temperature. This invention saves energy, and has no pollution to environment.
Description
(1) technical field under
The present invention relates to a kind of N, dinethylformamide (to call DMF in the following text) recovery, regeneration, process for purification, N behind particularly a kind of carbon five extraction desorptions, the renovation process of dinethylformamide.
(2) background technology
The petroleum cracking process of producing ethylene because of boiling point is close or identical, is difficult to directly obtain by rectificating method isoprene, m-pentadiene, the dicyclopentadiene of higher degree in the byproduct C5 component.And according to C5 component relative volatility difference in DMF, utilize extraction, parsing, rectificating method, then can obtain highly purified isoprene, m-pentadiene, dicyclopentadiene, but because of containing more active diolefine among the C5, part diene polymerization in this process makes and contains more polymkeric substance and tar among the DMF at the bottom of the Analytic Tower.Recycling then directly influences effect of extracting, and easily causes the obstruction of tower tray, reboiler.Abandon it, then cause environmental pollution, substantial contribution, the wasting of resources.
(3) summary of the invention
The present invention is in order to remedy the deficiencies in the prior art, provides N behind a kind of carbon five extraction desorptions that are easy to suitability for industrialized production, the renovation process of dinethylformamide.
The present invention is achieved through the following technical solutions:
N behind a kind of carbon five extraction desorptions, the renovation process of dinethylformamide, its special character is: may further comprise the steps:
(1) Analytic Tower still material enters the regeneration still, and working pressure is-0.065～-0.085MPa, 115～175 ℃ of temperature steam DMF
(2) DMF enters DMF through surge tank and reclaims treating tower, and working pressure is a normal pressure, 120～150 ℃ of temperature, and the cocurrent flow ratio is controlled at 8～12, reclaims refining Tata still and obtains the DMF of purity more than 95%.
N behind carbon five extraction desorptions of the present invention, the renovation process of dinethylformamide in step (1), when liquid is than thickness in observing the regeneration still, stops charging, begins to concentrate, and promotes still temperature to 175 ℃, the switching of the still of regenerating simultaneously gradually.
Analytic Tower still material component:
Light C5 0.25%, DMF 82.74%, and X3 0.53%, dicyclopentadiene 4.05%, X4 12.9%, dimer 1.54%, tripolymer 1.86%.(, replace with X3, X4 owing to can't detect concrete composition in detail.Down together.)
Analytic Tower still material enters the regeneration still, and under certain pressure and temperature, most of polymkeric substance, tar fall in the regeneration still.The material that comes out from the regeneration still enters DMF recovery treating tower through cooling, and under certain pressure and temperature, the tower still obtains the DMF of purity more than 95%.
The present invention reaches more than 95% by purification DMF purity, utilizes once more, can reach good effect of extracting, has save energy, protection environment, easy to operate advantage.
(4) description of drawings
The present invention is further illustrated below in conjunction with accompanying drawing.
Accompanying drawing is a process flow diagram of the present invention.
(5) embodiment
Embodiment 1:
Analytic Tower still material cooling is after be pumped into the regeneration still, control pressure-0.065MPa, and 115 ℃ of temperature steam components such as DMF, through cooling off laggard DMF surge tank.Material reclaims the treating tower feeding pump through DMF and sends into the recovery treating tower in the surge tank, and the recovery treating tower is an atmospheric operation, and temperature is controlled at 120 ℃, reflux ratio 8.Reclaim the treating tower still and then obtain following product: DMF95.85%, dicyclopentadiene 0.9%, X4 5.56%, dimer 2.71%, tripolymer 1.11%.
Because of the regeneration still is continuously feeding, of long duration, polymer/tar accumulates in the regeneration still, and polymer/tar lumps in still and can't discharge, and causes the regeneration still to scrap.Can be observed by visor that liquid is clamminess in the still, temperature in the kettle rises, and vapor pressure raises, and should stop charging this moment, begins to heat up to concentrate, and (pressure remains unchanged, and temperature raises 160～175 ℃ gradually) observes material bubble situation in the still, determines the coke discharging time.When the regeneration still stops charging, the switching of the still of should regenerating.
Embodiment 2:
Analytic Tower still material cooling is after be pumped into the regeneration still, control pressure-0.085MPa, and 175 ℃ of temperature steam components such as DMF, through cooling off laggard DMF surge tank.Material reclaims the treating tower feeding pump through DMF and sends into the recovery treating tower in the surge tank, and the recovery treating tower is an atmospheric operation, and temperature is controlled at 135 ℃, reflux ratio 10.Reclaim the treating tower still and then obtain following product: DMF97.4407%, dicyclopentadiene 0.6021%, X4 2.8582%, dimer 2.3058%, tripolymer 0.7852%.Other is identical with embodiment 1.
Embodiment 3:
Analytic Tower still material cooling is after be pumped into the regeneration still, control pressure-0.075MPa, and 145 ℃ of temperature steam components such as DMF, through cooling off laggard DMF surge tank.Material reclaims the treating tower feeding pump through DMF and sends into the recovery treating tower in the surge tank, and the recovery treating tower is an atmospheric operation, and temperature is controlled at 150 ℃, reflux ratio 12.Reclaim the treating tower still and then obtain following product: DMF99.07%, dicyclopentadiene 0.33%, X4 0.69%, dimer 0.82%.Other is identical with embodiment 1.
Claims (3)
1. N behind carbon five extraction desorptions, the renovation process of dinethylformamide is characterized in that: may further comprise the steps:
(1) Analytic Tower still material enters the regeneration still, and working pressure is-0.065～-0.085MPa, 115～175 ℃ of temperature steam DMF;
(2) DMF enters DMF through surge tank and reclaims treating tower, and working pressure is a normal pressure, 120～150 ℃ of temperature, and control of reflux ratio reclaims refining Tata still and obtains the DMF of purity more than 95% 8～12.
2. N behind carbon five extraction desorptions according to claim 1, the renovation process of dinethylformamide is characterized in that: in step (1), when liquid is than thickness in observing the regeneration still, stop charging, begin to concentrate, promote still temperature to 175 ℃, the switching of the still of regenerating simultaneously gradually.
3. N behind carbon five extraction desorptions according to claim 1, the renovation process of dinethylformamide is characterized in that: in step (2), 150 ℃ of temperature, reflux ratio are 12.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101311634A CN100432045C (en) | 2005-12-26 | 2005-12-26 | N, N-dimethylformamide regeneration method after C5 extraction desorption |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101311634A CN100432045C (en) | 2005-12-26 | 2005-12-26 | N, N-dimethylformamide regeneration method after C5 extraction desorption |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1803764A true CN1803764A (en) | 2006-07-19 |
| CN100432045C CN100432045C (en) | 2008-11-12 |
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| CNB2005101311634A Active CN100432045C (en) | 2005-12-26 | 2005-12-26 | N, N-dimethylformamide regeneration method after C5 extraction desorption |
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| CN (1) | CN100432045C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040533A (en) * | 2009-10-20 | 2011-05-04 | 中国石油化工股份有限公司 | Regeneration method for N,N-dimethyl formamide and application thereof |
| CN101397261B (en) * | 2007-09-24 | 2011-11-30 | 中国石油化工股份有限公司 | Regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 and use thereof |
| CN101450908B (en) * | 2007-12-07 | 2011-11-30 | 中国石油化工股份有限公司 | Fractional condensation and regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 |
| CN101450909B (en) * | 2007-12-07 | 2011-11-30 | 中国石油化工股份有限公司 | Segregation and fractionation regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 |
| CN101434556B (en) * | 2007-11-16 | 2012-08-29 | 中国石油化工股份有限公司 | Regeneration method of C5 fraction extracting solvent N,N-dimethylformamide |
| CN103570576A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工集团公司 | Regeneration system and regeneration method for circulating solvent of cracked C5 separation device |
| CN103566608A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工集团公司 | Regeneration system and regeneration method for solvent of cracked C5 separation device |
| CN106811223A (en) * | 2017-03-22 | 2017-06-09 | 福建省环境工程有限公司 | A kind of tar processing method and processing unit |
| CN109569004A (en) * | 2019-01-31 | 2019-04-05 | 成都沃枘科技有限公司 | Continuous separating and reclaiming device of organic solvent waste liquid and application thereof |
| CN114432725A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Process system and method for refining dimethylformamide serving as solvent extracted by carbon five separation device |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EG10431A (en) * | 1971-08-02 | 1976-03-31 | Leuna Werk Walter Ulbrich Veb | Method for preparation of butadien polymer |
| SU1018932A1 (en) * | 1982-01-11 | 1983-05-23 | Предприятие П/Я В-8873 | Process for purifying dimethylformamide |
-
2005
- 2005-12-26 CN CNB2005101311634A patent/CN100432045C/en active Active
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101397261B (en) * | 2007-09-24 | 2011-11-30 | 中国石油化工股份有限公司 | Regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 and use thereof |
| CN101434556B (en) * | 2007-11-16 | 2012-08-29 | 中国石油化工股份有限公司 | Regeneration method of C5 fraction extracting solvent N,N-dimethylformamide |
| CN101450908B (en) * | 2007-12-07 | 2011-11-30 | 中国石油化工股份有限公司 | Fractional condensation and regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 |
| CN101450909B (en) * | 2007-12-07 | 2011-11-30 | 中国石油化工股份有限公司 | Segregation and fractionation regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 |
| CN102040533A (en) * | 2009-10-20 | 2011-05-04 | 中国石油化工股份有限公司 | Regeneration method for N,N-dimethyl formamide and application thereof |
| CN102040533B (en) * | 2009-10-20 | 2014-08-06 | 中国石油化工股份有限公司 | Regeneration method for N,N-dimethyl formamide and application thereof |
| CN103566608A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工集团公司 | Regeneration system and regeneration method for solvent of cracked C5 separation device |
| CN103570576A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工集团公司 | Regeneration system and regeneration method for circulating solvent of cracked C5 separation device |
| CN103566608B (en) * | 2012-07-20 | 2015-08-12 | 中国石油化工集团公司 | A kind of regenerative system of cracking c_5 separator solvent and renovation process |
| CN103570576B (en) * | 2012-07-20 | 2016-06-15 | 中国石油化工集团公司 | A kind of cracking c_5 tripping device circulating solvent regeneration system rapidly and method |
| CN106811223A (en) * | 2017-03-22 | 2017-06-09 | 福建省环境工程有限公司 | A kind of tar processing method and processing unit |
| CN109569004A (en) * | 2019-01-31 | 2019-04-05 | 成都沃枘科技有限公司 | Continuous separating and reclaiming device of organic solvent waste liquid and application thereof |
| CN114432725A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Process system and method for refining dimethylformamide serving as solvent extracted by carbon five separation device |
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| Publication number | Publication date |
|---|---|
| CN100432045C (en) | 2008-11-12 |
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Denomination of invention: Regeneration method for N,N-dimethyl formamide and application thereof Effective date of registration: 20120719 Granted publication date: 20081112 Pledgee: Prudential Bank Ji'nan branch of Limited by Share Ltd Pledgor: Shandong Yuhuang Chemical Co., Ltd. Registration number: 2012990000387 |
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Effective date of registration: 20141126 Address after: 274000 Changjiang Road, Heze Development Zone, Shandong, China, No. 4666 Patentee after: Jade Emperor flourishing age chemical inc, Shandong Address before: 274500 Shandong city of Heze province Dongming County wusheng Township Development Zone Patentee before: Shandong Yuhuang Chemical Co., Ltd. |
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Denomination of invention: Regeneration method for N,N-dimethyl formamide and application thereof Effective date of registration: 20150910 Granted publication date: 20081112 Pledgee: China Minsheng Banking Corp Ji'nan branch Pledgor: Jade Emperor flourishing age chemical inc, Shandong Registration number: 2015370000047 |
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