CN1125039C - Process for rectifying recovery of diluted dimethyl formamide liquid generated in synthesizing artificial leather by wet method - Google Patents

Process for rectifying recovery of diluted dimethyl formamide liquid generated in synthesizing artificial leather by wet method Download PDF

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Publication number
CN1125039C
CN1125039C CN 00125092 CN00125092A CN1125039C CN 1125039 C CN1125039 C CN 1125039C CN 00125092 CN00125092 CN 00125092 CN 00125092 A CN00125092 A CN 00125092A CN 1125039 C CN1125039 C CN 1125039C
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China
Prior art keywords
rectifying
tower
recovery
dimethylformamide
dimethyl formamide
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Expired - Fee Related
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CN 00125092
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CN1282733A (en
Inventor
金根林
朱利国
王诗军
计国兴
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TIANHUI SYNTHETIC LEATHER FACTORY SHANGHAI
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TIANHUI SYNTHETIC LEATHER FACTORY SHANGHAI
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Priority to CN 00125092 priority Critical patent/CN1125039C/en
Publication of CN1282733A publication Critical patent/CN1282733A/en
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Abstract

The present invention relates to a rectifying recovery method of dimethylformamide thin liquid for synthesizing artificial leather by a wet method. The rectifying recovery method is characterized in that the phase-change boiling distillation is used for tower heating, and from the intermediate section of a rectifying tower, the gas phase part of dimethylformamide is leaded into the rectifying tower which is a plate type packing composite tower. Recovery technological process adopts circulation technology, and the generated heat energy is circularly utilized among finished product condensation working procedure, tower heating working procedure, rectification working procedure and reboiling working procedure. Acid impurities produced in the recovery technological process are neutralized by alkali, extracted by using organic solvent with the physical principle of similarity and intermiscibility and removed at the time of light and medium maintenance of the rectifying tower. The present invention has the advantages of simple technological process, simplified equipment and low energy consumption, and the recovery rate of dimethylformamide thin liquid can reach 99.95%.

Description

Process for rectifying recovery of diluted dimethyl formamide liquid generated in synthesizing artificial leather by wet method
The present invention relates to the recovery method of synthetic leather solvent, particularly relate to a kind of process for rectifying recovery of diluted dimethyl formamide liquid generated in synthesizing artificial leather by wet method.
At present, domestic have up to a hundred wet method leather production lines, mostly adopts dimethyl formamide as solvent, and dimethyl formamide is a kind of hazardous solvent, can reduce pollution to environment to its recycling.The domestic existing basic interruption method recovery technology that adopts, this technical matters flow process is simple, but can't continuous production, and the rate of recovery is low, easily causes environmental pollution.Chinese patent CN96116260.0 " solvent-resisting polysulfone hollow fiber ultrafiltration membrane system " has introduced a kind of dimethyl formamide as the Recovery of Organic Solvent technology, but it adopts the cellulosic ultrafiltration film as end-filtration, and cost is higher.In the world, gondola leather and synthetic leather processing technology maintain the leading position, and diluted dimethyl formamide liquid generated in synthesizing rectifying recovery technology is also advanced with Italy, but its double tower system flow process exists equipment complexity, shortcoming that energy consumption is high.
The object of the present invention is to provide that a kind of technical process is simple, simplified equipment, energy consumption is low, the rate of recovery is high process for rectifying recovery of diluted dimethyl formamide liquid generated in synthesizing artificial leather by wet method.
The object of the present invention is achieved like this: diluted dimethyl formamide liquid generated in synthesizing enters cooling condensation and finished product condensation operation by feed process, through the heating of tower still, adopt phase transformation boiling distillation, dimethyl formamide gas phase part enters rectifying tower and the operation of boiling again by the rectifying tower stage casing, rectifying tower adopts filler and board-like combination tower, the purification of dimethyl formamide comprises boils and separation circuit again, and the dimethyl formamide of rectifying is through finished product condensation operation, by going out the material process output.Circulation technology is adopted in recovery technical process of the present invention, the heat energy of generation in finished product condensation, the heating of tower still, rectifying, the recycle between the operation of boiling again.The present invention reclaims the acidic impurities that produces in the technical process and utilizes alkali to carry out neutralization reaction, utilizes the similar physical principle that mixes to extract with organic solvent then, and little, in remove when repairing.
The invention has the beneficial effects as follows: owing to adopted phase transformation boiling distillation technique, got rid of the forced circulation pump in the Italian technology, power consumption has reduced by 50%.Owing to adopted filler and board-like compound rectifying column, reduced tower height, solved stifled tower problem, product index reaches international standard.The present invention adopts the heat energy circulating technology, and the energy consumption amplitude is reduced greatly.Utilize chemical reaction to handle residue, got rid of treatment facilities such as skim gate with the similar physical principle that mixes.
Description of drawings
Fig. 1 is a process flow diagram of the present invention
The invention will be further described below in conjunction with accompanying drawing
Embodiment: 22% diluted dimethyl formamide liquid generated in synthesizing is entered cooling condensation and finished product condensation operation with 2.5 tons/hour by feed process, be heated to 110 ℃ through the tower still, adopt phase transformation boiling distillation, the dimethyl formamide gas phase partly enters rectifying, the operation of boiling again, rectifying tower adopts filler and board-like combination tower, tower height is 26 meters, tower vacuum tightness is 80000 handkerchiefs, rectifying dimethyl formamide cut is 105 ℃ by cutting out temperature in the middle of the tower, through finished product condensation operation, by going out the material process output, hourly output is 600 kilograms, and the purity of the dimethyl formamide of recovery reaches 99.95%.Part dimethyl formamide mixed solution through 125 ℃ of reflux of reboiler to rectifying tower, cyclical operation.Circulation technology is adopted in recovery technical process of the present invention, the heat energy of generation in finished product condensation, the heating of tower still, rectifying, the recycle between the operation of boiling again.The present invention reclaims the acidic impurities such as formic acid that produce in the technical process and utilizes 25% NaOH to carry out neutralization reaction, extract with 85% methyl alcohol again, and little, in remove when repairing.

Claims (3)

1, a kind of wet-method synthetic leather dimethylformamide thin liquid process for rectifying recovery comprises: charging, cools off cold liquid, finished product condensation, the heating of tower still, rectifying, separation, boils, goes out material process again, it is characterized in that,
A, tower still add thermal recovery phase transformation boiling distillation, and dimethyl formamide gas phase part enters rectifying tower by the rectifying tower stage casing;
B, rectifying tower adopt filler and board-like combination tower.
2, a kind of wet-method synthetic leather dimethylformamide thin liquid process for rectifying recovery according to claim 1 is characterized in that, the heat energy that in described recovery method, produces in finished product condensation, the heating of tower still, rectifying, the recycle between the operation of boiling again.
3, a kind of wet-method synthetic leather dimethylformamide thin liquid process for rectifying recovery according to claim 1, it is characterized in that, the acidic impurities that produces in described recovery method utilizes alkali to neutralize, extract with organic solvent then, and little, in remove in repairing.
CN 00125092 2000-09-07 2000-09-07 Process for rectifying recovery of diluted dimethyl formamide liquid generated in synthesizing artificial leather by wet method Expired - Fee Related CN1125039C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 00125092 CN1125039C (en) 2000-09-07 2000-09-07 Process for rectifying recovery of diluted dimethyl formamide liquid generated in synthesizing artificial leather by wet method

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Application Number Priority Date Filing Date Title
CN 00125092 CN1125039C (en) 2000-09-07 2000-09-07 Process for rectifying recovery of diluted dimethyl formamide liquid generated in synthesizing artificial leather by wet method

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CN1282733A CN1282733A (en) 2001-02-07
CN1125039C true CN1125039C (en) 2003-10-22

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100422142C (en) * 2005-12-06 2008-10-01 浙江禾欣实业集团股份有限公司 Dimethyl formylamine solution three-effect rectification recovery method for wet synthesis of leather
CN101838215A (en) * 2010-05-25 2010-09-22 刘伟斌 Process for separating acetic acid from DMAC azeotrope

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101386632B (en) * 2007-09-12 2011-03-09 盐城捷康三氯蔗糖制造有限公司 Method for recovering tert-amide solvent from sucrose trichloride production process
CN101759590B (en) * 2009-05-16 2012-11-21 石狮龙祥制革有限公司 DMF recycling method
CN101825220B (en) * 2010-05-07 2011-11-16 海宁瑞星皮革有限公司 DMF gas recovery device
CN103980143B (en) * 2014-04-29 2015-07-15 中节能清洁技术发展有限公司 Method and system for distillation recycling of dimethyl formamide rectified residual liquid

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100422142C (en) * 2005-12-06 2008-10-01 浙江禾欣实业集团股份有限公司 Dimethyl formylamine solution three-effect rectification recovery method for wet synthesis of leather
CN101838215A (en) * 2010-05-25 2010-09-22 刘伟斌 Process for separating acetic acid from DMAC azeotrope
CN101838215B (en) * 2010-05-25 2013-03-27 刘伟斌 Process for separating acetic acid from DMAC azeotrope

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