CN101712616B - Method for separating dimethyl benzene and butyl acetate from industrial waste solvent - Google Patents
Method for separating dimethyl benzene and butyl acetate from industrial waste solvent Download PDFInfo
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- CN101712616B CN101712616B CN 200810140329 CN200810140329A CN101712616B CN 101712616 B CN101712616 B CN 101712616B CN 200810140329 CN200810140329 CN 200810140329 CN 200810140329 A CN200810140329 A CN 200810140329A CN 101712616 B CN101712616 B CN 101712616B
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- butyl acetate
- industrial waste
- solvent
- waste solvent
- dimethyl benzene
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- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000002904 solvent Substances 0.000 title claims abstract description 50
- 239000002440 industrial waste Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 18
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 title abstract 6
- 238000010992 reflux Methods 0.000 claims abstract description 15
- 238000001577 simple distillation Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 241000282326 Felis catus Species 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000010887 waste solvent Substances 0.000 abstract 2
- 238000005265 energy consumption Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000003113 dilution method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- YTLYLLTVENPWFT-UHFFFAOYSA-N 3-aminoprop-2-enoic acid Chemical compound NC=CC(O)=O YTLYLLTVENPWFT-UHFFFAOYSA-N 0.000 description 1
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical compound CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a method for separating dimethyl benzene and butyl acetate from industrial waste solvent. The method comprises the following steps of: a, performing atmospheric simple distillation to the industrial waste solvent to obtain colorless and transparent waste solvent to be separated; b, mixing the waste solvent to be separated processed through simple atmospheric distillation with water in weight ratio of 1 to 3:1 to obtain a heterogeneous azeotropic system, and then performing rectification separation operation to the heterogeneous azeotropic system in a batch rectificationtower; and c, performing continuous reflux for 30 to 100 minutes after performing infinite reflux for 30 to 60 minutes in the batch rectification tower, and sequentially distilling off butyl acetate and dimethyl benzene from the top of the tower. The method for separating dimethyl benzene and butyl acetate from industrial waste solvent has the advantages that the separation effect is good, the heating temperature of the method is 50 to 80 DEG C lower than that of conventional homogeneous batch rectification, the yield coefficient of the butyl acetate is 80 to 99 percent, the yield coefficientof the dimethyl benzene is 84 to 87 percent, the separated dimethyl benzene and butyl acetate can be reused, the entrainer can be recycled, no pollution is produced during the separation process, theenergy consumption is low, and the processing cost is low.
Description
Technical field
The invention provides a kind of separation method of industrial waste solvent, especially a kind of from industrial waste solvent the method for separating dimethyl benzene and N-BUTYL ACETATE.
Background technology
Produce a large amount of industrial waste solvents in the industry production processes such as automobile and component, pesticide intermediate, paint, electronics, petrochemical complex, contain paint vehicles such as dimethylbenzene, N-BUTYL ACETATE and alkyd, amino, vinylformic acid in these solvent slops, volatile, inflammable, explosive, has strong toxicity, be listed in a class hazardous industry waste, there are harm greatly in environment and human health.But the solvent composition in the solvent slop has higher economic value.Along with the shortage of oil supply and the continuous increase of coating output and kind, the demand of countries in the world p-Xylol is in rising trend year by year, and its price rises to present 14000 yuan/ton by 4000 yuan/ton, and supply falls short of demand.Mainly adopt burning method, dilution method etc. to handle and adopt distillation under vacuum or solvent recovery machine to reclaim to solvent slop at present.Burning method not only causes the waste that important economic worth organic solvent is arranged in a large number, and combustion processes produces a large amount of poisonous fumes, and atmospheric environment is caused secondary pollution; Dilution method waste great amount of water resources, and cause serious water pollution easily, inadvisable in today of water resources worsening shortages.Equipment requirements height when underpressure distillation is reclaimed, energy consumption is big, the cost recovery height; Shortcomings such as solvent recovery machine exists energy consumption big, and processing power is low, and separation efficiency is low, and recovered solvent purity is low, especially for the multi-component complex mixture, resolution is relatively poor, can not obtain the higher technical grade solvent of quality.
Summary of the invention
Technical problem to be solved by this invention is, provide a kind of from industrial waste solvent the method for separating dimethyl benzene and N-BUTYL ACETATE, to improve separating effect, reduce separation costs.
The present invention is achieved in that the method for separating dimethyl benzene and N-BUTYL ACETATE from industrial waste solvent, and the step of described method is,
A, industrial waste solvent is carried out normal pressure simple distillation, distillation is 3-5 hour under 120-200 ℃ of temperature, remove suspended substance and high-boiling-point impurity in the industrial waste solvent, obtain water white solvent slop to be separated, the content sum of dimethylbenzene and N-BUTYL ACETATE is 93%-97% by mass percentage in the solvent slop to be separated, and other heavy seeds component is 3%-7% by mass percentage;
B, will be the mixed of 1～3:1 by weight through solvent slop to be separated and the water that obtains after the above-mentioned normal pressure simple distillation, form heteroazeotropic system, in batch fractionating tower, carry out the rectifying separation operation;
C, batch fractionating tower total reflux be after 30-60 minute, is that 5-15, tower reactor temperature are under the condition of 92-150 ℃, tower top temperature 89-100 ℃ keeping reflux ratio again, continues backflow 30-100 minute, distillates N-BUTYL ACETATE and dimethylbenzene successively from cat head.
This from industrial waste solvent the method for separating dimethyl benzene and N-BUTYL ACETATE, good separating effect, Heating temperature reduces 40-80 ℃ than conventional homogeneous phase batch fractionating, the N-BUTYL ACETATE yield is 80-99%, the dimethylbenzene yield is 84-87%, and isolated dimethylbenzene and N-BUTYL ACETATE can utilize again, and entrainer can be recycled, the pollution-free generation of sepn process, and the energy consumption of separating is low, processing cost is low.This method not only can be used for solving automobile and component industry, agricultural chemicals and the pollution problem of Paint Production solvent slop, and can be used for separating of field organic mixture systems such as petrochemical complex, pharmacy and electronics.Application Areas is extensive, remarkable in economical benefits.
Embodiment
Further specify the present invention below.
Described industrial waste solvent is carried out normal pressure simple distillation, in the common fillers batch fractionating tower, carry out.
To be the mixed of 1～3:1 by weight through solvent slop to be separated and the water that obtains after the normal pressure simple distillation.The mixed solution that forms is in the batch fractionating tower rectifying, and the initial stage overhead product is mainly N-BUTYL ACETATE, and along with the increase of time and temperature, the overhead product xylene content reaches more than 98% gradually, and N-BUTYL ACETATE content is reduced to below 2%.After the time surpassed 90 minutes, overhead product mainly was dimethylbenzene, and N-BUTYL ACETATE content is near 0.
Embodiment 1
A, industrial waste solvent is carried out normal pressure simple distillation, distillation is 3 hours under 120 ℃ of temperature, remove suspended substance and high-boiling-point impurity in the industrial waste solvent, obtain water white solvent slop to be separated, the content sum of dimethylbenzene and N-BUTYL ACETATE is 93% by mass percentage in the solvent slop to be separated, and other heavy seeds component is 7% by mass percentage;
B, will form heteroazeotropic system through the solvent slop to be separated that obtains after the above-mentioned normal pressure simple distillation and water by weight be the mixed of 1:1, and in batch fractionating tower, carry out rectifying separation and operate;
C, batch fractionating tower total reflux be after 30 minutes, again keep that reflux ratio is 5, the tower reactor temperature is under the condition of 89 ℃ of 92 ℃, tower top temperature, continues to reflux 30 minutes, distillates N-BUTYL ACETATE and dimethylbenzene successively from cat head.
Embodiment 2
A, industrial waste solvent is carried out normal pressure simple distillation, distillation is 5 hours under 200 ℃ of temperature, remove suspended substance and high-boiling-point impurity in the industrial waste solvent, obtain water white solvent slop to be separated, the content sum of dimethylbenzene and N-BUTYL ACETATE is 97% by mass percentage in the solvent slop to be separated, and other heavy seeds component is 3% by mass percentage;
B, will form heteroazeotropic system through the solvent slop to be separated that obtains after the above-mentioned normal pressure simple distillation and water by weight be the mixed of 3:1, and in batch fractionating tower, carry out rectifying separation and operate;
C, batch fractionating tower total reflux be after 60 minutes, again keep that reflux ratio is 15, the tower reactor temperature is under the condition of 100 ℃ of 150 ℃, tower top temperature, continues to reflux 100 minutes, distillates N-BUTYL ACETATE and dimethylbenzene successively from cat head.
Embodiment 3
A, industrial waste solvent is carried out normal pressure simple distillation, distillation is 4 hours under 150 ℃ of temperature, remove suspended substance and high-boiling-point impurity in the industrial waste solvent, obtain water white solvent slop to be separated, the content sum of dimethylbenzene and N-BUTYL ACETATE is 95% by mass percentage in the solvent slop to be separated, and other heavy seeds component is 5% by mass percentage;
B, will form heteroazeotropic system through the solvent slop to be separated that obtains after the above-mentioned normal pressure simple distillation and water by weight be the mixed of 2:1, and in batch fractionating tower, carry out rectifying separation and operate;
C, batch fractionating tower total reflux be after 45 minutes, again keep that reflux ratio is 10, the tower reactor temperature is under the condition of 92 ℃ of 120 ℃, tower top temperature, continues to reflux 70 minutes, distillates N-BUTYL ACETATE and dimethylbenzene successively from cat head.
Claims (2)
1. the method for separating dimethyl benzene and N-BUTYL ACETATE from industrial waste solvent is characterized in that, the step of described method is,
A, industrial waste solvent is carried out normal pressure simple distillation, distillation is 3-5 hour under 120-200 ℃ of temperature, remove suspended substance and high-boiling-point impurity in the industrial waste solvent, obtain water white solvent slop to be separated, the content sum of dimethylbenzene and N-BUTYL ACETATE is 93%-97% by mass percentage in the solvent slop to be separated, and other heavy seeds component is 3%-7% by mass percentage;
B, will be the mixed of 1～3:1 by weight through solvent slop to be separated and the water that obtains after the above-mentioned normal pressure simple distillation, form heteroazeotropic system, in batch fractionating tower, carry out the rectifying separation operation;
C, batch fractionating tower total reflux be after 30-60 minute, is that 5-15, tower reactor temperature are under the condition of 92-150 ℃, tower top temperature 89-100 ℃ keeping reflux ratio again, continues backflow 30-100 minute, distillates N-BUTYL ACETATE and dimethylbenzene successively from cat head.
As claimed in claim 1 from industrial waste solvent the method for separating dimethyl benzene and N-BUTYL ACETATE, it is characterized in that, described industrial waste solvent is carried out normal pressure simple distillation, in the common fillers batch fractionating tower, carry out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810140329 CN101712616B (en) | 2008-09-30 | 2008-09-30 | Method for separating dimethyl benzene and butyl acetate from industrial waste solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810140329 CN101712616B (en) | 2008-09-30 | 2008-09-30 | Method for separating dimethyl benzene and butyl acetate from industrial waste solvent |
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| Publication Number | Publication Date |
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| CN101712616A CN101712616A (en) | 2010-05-26 |
| CN101712616B true CN101712616B (en) | 2013-09-04 |
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| CN 200810140329 Expired - Fee Related CN101712616B (en) | 2008-09-30 | 2008-09-30 | Method for separating dimethyl benzene and butyl acetate from industrial waste solvent |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107619146B (en) * | 2017-10-30 | 2020-05-22 | 新中天环保股份有限公司 | Method for recovering waste solvent in automobile industry |
| CN107698420B (en) * | 2017-11-03 | 2021-01-05 | 新中天环保股份有限公司 | Waste solvent-oil separation process |
| CN110156556A (en) * | 2019-06-03 | 2019-08-23 | 新中天环保股份有限公司 | A kind of coating solvent slop withdrawal technique |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696098A (en) * | 2005-03-25 | 2005-11-16 | 扬子石油化工股份有限公司 | Method for recovering raw material, solvent and by-product generated in procedure of producing aromatic carboxylic acid |
| CN101024139A (en) * | 2006-12-31 | 2007-08-29 | 武汉旭日华科技发展有限公司 | Method and apparatus for absorbing and recovering volatile gas by active charcoal fiber |
| CN101168505A (en) * | 2007-11-30 | 2008-04-30 | 胡先念 | Preparation method for sec-butyl acetate with product separating and reclaiming technique |
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2008
- 2008-09-30 CN CN 200810140329 patent/CN101712616B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696098A (en) * | 2005-03-25 | 2005-11-16 | 扬子石油化工股份有限公司 | Method for recovering raw material, solvent and by-product generated in procedure of producing aromatic carboxylic acid |
| CN101024139A (en) * | 2006-12-31 | 2007-08-29 | 武汉旭日华科技发展有限公司 | Method and apparatus for absorbing and recovering volatile gas by active charcoal fiber |
| CN101168505A (en) * | 2007-11-30 | 2008-04-30 | 胡先念 | Preparation method for sec-butyl acetate with product separating and reclaiming technique |
Non-Patent Citations (2)
| Title |
|---|
| 李贞玉等.间歇精馏回收废溶剂油中二甲苯/醋酸丁酯实验及模拟.《滨州学院学报》.2007,第23卷(第6期),40-44. |
| 间歇精馏回收废溶剂油中二甲苯/醋酸丁酯实验及模拟;李贞玉等;《滨州学院学报》;20071231;第23卷(第6期);40-44 * |
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