CN104774132B - A kind of method of separation of extractive distillation hexanaphthene and n-propyl alcohol mixture - Google Patents
A kind of method of separation of extractive distillation hexanaphthene and n-propyl alcohol mixture Download PDFInfo
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- CN104774132B CN104774132B CN201510108091.5A CN201510108091A CN104774132B CN 104774132 B CN104774132 B CN 104774132B CN 201510108091 A CN201510108091 A CN 201510108091A CN 104774132 B CN104774132 B CN 104774132B
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- extraction
- propyl alcohol
- extraction agent
- hexanaphthene
- mixture
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000000203 mixture Substances 0.000 title claims abstract description 43
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000895 extractive distillation Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000000926 separation method Methods 0.000 title claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 100
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 88
- 238000011084 recovery Methods 0.000 claims abstract description 23
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 description 45
- 239000002904 solvent Substances 0.000 description 8
- WIRUZQNBHNAMAB-UHFFFAOYSA-N benzene;cyclohexane Chemical compound C1CCCCC1.C1=CC=CC=C1 WIRUZQNBHNAMAB-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pyrrole Compounds (AREA)
Abstract
The present invention discloses a kind of method of separation of extractive distillation hexanaphthene and n-propyl alcohol mixture. It is taking the mixture of dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone as extraction agent, hexanaphthene to be separated and n-propyl alcohol mixture enter in the extractive distillation column that 30-60 block theoretical stage is housed by 15-40 block theoretical stage, extraction agent is entered by 5-20 block theoretical stage, hexanaphthene is by extracting rectifying top of tower extraction, extraction agent and n-propyl alcohol are entered, by after extracting rectifying tower bottom extraction, the extraction agent recovery tower that 15-30 block theoretical stage is housed by 10-20 block theoretical stage, n-propyl alcohol is used by extraction Posterior circle bottom extraction agent recovery tower by extraction agent recovery tower top extraction, extraction agent. It is an advantage of the current invention that energy consumption is low, product purity and receipts rate height, technique is simple, safety, environmental protection, pollution-free, it may be achieved cleaner production.
Description
Technical field
The present invention relates to separating benzene-cyclohexane and the method for n-propyl alcohol mixture, particularly relate to a kind of method of separation of extractive distillation hexanaphthene and n-propyl alcohol mixture.
Background technology
Hexanaphthene is industrially mainly used in the solvent of rubber, coating, varnish, and the thinner of tackiness agent and oil extraction agent, also can be used for preparing the organism such as hexalin and pimelinketone. N-propyl alcohol is important industrial chemicals, is also the solvent of good properties, can be used for the production process of the products such as coating, printing-ink, makeup, medicine, agricultural chemicals, fodder additives, synthetic perfume.
In Chemical Manufacture, often produce the mixture of hexanaphthene and n-propyl alcohol, for reducing production cost, reduce environmental pollution, hexanaphthene need to be separated with the mixture of n-propyl alcohol, but hexanaphthene and n-propyl alcohol form azeotrope, cannot be separated with conventional distillation.
About being separated of hexanaphthene and n-propyl alcohol, Bai Peng etc. (modern chemical industry, 2013,33(6), 108) study, it is that extraction agent carries out batch extracting rectified taking DMF, cyclohexane product massfraction can reach 96.2%, and the rate of recovery is 72.2%. There is product purity and rate of recovery shortcoming all on the low side in this method separating benzene-cyclohexane and n-propyl alcohol.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of method of separation of extractive distillation hexanaphthene and n-propyl alcohol mixture.
By the method for separation of extractive distillation hexanaphthene and n-propyl alcohol mixture it is: taking the mixture of dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone as extraction agent, hexanaphthene to be separated and n-propyl alcohol mixture enter in the extractive distillation column that 30-60 block theoretical stage is housed by 15-40 block theoretical stage, extraction agent is entered by 5-20 block theoretical stage, hexanaphthene is by extracting rectifying top of tower extraction, extraction agent and n-propyl alcohol are entered, by after extracting rectifying tower bottom extraction, the extraction agent recovery tower that 15-30 block theoretical stage is housed by 10-20 block theoretical stage, n-propyl alcohol is by the top extraction of extraction agent recovery tower, extraction agent is used by extraction Posterior circle bottom extraction agent recovery tower, schema is as shown in Figure 1.
In the mixture of described dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone, mass percent shared by dimethyl sulfoxide (DMSO) is 40%-80%.
Described extraction agent is 2-5 with the ratio of mixture velocity to be separated, and mixture to be separated is made up of hexanaphthene and n-propyl alcohol. The reflux ratio of described extractive distillation column is 2-6, and the reflux ratio of described extraction agent recovery tower is 1-3.
It is an advantage of the current invention that energy consumption is low, product purity and receipts rate height, technique is simple, safety, environmental protection, pollution-free, it may be achieved cleaner production.
Accompanying drawing explanation
Fig. 1 is with the schema of separation of extractive distillation hexanaphthene and n-propyl alcohol mixture.
Embodiment
By the method for separation of extractive distillation hexanaphthene and n-propyl alcohol mixture it is: taking the mixture of dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone as extraction agent, hexanaphthene to be separated and n-propyl alcohol mixture enter in the extractive distillation column that 30-60 block theoretical stage is housed by 15-40 block theoretical stage, extraction agent is entered by 5-20 block theoretical stage, hexanaphthene is by extracting rectifying top of tower extraction, extraction agent and n-propyl alcohol are entered, by after extracting rectifying tower bottom extraction, the extraction agent recovery tower that 15-30 block theoretical stage is housed by 10-20 block theoretical stage, n-propyl alcohol is by the top extraction of extraction agent recovery tower, extraction agent is used by extraction Posterior circle bottom extraction agent recovery tower.
In the mixture of described dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone, mass percent shared by dimethyl sulfoxide (DMSO) is 40%-80%.
Described extraction agent is 2-5 with the ratio of mixture velocity to be separated, and mixture to be separated is made up of hexanaphthene and n-propyl alcohol. The reflux ratio of described extractive distillation column is 2-6. The reflux ratio of described extraction agent recovery tower is 1-3.
Embodiment 1
At an internal diameter 50mm, it is equipped with in the extractive distillation column of 60 pieces of theoretical stages, hexanaphthene and n-propyl alcohol mixture (mass content is respectively 60% and 40%) enter this tower with the speed of 5ml/min at the 40th piece of theoretical stage, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 40%) of extraction agent dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone is taking 15ml/min(and solvent ratio as 3) speed enter this tower at the 20th piece of theoretical stage, control reflux ratio is 2, hexanaphthene with the speed of 3.0ml/min from overhead extraction, purity is 99.2%, extraction agent and n-propyl alcohol enter extraction agent recovery tower (internal diameter 50mm by after extraction at the bottom of tower at the 10th piece of theoretical stage, 15 pieces of theoretical stages are housed) in, control reflux ratio is 3, n-propyl alcohol with the speed of 2.0ml/min from overhead extraction, purity is 99.4%, extraction agent uses from extraction Posterior circle at the bottom of tower.
Embodiment 2
At an internal diameter 50mm, it is equipped with in the extractive distillation column of 48 pieces of theoretical stages, hexanaphthene and n-propyl alcohol mixture (mass content is respectively 70% and 30%) enter this tower with the speed of 5ml/min at the 33rd piece of theoretical stage, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 50%) of extraction agent dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone is taking 10ml/min(and solvent ratio as 2) speed enter this tower at the 8th piece of theoretical stage, control reflux ratio is 2, hexanaphthene with the speed of 3.5ml/min from overhead extraction, purity is 99.5%, extraction agent and n-propyl alcohol enter extraction agent recovery tower (internal diameter 50mm by after extraction at the bottom of tower at the 10th piece of theoretical stage, 15 pieces of theoretical stages are housed) in, control reflux ratio is 3, n-propyl alcohol with the speed of 1.5ml/min from overhead extraction, purity is 99.3%, extraction agent uses from extraction Posterior circle at the bottom of tower.
Embodiment 3
At an internal diameter 50mm, it is equipped with in the extractive distillation column of 48 pieces of theoretical stages, hexanaphthene and n-propyl alcohol mixture (mass content is respectively 80% and 20%) enter this tower with the speed of 5ml/min at the 33rd piece of theoretical stage, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 60%) of extraction agent dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone is taking 10ml/min(and solvent ratio as 2) speed enter this tower at the 8th piece of theoretical stage, control reflux ratio is 3, hexanaphthene with the speed of 4.0ml/min from overhead extraction, purity is 99.8%, extraction agent and n-propyl alcohol enter extraction agent recovery tower (internal diameter 50mm by after extraction at the bottom of tower at the 15th piece of theoretical stage, 25 pieces of theoretical stages are housed) in, control reflux ratio is 2, n-propyl alcohol with the speed of 1.0ml/min from overhead extraction, purity is 99.5%, extraction agent uses from extraction Posterior circle at the bottom of tower.
Embodiment 4
At an internal diameter 50mm, it is equipped with in the extractive distillation column of 40 pieces of theoretical stages, hexanaphthene and n-propyl alcohol mixture (mass content is respectively 80% and 20%) enter this tower with the speed of 5ml/min at the 20th piece of theoretical stage, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 70%) of extraction agent dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone is taking 25ml/min(and solvent ratio as 5) speed enter this tower at the 5th piece of theoretical stage, control reflux ratio is 4, hexanaphthene with the speed of 4.0ml/min from overhead extraction, purity is 99.1%, extraction agent and n-propyl alcohol enter extraction agent recovery tower (internal diameter 50mm by after extraction at the bottom of tower at the 15th piece of theoretical stage, 25 pieces of theoretical stages are housed) in, control reflux ratio is 2, n-propyl alcohol with the speed of 1.0ml/min from overhead extraction, purity is 99.2%, extraction agent uses from extraction Posterior circle at the bottom of tower.
Embodiment 5
At an internal diameter 50mm, it is equipped with in the extractive distillation column of 30 pieces of theoretical stages, hexanaphthene and n-propyl alcohol mixture (mass content is respectively 90% and 10%) enter this tower with the speed of 5ml/min at the 15th piece of theoretical stage, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 60%) of extraction agent dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone is taking 20ml/min(and solvent ratio as 4) speed enter this tower at the 5th piece of theoretical stage, control reflux ratio is 6, hexanaphthene with the speed of 4.5ml/min from overhead extraction, purity is 99.4%, extraction agent and n-propyl alcohol enter extraction agent recovery tower (internal diameter 50mm by after extraction at the bottom of tower at the 20th piece of theoretical stage, 30 pieces of theoretical stages are housed) in, control reflux ratio is 1, n-propyl alcohol with the speed of 0.5ml/min from overhead extraction, purity is 99.1%, extraction agent uses from extraction Posterior circle at the bottom of tower.
Embodiment 6
At an internal diameter 50mm, it is equipped with in the extractive distillation column of 40 pieces of theoretical stages, hexanaphthene and n-propyl alcohol mixture (mass content is respectively 50% and 50%) enter this tower with the speed of 5ml/min at the 20th piece of theoretical stage, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 80%) of extraction agent dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone is taking 15ml/min(and solvent ratio as 3) speed enter this tower at the 10th piece of theoretical stage, control reflux ratio is 5, hexanaphthene with the speed of 2.5ml/min from overhead extraction, purity is 99.2%, extraction agent and n-propyl alcohol enter extraction agent recovery tower (internal diameter 50mm by after extraction at the bottom of tower at the 20th piece of theoretical stage, 30 pieces of theoretical stages are housed) in, control reflux ratio is 1, n-propyl alcohol with the speed of 2.5ml/min from overhead extraction, purity is 99.1%, extraction agent uses from extraction Posterior circle at the bottom of tower.
Claims (3)
1. one kind by the method for separation of extractive distillation hexanaphthene and n-propyl alcohol mixture, it is characterized in that taking the mixture of dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone as extraction agent, hexanaphthene to be separated and n-propyl alcohol mixture enter in the extractive distillation column that 30-60 block theoretical stage is housed by 15-40 block theoretical stage, extraction agent is entered by 5-20 block theoretical stage, hexanaphthene is by extracting rectifying top of tower extraction, extraction agent and n-propyl alcohol are entered, by after extracting rectifying tower bottom extraction, the extraction agent recovery tower that 15-30 block theoretical stage is housed by 10-20 block theoretical stage, n-propyl alcohol is by the top extraction of extraction agent recovery tower, extraction agent is used by extraction Posterior circle bottom extraction agent recovery tower, in described dimethyl sulfoxide (DMSO) and the mixture of N-Methyl pyrrolidone, mass percent shared by dimethyl sulfoxide (DMSO) is 40%-80%, described extraction agent is 2-5 with the ratio of mixture velocity to be separated, and mixture to be separated is made up of hexanaphthene and n-propyl alcohol.
2. by the method for a kind of separation of extractive distillation hexanaphthene according to claim 1 and n-propyl alcohol mixture, it is characterised in that the reflux ratio of described extractive distillation column is 2-6.
3. by the method for a kind of separation of extractive distillation hexanaphthene according to claim 1 and n-propyl alcohol mixture, it is characterised in that the reflux ratio of described extraction agent recovery tower is 1-3.
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| CN105503501B (en) * | 2016-01-17 | 2017-12-12 | 济南大学 | A kind of butanol hexamethylene azeotropic mixture extraction rectifying method |
| CN106431841B (en) * | 2016-09-19 | 2019-01-08 | 青岛科技大学 | A method of being thermally integrated separation of extractive distillation isobutanol and normal heptane mixture |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4921581A (en) * | 1989-05-26 | 1990-05-01 | Phillips Petroleum Company | Extractive distillation of hydrocarbons employing solvent mixture |
| CN103896713A (en) * | 2014-04-17 | 2014-07-02 | 河北工业大学 | Process for extracting, rectifying and separating cyclohexane-ethanol system by using ionic liquid |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4921581A (en) * | 1989-05-26 | 1990-05-01 | Phillips Petroleum Company | Extractive distillation of hydrocarbons employing solvent mixture |
| CN103896713A (en) * | 2014-04-17 | 2014-07-02 | 河北工业大学 | Process for extracting, rectifying and separating cyclohexane-ethanol system by using ionic liquid |
Non-Patent Citations (1)
| Title |
|---|
| 间歇萃取精馏分离环己烷-正丙醇的研究;孙畅等;《现代化工》;20130630;第33卷(第6期);第108-111页 * |
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