CN104774132A - Extraction and rectification method for separating mixture of cyclohexane and n-propanol - Google Patents
Extraction and rectification method for separating mixture of cyclohexane and n-propanol Download PDFInfo
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- CN104774132A CN104774132A CN201510108091.5A CN201510108091A CN104774132A CN 104774132 A CN104774132 A CN 104774132A CN 201510108091 A CN201510108091 A CN 201510108091A CN 104774132 A CN104774132 A CN 104774132A
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Abstract
The invention discloses an extraction and rectification method for separating a mixture of cyclohexane and n-propanol. A mixture of dimethyl sulfoxide and N,N-dimethyl acetamide is taken as the extractant, a mixture of cyclohexane and n-propanol enters a extraction and rectification tower with 30 to 60 theoretical plates from the 15th-40th theoretical plate, the extractant enters the tower from the 5th-20th theoretical plate, the cyclohexane is discharged from the top of the extraction and rectification tower, the mixture of extractant and n-propanol is discharged from the bottom of the extraction and rectification tower and then fed into an extractant recovery tower with 15 to 30 theoretical plates from the 10th-20th plate, n-propanol is discharged from the top of the extractant recovery tower, and the extractant is discharged from the bottom of the extractant recovery tower and recovered. The method has the advantages of low energy consumption, high purity, high yield, simple technology, safety, environment-friendliness, and no pollution, and is capable of achieving clean production.
Description
Technical field
The present invention relates to the method for separating benzene-cyclohexane and 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, 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, need be separated with the mixture of n-propyl alcohol hexanaphthene, 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) be studied, be that extraction agent carries out batch extracting rectified with DMF, hexanaphthene quality product mark 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
The object of the invention is to overcome the deficiencies in the prior art, a kind of method of separation of extractive distillation hexanaphthene and n-propyl alcohol mixture is provided.
By the method for separation of extractive distillation hexanaphthene and n-propyl alcohol mixture be: with the mixture of dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone for extraction agent, hexanaphthene to be separated and n-propyl alcohol mixture entered by 15-40 block theoretical stage 30-60 block theoretical stage is housed extractive distillation column in, extraction agent is entered by 5-20 block theoretical stage, hexanaphthene is by the extraction of extracting rectifying top of tower, extraction agent and n-propyl alcohol enter by 10-20 block theoretical stage the extraction agent recovery tower that 15-30 block theoretical stage is housed by after the extraction of extracting rectifying tower bottom, 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 as shown in Figure 1.
Mass percent in the mixture of described dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone 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.
The invention has the advantages that energy consumption is low, product purity and yield high, technique is simple, safety, environmental protection, pollution-free, can realize cleaner production.
Accompanying drawing explanation
Fig. 1 is the schema with 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 be: with the mixture of dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone for extraction agent, hexanaphthene to be separated and n-propyl alcohol mixture entered by 15-40 block theoretical stage 30-60 block theoretical stage is housed extractive distillation column in, extraction agent is entered by 5-20 block theoretical stage, hexanaphthene is by the extraction of extracting rectifying top of tower, extraction agent and n-propyl alcohol enter by 10-20 block theoretical stage the extraction agent recovery tower that 15-30 block theoretical stage is housed by after the extraction of extracting rectifying tower bottom, 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.
Mass percent in the mixture of described dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone 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, be 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 with 15ml/min(and solvent ratio for 3) speed enter this tower at the 20th piece of theoretical stage, controlling 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, controlling 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, be 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 with 10ml/min(and solvent ratio for 2) speed enter this tower at the 8th piece of theoretical stage, controlling 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, controlling 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, be 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 with 10ml/min(and solvent ratio for 2) speed enter this tower at the 8th piece of theoretical stage, controlling 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, controlling 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, be 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 with 25ml/min(and solvent ratio for 5) speed enter this tower at the 5th piece of theoretical stage, controlling 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, controlling 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, be 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 with 20ml/min(and solvent ratio for 4) speed enter this tower at the 5th piece of theoretical stage, controlling 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, controlling 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, be 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 with 15ml/min(and solvent ratio for 3) speed enter this tower at the 10th piece of theoretical stage, controlling 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, controlling 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 (5)
1. the method with separation of extractive distillation hexanaphthene and n-propyl alcohol mixture, it is characterized in that with the mixture of dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone for extraction agent, hexanaphthene to be separated and n-propyl alcohol mixture entered by 15-40 block theoretical stage 30-60 block theoretical stage is housed extractive distillation column in, extraction agent is entered by 5-20 block theoretical stage, hexanaphthene is by the extraction of extracting rectifying top of tower, extraction agent and n-propyl alcohol enter by 10-20 block theoretical stage the extraction agent recovery tower that 15-30 block theoretical stage is housed by after the extraction of extracting rectifying tower bottom, 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.
2. press the method for a kind of separation of extractive distillation hexanaphthene according to claim 1 and n-propyl alcohol mixture, it is characterized in that the mass percent in the mixture of described dimethyl sulfoxide (DMSO) and N-Methyl pyrrolidone shared by dimethyl sulfoxide (DMSO) is 40%-80%.
3. press the method for a kind of separation of extractive distillation hexanaphthene according to claim 1 and n-propyl alcohol mixture, it is characterized in that described extraction agent is 2-5 with the ratio of mixture velocity to be separated, mixture to be separated is made up of hexanaphthene and n-propyl alcohol.
4. press the method for a kind of separation of extractive distillation hexanaphthene according to claim 1 and n-propyl alcohol mixture, it is characterized in that the reflux ratio of described extractive distillation column is 2-6.
5. press the method for a kind of separation of extractive distillation hexanaphthene according to claim 1 and n-propyl alcohol mixture, it is characterized in that the reflux ratio of described extraction agent recovery tower is 1-3.
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| CN201510108091.5A CN104774132B (en) | 2015-03-12 | 2015-03-12 | A kind of method of separation of extractive distillation hexanaphthene and n-propyl alcohol mixture |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503501A (en) * | 2016-01-17 | 2016-04-20 | 济南大学 | Butanol-cyclohexane azeotropic mixture extractive distillation method |
| CN106431841A (en) * | 2016-09-19 | 2017-02-22 | 青岛科技大学 | Method for separating isobutanol and n-heptane mixture through heat integration extractive distillation |
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 |
-
2015
- 2015-03-12 CN CN201510108091.5A patent/CN104774132B/en active Active
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)
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| 孙畅等: "间歇萃取精馏分离环己烷-正丙醇的研究", 《现代化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503501A (en) * | 2016-01-17 | 2016-04-20 | 济南大学 | Butanol-cyclohexane azeotropic mixture extractive distillation method |
| CN105503501B (en) * | 2016-01-17 | 2017-12-12 | 济南大学 | A kind of butanol hexamethylene azeotropic mixture extraction rectifying method |
| CN106431841A (en) * | 2016-09-19 | 2017-02-22 | 青岛科技大学 | Method for separating isobutanol and n-heptane mixture through heat integration extractive distillation |
| 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 |
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