CN104774130A - Extraction and rectification method for separating mixture of cyclohexane and isopropanol - Google Patents
Extraction and rectification method for separating mixture of cyclohexane and isopropanol Download PDFInfo
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- CN104774130A CN104774130A CN201510108138.8A CN201510108138A CN104774130A CN 104774130 A CN104774130 A CN 104774130A CN 201510108138 A CN201510108138 A CN 201510108138A CN 104774130 A CN104774130 A CN 104774130A
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Abstract
The invention discloses an extraction and rectification method for separating a mixture of cyclohexane and isopropanol. A mixture of dimethyl sulfoxide and N,N-dimethyl acetamide is taken as the extractant, a mixture of cyclohexane and isopropanol 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 6th-20th theoretical plate, the cyclohexane is discharged from the top of the extraction and rectification tower, the mixture of extractant and isopropanol 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, isopropanol 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 recovery rate, 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 isopropanol mixture, particularly relate to a kind of method of separation of extractive distillation hexanaphthene and isopropanol 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.Virahol is at chemical industry, medicine, fine chemistry industry, the fields such as electronic industry have extensive use, can be used as industrial chemicals and produce acetone, hydrogen peroxide, methyl iso-butyl ketone (MIBK), diisobutyl ketone, isopropyl ether, Isopropylamine, isopropyl alcohol ether, isopropyl chloride compound, isopropyl fatty acid ester and chloro fat isopropyl propionate etc., also can be used as solvent manufacture of ink, coating, extraction agent, aerosol agent etc., also can be used as sanitising agent, frostproofer, dewatering agent, the dispersion agent of pigment production, the additive of blended gasoline, the thinner of sizing agent, the fixing agent of printing and dyeing industry, the antifogging agent of glass and transparent plastics.
In Chemical Manufacture, often produce the mixture of hexanaphthene and Virahol, for reducing production cost, reduce environmental pollution, need be separated with the mixture of Virahol hexanaphthene, but hexanaphthene and Virahol form azeotrope, cannot be separated with conventional distillation.
About being separated of hexanaphthene and Virahol, (Hebei Normal University Journal (natural science edition), 1997 such as Liu Jinmei, 21(2), 174) adopt aqueous extraction method to be studied, first extract with water, after by upper strata anhydrous sodium sulfate drying, obtain the hexanaphthene that purity is higher, the rate of recovery is 90%, and lower floor is carried out rectifying, overhead product is moisture, Virahol and hexanaphthene, carry out distillation after adding calcium oxide reflux dewatering again and obtain Virahol, content is 98%, and the rate of recovery is 85%.Chen Liping etc. (laboratory study and exploration, 2007,26(9), 30) this is also studied, first extract with water, obtain thick hexanaphthene and isopropanol-water solutions, thicker hexanaphthene is carried out rectification and purification, isopropanol-water solutions carries out azeotropic distillation.Although above-mentioned two kinds of methods achieve being separated of hexanaphthene and Virahol, because people is for introducing isopropanol-water azeotropic system, increase separating difficulty, and flow process is complicated.(chemical industry and the engineering such as Bai Peng, 2013,30(2), 58) extraction fractional distillation is adopted to be studied with being separated of Virahol hexanaphthene, the display of simulative optimization result is extraction agent with furfural, being separated of hexanaphthene and Virahol can be realized, but the non-experimental results of this research, and the thermostability of extraction agent furfural is not good enough.In addition, also there are investigator's proposition variable-pressure rectification and salt adding variable-pressure rectification separating benzene-cyclohexane and Virahol, but there is the shortcomings such as equipment requirements is higher, investment is larger.
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 isopropanol mixture is provided.
By the method for separation of extractive distillation hexanaphthene and isopropanol mixture be: with dimethyl sulfoxide (DMSO) and N, the mixture of N-N,N-DIMETHYLACETAMIDE is extraction agent, hexanaphthene to be separated and isopropanol mixture entered by 15-40 block theoretical stage 30-60 block theoretical stage is housed extractive distillation column in, extraction agent is entered by 6-20 block theoretical stage, hexanaphthene is by the extraction of extracting rectifying top of tower, extraction agent and Virahol 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, Virahol 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,N-dimethylacetamide shared by dimethyl sulfoxide (DMSO) is 30%-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 Virahol.The reflux ratio of described extractive distillation column is 2-6.The reflux ratio of described extraction agent recovery tower is 1-3.
The invention has the advantages that energy consumption is low, the rate of recovery is high, and 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 isopropanol mixture.
Embodiment
By the method for separation of extractive distillation hexanaphthene and isopropanol mixture be: with dimethyl sulfoxide (DMSO) and N, the mixture of N-N,N-DIMETHYLACETAMIDE is extraction agent, hexanaphthene to be separated and isopropanol mixture entered by 15-40 block theoretical stage 30-60 block theoretical stage is housed extractive distillation column in, extraction agent is entered by 6-20 block theoretical stage, hexanaphthene is by the extraction of extracting rectifying top of tower, extraction agent and Virahol 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, Virahol 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,N-dimethylacetamide shared by dimethyl sulfoxide (DMSO) is 30%-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 Virahol.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 isopropanol mixture (mass content is respectively 60% and 40%) enter this tower with the speed of 5ml/min at the 40th piece of theoretical stage, extraction agent dimethyl sulfoxide (DMSO) and N, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 30%) of N-N,N-DIMETHYLACETAMIDE 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 99.3%, extraction agent and Virahol 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, Virahol with the speed of 2.0ml/min from overhead extraction, purity is 99.1%, 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 isopropanol mixture (mass content is respectively 70% and 30%) enter this tower with the speed of 5ml/min at the 33rd piece of theoretical stage, extraction agent dimethyl sulfoxide (DMSO) and N, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 40%) of N-N,N-DIMETHYLACETAMIDE 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 99.0%, extraction agent and Virahol 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, Virahol with the speed of 1.5ml/min from overhead extraction, purity is 99.5%, 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 isopropanol mixture (mass content is respectively 80% and 20%) enter this tower with the speed of 5ml/min at the 33rd piece of theoretical stage, extraction agent dimethyl sulfoxide (DMSO) and N, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 50%) of N-N,N-DIMETHYLACETAMIDE 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 98.7%, extraction agent and Virahol 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, Virahol with the speed of 1.0ml/min from overhead extraction, purity is 99.0%, 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 isopropanol mixture (mass content is respectively 67% and 33%) enter this tower with the speed of 5ml/min at the 20th piece of theoretical stage, extraction agent dimethyl sulfoxide (DMSO) and N, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 60%) of N-N,N-DIMETHYLACETAMIDE with 25ml/min(and solvent ratio for 5) speed enter this tower at the 6th piece of theoretical stage, controlling reflux ratio is 4, hexanaphthene with the speed of 3.3ml/min from overhead extraction, purity is 99.4%, extraction agent and Virahol 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, Virahol with the speed of 1.7ml/min from overhead extraction, purity is 98.8%, 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 isopropanol mixture (mass content is respectively 50% and 50%) enter this tower with the speed of 5ml/min at the 15th piece of theoretical stage, extraction agent dimethyl sulfoxide (DMSO) and N, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 70%) of N-N,N-DIMETHYLACETAMIDE with 20ml/min(and solvent ratio for 4) speed enter this tower at the 6th piece of theoretical stage, controlling reflux ratio is 6, hexanaphthene with the speed of 2.5ml/min from overhead extraction, purity is 99.0%, extraction agent and Virahol 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, Virahol with the speed of 2.5ml/min from overhead extraction, purity is 99.3%, 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 isopropanol mixture (mass content is respectively 40% and 60%) enter this tower with the speed of 5ml/min at the 20th piece of theoretical stage, extraction agent dimethyl sulfoxide (DMSO) and N, the mixture (mass percent shared by dimethyl sulfoxide (DMSO) is 80%) of N-N,N-DIMETHYLACETAMIDE 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 2.0ml/min from overhead extraction, purity is 98.9%, extraction agent and Virahol 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, Virahol with the speed of 3.0ml/min from overhead extraction, purity is 99.2%, extraction agent uses from extraction Posterior circle at the bottom of tower.
Claims (5)
1. the method with separation of extractive distillation hexanaphthene and isopropanol mixture, it is characterized in that with dimethyl sulfoxide (DMSO) and N, the mixture of N-N,N-DIMETHYLACETAMIDE is extraction agent, hexanaphthene to be separated and isopropanol mixture entered by 15-40 block theoretical stage 30-60 block theoretical stage is housed extractive distillation column in, extraction agent is entered by 6-20 block theoretical stage, hexanaphthene is by the extraction of extracting rectifying top of tower, extraction agent and Virahol 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, Virahol 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 isopropanol mixture, it is characterized in that the mass percent in the mixture of described dimethyl sulfoxide (DMSO) and N,N-dimethylacetamide shared by dimethyl sulfoxide (DMSO) is 30%-80%.
3. press the method for a kind of separation of extractive distillation hexanaphthene according to claim 1 and isopropanol 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 Virahol.
4. press the method for a kind of separation of extractive distillation hexanaphthene according to claim 1 and isopropanol 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 isopropanol mixture, it is characterized in that the reflux ratio of described extraction agent recovery tower is 1-3.
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Cited By (3)
| 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 |
| CN110052052A (en) * | 2019-05-29 | 2019-07-26 | 天津赫普菲乐新材料有限公司 | Multicomponent batch fractionating intelligence control system and control method |
| CN111377804A (en) * | 2020-03-27 | 2020-07-07 | 山东省特种设备检验研究院潍坊分院 | Device and method for separating diisopropyl ether-isopropanol mixture by binary mixed extractant |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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- 2015-03-12 CN CN201510108138.8A patent/CN104774130B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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| 王婧娴等: "异丙醇-环己烷萃取精馏过程模拟与优化", 《化学工业与工程》 * |
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 |
| CN110052052A (en) * | 2019-05-29 | 2019-07-26 | 天津赫普菲乐新材料有限公司 | Multicomponent batch fractionating intelligence control system and control method |
| CN111377804A (en) * | 2020-03-27 | 2020-07-07 | 山东省特种设备检验研究院潍坊分院 | Device and method for separating diisopropyl ether-isopropanol mixture by binary mixed extractant |
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