CN103193579A - Method for separating mixture of normal hexane and tetrahydrofuran through extractive distillation - Google Patents
Method for separating mixture of normal hexane and tetrahydrofuran through extractive distillation Download PDFInfo
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- CN103193579A CN103193579A CN2013100898759A CN201310089875A CN103193579A CN 103193579 A CN103193579 A CN 103193579A CN 2013100898759 A CN2013100898759 A CN 2013100898759A CN 201310089875 A CN201310089875 A CN 201310089875A CN 103193579 A CN103193579 A CN 103193579A
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Abstract
The invention discloses a method for separating a mixture of normal hexane and tetrahydrofuran through extractive distillation. The method takes an N-substituted lactam compound as an extracting agent, and comprises the following steps of: allowing the mixture of normal hexane and tetrahydrofuran to be separated to enter an extractive distillation tower filled with 30-60 theoretical plates from the 15th to 40th theoretical plates, allowing the extracting agent to enter the tower from the 3rd to 20th theoretical plates, extracting the normal hexane from the top of the extractive distillation tower, extracting the extracting agent and the tetrahydrofuran from the bottom of the extractive distillation tower, allowing the extracting agent and the tetrahydrofuran to enter an extracting agent recovery tower filled with 12-30 theoretical plates from the 5th to 20th theoretical plates, extracting the tetrahydrofuran from the top of the extracting agent recovery tower, and extracting the extracting agent from the bottom of the extracting agent recovery tower for recycling. The method has the advantages of low energy consumption, high product purity, high recovery rate, simple process, high safety, environment friendliness and zero pollution, and clean production can be realized.
Description
Technical field
The present invention relates to separate the method for normal hexane and tetrahydrofuran compound, relate in particular to a kind of method of separating normal hexane and tetrahydrofuran compound with extracting rectifying.
Background technology
Normal hexane is industrial main as solvent, be used for the preparation viscose glue with cement footwear leather, case and bag, be usually used in the wiping clean-out operation in the electronics and information industry production process, the thick oil immersion of foodstuff manufacturing goes out, the industries such as fragrance of a flower solvent extraction the when extraction agent in the manufacturing propylene solvent recuperation of plastics, chemical experiment and household chemicals are produced are also used normal hexane.Tetrahydrofuran (THF) is a kind of valuable organic solvent of excellent property, is again a kind of important organic synthesis intermediate, is widely used in fields such as pharmacy, coating, leathers.
In Chemical Manufacture, tend to produce the mixture of normal hexane and tetrahydrofuran (THF), for reducing production costs, reduce environmental pollution, need the mixture of normal hexane and tetrahydrofuran (THF) is separated, but normal hexane and tetrahydrofuran (THF) form azeotrope, can't separate with conventional distillation.
Document (is used chemical industry at present, 2008,37(9): 1106) method of separating with tetrahydrofuran compound about normal hexane is at first the mixture of normal hexane and tetrahydrofuran (THF) to be washed, utilize normal hexane and tetrahydrofuran (THF) solubleness different in water, through repeatedly washing, the content of tetrahydrofuran (THF) in normal hexane and the tetrahydrofuran compound is reduced, adopt anhydrous MgCl then
2Perhaps the 13X molecular sieve carries out fractionation by adsorption.Need a large amount of water when this method is separated normal hexane and tetrahydrofuran compound, wash laggard tetrahydrofuran (THF) of going into aqueous phase because can and water formation azeotrope, can't directly obtain qualified tetrahydrofuran (THF), anhydrous MgCl of while
2Perhaps the 13X molecular sieve also needs could use after the regeneration, so this method complex operation, only is applicable to the separation of a small amount of tetrahydrofuran (THF) in the normal hexane.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method of separating normal hexane and tetrahydrofuran compound with extracting rectifying is provided.
The method of separating normal hexane and tetrahydrofuran compound with extracting rectifying is: be extraction agent with the N-substituted lactams compounds, normal hexane to be separated and tetrahydrofuran compound are entered in the extractive distillation column that 30-60 piece theoretical stage is housed by 15-40 piece theoretical stage, extraction agent is entered by 3-20 piece theoretical stage, normal hexane is by the extraction of extracting rectifying top of tower, extraction agent and tetrahydrofuran (THF) enter the extraction agent recovery tower that 12-30 piece theoretical stage is housed by 5-20 piece theoretical stage after by the extraction of extracting rectifying tower bottom, tetrahydrofuran (THF) is by the top extraction of extraction agent recovery tower, and extraction agent recycles after the extraction bottom the extraction agent recovery tower.
Described N-substituted lactams compounds is N-N-methyl-2-2-pyrrolidone N-, N-methyl-2-piperidone or N-methyl caprolactam.Described extraction agent is that solvent ratio is 2-6 with the ratio of normal hexane to be separated and tetrahydrofuran compound flow, and the reflux ratio of described extractive distillation column is 2-5, and the reflux ratio of described extraction agent recovery tower is 1.5-4.
The invention has the advantages that energy consumption is low, product purity and rate of recovery height, technology is simple, safety, environmental protection, pollution-free, can realize cleaner production.
Description of drawings
Fig. 1 is the schema that separates normal hexane and tetrahydrofuran compound with extracting rectifying.
Embodiment
As shown in Figure 1, the method of separating normal hexane and tetrahydrofuran compound with extracting rectifying is: be extraction agent with the N-substituted lactams compounds, normal hexane to be separated and tetrahydrofuran compound are entered in the extractive distillation column that 30-60 piece theoretical stage is housed by 15-40 piece theoretical stage, extraction agent is entered by 3-20 piece theoretical stage, normal hexane is by the extraction of extracting rectifying top of tower, extraction agent and tetrahydrofuran (THF) enter the extraction agent recovery tower that 12-30 piece theoretical stage is housed by 5-20 piece theoretical stage after by the extraction of extracting rectifying tower bottom, tetrahydrofuran (THF) is by the top extraction of extraction agent recovery tower, and extraction agent recycles after the extraction bottom the extraction agent recovery tower.
Described N-substituted lactams compounds is N-N-methyl-2-2-pyrrolidone N-, N-methyl-2-piperidone or N-methyl caprolactam.Described extraction agent is that solvent ratio is 2-6 with the ratio of normal hexane to be separated and tetrahydrofuran compound flow, and the reflux ratio of described extractive distillation column is 2-5, and the reflux ratio of described extraction agent recovery tower is 1.5-4.
Embodiment 1
At an internal diameter 50mm, be equipped with in the extractive distillation column of 37 theoretical stages, normal hexane and tetrahydrofuran compound (mass content is respectively 43% and 57%) enter this tower with the speed of 5ml/min at the 20th theoretical stage, extraction agent N-N-methyl-2-2-pyrrolidone N-is that solvent ratio is 4 with 20ml/min() speed enter this tower at the 3rd theoretical stage, the control reflux ratio is 2, normal hexane with the speed of 2.4ml/min from the cat head extraction, purity is 99.0%, N-N-methyl-2-2-pyrrolidone N-and tetrahydrofuran (THF) enter extraction agent recovery tower (internal diameter 50mm at the 5th theoretical stage after the extraction at the bottom of by tower, 12 theoretical stages are housed) in, the control reflux ratio is 2, tetrahydrofuran (THF) with the speed of 2.6ml/min from the cat head extraction, to be 99.3%, N-N-methyl-2-2-pyrrolidone N-recycle after the extraction at the bottom of the tower purity.
Embodiment 2
At an internal diameter 50mm, be equipped with in the extractive distillation column of 45 theoretical stages, normal hexane and tetrahydrofuran compound (mass content is respectively 40% and 60%) enter this tower with the speed of 5ml/min at the 30th theoretical stage, extraction agent N-methyl-2-piperidone is that solvent ratio is 2.4 with 12ml/min() speed enter this tower at the 10th theoretical stage, the control reflux ratio is 5, normal hexane with the speed of 2.3ml/min from the cat head extraction, purity is 99.1%, N-methyl-2-piperidone and tetrahydrofuran (THF) enter extraction agent recovery tower (internal diameter 50mm at the 6th theoretical stage after the extraction at the bottom of by tower, 15 theoretical stages are housed) in, the control reflux ratio is 4, tetrahydrofuran (THF) with the speed of 2.7ml/min from the cat head extraction, to be 99.3%, N-methyl-2-piperidone recycle after the extraction at the bottom of the tower purity.
Embodiment 3
At an internal diameter 50mm, be equipped with in the extractive distillation column of 30 theoretical stages, normal hexane and tetrahydrofuran compound (mass content is respectively 60% and 40%) enter this tower with the speed of 5ml/min at the 15th theoretical stage, extraction agent N-methyl-2-piperidone is that solvent ratio is 6 with 30ml/min() speed enter this tower at the 5th theoretical stage, the control reflux ratio is 2, normal hexane with the speed of 3.5ml/min from the cat head extraction, purity is 99.2%, N-methyl-2-piperidone and tetrahydrofuran (THF) enter extraction agent recovery tower (internal diameter 50mm at the 8th theoretical stage after the extraction at the bottom of by tower, 20 theoretical stages are housed) in, the control reflux ratio is 3, tetrahydrofuran (THF) with the speed of 1.5ml/min from the cat head extraction, to be 99.4%, N-methyl-2-piperidone recycle after the extraction at the bottom of the tower purity.
Embodiment 4
At an internal diameter 50mm, be equipped with in the extractive distillation column of 55 theoretical stages, normal hexane and tetrahydrofuran compound (mass content is respectively 40% and 60%) enter this tower with the speed of 5ml/min at the 30th theoretical stage, extraction agent N-methyl caprolactam is that solvent ratio is 4 with 20ml/min() speed enter this tower at the 10th theoretical stage, the control reflux ratio is 2, normal hexane with the speed of 2.3ml/min from the cat head extraction, purity is 99.1%, N-methyl caprolactam and tetrahydrofuran (THF) enter extraction agent recovery tower (internal diameter 50mm at the 8th theoretical stage after the extraction at the bottom of by tower, 20 theoretical stages are housed) in, the control reflux ratio is 3, tetrahydrofuran (THF) with the speed of 2.7ml/min from the cat head extraction, to be 99.5%, N-methyl caprolactam recycle after the extraction at the bottom of the tower purity.
Embodiment 5
At an internal diameter 50mm, be equipped with in the extractive distillation column of 45 theoretical stages, normal hexane and tetrahydrofuran compound (mass content is respectively 60% and 40%) enter this tower with the speed of 5ml/min at the 25th theoretical stage, extraction agent N-methyl caprolactam is that solvent ratio is 3 with 15ml/min() speed enter this tower at the 10th theoretical stage, the control reflux ratio is 3, normal hexane with the speed of 3.5ml/min from the cat head extraction, purity is 99.0%, N-methyl caprolactam and tetrahydrofuran (THF) enter extraction agent recovery tower (internal diameter 50mm at the 20th theoretical stage after the extraction at the bottom of by tower, 30 theoretical stages are housed) in, the control reflux ratio is 1.5, tetrahydrofuran (THF) with the speed of 1.5ml/min from the cat head extraction, to be 99.4%, N-methyl caprolactam recycle after the extraction at the bottom of the tower purity.
Embodiment 6
At an internal diameter 50mm, be equipped with in the extractive distillation column of 60 theoretical stages, normal hexane and tetrahydrofuran compound (mass content is respectively 20% and 80%) enter this tower with the speed of 5ml/min at the 40th theoretical stage, extraction agent N-N-methyl-2-2-pyrrolidone N-is that solvent ratio is 2 with 10ml/min() speed enter this tower at the 20th theoretical stage, the control reflux ratio is 3.5, normal hexane with the speed of 1.2ml/min from the cat head extraction, purity is 99.3%, N-N-methyl-2-2-pyrrolidone N-and tetrahydrofuran (THF) enter extraction agent recovery tower (internal diameter 50mm at the 15th theoretical stage after the extraction at the bottom of by tower, 30 theoretical stages are housed) in, the control reflux ratio is 1.5, tetrahydrofuran (THF) with the speed of 3.8ml/min from the cat head extraction, to be 99.5%, N-N-methyl-2-2-pyrrolidone N-recycle after the extraction at the bottom of the tower purity.
Claims (5)
1. method of separating normal hexane and tetrahydrofuran compound with extracting rectifying, it is characterized in that with the N-substituted lactams compounds be extraction agent, normal hexane to be separated and tetrahydrofuran compound are entered in the extractive distillation column that 30-60 piece theoretical stage is housed by 15-40 piece theoretical stage, extraction agent is entered by 3-20 piece theoretical stage, normal hexane is by the extraction of extracting rectifying top of tower, extraction agent and tetrahydrofuran (THF) enter the extraction agent recovery tower that 12-30 piece theoretical stage is housed by 5-20 piece theoretical stage after by the extraction of extracting rectifying tower bottom, tetrahydrofuran (THF) is by the top extraction of extraction agent recovery tower, and extraction agent recycles after the extraction bottom the extraction agent recovery tower.
2. by the described a kind of method of separating normal hexane and tetrahydrofuran compound with extracting rectifying of claim 1, it is characterized in that described N-substituted lactams compounds is N-N-methyl-2-2-pyrrolidone N-, N-methyl-2-piperidone or N-methyl caprolactam.
3. by the described a kind of method of separating normal hexane and tetrahydrofuran compound with extracting rectifying of claim 1, it is characterized in that described extraction agent and the ratio of normal hexane to be separated and tetrahydrofuran compound flow are 2-6.
4. by the described a kind of method of separating normal hexane and tetrahydrofuran compound with extracting rectifying of claim 1, the reflux ratio that it is characterized in that described extractive distillation column is 2-5.
5. by the described a kind of method of separating normal hexane and tetrahydrofuran compound with extracting rectifying of claim 1, the reflux ratio that it is characterized in that described extraction agent recovery tower is 1.5-4.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965008A (en) * | 2014-04-25 | 2014-08-06 | 浙江大学 | Method for separating mixture of cyclohexane and ethyl acetate through extractive distillation |
| CN106518598A (en) * | 2016-10-09 | 2017-03-22 | 大连理工大学 | Device and method for purifying n-hexane with N,N-dimethylacetamide solvent |
| CN111116522A (en) * | 2020-01-20 | 2020-05-08 | 福州大学 | Device and method for separating tetrahydrofuran-water mixture by single-tower extractive distillation |
| CN111960914A (en) * | 2020-07-27 | 2020-11-20 | 南京师范大学 | Method for separating n-hexane from n-hexane-tert-butyl alcohol-tetrahydrofuran mixed solvent by liquid-liquid extraction |
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| GB1221902A (en) * | 1969-09-11 | 1971-02-10 | Leuna Werke Veb | Process for production of pure hydrocarbons |
| CN102701929A (en) * | 2012-05-17 | 2012-10-03 | 浙江大学 | Method for separating acetone-tetrahydrofuran mixture through extractive distillation |
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- 2013-03-20 CN CN201310089875.9A patent/CN103193579B/en active Active
Patent Citations (2)
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| GB1221902A (en) * | 1969-09-11 | 1971-02-10 | Leuna Werke Veb | Process for production of pure hydrocarbons |
| CN102701929A (en) * | 2012-05-17 | 2012-10-03 | 浙江大学 | Method for separating acetone-tetrahydrofuran mixture through extractive distillation |
Non-Patent Citations (1)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965008A (en) * | 2014-04-25 | 2014-08-06 | 浙江大学 | Method for separating mixture of cyclohexane and ethyl acetate through extractive distillation |
| CN106518598A (en) * | 2016-10-09 | 2017-03-22 | 大连理工大学 | Device and method for purifying n-hexane with N,N-dimethylacetamide solvent |
| CN111116522A (en) * | 2020-01-20 | 2020-05-08 | 福州大学 | Device and method for separating tetrahydrofuran-water mixture by single-tower extractive distillation |
| CN111116522B (en) * | 2020-01-20 | 2023-01-10 | 福州大学 | Device and method for separating tetrahydrofuran-water mixture by single-tower extractive distillation |
| CN111960914A (en) * | 2020-07-27 | 2020-11-20 | 南京师范大学 | Method for separating n-hexane from n-hexane-tert-butyl alcohol-tetrahydrofuran mixed solvent by liquid-liquid extraction |
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