CN102942434B - Method extracting high purity n-hexane by integrating rectification and extraction - Google Patents
Method extracting high purity n-hexane by integrating rectification and extraction Download PDFInfo
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- CN102942434B CN102942434B CN201210497953.4A CN201210497953A CN102942434B CN 102942434 B CN102942434 B CN 102942434B CN 201210497953 A CN201210497953 A CN 201210497953A CN 102942434 B CN102942434 B CN 102942434B
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Abstract
The invention relates to a method extracting high purity n-hexane by integrating rectification and extraction. The method utilizes aromatic hydrocarbon raffinate oil as a raw material and adopts a three-tower technological process which combines continuous rectification and extractive distillation. Firstly, distillate lighter than n-hexane is removed in a rectifying tower, and n-hexane distillate which is around 80% in content is obtained at the bottom of the tower. The distillate at the bottom of the tower is adopted as the raw material of an extractive distillation tower, N-methyl pyrrolidone is adopted as an extracting solvent to be delivered into the extractive distillation tower, and the proportion of the N-methyl pyrrolidone and raw oil is 8:1, after extractive distillation, high purity n-hexane is extracted at the top of the tower by integrating rectification and extraction, and heavy components which are rich in methylcyclopentane and the extracting solvent are at the bottom of the tower. Materials at the bottom of the tower are delivered into a solvent recovery tower, distillate oil which is rich in methylcyclopentane is separated at the top of the tower, and N-methyl pyrrolidone solvent is at the bottom of the tower and sent back to the extractive distillation tower to be recycled. By means of the method, n-hexane content can achieve 99%, no extracting solvent is contained in products, solvent consumption is smaller than 0.1%, one-off yield of n-hexane is larger than 95%, and compared with traditional rectification, energy consumption can be saved over 50%.
Description
Technical field
The present invention relates to a kind of chemical solvents and produce, more particularly mainly as extraction solvent, the solvent of solvent, rubber and coating and the thinner of pigment etc. for pharmaceutical extraction of solvent, edible vegetable oil for olefin polymerization catalysis.
Background technology
Hexane solvent is applied to the content requirement difference of different industries to normal hexane, and as food plant oil extraction solvent, hexane content reaches more than 60% and can meet the demands.And the hexane solvent that chemical process polymerization is used requires hexane content to reach more than 99% (as CSPC ethylene unit chemical industry polymerization hexane solvent).The normal hexane solvent that domestic purity used is 99% is at present all from external import, and price is high.Approximately 10000 tons of current domestic import volumes, this products substitution imported product, in the Changjiang river areas to the south, is developed in principal market, meets domestic market demand, has good economic benefit and social benefit.
The raw material that this project adopts is that the aromatic hydrocarbons that oil refining apparatus is produced is raffinated oil, and raw material main ingredient is C
5～C
8, wherein normal hexane content is 25%, methylcyclopentane content is 2.5%.Because normal hexane and methylcyclopentane boiling point approach, if adopt conventional rectification method, not only energy consumption is large, and separation accuracy does not reach requirement, is difficult to obtain more than 99% normal hexane.
Summary of the invention
The object of this invention is to provide a kind of rectifying and the method that extracts integrated extraction high purity normal hexane, the three tower process flow processs that it adopts continuous rectification to combine with extractive distillation, the key of continuous rectification process is component lighter than normal hexane in raw material to excise, and extractive distillation charging is the normal hexane fraction (control isohexane content and be less than 0.1%) of 80% left and right; Obtain 99% normal hexane through extractive distillation, product separates with extraction solvent is easy, do not carry phenomenon secretly, in product, do not contain extraction solvent, do not affect quality product, extraction solvent consumption is less than 0.1%, and in product, normal hexane content is more than 99%, yield of product is greater than 95%, can energy efficient compared with traditional rectifying more than 50%.
Technical solution of the present invention is to adopt continuous rectifying tower, extraction distillation column and extraction solvent recovery tower three tower process flow and methods, with oil refining apparatus produce aromatic hydrocarbons raffinate oil as raw material, first by component excision lighter than normal hexane in raw material, tower top is lighting end, and at the bottom of tower, discharging is the normal hexane fraction (isohexane content is less than 0.1%) of 80% left and right; At the bottom of tower, fraction is as extraction distillation column stock oil, and stock oil is from the charging of extraction distillation column middle and lower part; Taking high boiling point N-Methyl pyrrolidone as extraction solvent and stock oil in 8:1 ratio simultaneously continuously from the charging of extraction distillation column middle and upper part, after extractive distillation column separates, tower top obtains more than 99% normal hexane, is heavy constituent and extraction solvent that methylcyclopentane content is higher at the bottom of extraction distillation column; Last taking the material at the bottom of extraction distillation column as extraction solvent recovery tower raw material, extraction solvent recovery tower ejects material for the higher distillate of methylcyclopentane content, at the bottom of extraction solvent recovery tower tower, is extraction solvent, and extraction solvent is circulated to extraction distillation column, recycles.
The aromatic hydrocarbons that the above raw material adopts oil refining apparatus to produce is raffinated oil, foreign matter content extremely low (sulphur content is less than 1.0PPM, and olefin(e) centent is less than 10PPM, and aromaticity content is less than 50PPM) in raw material, and raw material main ingredient is C
5～C
8, wherein normal hexane content is 25%, methylcyclopentane content is 2.5%.
Three tower indices of the present invention are as follows above:
1, continuous rectifying tower of the present invention (T-1 tower) adopts band press operation, working pressure is 160kPa(a), design tower diameter is φ 1400mm, adopt efficient DZ-II type filler, packing section height is 35200mm, be divided into into eight sections, each section is highly respectively 4000mm, 4000mm, 4800mm, 4800mm, 4800mm, 4800mm, 4000mm, 4000mm, between tower top and packing section, adopt high-efficiency liquid distributor, in tower, configure snappiness liquid header, opening for feed is arranged between second segment and the 3rd section of filler, side is adopted mouth and is arranged between the 6th section and the 7th section of filler.
2, extractive distillation column of the present invention (T-2 tower) adopts decompression operation, working pressure is 70kPa(a), design tower diameter is φ 1200mm, adopt efficient DZ-III type filler, total filler height is 30100mm, be divided into into seven sections, each section is highly respectively 3000mm, 4600mm, 4600mm, 4700mm, 4400mm, 4400mm, 4400mm, between tower top and packing section, adopt high-efficiency liquid distributor, in tower, configure snappiness liquid header, extractant feed mouth is arranged between first paragraph filler and second segment filler, material inlet is arranged between the 4th section of filler and the 5th section of filler.
3, extraction solvent recovery tower of the present invention (T-3 tower) adopts decompression operation, and working pressure is 40kPa(a), design tower diameter is φ 1000mm, rectifying section adopts efficient DZ-III type filler, be highly 5000mm, stripping section adopts DZ-II type filler, packed height 5500mm.Between tower top and packing section, adopt high-efficiency liquid distributor, configure snappiness liquid header in tower, opening for feed is arranged between two sections of fillers.
In the selected raw material of the present invention, hexane is different from the content of methylcyclopentane, and the working ability on rectifying and extractive distillation, the consumption of extraction solvent, product yield and energy consumption all have impact, so preferred feedstock of the present invention has very large meaning.
Advantage of the present invention is raw material and the extraction solvent wide material sources of selecting.Both easily separate, and do not carry phenomenon secretly, do not contain extraction solvent in product, normal hexane content is more than 99%, and yield of product is greater than 95%, extraction solvent Heat stability is good, extraction solvent consumption is less than 0.1%, can save energy compared with traditional precision fractional distillation more than 50%.
Brief description of the drawings:
Fig. 1 process flow diagram of the present invention.
Embodiment:
1, technical process explanation
Shown in Fig. 1, the raw material of feed sump 1 is entered from the middle part of continuous rectifying tower T1 continuously, the cut 2 being obtained by continuous rectifying tower T1 tower top is the light constituent (light constituent below normal hexane, as 3-methylpentane), control isohexane content by T1 continuous rectifying tower tower reactor extraction feed liquid 3(and be less than 0.1%) send into T2 extraction distillation column, taking N-Methyl pyrrolidone as extraction solvent, from the charging of extractive distillation top, obtaining cut 4(mass content from T2 column overhead is more than 99% normal hexane) be qualified product, be sent to T3 extraction solvent recovery tower by the material 5 of extraction at the bottom of T2 extraction distillation column tower, the discharging 6 of T3 column overhead for methylcyclopentane be main heavy distillate, the extraction solvent 7(extraction solvent content being reclaimed by T3 tower tower reactor is more than 99.9%) after cooling, circulate and enter T2 extraction distillation column.
2, processing condition
Major technique is in table 1.
The main design of table 1 and operating parameters
3, three tower designs
3.1 T1 continuous rectifying towers
T1 continuous rectifying tower adopts band press operation, working pressure is 160kPa(a), design tower diameter is φ 1400mm, adopt efficient DZ-II type filler, packing section height is 35200mm, be divided into into eight sections, each section is highly respectively 4000mm, 4000mm, 4800mm, 4800mm, 4800mm, 4800mm, 4000mm, 4000mm.Between tower top and packing section, adopt high-efficiency liquid distributor, in tower, configure snappiness liquid header.Opening for feed is arranged between second segment and the 3rd section of filler, and side is adopted mouth and is arranged between the 6th section and the 7th section of filler.
3.2 T2 extraction distillation columns
T2 extraction distillation column adopts decompression operation, working pressure is 70kPa(a), design tower diameter is φ 1200mm, adopt efficient DZ-III type filler, total filler height is 30100mm, be divided into into seven sections, each section is highly respectively 3000mm, 4600mm, 4600mm, 4700mm, 4400mm, 4400mm, 4400mm.Between tower top and packing section, adopt high-efficiency liquid distributor, in tower, configure snappiness liquid header.Extractant feed mouth is arranged between first paragraph filler and second segment filler, and material inlet is arranged between the 4th section of filler and the 5th section of filler.
3.3 T3 extraction solvent recovery towers
T3 extraction solvent recovery tower adopts decompression operation, and working pressure is 40kPa(a), design tower diameter is φ 1000mm, and rectifying section adopts efficient DZ-III type filler, is highly 5000mm, and stripping section adopts DZ-II type filler, packed height 5500mm.Between tower top and packing section, adopt high-efficiency liquid distributor, in tower, configure snappiness liquid header.Opening for feed is arranged between two sections of fillers.
4, raw material scheme
The aromatic hydrocarbons that oil refining apparatus is produced raffinates oil 1 as raw material.
5, intermediates scheme
At the bottom of continuous rectifying tower tower, obtaining entering extraction distillation column containing 80% hexane fraction 3 (the light constituent content below normal hexane is controlled at below 0.1%) purifies again, the material 5 obtaining at the bottom of extraction distillation column tower enters extraction solvent recovery tower, at the bottom of extraction solvent recovery tower tower, extraction solvent 7 enters continuous rectifying tower again, recycles.
6, the finished product scheme
99% above normal hexane cut 4 is qualified normal hexane solvent, as the solvent of for olefines polymerization, the solvent of extraction agent, rubber and coating and the thinner of pigment of edible vegetable oil.
Claims (1)
1. rectifying and the method that extracts integrated extraction high purity normal hexane, the aromatic hydrocarbons of producing taking oil refining apparatus is raffinated oil as raw material, and raw material main ingredient is C
5～C
8wherein normal hexane content is 25%, methylcyclopentane content is 2.5%, the three tower process flow processs that adopt continuous rectification to combine with extractive distillation, first by component excision lighter than normal hexane in raw material, tower top is lighting end, and at the bottom of tower, discharging is the normal hexane fraction that isohexane content is less than 0.1% 80% left and right; At the bottom of tower, fraction is as extraction distillation column stock oil, and stock oil is from the charging of extraction distillation column middle and lower part; Taking high boiling point N-Methyl pyrrolidone as extraction solvent and stock oil in 8:1 ratio continuously from the charging of extraction distillation column middle and upper part, after extractive distillation column separates, tower top obtains more than 99% normal hexane, is heavy constituent and extraction solvent that methylcyclopentane content is high at the bottom of extraction distillation column; Last taking the material at the bottom of extraction distillation column as extraction solvent recovery tower raw material, extraction solvent recovery tower ejects material for the high distillate of methylcyclopentane content, at the bottom of extraction solvent recovery tower tower, is extraction solvent, and extraction solvent is circulated to extraction distillation column, recycles;
It is characterized in that adopting three tower process flow processs, rectifying tower T-1 adopts band press operation, working pressure is 160kPaA, design tower diameter is φ 1400mm, adopt efficient DZ-II type filler, packing section height is 35200mm, be divided into into eight sections, each section is highly respectively 4000mm, 4000mm, 4800mm, 4800mm, 4800mm, 4800mm, 4000mm, 4000mm, between tower top and packing section, adopt high-efficiency liquid distributor, in tower, configure snappiness liquid header, opening for feed is arranged between second segment and the 3rd section of filler, side is adopted mouth and is arranged between the 6th section and the 7th section of filler, extractive distillation column T-2 adopts decompression operation, working pressure is φ 1200mm for 70kPaA designs tower diameter, adopt efficient DZ-III type filler, total filler height is 30100mm, be divided into into seven sections, each section is highly respectively 3000mm, 4600mm, 4600mm, 4700mm, 4400mm, 4400mm, 4400mm, between tower top and packing section, adopt high-efficiency liquid distributor, in tower, configure snappiness liquid header, extractant feed mouth is arranged between first paragraph filler and second segment filler, and material inlet is arranged between the 4th section of filler and the 5th section of filler, extraction solvent recovery tower T-3 adopts decompression operation, working pressure is 40kPaA, design tower diameter is φ 1000mm, rectifying section adopts efficient DZ-III type filler, is highly 5000mm, and stripping section adopts DZ-II type filler, packed height 5500mm, between tower top and packing section, adopt high-efficiency liquid distributor, configure snappiness liquid header in tower, opening for feed is arranged between two sections of fillers.
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| CN201210497953.4A CN102942434B (en) | 2012-11-29 | 2012-11-29 | Method extracting high purity n-hexane by integrating rectification and extraction |
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| CN201210497953.4A CN102942434B (en) | 2012-11-29 | 2012-11-29 | Method extracting high purity n-hexane by integrating rectification and extraction |
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| CN102942434B true CN102942434B (en) | 2014-12-03 |
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Families Citing this family (9)
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| CN104045500B (en) * | 2013-03-15 | 2016-04-13 | 中石化广州工程有限公司 | A kind of production method of high purity polymerization-grade normal hexane |
| CN103242120B (en) * | 2013-04-27 | 2015-11-04 | 天津大学 | Extraction agent circulation device and process for purification in a kind of normal hexane, isohexane and benzene sepn process |
| CN103664446A (en) * | 2013-12-17 | 2014-03-26 | 赛鼎工程有限公司 | Technology for separating n-hexane-methylcyclopentane through extractive distillation |
| CN105085140B (en) * | 2014-05-16 | 2018-03-06 | 上海星可高纯溶剂有限公司 | The method of purification of liquid chromatography mass combined instrument n-hexane |
| CN105085142B (en) * | 2014-05-20 | 2018-03-20 | 中石化广州工程有限公司 | A kind of production method of high-purity n-hexane |
| CN105194899A (en) * | 2015-10-16 | 2015-12-30 | 青岛科技大学 | Variable-diameter rectifying device and method for separating methylbenzene-isobutylbenzene mixture |
| CN107698481A (en) * | 2017-11-06 | 2018-02-16 | 黄河三角洲京博化工研究院有限公司 | A kind of renovation process of n-hexane, isohexane separator extractant |
| CN110256190A (en) * | 2019-06-20 | 2019-09-20 | 山东京博石油化工有限公司 | A kind of production method of food-grade n-hexane |
| CN110386866B (en) * | 2019-07-26 | 2021-04-27 | 厦门金达威维生素有限公司 | Continuous extraction and drying device and method for butenone |
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