CN1280976A - Process for separating butane from butene with dimethyl formamide and its mixture - Google Patents

Process for separating butane from butene with dimethyl formamide and its mixture Download PDF

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Publication number
CN1280976A
CN1280976A CN 99108743 CN99108743A CN1280976A CN 1280976 A CN1280976 A CN 1280976A CN 99108743 CN99108743 CN 99108743 CN 99108743 A CN99108743 A CN 99108743A CN 1280976 A CN1280976 A CN 1280976A
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China
Prior art keywords
tower
solvent
butylene
dmf
mixture
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CN 99108743
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CN1139560C (en
Inventor
任万忠
许文有
王文华
陈小平
虞乐舜
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CHEMICAL DEPARTMENT OF YANTAI UNIV
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CHEMICAL DEPARTMENT OF YANTAI UNIV
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Abstract

A process for separating butane and butene uses the mixture of dimethyl formamide (DMF) and another one or more solvents as its solvent and a two-tower route for separation. Two towers are operated under pressure. The output product from tower top can be condensed by circulating water and the tower still temp. is lower than 170 deg.C. The DMF is not decomposed. The added solvent also has separation action, but the boiling point is relatively low.

Description

Method with dimethyl formamide and composition thereof separating butane and butylene
The present invention relates to use N, dinethylformamide (hereinafter to be referred as DMF) and with the mixture as solvent of another or multiple solvent, the method for two tower flow process extracting rectifying separating butanes and butylene.
The method of making solvent extraction rectifying separation hydro carbons with DMF has been mature technology in the extracting of divinyl, but it is then rare with separating of n-butene to be used for butane, and known method with DMF separating butane and butylene is three-column process flow (IFP Ep0501 848 A1).The C4 mixture contacts with DMF in the extractive distillation column of a pressurized operation, the overhead collection butane, the solvent that contains butylene enters second tower of a pressurized operation after the extraction of tower still, butylene is by the part desorb in this tower, in overhead collection, the solvent that still contains some butylene is purified at the 3rd tower of an atmospheric operation, obtains qualified solvent at the tower still of this tower and introduces extractive distillation column and recycle, cat head vapour phase production is sent the bottom of second tower back to again through overdraft.The shortcoming of this method is a complicated operation, the energy consumption height.
And if solvent recuperation is finished, promptly to obtain qualified butylene in the solvent recuperation column overhead in a tower, the tower still will obtain qualified solvent, if pressurized operation, tower still temperature is higher, surpasses 170 ℃, and at this more than temperature, DMF decomposes easily, influences the butylene quality, increases the loss of solvent.If atmospheric operation is the overhead condensation difficulty of butylene then, need deep cooling or compression.Therefore how solvent recuperation was divided into for two steps, promptly adopts three-column process flow.
The task of this patent is to set up a kind of two tower flow processs solvent recuperation is finished in a tower, and solvent recovery tower is operated (the assurance butylene can be used water condensation) under pressurized conditions, and tower still temperature lower (being lower than 1.70 ℃), DMF does not decompose.
Method of the present invention with reference to the accompanying drawings, butane and butene mixture (3) are added by extractive distillation column (1 tower) middle part, add by the mixed solvent (4) of DMF and another solvent or other multiple solvent composition top by 1 tower, butane (3) is from the top extraction of extractive distillation column, the solvent that contains butylene is from 1 Tata still extraction, the solvent recovery tower (2 tower) that connects after the solvent that contains alkene causes after the bottom extraction of 1 tower, by distilling with alkene and separated from solvent, butylene (5) is from 2 column overhead extraction, solvent (6) is introduced 1 tower again again and is recycled from 2 Tata still extraction.
The method of above-mentioned extracting rectifying has been successfully applied to the butane of various raw materials compositions and separating of butene mixture.
Characteristics of the present invention are:
A). adopt two tower flow process separating butane and butylene.
B). all operations under pressurization of two towers, the cat head production can be used the recirculated water condensation.
C). tower still temperature is lower than 170 ℃.
D). having added has centrifugation equally, but the second lower solvent of boiling point, or multiple other solvent.
Example as this patent is to add the second solvent butanone.Because the boiling point of butanone is lower, can reduce the temperature of tower still greatly, the amplitude of reduction is relevant with the amount that adds butanone.
Use this patent method, the concentration of the butylene of being produced can reach about 97% (Wt), can be higher than 97% in case of necessity, and this is mainly decided by solvent ratio and stage number.
It below is an example of this patent.
Example:
Handled C4 mixture is C4 after the etherificate, promptly produces the hybrid C 4 behind the MTBE, and solvent for use is the mixture of DMF (N, dinethylformamide) and butanone, and the ratio of DMF and butanone is 30/70~70/30.Main experimental results reduction is in table one.
Table one DMF and butanone are made separated from solvent butane and butylene
The DMF charging ??kg/hr ????10.1
Cat head is formed (not containing solvent)
N-propane Trimethylmethane normal butane 1-butylene is anti--and 2-butylene is suitable-2-butylene C 4Feed composition Weight, % weight, % weight, % weight, % weight, % weight, % ??1.33 ?65.57 ?26.63 ??6.47 ??0.00 ??0.00
N-propane iso-butane normal butane 1-butylene Trans-2-butene cis-2-butene tower reactor forms (not containing solvent) Weight, % weight, % weight, % weight, % weight, % weight, % ??0.56 ?27.76 ?12.43 ?33.35 ?18.71 ??7.19
N-propane Trimethylmethane normal butane 1-butylene is anti--and 2-butylene is suitable-2-butylene Weight, % weight, % weight, % weight, % weight, % weight, % ??0.33 ??2.13 ?52.86 ?32.29
Used extractive distillation column (1 tower) is a packing tower: the material carbon steel, and tower diameter 50mm, filler are the Stainless Steel Wire ring filler;
Solvent recovery tower (2 tower) also is a packing tower: the material carbon steel, and tower diameter 50mm, filler are the θ ring filler;
The equal adiabatic heat-insulation of two towers;
Hybrid C 4 adds temperature 30-50 ℃ by the middle part of 1 tower;
Solvent ratio: 10-19;
1 tower working pressure: 0.4-0.6MPa;
2 tower reflux ratio: 2.5-8;
2 tower working pressure: 0.4-0.6MPa;
1 Tata still temperature: 110-150 ℃;
2 Tata still temperature: 140-165 ℃;

Claims (4)

1. utilize DMF and composition thereof to make the method for solvent two tower flow process separating butanes and butylene, it is characterized in that adopting the mixture as solvent of DMF and another or multiple solvent, second solvent boiling point is lower.
2. by the described method of claim 1, it is characterized in that adopting two tower flow processs, hybrid C 4 adds from 1 tower middle part, and solvent adds from 1 top of tower, and butane is from 1 top of tower extraction, and butylene is from 2 top of tower extraction, and 2 Tata still solvents return 1 tower after energy recovery.
3. by the described method of claim 1, it is characterized in that two towers all operate under pressurized conditions, the cat head production can be used the recirculated water condensation.
By claim 1 fast method, it is characterized in that tower still temperature is lower than 170 ℃.
CNB991087437A 1999-07-14 1999-07-14 Process for separating butane from butene with dimethyl formamide and its mixture Expired - Fee Related CN1139560C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB991087437A CN1139560C (en) 1999-07-14 1999-07-14 Process for separating butane from butene with dimethyl formamide and its mixture

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Application Number Priority Date Filing Date Title
CNB991087437A CN1139560C (en) 1999-07-14 1999-07-14 Process for separating butane from butene with dimethyl formamide and its mixture

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CN1280976A true CN1280976A (en) 2001-01-24
CN1139560C CN1139560C (en) 2004-02-25

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102603454A (en) * 2011-12-22 2012-07-25 烟台大学 Iso-butane, n-butane and butylene separation and purification method
CN103193577A (en) * 2013-03-25 2013-07-10 烟台大学 Method for extracting, rectifying and separating butane from butylene by ternary mixed solvent
CN103641693A (en) * 2013-12-05 2014-03-19 河北海特伟业石化有限公司 Low-energy-consumption MTBE (methyl tert-butyl ether) production method
US9266808B2 (en) 2006-11-30 2016-02-23 Basf Se Method for the hydroformylation of olefins
CN106966852A (en) * 2016-01-14 2017-07-21 天津大学 The method that continuous extraction rectifying separates high-carbon n-alkane and normal olefine

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9266808B2 (en) 2006-11-30 2016-02-23 Basf Se Method for the hydroformylation of olefins
CN102603454A (en) * 2011-12-22 2012-07-25 烟台大学 Iso-butane, n-butane and butylene separation and purification method
CN103193577A (en) * 2013-03-25 2013-07-10 烟台大学 Method for extracting, rectifying and separating butane from butylene by ternary mixed solvent
CN103641693A (en) * 2013-12-05 2014-03-19 河北海特伟业石化有限公司 Low-energy-consumption MTBE (methyl tert-butyl ether) production method
CN106966852A (en) * 2016-01-14 2017-07-21 天津大学 The method that continuous extraction rectifying separates high-carbon n-alkane and normal olefine
CN106966852B (en) * 2016-01-14 2019-10-25 天津大学 The method of continuous extraction rectifying separation high-carbon n-alkane and normal olefine

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