CN101134736A - Method for separating carbinol acetonitrile azeotrope - Google Patents
Method for separating carbinol acetonitrile azeotrope Download PDFInfo
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- CN101134736A CN101134736A CNA2007100612883A CN200710061288A CN101134736A CN 101134736 A CN101134736 A CN 101134736A CN A2007100612883 A CNA2007100612883 A CN A2007100612883A CN 200710061288 A CN200710061288 A CN 200710061288A CN 101134736 A CN101134736 A CN 101134736A
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Abstract
The present invention relates to method of separating methanol-acetonitrile azeotrope. By means of the feature of methanol-acetonitrile azeotrope system with positive deviation to Raoult's law, the pressure of the system is lowered or raised to shift the binary azeotropic point and alter the composition of the azeotrope system, so as to reach the separation aim. The decompressing rectification tower has a theoretical plate number of at least 40 and top pressure of 0.3-0.5atm, and compressing rectification tower has a theoretical plate number of at least 25 and top pressure of 5-10 atm. The method can obtain separated methanol and acetonitrile products of purity over 99.5 wt%, has short technological process, easy control and other advantages, and is suitable for separating methanol-acetonitrile solution in different ratio.
Description
Technical field
The present invention relates to the separation technology field of methyl alcohol, specifically a kind of method of separation of methanol acetonitrile azeotrope.
Technical background
Methyl alcohol is widely used in industry such as medicine, agricultural chemicals, dyestuff, synthon, synthetic rubber, synthetic plastics and synthetic resins, and its output is only second to synthetic ammonia and ethene, occupies the third place in the world.Acetonitrile (methyl nitrile) is a kind of important Organic Chemicals.Because acetonitrile has distinctive functional group itrile group, as solvent, it also has than better partition ratio of alcohols and desorption ability except the characteristic that has ethanol, methyl alcohol equal solvent and had.The extractant of Chang Zuowei divinyl, isoprene cut in petrochemical complex; Be important medicine, agricultural chemicals, dyestuff and synthetic perfume raw material or intermediate, also can be used as analytical reagent and be used for high pressure liquid chromatographic analysis.
Acetonitrile and methyl alcohol infinitely dissolve each other, and there is azeotrope, azeotropic under the normal pressure consists of and contains methyl alcohol 79%～80% (wt), azeotropic temperature is 63.4～63.7 ℃, therefore what obtain from cat head by atmospheric distillation is the binary azeotrope of methyl alcohol-acetonitrile, contain a large amount of acetonitriles in this azeotrope, how the methyl alcohol of Separation and Recovery high density and acetonitrile are the problems that needs solve from this azeotrope.At the separation of this system, do not see the industrialization report at present.
Summary of the invention
The object of the present invention is to provide the method for a kind of separation of methanol and acetonitrile azeotrope.Technical process of the present invention is short, facility investment is few, easy to operate, be easy to control, be applicable to arbitrarily than blended methyl alcohol-acetonitrile mixed solution.
The method of separation of methanol provided by the invention and acetonitrile azeotrope is characterized in that its process following steps:
1) in the rectification under vacuum tower, carry out underpressure distillation, theoretical plate number at least 40, tower top pressure 0.3～0.5atm, azeotrope continuously feeding in the room temperature tower, cat head is 2～6 continuous dischargings with reflux ratio, sends into the compression rectification tower and carries out pressure distillation, further handles; The continuous discharging of tower still obtains methanol product.
2) send into the compression rectification tower and carry out in the pressure distillation, theoretical plate number at least 25, tower top pressure 5～10atm, continuously feeding in the tower, the trim the top of column ratio is 2～6 continuous dischargings, enters the rectification under vacuum tower again and further carries out the underpressure distillation recycle; The continuous discharging of tower still obtains the acetonitrile product.
The method of separation of methanol provided by the invention and acetonitrile azeotrope may further comprise the steps:
1) in the rectification under vacuum tower, theoretical plate number at least 40, tower top pressure 0.3～0.5atm, azeotrope continuously feeding in the room temperature tower, wherein methanol quality concentration 79%～80%, and cat head is 2～5 continuous dischargings with reflux ratio, sends into the compression rectification tower and further handles; The continuous discharging of tower still obtains methanol quality concentration greater than 99.5% methanol product.
2) send in the compression rectification tower, theoretical plate number at least 25, tower top pressure 5～10atm, continuously feeding in the tower, the trim the top of column ratio is 2～4 continuous dischargings, enters the further recycle of rectification under vacuum tower; The continuous discharging of tower still obtains the acetonitrile mass concentration greater than 99.5% acetonitrile product.
The present invention is applicable to arbitrarily that than blended methyl alcohol-acetonitrile mixed solution particularly azeotropic is formed the mixed solution under (methanol quality concentration 79%～80%).
The present invention utilizes methyl alcohol-acetonitrile system Raoult's law to be produced the characteristics of plus deviation, reduction or pressurize can be broken the binary azeotropic point that methyl alcohol under the normal pressure-acetonitrile forms, change azeotrope and form, thereby methyl alcohol is separated with acetonitrile, obtain highly purified methyl alcohol and acetonitrile.
The present invention is characterized in that comprising following process: under reduced pressure, cat head can obtain the azeotrope based on methyl alcohol, obtains highly purified methanol product at the bottom of the tower.The azeotrope that is come out by the vacuum distillation tower cat head carries out rectifying under pressurized conditions, obtain highly purified acetonitrile product at the bottom of the tower.The mass concentration of methanol product and acetonitrile product all can reach more than 99.5%.Technical process of the present invention is short, facility investment is few, easy to operate, be easy to control.
Description of drawings
Accompanying drawing 1 is the process flow sheet of the present invention's decompression-pressurization separation of methanol-acetonitrile.
Embodiment
As shown in the figure, T1, T2 are respectively rectification under vacuum tower and compression rectification tower, and H1, H2 are respectively the tower still reboilers of rectification under vacuum tower and compression rectification tower, and C1, C2 are respectively the overhead condensers of rectification under vacuum tower and compression rectification tower.
The normal pressure azeotrope warp 1 of methyl alcohol-acetonitrile adds rectification under vacuum tower T1, and after T1 tower rectifying separation, the high purity methanol product that obtains of purifying leaves system by line 3, and the azeotrope warp 2 under the decompression of cat head extraction enters compression rectification tower T2.After T2 tower rectifying separation, the acetonitrile of high purity product obtain of purifying leaves system by line 5, the adding of cat head extraction the azeotrope warp 4 depressed with after the normal pressure azeotrope mixes, enter rectification under vacuum tower T1.By flow process shown in Figure 1, can obtain purity all greater than the methanol product and the acetonitrile product of 99.5% (wt).
The equipment structure:
| The T1 tower | The T2 tower | |
| Internal diameter (mm) | 400 | 350 |
| Rectifying section height (m) | 6 | 5 |
| Stripping section height (m) | 5 | 3 |
| Rectifying section stage number (piece) | 22 | 17 |
| Stripping section stage number (piece) | 18 | 8 |
Operational stage: two tower operate continuouslys, raw material azeotropic treatment capacity 700kg/h.
| Feeding temperature (℃) | Working pressure/atm | Reflux ratio | |||
| T1 | T2 | | T2 | ||
| Embodiment | |||||
| 1 | 35 | 0.3 | 5 | 3.5 | 2 |
| |
35 | 0.4 | 5 | 3.5 | 3 |
| |
35 | 0.4 | 10 | 4 | 2 |
Operating result:
| The T1 top | The T1 still | The T2 top | The T2 still | |||||
| Methyl alcohol | Acetonitrile | Methyl alcohol | Acetonitrile | Methyl alcohol | Acetonitrile | Methyl | Acetonitrile | |
| Embodiment | ||||||||
| 1 | 0.663 | 0.337 | 0.997 | 0.003 | 0.873 | 0.127 | 0.003 | 0.997 |
| |
0.687 | 0.313 | 0.996 | 0.004 | 0.890 | 0.110 | 0.003 | 0.997 |
| Embodiment 3 | 0.694 | 0.306 | 0.997 | 0.003 | 0.914 | 0.086 | 0.003 | 0.997 |
The present invention utilizes methyl alcohol-acetonitrile system to the characteristics of Raoult's law generation overgauge, reduces or improves pressure and can break the binary azeotropic point that methyl alcohol under the normal pressure-acetonitrile forms, thereby change the azeotropic mixture composition, reaches the separation purpose. The advantages such as the method has that technological process is short, equipment investment is few, easy to operate, easy control.
Claims (2)
1. the method for separation of methanol and acetonitrile azeotrope is characterized in that it is through following steps:
1) in the rectification under vacuum tower, carry out underpressure distillation, theoretical plate number at least 40, tower top pressure 0.3～0.5atm, azeotrope continuously feeding in the room temperature tower, cat head is 2～6 continuous dischargings with reflux ratio, sends into the compression rectification tower and carries out pressure distillation, further handles; The continuous discharging of tower still obtains methanol product.
2) send into the compression rectification tower and carry out in the pressure distillation, theoretical plate number at least 25, tower top pressure 5～10atm, continuously feeding in the tower, the trim the top of column ratio is 2～6 continuous dischargings, enters the rectification under vacuum tower again and further carries out the underpressure distillation recycle; The continuous discharging of tower still obtains the acetonitrile product.
2. the method for separation of methanol and acetonitrile azeotrope is characterized in that it is through following steps:
1) in the rectification under vacuum tower, theoretical plate number at least 40, tower top pressure 0.3～0.5atm, azeotrope continuously feeding in the room temperature tower, wherein methanol quality concentration 79%～80%, and cat head is 2～5 continuous dischargings with reflux ratio, sends into the compression rectification tower and further handles; The continuous discharging of tower still obtains methanol quality concentration greater than 99.5% methanol product;
2) send in the compression rectification tower, theoretical plate number at least 25, tower top pressure 5～10atm, continuously feeding in the tower, the trim the top of column ratio is 2～4 continuous dischargings, enters the further recycle of rectification under vacuum tower; The continuous discharging of tower still obtains the acetonitrile mass concentration greater than 99.5% acetonitrile product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100612883A CN100548972C (en) | 2007-09-28 | 2007-09-28 | A kind of method of separation of methanol acetonitrile azeotrope |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100612883A CN100548972C (en) | 2007-09-28 | 2007-09-28 | A kind of method of separation of methanol acetonitrile azeotrope |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101134736A true CN101134736A (en) | 2008-03-05 |
| CN100548972C CN100548972C (en) | 2009-10-14 |
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| CNB2007100612883A Expired - Fee Related CN100548972C (en) | 2007-09-28 | 2007-09-28 | A kind of method of separation of methanol acetonitrile azeotrope |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102068831A (en) * | 2010-12-15 | 2011-05-25 | 天津大学 | Batch extractive distillation device and separation method for acetonitrile-methanol azeotropic mixture |
| CN102225963A (en) * | 2011-05-13 | 2011-10-26 | 周逸明 | Method for reducing acetonitrile residue in polypeptide medicament |
| CN103214345A (en) * | 2013-04-22 | 2013-07-24 | 河北工业大学 | Technological method for separating methanol, acetonitrile and benzene tertiary mixture |
| CN103386211A (en) * | 2013-07-12 | 2013-11-13 | 中山大学 | Device and method for separating acetonitrile-water-methanol mixture |
| CN105906479A (en) * | 2016-05-24 | 2016-08-31 | 济南大学 | Method for separating butanol-butyronitrile mixture |
| CN106008159A (en) * | 2016-05-24 | 2016-10-12 | 济南大学 | Method for separating isopropyl alcohol-propionitrile mixture |
| CN106492495A (en) * | 2015-09-07 | 2017-03-15 | 中国石油化工股份有限公司 | Improved vacuum distillation tower and acetonitrile refining system |
| CN107011171A (en) * | 2017-04-14 | 2017-08-04 | 长江师范学院 | The system and method for variable-pressure rectification separating ethyl acetate and n-hexane azeotropic system |
| CN113582875A (en) * | 2021-08-10 | 2021-11-02 | 上海应用技术大学 | Treatment process of acetonitrile waste liquid containing methanol, ethanol and water |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3292311B2 (en) * | 1992-06-18 | 2002-06-17 | 日本パイオニクス株式会社 | Purification method of methanol |
| US5346593A (en) * | 1993-06-18 | 1994-09-13 | The M. W. Kellogg Company | Intermediate reboiler for a methanol plant |
| CN1075481C (en) * | 1999-09-17 | 2001-11-28 | 清华大学 | Process for refining high-purity reagent by raction extractive reactification |
-
2007
- 2007-09-28 CN CNB2007100612883A patent/CN100548972C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102068831B (en) * | 2010-12-15 | 2012-11-21 | 天津大学 | Batch extractive distillation device and separation method for acetonitrile-methanol azeotropic mixture |
| CN102068831A (en) * | 2010-12-15 | 2011-05-25 | 天津大学 | Batch extractive distillation device and separation method for acetonitrile-methanol azeotropic mixture |
| CN102225963A (en) * | 2011-05-13 | 2011-10-26 | 周逸明 | Method for reducing acetonitrile residue in polypeptide medicament |
| CN103214345B (en) * | 2013-04-22 | 2014-09-17 | 河北工业大学 | Technological method for separating methanol, acetonitrile and benzene tertiary mixture |
| CN103214345A (en) * | 2013-04-22 | 2013-07-24 | 河北工业大学 | Technological method for separating methanol, acetonitrile and benzene tertiary mixture |
| CN103386211B (en) * | 2013-07-12 | 2015-08-12 | 中山大学 | A kind of separator of acetonitrile-water-carbinol mixture and separation method |
| CN103386211A (en) * | 2013-07-12 | 2013-11-13 | 中山大学 | Device and method for separating acetonitrile-water-methanol mixture |
| CN106492495A (en) * | 2015-09-07 | 2017-03-15 | 中国石油化工股份有限公司 | Improved vacuum distillation tower and acetonitrile refining system |
| CN105906479A (en) * | 2016-05-24 | 2016-08-31 | 济南大学 | Method for separating butanol-butyronitrile mixture |
| CN106008159A (en) * | 2016-05-24 | 2016-10-12 | 济南大学 | Method for separating isopropyl alcohol-propionitrile mixture |
| CN105906479B (en) * | 2016-05-24 | 2019-01-22 | 济南大学 | A kind of separation method of butanol-butyronitrile mixture |
| CN106008159B (en) * | 2016-05-24 | 2019-01-22 | 济南大学 | A kind of separation method of isopropanol-propionitrile mixture |
| CN107011171A (en) * | 2017-04-14 | 2017-08-04 | 长江师范学院 | The system and method for variable-pressure rectification separating ethyl acetate and n-hexane azeotropic system |
| CN113582875A (en) * | 2021-08-10 | 2021-11-02 | 上海应用技术大学 | Treatment process of acetonitrile waste liquid containing methanol, ethanol and water |
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| Publication number | Publication date |
|---|---|
| CN100548972C (en) | 2009-10-14 |
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Granted publication date: 20091014 Termination date: 20100928 |