CN101372442B - Apparatus and method for separating tert-butanol and water using batch fractionating and pervaporation - Google Patents
Apparatus and method for separating tert-butanol and water using batch fractionating and pervaporation Download PDFInfo
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- CN101372442B CN101372442B CN2008101518101A CN200810151810A CN101372442B CN 101372442 B CN101372442 B CN 101372442B CN 2008101518101 A CN2008101518101 A CN 2008101518101A CN 200810151810 A CN200810151810 A CN 200810151810A CN 101372442 B CN101372442 B CN 101372442B
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Abstract
The invention relates to a device and a method for separating tert-butyl alcohol from water by combining batch rectification and pervaporation. The device mainly comprises a rectification tower body, a rectification tower kettle, a condenser, a membrane separator, a water jet pump, a condensate storage tank and a circulating pump. The tert-butyl alcohol aqueous solution is added to the batch rectification tower kettle, and firstly total-reflux operation is carried out in the batch rectification tower by switching a valve positioned at the condensate outlet at the tower top; after the mixture in the tower becomes stable, azeotrope of the tert-butyl alcohol and the water enters the membrane separator by the condenser for further dehydration and separation; osmotic lateral pressure is kept at 1000Pa by the jetting of the water jet pump, thus the tert-butyl alcohol and the water in the tert-butyl alcohol aqueous solution are separated by the membrane separator; the high-concentration tert-butyl product can be obtained from the rectification tower kettle, and the water is vaporized at the downstream of the membrane separator by an osmotic membrane; after vaporization and condensation, the high-concentration tert-butyl product is put in the condensate storage tank, and then cooled by the condenser and sent to the water jet pump by the circulating pump for circulation. The method has the advantages of simple operations and high tert-butyl alcohol yield without adding other solvents.
Description
Technical field
The present invention relates to the separation of azeotrope, the apparatus and method of particularly a kind of batch fractionating and shared separating tert-butanol of infiltration evaporation and water specifically are the method and apparatus of total reflux batch fractionating-water-jetting type decompress osmosis vaporization coupling separating tert-butanol-water.
Background technology
The trimethyl carbinol (TBA) has another name called the butyl alcohol-tert trimethyl carbinol, the colourless crystallization or the transparent liquid of camphor smell are arranged under the normal temperature, have water absorbability, dissolve in most of organic solvents, as alcohol, ester, ether, aliphatic hydrocarbon, arene, be solvent and additive important in the industrial production.The trimethyl carbinol uses quite extensive as solvent, can make wax with the solvent of solvent, paint solvent, medical solvent, soluble cotton and synthetic resins and thinner etc.The raw material that also can be used as synthetic musk also is used for synthetic fruit essence, synthetic drugs, system TERTIARY BUTYL AMINE etc.The trimethyl carbinol can be miscible and can form constant boiling mixture with arbitrary proportion with water, and azeotropic point is 62.5 ℃, and wherein the massfraction of water is 11.76%, is difficult to dehydration, can't obtain the highly purified trimethyl carbinol with the method for conventional distillation.
At present large-scale application is azeotropic distillation and extracting rectifying in industrial separating tert-butanol-water.U.S. Pat 4239926 at first proposes water and the dimethylbenzene combination is removed water as extraction agent.5084142 of U.S. Pat have been carried out the measurement of relative volatility to big quantity of material, have screened some and have been suitable for the entrainment agent that separates this tertiary butanol and water.Studies show that the entrainment agent that is applicable to azeotropic distillation is vinyl n-butyl ether and Propylene Glycol Dimethyl Ether, the extraction agent suitable to extracting rectifying is 1,3 butylene glycol and triglycol.Chinese patent CN1634820A has introduced the novel process that the infiltration evaporation method is produced the trimethyl carbinol.CN1760165A discloses the method for heterogeneous azeotropic rectification separating tert-butanol and water, this method is introduced the third material cyclohexane, cyclohexane give is a solvent important in the industrial production, need reclaim it, the purity that obtains the trimethyl carbinol from cat head is 98.2% simultaneously, quality product is not very high, and yield is 52%, and yield is low.
Summary of the invention
The apparatus and method that the purpose of this invention is to provide shared separating tert-butanol of a kind of batch fractionating and infiltration evaporation and water, from the trimethyl carbinol aqueous solution, the trimethyl carbinol is separated with water, utilize total reflux batch fractionating-water-jetting type decompress osmosis vaporization coupling isolation technique purification, spissated t-butanol solution, obtain moisture 0.01～5% high concentration tert-butyl alcohol, reduce production cost of products, improve the quality of products.
The device of a kind of batch fractionating provided by the invention and shared separating tert-butanol of infiltration evaporation and water mainly comprises: rectifying tower body of the tower, rectifying Tata still, condenser, membrane separation apparatus, water jet pump, phlegma storage tank and recycle pump.
The batch fractionating column overhead is connected and installed first condenser, and cat head first condenser is communicated with first phlegma storage tank and the membrane separation apparatus, and membrane separation apparatus connects water jet pump and recycle pump; Water jet pump below is established and is connected with the second phlegma storage tank, is connected second condenser between the second phlegma storage tank and the recycle pump.
In the disposable input rectifying of the material Tata still, carrying out gas-liquid mass transfer at the rectifying tower body of the tower separates, after cat head first condenser condenses, obtain the tertiary butanol and water azeotrope and be introduced into the first phlegma storage tank and carry out total reflux operation, treat in the tower stable after, cat head tertiary butanol and water phlegma enters membrane separation apparatus.Separation through membrane separation apparatus, the spissated trimethyl carbinol of film upside all passes back into rectifying Tata internal recycle, gas after the vaporization of film downside directly enters water jet pump, behind vaporization and condensation, enter the second phlegma storage tank, the second phlegma storage tank is connected with second condenser, enter recycle pump after cooling, cooled liquid enters water jet pump once more through recycle pump and circulates.
The parameter of described batch fractionating tower is: effective packing tower height 1m, king-post diameter 30mm, the efficient stainless steel θ ring filler of interior dress 3mm * 3mm; The tower still is 1000ml; With electro-magnet and rly. control reflux ratio, thief hatch is arranged at cat head; The tower still has companion's thermic devices, and body of the tower is incubated with the heating zone,
The number of theoretical plate of described batch fractionating tower is at least 20.
Described infiltrating and vaporizing membrane adopts water permeable membrane, described water permeable membrane is selected from: and NaA type molecular screen membrane, polyvinyl alcohol, chitosan blend composite membrane (PVA-CS, PSF), algae plays acid, carboxymethyl cellulose or based on the polyion compound film material of polyacrylic acid.
The method of a kind of batch fractionating provided by the invention and shared separating tert-butanol of infiltration evaporation and water may further comprise the steps:
At first tertiary butanol and water solution is joined number of theoretical plate and be in the batch fractionating Tata still more than 20, make the whole experiment device system keep sealing; Close the valve B in overhead condensation liquid exit, open valve A, feed water coolant, open the rectifying tower well heater, treat to carry out total reflux operation after cat head has backflow the heating of tower still to overhead condenser; Stable in the tower, tower top temperature is stable; Valve-off A, open valve B, at this moment the phlegma that obtains of cat head enters the separation of further dewatering in the membrane separation apparatus, hold back the spissated trimethyl carbinol of side and then enter the tower internal recycle, per-meate side volleys by water jet pump, per-meate side obtains water and the micro-trimethyl carbinol is vaporized under this vacuum condition, gas after the vaporization enters the suction chamber of water jet pump to be mixed with high-speed jet from water jet pump, mixed flow then enters the expansion chambers of water jet pump, behind vaporization and condensation, enter the phlegma storage tank, enter water-circulating pump through the supercooler cooling again and recycle.
Described batch fractionating column overhead working pressure is 600～7000Pa.The pressure-stabilisation that described per-meate side volleys by water jet pump is at 1000Pa.
1-2 hour described total reflux time.The overhead condensation liquid temp is at 60～105 ℃.Be preferably 62.5 ℃.
Described tertiary butanol and water solution is to contain the above tertiary butanol and water solution of the 80-92% trimethyl carbinol.
Advantage of the present invention: applied widely, need not introduce other solvent, trimethyl carbinol purity height, yield easy to operate, that obtain are big; Adopt the water jet pump to keep the vacuum tightness of per-meate side, having effectively utilized vaporization is coupling between the water for the medium of water and water jet pump mutually.The present invention is applicable to the tertiary butanol and water system that any azeotropic is formed.
Description of drawings
Fig. 1 is an Experimental equipment of the present invention.
Embodiment
As shown in Figure 1,1 is rectifying Tata still, and 2 is the rectifying tower body of the tower, and 3,8 is condenser, and 4,7 is the phlegma storage tank, and 5 is membrane separation apparatus, and 6 is water jet pump, and 9 is recycle pump.
The device of a kind of batch fractionating provided by the invention and shared separating tert-butanol of infiltration evaporation and water comprises: rectifying tower body of the tower 2, rectifying Tata still 1, condenser 3,8, membrane separation apparatus 5, water jet pump 6, phlegma storage tank 4,7 and recycle pump 9.In the disposable input rectifying of the material Tata still 1, carrying out gas-liquid mass transfer at rectifying tower body of the tower 2 separates, after overhead condenser 3 condensations, obtain the tertiary butanol and water azeotrope and be introduced into phlegma storage tank 4 and carry out total reflux operation, treat in the tower stable after, cat head tertiary butanol and water phlegma enters membrane separation apparatus 5.Separation through membrane separation apparatus, the spissated trimethyl carbinol of film upside all passes back into rectifying Tata internal recycle, gas after the vaporization of film downside directly enters water jet pump 6, behind vaporization and condensation, enter phlegma storage tank 7, the phlegma storage tank is connected with water cooler 8, enter recycle pump 9 after cooling, cooled liquid enters water jet pump once more through recycle pump and circulates.
Application Example
Embodiment 1
Setting drawing as shown in Figure 1.The tertiary butanol and water solution 600ml that will contain 80% trimethyl carbinol puts in the batch fractionating Tata still stopping property of check system.Close the valve B in overhead condensation liquid exit earlier, open valve A, after overhead condenser feeds water coolant, connect heating power supply to the heating of tower still, treat to carry out total reflux operation after cat head has backflow, total reflux 1.5 hours, vapor liquid equilibrium is stable in the tower, and the overhead condensation liquid temp is stabilized in 62.5 ℃.Switch the condensate outlet valve, valve-off A, open valve B, make the azeotrope of tertiary butanol and water enter membrane separation apparatus, the separation of in membrane separation apparatus, further dewatering, hold back the spissated trimethyl carbinol of side and enter rectifying Tata internal recycle, per-meate side employing water jet pump volleys makes its pressure-stabilisation about 1000Pa, the water that per-meate side obtains and the micro-trimethyl carbinol are vaporized under this vacuum condition, gas after the vaporization enters water jet pump, behind vaporization and condensation, enter the phlegma storage tank, again through cooling off after recycle pump recycles to water jet pump.The trimethyl carbinol aqueous solution is constantly circulation in rectifying tower, and the water in the rectifying tower can obtain containing the product of the trimethyl carbinol 98.5% in continuous minimizing at the bottom of tower.
Setting drawing as shown in Figure 1.The tertiary butanol and water solution 600ml that will contain 88% trimethyl carbinol puts in the batch fractionating Tata still stopping property of check system.Close the valve B in overhead condensation liquid exit earlier, open valve A, after overhead condenser feeds water coolant, connect heating power supply to the heating of tower still, treat to carry out total reflux operation after cat head has backflow, total reflux 1.5 hours, vapor liquid equilibrium is stable in the tower, and the overhead condensation liquid temp is stabilized in 62.5 ℃.Switch the condensate outlet valve, valve-off A, open valve B, make the azeotrope of tertiary butanol and water enter membrane separation apparatus, the separation of in membrane separation apparatus, further dewatering, hold back the spissated trimethyl carbinol of side and enter rectifying Tata internal recycle, per-meate side employing water jet pump volleys makes its pressure-stabilisation about 1000Pa, the water that per-meate side obtains and the micro-trimethyl carbinol are vaporized under this vacuum condition, gas after the vaporization enters water jet pump, behind vaporization and condensation, enter the phlegma storage tank, again through cooling off after recycle pump recycles to water jet pump.The trimethyl carbinol aqueous solution is constantly circulation in rectifying tower, and the water in the rectifying tower can obtain containing the product of the trimethyl carbinol 99.5% in continuous minimizing at the bottom of tower.
Setting drawing as shown in Figure 3.The tertiary butanol and water solution 600ml that will contain 92% trimethyl carbinol puts in the batch fractionating Tata still stopping property of check system.Close the valve B at overhead condenser place earlier, open valve A, after overhead condenser feeds water coolant, connect heating power supply to the heating of tower still, treat to carry out total reflux operation after cat head has backflow, total reflux 1.5 hours, vapor liquid equilibrium is stable in the tower, and the overhead condensation liquid temp is stabilized in 62.5 ℃.Switch the condensate outlet valve, valve-off A, open valve B, make the azeotrope of tertiary butanol and water enter membrane separation apparatus, the separation of in membrane separation apparatus, further dewatering, hold back the spissated trimethyl carbinol of side and enter rectifying Tata internal recycle, per-meate side employing water jet pump volleys makes its pressure-stabilisation about 1000Pa, the water that per-meate side obtains and the micro-trimethyl carbinol are vaporized under this vacuum condition, gas after the vaporization enters water jet pump, behind vaporization and condensation, enter the phlegma storage tank, again through cooling off after recycle pump recycles to water jet pump.The trimethyl carbinol aqueous solution is constantly circulation in rectifying tower, and the water in the rectifying tower can obtain containing the product of 99.9% trimethyl carbinol in continuous minimizing at the bottom of tower.
Claims (7)
1. the device of a batch fractionating and shared separating tert-butanol of infiltration evaporation and water is characterized in that mainly comprising: rectifying tower body of the tower, rectifying Tata still, condenser, membrane separation apparatus, water jet pump, phlegma storage tank and recycle pump;
The batch fractionating column overhead is connected and installed first condenser, and cat head first condenser is communicated with first phlegma storage tank and the membrane separation apparatus, and membrane separation apparatus connects water jet pump and recycle pump; Water jet pump below is established and is connected with the second phlegma storage tank, is connected second condenser between the second phlegma storage tank and the recycle pump;
Obtaining the tertiary butanol and water azeotrope after cat head first condenser condenses is introduced into the first phlegma storage tank and carries out total reflux operation, after treating to stablize in the tower, cat head tertiary butanol and water phlegma enters membrane separation apparatus, through the separation of membrane separation apparatus, the spissated trimethyl carbinol of film upside all passes back into rectifying Tata internal recycle.
2. device according to claim 1 is characterized in that the parameter of described batch fractionating tower is: effective packing tower height 1m, king-post diameter 30mm, the efficient stainless steel θ ring filler of interior dress 3mm * 3mm; The tower still is 1000ml.
3. device according to claim 1 is characterized in that the number of theoretical plate of described batch fractionating tower is at least 20.
4. the method for a batch fractionating and shared separating tert-butanol of infiltration evaporation and water is characterized in that may further comprise the steps:
At first tertiary butanol and water solution is joined number of theoretical plate and be in the batch fractionating Tata still more than 20, make the whole experiment device system keep sealing; Close the valve in overhead condensation liquid exit, open valve, feed water coolant, open the rectifying tower well heater, treat to carry out total reflux operation after cat head has backflow the heating of tower still to overhead condenser; Stable in the tower, tower top temperature is stable; Valve-off, open valve, at this moment the phlegma that obtains of cat head enters the separation of further dewatering in the membrane separation apparatus, hold back the spissated trimethyl carbinol of side and then enter the tower internal recycle, per-meate side volleys by water jet pump, the pressure-stabilisation that water jet pump volleys is at 1000Pa, per-meate side obtains water and the micro-trimethyl carbinol is vaporized under this vacuum condition, gas after the vaporization enters the suction chamber of water jet pump to be mixed with high-speed jet from water jet pump, mixed flow then enters the expansion chambers of water jet pump, behind vaporization and condensation, enter the phlegma storage tank, enter water-circulating pump through the supercooler cooling again and recycle.
5. method according to claim 4 is characterized in that described batch fractionating column overhead working pressure is 600～7000Pa.
6. method according to claim 4 is characterized in that 1-2 hour described total reflux time.
7. method according to claim 4 is characterized in that the overhead condensation liquid temp is at 60～105 ℃.
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| CN101805754B (en) * | 2010-03-31 | 2012-06-27 | 南京工业大学 | Process for separating acetone, butanol and ethanol in situ by coupling biomass fermentation and pervaporation |
| CN102120093A (en) * | 2010-12-28 | 2011-07-13 | 南京工业大学 | Solvent recovery process in pharmaceutical industry |
| CN102206197A (en) * | 2011-03-31 | 2011-10-05 | 天津大学 | Intermediate storage tank-carrying batch distillation and pervaporation coupling method for separating tetrahydrofuran from water and device thereof |
| CN104027996A (en) * | 2013-12-27 | 2014-09-10 | 江苏九天高科技股份有限公司 | A pervaporation rectification coupled system and a use thereof |
| CN104262089B (en) * | 2014-09-01 | 2016-08-24 | 南京工业大学 | The method and device that the dehydration of a kind of bio-fuel is refined |
| CN105561620B (en) * | 2014-10-09 | 2017-11-28 | 中国石油化工股份有限公司 | Aqueous high boiling solvent recovery process and device |
| CN108452553B (en) * | 2018-04-01 | 2023-12-15 | 重庆梁彬新材料技术有限公司 | Alcohol water recovery unit for aerogel |
| CN112044231A (en) * | 2020-09-16 | 2020-12-08 | 湖南一代伟仁科技有限公司 | Efficient method for recovering solvent by tail gas refrigeration |
| CN113045386A (en) * | 2021-03-11 | 2021-06-29 | 南京师范大学 | Process method for separating tert-butyl alcohol-tetrahydrofuran-water mixed solvent by rectification-membrane separation integrated process |
| CN114011108A (en) * | 2021-12-06 | 2022-02-08 | 兰州理工大学 | System and method for separating methanol-water by rectification coupling membrane |
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| CN1681757A (en) * | 2002-09-10 | 2005-10-12 | 奥克森诺奥勒芬化学股份有限公司 | Method of producting waterless tert-butanol |
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