CN101607870A - A kind of method of separating tert-butanol-water - Google Patents
A kind of method of separating tert-butanol-water Download PDFInfo
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- CN101607870A CN101607870A CNA2009100174178A CN200910017417A CN101607870A CN 101607870 A CN101607870 A CN 101607870A CN A2009100174178 A CNA2009100174178 A CN A2009100174178A CN 200910017417 A CN200910017417 A CN 200910017417A CN 101607870 A CN101607870 A CN 101607870A
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- butanol
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Abstract
The present invention relates to the method for azeotrope separation method, particularly a kind of separating tert-butanol-water, this method reaches the trimethyl carbinol and water sepn by total reflux batch fractionating and infiltration evaporation coupled method.Employing comprises batch fractionating tower, the device of infiltration vaporization membrane module and water jet pump, it is characterized in that: separating technology may further comprise the steps, the trimethyl carbinol aqueous solution is put in the batch fractionating Tata still, at first in batch fractionating tower, carry out total reflux operation, the azeotrope for the treatment of tertiary butanol and water is after cat head is assembled, enter the separation of further dewatering in the membrane separation apparatus through condenser, volley the absolute pressure that makes osmotic lateral pressure maintenance 700～7500Pa by water jet pump, trimethyl carbinol aqueous solution process membrane separation apparatus is with the trimethyl carbinol and water sepn, in rectifying Tata still, can obtain the trimethyl carbinol product of high density, water, is separated from the trimethyl carbinol through vaporization and condensation under vacuum low-pressure in vapour phase chamber, membrane separation apparatus downstream side through membrane permeation.The present invention has convenient production process operation, does not introduce other solvents, and the high advantage of trimethyl carbinol yield has certain popularization value.
Description
Technical field:
The present invention relates to the method for azeotrope separation method, particularly a kind of separating tert-butanol-water.
Background technology:
The trimethyl carbinol (TBA) has another name called the butyl alcohol-tert trimethyl carbinol, and the colourless crystallization of camphor smell is arranged under the normal temperature, then is liquid when less water exists.Have water absorbability, dissolve in most of organic solvents, as alcohol, ester, ether, aliphatic hydrocarbon, arene.Be used as emulsifying agent, dye dispersant, dewatering agent, paint remover, industrial detergent etc., also be used as softening agent, weedicide, oil extraction agent.Because these character make the trimethyl carbinol be used as that nitro sprays paint, the solubility promoter of thinner for nitrocellulose finishes.The trimethyl carbinol and water can form azeotropic mixture, and 82.5 ℃ of azeotropic boiling points, the massfraction of water are 11.76%, 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.US4239926 at first proposes water and the dimethylbenzene combination is removed water as extraction agent.US5084142 has then carried out the measurement of relative volatility to big quantity of material, screened some and be suitable for the entrainment agent that separates this tertiary butanol and water.Studies show that the entrainment agent suitable for azeotropic distillation is vinyl n-butyl ether and Propylene Glycol Dimethyl Ether, the extraction agent suitable for extracting rectifying is 1,3 butylene glycol and triglycol.CN1634820A has introduced the novel process that the infiltration evaporating method is produced the trimethyl carbinol.Production cost height, quality product and the yield of above handicraft product are low.
Summary of the invention:
The novel process of the separating tert-butanol-water that the purpose of this invention is to provide that a kind of production cost is low, quality and yield is high.
Technology of the present invention is achieved in that a kind of novel process of producing high purity tert-butyl alcohol with total reflux batch fractionating and infiltration evaporation coupled method, from the trimethyl carbinol aqueous solution, the trimethyl carbinol is separated with water, adopt jet of water decompress osmosis vaporization coupled total reflux batch fractionating isolation technique, its special character is that separation process scheme may further comprise the steps:
1. putting valve is closing condition, be that the tertiary butanol and water mixture of 11.76% (azeotropic composition) is put in the batch fractionating Tata still with the water content mass percent, and carry out total reflux operation, and control phegma temperature is 70-75 ℃;
2. start recycle pump, make recirculated water be in recurrent state, and regulate the cooling water flow of water cooler, the Control Circulation water temp is 30-35 ℃, regulates the flow of recycle pump, makes absolute pressure remain on 2500～5000Pa;
3. when cat head gas phase temperature-stable during, open valve, make the trimethyl carbinol infiltration of contained water of phegma and denier pass film, and vaporization enters water jet pump, be recycled water condensation and absorption at 79.9 ℃;
4. aforesaid operations continues to that the cat head gas phase temperature rises gradually and (determine) EO when being stabilized in 82.0-82.5 ℃ according to concrete product purity.This moment valve-off, recycle pump is out of service, the rectifying tower shut-down operation;
5. open valve and emit high purity tert-butyl alcohol product in the tower still, open valve and emit the water that increases newly in the recirculated water storage tank, make liquid level get back to original position.
It has characteristics, and its special character is to select for use the water permeable membrane separator, and it is 700～7000Pa that water permeable membrane keep-ups pressure through side, the tertiary butanol and water azeotrope that condensation is got off, and behind the water permeable membrane separator, water sees through film, holds back side and obtains the spissated trimethyl carbinol.
It has characteristics, holds back the spissated trimethyl carbinol of side and is back in the rectifying tower.
It has characteristics, described jet of water decompress osmosis gasification coupled total reflux batch distillation process can be a process of dehydration in batches, tertiary butanol and water by rectifying tower, condenser, composite membrane assembly,, water jet pump and interchanger form dehydration cycle in the loop that constitutes, up to the concentration of water drop to target value with the recirculated water storage tank under.
It has characteristics, and described step rectifying tower condensate temperature is at 60～105 ℃, and seeing through wall pressure is 700～7500Pa.
It also has characteristics, and described rectifying tower number of theoretical plate is the rectifying tower more than 20, and the cat head working pressure is 600～7000Pa.
Wherein experiment adopts the parameter of batch fractionating tower to be: effective packing section height 1m, king-post diameter 30mm, the stainless steel θ of the colleges and universities ring filler of interior dress 3mm * 3mm; The tower still is the there-necked flask of 1000ml, connects tower body, thermometer and plug respectively; 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, and this tower number of theoretical plate is 20, and wherein infiltrating and vaporizing membrane adopts water permeable membrane.Described water permeable membrane be selected from Na A type molecular sieve film, polyvinyl alcohol, chitosan blend composite membrane (PVA-CS, PSF), algae plays acid, carboxymethyl cellulose and based on the polyion compound film material of polyacrylic acid.
The present invention is applicable to the azeotropic that contains trimethyl carbinol water composition or is below or above the mixture that azeotrope is formed.
Advantage of the present invention is applied widely, need not introduce other solvent, trimethyl carbinol purity height, yield easy to operate, that obtain are big.
Description of drawings
Fig. 1 is an Experimental equipment of the present invention
Wherein: 1 is the rectifying tower body of the tower, and 2 are rectifying Tata still, and 3 is condenser, and 4 is membrane separation apparatus, and 5 is water jet pump, 6 is the recirculated water storage tank, and 7 is recycle pump, and 8 is water cooler, 9,10,11,12-is valve, 13,14,15-is thermometer, 16-is a vacuum meter, and F is a raw material, and P is a product, and W is a water.
Embodiment:
Embodiment 1: setting drawing as shown in Figure 1.The tertiary butanol and water solution F600ml that will contain 80% (wt%) trimethyl carbinol puts in the batch fractionating Tata still 2, check everywhere whether good seal of interface, valve 9-10 is a closing condition, after overhead condenser 3 feeds water coolant, connecting heating power supply heats reboiler, treat that cat head has the total reflux operation of the back of backflow, and control phegma temperature is 70-75 ℃.
Start recycle pump 7, make recirculated water be in recurrent state, and regulate the cooling water flow of water cooler (8), the Control Circulation water temp is 30-35 ℃, regulates the flow of recycle pump (7), makes absolute pressure remain on 2500～5000Pa; The azeotrope of tertiary butanol and water is after cat head is assembled, and water cooler (8) is with the liquid of trimethyl carbinol water cooling to 70～75 ℃.
When cat head gas phase temperature-stable during at 79.9 ℃, open valve 9, the phlegma separation of in entering membrane separation apparatus 4, further dewatering, per-meate side can obtain the trimethyl carbinol of water and trace, enters water tank 6 through water jet pump 5.
Aforesaid operations continues to that the cat head gas phase temperature rises gradually and (determine) EO when being stabilized in 82.0-82.5 ℃ according to concrete product purity.This moment valve-off 9, recycle pump 7 is out of service, the rectifying tower shut-down operation; At the bottom of tower, can obtain containing the product P of the trimethyl carbinol 95～99%.
After overhead condenser 3 feeds water coolant, connect heating power supply reboiler is heated, treat that cat head has the total reflux operation of the back of backflow, and control phegma temperature is 70-75 ℃.
Start recycle pump 7, make recirculated water be in recurrent state, and regulate the cooling water flow of water cooler 8, the Control Circulation water temp is 30-35 ℃, regulates the flow of recycle pump 7, makes absolute pressure remain on 2500～5000Pa; The azeotrope of tertiary butanol and water is after cat head is assembled, and water cooler (8) is with the liquid of trimethyl carbinol water cooling to 70～75 ℃.
When cat head gas phase temperature-stable during at 79.9 ℃, open valve 9, the phlegma separation of in entering membrane separation apparatus 4, further dewatering, per-meate side can obtain the trimethyl carbinol of water and trace, enters water tank 6 through water jet pump 5.
Aforesaid operations continues to that the cat head gas phase temperature rises gradually and (determine) EO when being stabilized in 82.0-82.5 ℃ according to concrete product purity.This moment valve-off 9, recycle pump 7 is out of service, the rectifying tower shut-down operation; At the bottom of tower, can obtain containing the product P of the trimethyl carbinol 95～99%.
Start recycle pump 7, make recirculated water be in recurrent state, and regulate the cooling water flow of water cooler 8, the Control Circulation water temp is 30-35 ℃, regulates the flow of recycle pump 7, makes absolute pressure remain on 2500～5000Pa; The azeotrope of tertiary butanol and water is after cat head is assembled, and water cooler 8 is with the liquid of trimethyl carbinol water cooling to 70～75 ℃.
When cat head gas phase temperature-stable during at 79.9 ℃, open valve 9, the phlegma separation of in entering membrane separation apparatus 4, further dewatering, per-meate side can obtain the trimethyl carbinol of water and trace, enters water tank 6 through water jet pump 5.
Aforesaid operations continues to that the cat head gas phase temperature rises gradually and (determine) EO when being stabilized in 82.0-82.5 ℃ according to concrete product purity.This moment valve-off 9, recycle pump 7 is out of service, the rectifying tower shut-down operation; At the bottom of tower, can obtain containing the product P of the trimethyl carbinol 95～99%.
Open valve (11) and emit high purity tert-butyl alcohol product in the tower still 2, open valve 12 and emit the water W that increases newly in the recirculated water storage tank 6, make liquid level get back to original position.
Claims (6)
1. the method for a separating tert-butanol-water is characterized in that described method steps is as follows:
1. putting valve 9-10 is closing condition, be that the tertiary butanol and water mixture of 11.76% (azeotropic composition) is put in the batch fractionating Tata still (2) with the water content mass percent, and carry out total reflux operation, and control phegma temperature (14) is 70-75 ℃;
2. start recycle pump (7), make recirculated water be in recurrent state, and regulate the cooling water flow of water cooler (8), Control Circulation water temp (15) is 30-35 ℃, regulates the flow of recycle pump (7), makes absolute pressure (16) remain on 2500～5000Pa;
3. when cat head gas phase temperature (13) is stabilized in 79.9 ℃, open valve (9), make the trimethyl carbinol infiltration of contained water of phegma and denier pass film, and vaporization enters water jet pump (5), be recycled water condensation and absorption;
4. aforesaid operations continues to that cat head gas phase temperature (13) rises gradually and (determine) EO when being stabilized in 82.0-82.5 ℃ according to concrete product purity.This moment valve-off (9), recycle pump (7) is out of service, the rectifying tower shut-down operation;
5. open valve (11) and emit high purity tert-butyl alcohol product in the tower still (2), open valve (12) and emit the water that increases newly in the recirculated water storage tank, make liquid level get back to original position.
2. according to the method for the described a kind of separating tert-butanol-water of claim 1, it is characterized in that: select water permeable membrane separator (4) for use, it is 700～7000Pa that water permeable membrane keep-ups pressure through side, the tertiary butanol and water azeotrope that condensation is got off, behind water permeable membrane separator (4), water sees through film, holds back side and obtains the spissated trimethyl carbinol.
3. the method for a kind of separating tert-butanol-water according to claim 1 is characterized in that: hold back the spissated trimethyl carbinol of side and be back in the rectifying tower (1).
4. the method for a kind of separating tert-butanol-water according to claim 1, it is characterized in that: described jet of water decompress osmosis gasification coupled total reflux batch distillation process can be a process of dehydration in batches, tertiary butanol and water is dehydration cycle in be made of the loop that constitutes rectifying tower (1), condenser (3), composite membrane assembly (4), recirculated water storage tank (6), water jet pump (5) and interchanger (8), drops to below the target value up to the concentration of water.
5. the method for a kind of separating tert-butanol-water according to claim 1 is characterized in that: described step rectifying tower condensate temperature is at 60～105 ℃, and seeing through wall pressure is 700～7500Pa.
6.. the method for a kind of separating tert-butanol-water according to claim 1 is characterized in that: described rectifying tower number of theoretical plate is the rectifying tower more than 20, and the cat head working pressure is 600～7000Pa.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2009100174178A CN101607870A (en) | 2009-07-24 | 2009-07-24 | A kind of method of separating tert-butanol-water |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
-
2009
- 2009-07-24 CN CNA2009100174178A patent/CN101607870A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
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Application publication date: 20091223 |