CN1760165A - Method for separating tertiary butyl alcohol from water through azeotropy rectification in non-homogeneous phase - Google Patents
Method for separating tertiary butyl alcohol from water through azeotropy rectification in non-homogeneous phase Download PDFInfo
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- CN1760165A CN1760165A CN 200510016030 CN200510016030A CN1760165A CN 1760165 A CN1760165 A CN 1760165A CN 200510016030 CN200510016030 CN 200510016030 CN 200510016030 A CN200510016030 A CN 200510016030A CN 1760165 A CN1760165 A CN 1760165A
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- trimethyl carbinol
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Abstract
A process for separating tert-butanol from water by heterogeneous azeotropic rectifying in a rectifying system including rectifying tower includes such steps as proportionally adding the mixture of tert-butanol and water and the cyclohexane to rectifying tower, full reflux at 60-80 deg.C, tapping water from phase separator, tapping three-element azeotrope at particular temp, collecting it in phase separator, tapping cyclohexane and tert-butanol from upper layer of phase separator, tapping the mixture of cyclohexane-water and less cyclohexane-tert-butanol from tower top at another particular temp, and tapping high-purity (98.2 Wt%) tert-butanol from tower top at 82-83 deg.C for tower top. Its advantage is high output rate of tert-butanol.
Description
Technical field
The present invention relates to a kind of heterogeneous azeotropic rectification separating tert-butanol and water method, belong to the trimethyl carbinol and water separation technology.
Technical background
The trimethyl carbinol (TBA) has another name called trimethyl carbinol, and normal temperature for colourless crystallization or transparent liquid, has the camphor smell, 82.5 ℃ of boiling points, tool water absorbability down.The trimethyl carbinol dissolves in most of organic solvents, as alcohol, ester, ether, aliphatic hydrocarbon, arene.These character make the trimethyl carbinol become useful solvent and additive, can be used as the solubilizing agent of paraffin remover, methylated spirits, are used for the stabilized chlorine hydro carbons.Hydroxyl on the trimethyl carbinol molecule is easy to be substituted and generates tertiary butyl halogenide or superoxide, makes the trimethyl carbinol become important alkylating agent, is particularly useful for aromatic hydrocarbon and phenols, can produce multiple fine chemicals, as medicine, agricultural chemicals and various auxiliary agent.The trimethyl carbinol can be miscible and form constant boiling mixture (massfraction of water is 11.76%) by arbitrary proportion with water, can't obtain high purity tert-butyl alcohol with common rectificating method.
Separating tert-butanol---the main method of water has azeotropic distillation at present, extracting rectifying, and adsorptive distillation, salting-out process and pervaporation method, large-scale application is azeotropic distillation and extracting rectifying in industry.US4239926 has at first studied the process for purification of the trimethyl carbinol, produces in the process of the trimethyl carbinol in oxidation of isobutane, and trimethyl carbinol product contains acetone, water and other high-boiling-point impurity.He 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 trimethyl carbinol-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.CN1621399 employing alcohol or alcohol and salt or alkaline mixture carry out extracting rectifying as extraction agent, obtain crossing over the trimethyl carbinol that azeotropic is formed, for the further purification of the follow-up trimethyl carbinol lays the foundation, make the anhydrous tertiary butanol that is not contained impurity such as dipolymer become possibility.The industrial trimethyl carbinol of forming near azeotropic for water content adopts the ternary azeotropic compositions of forming with benzene to carry out the azeotropic distillation dehydration usually, but the toxicity of benzene is bigger, long-term work in the bigger environment of benzene vapour concentration can work the mischief to the healthy of people, various countries have avoided using benzene now, seek new substitute and put forth effort on.
Summary of the invention
The purpose of this invention is to provide the method for a kind of heterogeneous azeotropic rectification separating tert-butanol and water, the consumption of this method entrainer is few, has saved energy consumption.
The present invention is realized by the following technical programs: the method for a kind of heterogeneous azeotropic rectification separating tert-butanol and water, this method adopts by rectifying tower, condenser, the rectifier unit that phase splitter and product storage tank constitute, realize heterogeneous azeotropic rectification separating tert-butanol and water, it is characterized in that comprising following process: the azeotrope of under the normal pressure trimethyl carbinol and water being formed or the trimethyl carbinol and the water composition mixture formed near azeotropic, mass ratio by azeotrope or mixture and entrainer hexanaphthene is 0.3～1.5, together adding number of theoretical plate is in the tower still of 30～50 rectifying tower, being 60-80 ℃ in tower still temperature carried out total reflux operation 0.5-2 hour, behind the total reflux end of processing, the water of enrichment will be in time from phase splitter bottom extraction in the cat head phase splitter, when tower top temperature at 64～83 ℃, tower still temperature is at 70～87 ℃, with reflux ratio is 1～5, be collected in the phase splitter from the tertiary butanol and water-hexanaphthene ternary azeotrope of cat head extraction, standing demix, wherein the hexanaphthene on phase splitter upper strata and the extraction of trimethyl carbinol organic phase continue to use in next batch azeotropic distillation process in another storage tank.Again with reflux ratio 1-4, behind the mixture by cat head extraction hexanaphthene-water and a small amount of hexanaphthene-trimethyl carbinol under tower top temperature 62-82 ℃,, obtain the trimethyl carbinol product that purity is 98.2wt% from cat head under tower top temperature 82-83 ℃ 82-88 ℃ of tower still.
Method of the present invention is applicable to azeotrope that the trimethyl carbinol and water are formed or the mixture of forming near azeotropic.
Advantage of the present invention is: adopt hexanaphthene to substitute benzene, strengthened the security of operating process, and the price of hexanaphthene and benzene and performance are approaching, need not carry out scrap build.Adopted new-type condenser, just can the extraction portion water in the total reflux process, the water of participating in backflow is reduced, reduced the consumption of entrainer, increased a yield of the trimethyl carbinol, improved economic benefit.
Description of drawings
Fig. 1 is apparatus of the present invention synoptic diagram.
Wherein 1 is the rectifying tower body of the tower, and 2 is thermal insulation layer, and 3 are rectifying Tata still, and 4 is heating jacket, and 5 is condenser, and 6 is phase splitter, and 7 is the product storage tank.
Embodiment
Experiment adopts the parameter of batch fractionating tower to be: effective packing section height 1.5m, king-post diameter 30mm, the efficient stainless steel θ ring filler of interior dress 3mm * 3mm; The tower still is the there-necked flask of 250ml, peg graft respectively tower body, thermometer and glass stopper; Reflux ratio is sampled at cat head with rly. and magnet control; The heating of tower still electricity consumption heating jacket, heating power 200W, body of the tower is incubated with the heat tracing band, and tower top is condensed to room temperature with tap water; The theoretical plate number of this tower is 45.Open opening for feed, add 60ml hexanaphthene and 120ml raw material (moisture 12.93wt%).Check everywhere whether good seal of interface, after overhead condenser feeds water coolant, connect heating power supply reboiler is heated, reach 75 ℃, keep total reflux 1.5h, in the total reflux process, the hydromining in the phase splitter should be gone out in tower still temperature.When tower top temperature at 65-80 ℃, regulate reflux ratio controller, be 3 the speed extraction hexanaphthene-water and the mixture cut of a small amount of hexanaphthene-trimethyl carbinol with reflux ratio.Reached before 82 ℃ in tower top temperature, the product of extraction should be collected in the another one product collector, standing demix, and hexanaphthene wherein and trimethyl carbinol organic phase can continue to use in the tertiary butanol and water azeotropic distillation process of next batch.The final trimethyl carbinol product that is obtained by the tower still is a colourless transparent liquid, and t butanol content is 98.2wt%, and one time yield is 52%.
Claims (1)
1. the method for heterogeneous azeotropic rectification separating tert-butanol and water, this method adopts by rectifying tower, condenser, the rectifier unit that phase splitter and product storage tank constitute, realize heterogeneous azeotropic rectification separating tert-butanol and water, it is characterized in that comprising following process: the azeotrope of under the normal pressure trimethyl carbinol and water being formed or the trimethyl carbinol and the water composition mixture formed near azeotropic, mass ratio by azeotrope or mixture and entrainer cyclohexane is 0.3～1.5, together add number of theoretical plate and be in the tower still of 30～50 rectifying tower, being 60-80 ℃ in tower still temperature carried out total reflux operation 0.5-2 hour, behind the total reflux end of processing, the water of enrichment will be in time from phase splitter bottom extraction in the cat head phase splitter, when tower top temperature at 64～83 ℃, tower still temperature is at 70～87 ℃, with reflux ratio is 1～5, be collected in the phase splitter from the tertiary butanol and water-hexanaphthene ternary azeotrope of cat head extraction, standing demix, wherein the hexanaphthene on phase splitter upper strata and the extraction of trimethyl carbinol organic phase are in another storage tank, in next batch azeotropic distillation process, continue to use, again with reflux ratio 1-4, behind the mixture by cat head extraction hexanaphthene-water and a small amount of hexanaphthene-trimethyl carbinol under tower top temperature 62-82 ℃, 82-88 ℃ of tower still, obtain the trimethyl carbinol product that purity is 98.2wt% from cat head under tower top temperature 82-83 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510016030 CN1760165A (en) | 2005-11-11 | 2005-11-11 | Method for separating tertiary butyl alcohol from water through azeotropy rectification in non-homogeneous phase |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510016030 CN1760165A (en) | 2005-11-11 | 2005-11-11 | Method for separating tertiary butyl alcohol from water through azeotropy rectification in non-homogeneous phase |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101596371B (en) * | 2009-06-29 | 2011-04-06 | 天津大学 | Device for purifying formic acid solution with interval azeotropic distillation and method thereof |
| CN102935294A (en) * | 2012-11-12 | 2013-02-20 | 南京蓝星化工新材料有限公司 | Continuous still standing separation and purification device and method for butanol and water mixed liquor |
| CN106823437A (en) * | 2017-03-31 | 2017-06-13 | 江苏华益科技有限公司 | One kind is saltoutd rectifying coupled method dewatering and device |
| CN110035988A (en) * | 2016-12-02 | 2019-07-19 | 霍尼韦尔国际公司 | Method for drying HCFO-1233ZD |
| CN110937980A (en) * | 2019-12-20 | 2020-03-31 | 江苏天泽新材料有限公司 | Continuous production process of potassium tert-butoxide |
| CN111039757A (en) * | 2019-12-20 | 2020-04-21 | 江苏天泽新材料有限公司 | High-purity tert-butyl alcohol on-line recovery process for continuously producing potassium tert-butoxide |
-
2005
- 2005-11-11 CN CN 200510016030 patent/CN1760165A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101596371B (en) * | 2009-06-29 | 2011-04-06 | 天津大学 | Device for purifying formic acid solution with interval azeotropic distillation and method thereof |
| CN102935294A (en) * | 2012-11-12 | 2013-02-20 | 南京蓝星化工新材料有限公司 | Continuous still standing separation and purification device and method for butanol and water mixed liquor |
| CN102935294B (en) * | 2012-11-12 | 2014-09-03 | 南京蓝星化工新材料有限公司 | Continuous still standing separation and purification device and method for butanol and water mixed liquor |
| CN110035988A (en) * | 2016-12-02 | 2019-07-19 | 霍尼韦尔国际公司 | Method for drying HCFO-1233ZD |
| CN106823437A (en) * | 2017-03-31 | 2017-06-13 | 江苏华益科技有限公司 | One kind is saltoutd rectifying coupled method dewatering and device |
| CN110937980A (en) * | 2019-12-20 | 2020-03-31 | 江苏天泽新材料有限公司 | Continuous production process of potassium tert-butoxide |
| CN111039757A (en) * | 2019-12-20 | 2020-04-21 | 江苏天泽新材料有限公司 | High-purity tert-butyl alcohol on-line recovery process for continuously producing potassium tert-butoxide |
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