CN101492345A - Method for extractive distillation with salt of acetone and methanol - Google Patents
Method for extractive distillation with salt of acetone and methanol Download PDFInfo
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- CN101492345A CN101492345A CNA2008100329259A CN200810032925A CN101492345A CN 101492345 A CN101492345 A CN 101492345A CN A2008100329259 A CNA2008100329259 A CN A2008100329259A CN 200810032925 A CN200810032925 A CN 200810032925A CN 101492345 A CN101492345 A CN 101492345A
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Abstract
The invention relates to a method for separating acetone from methanol by extractive rectification with salt. The method mainly solves the technical problem in the prior art that the separation is difficult during the process of separating an acetone-methanol azeotrope. The invention solves the problem well by the technical proposal which comprises the steps as follows: solvent containing salt and the acetone-methanol azeotrope are respectively put into the upper part and the middle part of an extractive distillation column for the extractive rectification with salt; pure acetone is extracted from the top of the column; and a mixture of the methanol, the salt and the solvent is obtained at the bottom of the column; the mixture of the methanol, the salt and the solvent is put into a solvent recovery tower; distillate at the top of the tower is pure acetic acid; and the solvent containing the salt is obtained at the bottom of the tower. The invention can be used in the industrial application for recycling the acetone and the methanol.
Description
Technical field
The present invention relates to the method for a kind of extractive distillation with salt of acetone and methyl alcohol.
Background technology
Along with based on the increase of the liquid fuel demand of oil and the minimizing of petroleum resources usable reserves, the method for being produced the available liquid fuel by solid fuels such as coals more and more is subject to people's attention.Solid-fuelled liquefaction has two kinds of different technological lines, and a kind of is direct liquefaction, and a kind of is indirect liquefaction.Direct liquefaction is under High Temperature High Pressure, solid fuels such as coal is converted into the technology of liquefaction oil under the effect of solvent and catalyzer.Direct liquefaction operational condition harshness is strong to the dependency of raw material.Indirect liquefaction is that the Fischer-Tropsch of common indication is synthetic, be at iron-based, bore under the condition of base or the catalyst based existence of anvil, the synthetic gas that comprises carbon monoxide and hydrogen that will produce by solid fuels such as coals, under certain temperature and pressure, the technology of directional catalyzing synthin fuel and industrial chemicals.Indirect liquefaction is strong to the suitability of raw material, and range of product is many, institute's produce oil product quality height.
Fischer-Tropsch synthetic raw material is the synthetic gas based on carbon monoxide and hydrogen, and synthetic gas is to be obtained by solid fuel gasifications such as coals.Need before the solid fuel gasification to mix to roll with water earlier to make slurry.Mainly be carbon monoxide and hydrogen generate methane and higher carbon number under the catalyst based effect of iron-based, brill base or anvil hydro carbons in the fischer-tropsch reaction process, generate alcohol, other hydrocarbon oxide and reaction water simultaneously.
Reaction water can be separated easily with Fischer-Tropsch synthetic principal product hydrocarbon, but because hydrocarbon oxides such as alcohol have certain solubleness in water, so isolated reaction water contains organic oxygen-containing compounds such as certain alcohol, aldehyde, ketone and acid from Fischer-Tropsch synthetic.The amount of reaction water is bigger, it emitted, and obviously be uneconomic, be necessary its separation, obtain each organic oxygen-containing compound product.Wherein separate one of difficult point and be exactly the separating of acetone and methyl alcohol, methyl alcohol (64.7 ℃ of boiling points) and acetone (56.29 ℃ of boiling points) can form azeotrope, and azeotropic consists of and contains acetone 88wt%, and azeotropic temperature is 55.5 ℃, can not isolate pure component with conventional distillation.
Introduced the method for extracting rectifying separation of methanol and acetone in 3291～3033 pages of periodical Separation Science and Technology 2002 the 14th phases, this paper studies the isolating operational condition of water as solvent extracting rectifying.Provided the degree of aqueous solvent to methyl alcohol and the change of acetone relative volatility in the literary composition, the relative volatility of methyl alcohol and acetone is less during extracting rectifying, needs more number of theoretical plate to separate fully.
Summary of the invention
Technical problem to be solved by this invention is the problem that has separation difficulty in the sepn process of methyl alcohol and acetone azeotrope, and a kind of new extractive distillation with salt of acetone and the method for methyl alcohol are provided.This method has the high characteristics of separation efficiency.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: the method for a kind of extractive distillation with salt of acetone and methyl alcohol, may further comprise the steps: a) contain top, the middle part that salt solvent, acetone and methanol azeotrope enter extractive distillation column respectively and carry out extractive distillation with salt, cat head extraction pure acetone, the tower still obtains the mixture stream passes I of methyl alcohol, salt, solvent, wherein solvent is selected from least a in the polar solvent, salt is selected from least a in halide salt, acetate or the nitrate, and the content of salt is 3～20% in the solvent; B) stream I enters solvent recovery tower, and overhead distillate is a methyl alcohol, and the tower still obtains containing salt solvent.
In technique scheme, the theoretical plate number preferable range of extractive distillation column is 15～40, and the solvent ratio preferable range is 0.5～3, and the reflux ratio preferable range is 0.2～4, and control tower top temperature preferable range is 56～56.5 ℃; The theoretical plate number preferable range of solvent recovery tower is 10～50, and the reflux ratio preferable range is 0.3～6, and control tower top temperature preferable range is 64.5～65 ℃; Solvent is at least a in water, ethylene glycol preferably; Salt in the solvent is at least a in Repone K, Potassium ethanoate or saltpetre preferably; The mass percent preferable range of salt is 5～10% in the solvent.
Because acetone and methyl alcohol form azeotrope, adopt the method for conventional distillation can't obtain pure separately product, must adopt senior rectificating method could separate them.Extractive distillation with salt is to grow up on the basis of analysis-by-synthesis extracting rectifying and dissolved salt rectifying relative merits.Utilize the effective advantage of dissolved salt extraction agent, improve the shortcoming of extraction distillation solvent weak effect, utilizing extraction distillation solvent is that the liquids recovery circulation is convenient, the industrial advantage that is easy to realize, and salt is shortcomings such as Solid Conveying and Melting difficulty when overcoming dissolved salt rectifying.
Since solvent with salt after the relative volatility of acetone and methyl alcohol increase greatlyyer than simple solvent-applied, improved separating effect greatly, thereby made number of theoretical plate, solvent ratio and the reflux ratio of extractive distillation column reduce.The present invention has reached the purpose that improves separation efficiency by adopting the scheme of extractive distillation with salt, has obtained better technical effect.
Description of drawings
Fig. 1 is the process flow diagram of extractive distillation with salt of acetone and methyl alcohol.
1 is extractive distillation column among Fig. 1, and 2 is solvent recovery tower, and 3 for containing salt solvent, and 4 is acetone and carbinol mixture, and 5 is acetone, and 6 is the mixture of methyl alcohol, salt, solvent, and 7 is methyl alcohol, and 8 for containing salt solvent.
By flow process shown in Figure 1, add salt solvent 3, acetone and carbinol mixture 4 respectively from the top of extractive distillation column 1, The middle part enters, and overhead distillate is acetone 5, and tower reactor obtains the mixture 6 of methyl alcohol, salt, solvent, methyl alcohol, salt, solvent Mixture 6 enter solvent recovery tower 2, overhead distillate is methyl alcohol 7, tower reactor obtains containing salt solvent 8.
The present invention is further illustrated below by specific embodiment, and still, scope of the present invention has more than and is limited to enforcement The scope that example covers.
Embodiment
[embodiment 1]
The theoretical plate number of extractive distillation column is 15 (stage number is counted from top to bottom), select for use the ethylene glycol (massfraction 20% of ethylene glycol) that contains lithium chloride for adding salt solvent, add from the 3rd theoretical stage, flow is 30 gram/minute, acetone and carbinol mixture add from the 8th block of theoretical tray, the massfraction of acetone is 85%, and the massfraction 15% of methyl alcohol, flow are 10 gram/minute.Extractive distillation column trim the top of column ratio is 0.2, and tower top temperature is controlled at 56～56.5 ℃, analyzes overhead product, and the massfraction of acetone is 99.95%, and the massfraction of methyl alcohol is 0.05%.The discharging of extracting rectifying Tata still is that methyl alcohol, salt, solvent mixture enter solvent recovery tower, solvent recovery tower has 10 blocks of theoretical trays, feed entrance point is the 5th a block of theoretical tray, the trim the top of column ratio is 6, and tower top temperature is controlled at 64.5～65 ℃, behind the stable operation, analyze overhead distillate, the massfraction of methyl alcohol is 99.93%, and the mass percent of ethylene glycol is 0.07%, the tower still obtain containing the methanol quality mark be 0.02% with the salt ethylene glycol solution.
[embodiment 2]
The theoretical plate number of extractive distillation column is 40 (stage number is counted from top to bottom), select for use the aqueous solution (massfraction 3% of sodium-acetate) that contains sodium-acetate for adding salt solvent, add from the 6th theoretical stage, flow is 5 gram/minute, acetone and carbinol mixture add from the 20th block of theoretical tray, the massfraction of acetone is 85%, and the massfraction 15% of methyl alcohol, flow are 10 gram/minute.Extractive distillation column trim the top of column ratio is 4, and tower top temperature is controlled at 56～56.5 ℃, analyzes overhead product, and the massfraction of acetone is 99.97%, and the massfraction of methyl alcohol is 0.03%.The discharging of extracting rectifying Tata still is that methyl alcohol, salt, solvent mixture enter solvent recovery tower, solvent recovery tower has 50 blocks of theoretical trays, feed entrance point is the 30th a block of theoretical tray, the trim the top of column ratio is 0.3, and tower top temperature is controlled at 64.5～65 ℃, behind the stable operation, analyze overhead distillate, the massfraction of methyl alcohol is 99.96%, and the mass percent of water is 0.04%, and it is 0.01% the salt brine solution that adds that the tower still obtains containing the methanol quality mark.
[embodiment 3]
The theoretical plate number of extractive distillation column is 25 (stage number is counted from top to bottom), select for use the aqueous solution (massfraction 5% of sodium-acetate) that contains saltpetre for adding salt solvent, add from the 5th theoretical stage, flow is 15 gram/minute, acetone and carbinol mixture add from the 12nd block of theoretical tray, the massfraction of acetone is 85%, and the massfraction 15% of methyl alcohol, flow are 10 gram/minute.Extractive distillation column trim the top of column ratio is 2, and tower top temperature is controlled at 56～56.5 ℃, analyzes overhead product, and the massfraction of acetone is 99.94%, and the massfraction of methyl alcohol is 0.06%.The discharging of extracting rectifying Tata still is that methyl alcohol, salt, solvent mixture enter solvent recovery tower, solvent recovery tower has 30 blocks of theoretical trays, feed entrance point is the 20th a block of theoretical tray, the trim the top of column ratio is 3, and tower top temperature is controlled at 64.5～65 ℃, behind the stable operation, analyze overhead distillate, the massfraction of methyl alcohol is 99.95%, and the mass percent of water is 0.05%, and it is 0.02% the salt brine solution that adds that the tower still obtains containing the methanol quality mark.
[comparative example 1]
The theoretical plate number of extractive distillation column is 40 (stage number is counted from top to bottom), aqueous solvent adds from the 6th theoretical stage, flow is 40 gram/minute, acetone and carbinol mixture add from the 20th block of theoretical tray, the massfraction of acetone is 85%, the massfraction 15% of methyl alcohol, flow are 10 gram/minute.Extractive distillation column trim the top of column ratio is 3, and tower top temperature is controlled at 56.5～57 ℃, analyzes overhead product, and the massfraction of acetone is 99.5%, and the massfraction of methyl alcohol is 0.5%.The discharging of extracting rectifying Tata still is that the methanol aqueous solution that contains small amount of acetone enters solvent recovery tower, solvent recovery tower has 50 blocks of theoretical trays, feed entrance point is the 30th a block of theoretical tray, and the trim the top of column ratio is 0.3, and tower top temperature is controlled at 63.5～64.5 ℃, behind the stable operation, analyze overhead distillate, the massfraction of methyl alcohol is 99.36%, and the massfraction of acetone is 0.6%, the mass percent of water is 0.04%, and it is 0.02% the aqueous solution that the tower still obtains containing the methanol quality mark.
[comparative example 2]
The theoretical plate number of extractive distillation column is 40 (stage number is counted from top to bottom), solvent ethylene glycol adds from the 3rd theoretical stage, flow is 40 gram/minute, acetone and carbinol mixture add from the 20th block of theoretical tray, the massfraction of acetone is 85%, the massfraction 15% of methyl alcohol, flow are 10 gram/minute.Extractive distillation column trim the top of column ratio is 3, and tower top temperature is controlled at 56.5～57 ℃, analyzes overhead product, and the massfraction of acetone is 99.2%, and the massfraction of methyl alcohol is 0.8%.The discharging of extracting rectifying Tata still is that the methyl alcohol ethylene glycol solution that contains small amount of acetone enters solvent recovery tower, solvent recovery tower has 30 blocks of theoretical trays, feed entrance point is the 20th a block of theoretical tray, and the trim the top of column ratio is 1.5, and tower top temperature is controlled at 63.5～64.5 ℃, behind the stable operation, analyze overhead distillate, the massfraction of methyl alcohol is 98.98%, and the massfraction of acetone is 1.0%, the mass percent of ethylene glycol is 0.02%, and it is 0.01% the aqueous solution that the tower still obtains containing the methanol quality mark.
Claims (6)
1, the method for a kind of extractive distillation with salt of acetone and methyl alcohol may further comprise the steps successively:
A, contain top, the middle part that salt solvent, acetone and methanol azeotrope enter extractive distillation column respectively and carry out extractive distillation with salt, cat head extraction pure acetone, the tower still obtains the mixture stream passes I of methyl alcohol, salt, solvent, wherein solvent is selected from least a in the polar solvent, salt is selected from least a in halide salt, acetate or the nitrate, and the content of salt is 3～20% in the solvent;
B, stream I enter solvent recovery tower, and overhead distillate is a methyl alcohol, and the tower still obtains containing salt solvent.
2, according to the method for right 1 described extractive distillation with salt of acetone and methyl alcohol, the theoretical plate number that it is characterized in that extractive distillation column is 15～40, and solvent ratio is 0.5～3, and reflux ratio is 0.2～4,56～56.5 ℃ of control tower top temperatures.
3, according to the method for right 1 described extractive distillation with salt of acetone and methyl alcohol, the theoretical plate number that it is characterized in that solvent recovery tower is 10～50, and reflux ratio is 0.3～6,64.5～65 ℃ of control tower top temperatures.
4,, it is characterized in that solvent is selected from least a in water, the ethylene glycol according to the method for right 1 described extractive distillation with salt of acetone and methyl alcohol.
5,, it is characterized in that salt in the solvent is selected from least a in Repone K, Potassium ethanoate or the saltpetre according to the method for right 1 described extractive distillation with salt of acetone and methyl alcohol.
6, according to the method for right 1 described extractive distillation with salt of acetone and methyl alcohol, the mass percent that it is characterized in that salt in the solvent is 5～10%.
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| CN2008100329259A CN101492345B (en) | 2008-01-23 | 2008-01-23 | Method for extractive distillation with salt for separating acetone and methanol |
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| CN2008100329259A CN101492345B (en) | 2008-01-23 | 2008-01-23 | Method for extractive distillation with salt for separating acetone and methanol |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914001A (en) * | 2010-08-05 | 2010-12-15 | 南京师范大学 | Method for extracting acetone from acetone-dichloromethane-methanol-water mixed liquor by azeotropy and composite extraction reditification integration and equipment thereof |
| CN102190557A (en) * | 2011-03-25 | 2011-09-21 | 吉林大学 | Composite extractant for separating azeotrope of acetone methanol azeotrope and use method thereof |
| CN102190558A (en) * | 2011-04-01 | 2011-09-21 | 扬州市丽邦化工有限公司 | Method for separating acetone and methanol mixture |
| CN102816178A (en) * | 2012-09-14 | 2012-12-12 | 南通鸿志化工有限公司 | Method and special device for separating trimethyl borate from carbinol mixture |
| CN104387231A (en) * | 2014-11-25 | 2015-03-04 | 沈阳化工大学 | Device for separating acetone-methanol by using two-step extractive distillation and method thereof |
| CN107445817A (en) * | 2017-08-14 | 2017-12-08 | 青岛科技大学 | A kind of method with ion liquid abstraction rectifying acetone and methanol |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4620901A (en) * | 1985-11-04 | 1986-11-04 | Lloyd Berg | Separation of acetone from methanol by extractive distillation |
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2008
- 2008-01-23 CN CN2008100329259A patent/CN101492345B/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914001A (en) * | 2010-08-05 | 2010-12-15 | 南京师范大学 | Method for extracting acetone from acetone-dichloromethane-methanol-water mixed liquor by azeotropy and composite extraction reditification integration and equipment thereof |
| CN101914001B (en) * | 2010-08-05 | 2013-02-13 | 南京师范大学 | Method for extracting acetone from acetone-dichloromethane-methanol-water mixed liquor by azeotropy and composite extraction reditification integration and equipment thereof |
| CN102190557A (en) * | 2011-03-25 | 2011-09-21 | 吉林大学 | Composite extractant for separating azeotrope of acetone methanol azeotrope and use method thereof |
| CN102190557B (en) * | 2011-03-25 | 2014-01-01 | 吉林大学 | Composite extractant for separating azeotrope of acetone methanol azeotrope and use method thereof |
| CN102190558A (en) * | 2011-04-01 | 2011-09-21 | 扬州市丽邦化工有限公司 | Method for separating acetone and methanol mixture |
| CN102816178A (en) * | 2012-09-14 | 2012-12-12 | 南通鸿志化工有限公司 | Method and special device for separating trimethyl borate from carbinol mixture |
| CN102816178B (en) * | 2012-09-14 | 2015-10-28 | 南通鸿志化工有限公司 | A kind of method and special purpose device thereof being separated trimethyl borate and carbinol mixture |
| CN104387231A (en) * | 2014-11-25 | 2015-03-04 | 沈阳化工大学 | Device for separating acetone-methanol by using two-step extractive distillation and method thereof |
| CN107445817A (en) * | 2017-08-14 | 2017-12-08 | 青岛科技大学 | A kind of method with ion liquid abstraction rectifying acetone and methanol |
| CN107445817B (en) * | 2017-08-14 | 2020-08-28 | 青岛科技大学 | Method for separating acetone and methanol by using ionic liquid extraction and rectification |
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