CN101284770A - Extraction and rectification separation method for alkali solution in butanone-water system - Google Patents
Extraction and rectification separation method for alkali solution in butanone-water system Download PDFInfo
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- CN101284770A CN101284770A CNA2008100254638A CN200810025463A CN101284770A CN 101284770 A CN101284770 A CN 101284770A CN A2008100254638 A CNA2008100254638 A CN A2008100254638A CN 200810025463 A CN200810025463 A CN 200810025463A CN 101284770 A CN101284770 A CN 101284770A
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Abstract
The invention relates to a composite extractive distillation and separation method for butanone-water system soluble alkali. The method comprises the following steps: butanone-water mixture is used as the raw material, potassium hydrate is dissolved in ethylene glycol to be used as the soluble alkali composite extraction solvent, and is added into an extractive distillation column with the raw material mixed liquor, and the extractive distillation operation is performed; after the separation, butanone with the purity being larger than or equal to 99.5 percent is at the column top, and soluble alkali composite extraction solvent and water are at the column bottom; the material at the column bottom is delivered to a solvent regenerating column, and the distillation and dehydration operation is performed to the material, the produced material from the column top is water, and the regenerated soluble alkali composite extraction solvent is at the column bottom, which is delivered back to the extractive distillation column to be circularly used. Compared with the traditional common distillation and the azeotropic distillation methods, because the novel soluble alkali composite extraction solvent is adopted, the method has the advantages that the dehydration effect is more obvious, the product purity is higher, the recovery ratio is higher, and the butanone product with the purity being larger than or equal to 99.5 percent can be obtained. The energy consumption is lower. Meanwhile, because the soluble alkali composite extraction solvent can be circularly used during the entire process, the production cost is lower, and no pollution to the environment is caused.
Description
Technical field
The present invention relates to the molten alkali composite extraction and rectification separation method of a kind of separation method of chemical industry, particularly a kind of butanone-aqueous systems.
Background technology
Butanone is an important chemical material, it is a kind of excellent property, low boiling point organic solvent satisfactory for result, be widely used in industries such as oil refining, dyestuff, coating, tackiness agent, medicine and lubricating oil dewaxing, electronic component, cleaning, and can be used for plant extraction and azeotropic distillation, Application Areas is very extensive, and countries in the world sharply increase its consumption in recent years.Produce in the purification process at butanone, water is main impurity, must separate and remove, but owing to dissolve each other in butanone and water low temperature lower section, form azeotrope during distillation again, brought difficulty for the separation of butanone-aqueous systems, the conventional distillation mode is difficult to obtain high purity butanone product.Therefore develop effective separating technology, not only help product purity and improve, more help cutting down the consumption of energy and the further Application and Development of butanone product.
Summary of the invention
The molten alkali composite extraction and rectification separation method that the purpose of this invention is to provide a kind of butanone-aqueous systems is to overcome the isolating difficulty of butanone-aqueous systems in the prior art.Compare with traditional technology, the novel method processing step is fairly simple, constant product quality, and energy consumption reduces, and stock liquid can once obtain the butanone more than 99.5% behind molten alkali composite extraction and rectification, and simultaneously molten alkali compound extracting solvent cycle is utilized.
The technical scheme of finishing the foregoing invention task is: a kind of molten alkali composite extraction and rectification separation method of butanone-aqueous systems is characterized in that step is as follows:
With butanone-water mixture is raw material (containing 90% butanone, 10% water), and dissolving in ethylene glycol with potassium hydroxide is molten alkali compound extracting solvent, and itself and raw material mixed solution are added extractive distillation column with certain proportioning, carries out the extracting rectifying operation;
After the separation, cat head is high purity butanone (〉=99.5%), and the tower still is molten alkali compound extracting solvent+water;
Tower still material is sent into solvent regeneration tower and is carried out the distillation dehydration operation, and the cat head production is a water, and the tower still is the molten alkali compound extracting solvent after regenerating;
The compound extracting solvent is sent extractive distillation column back to and is recycled.
Described compound extracting solvent with the ratio of the mass rate of raw material is: 2.5/1～5/1, and wherein, optimum proportion is 3/1.
The technical process of sepn process is seen shown in Figure 1, and separating apparatus adopt to optimize that processing condition see Table 1, shown in the table 2, can obtain the high purity butanone after the separation.
Dissolve in the molten alkali compound extracting solvent that ethylene glycol forms with potassium hydroxide, have following reversible reaction to exist:
Promptly in the extracting rectifying process, ethylene glycol potassium can react with the water in the separated system, thereby make ethanol-water system obtain more effective separation, and the water of reaction can be removed in follow-up solvent reclamation process with it, do not influence recycling of solvent, be equivalent to ethylene glycol potassium the water in the system is constantly carried, and itself does not change, only play the carrier function of migration moisture, thereby make dehydrating effect more obvious.
Advantage of the present invention: adopt technical process shown in Figure 1 and optimized parameters, raw material is butanone-water mixture (containing 90% butanone, 10% water), dissolving in ethylene glycol with potassium hydroxide is molten alkali compound extracting solvent, at first carry out the extracting rectifying operation through extractive distillation column T1, overhead product is the butanone of purity 〉=99.5%, tower kettle product carries out distillation dehydration through solvent regeneration tower T2 to be handled, molten alkali compound extracting solvent is recycled, by the operation of two towers, can obtain the butanone product of purity 〉=99.5%.Compare with common distillation, Azotropic distillation method that routine is used, owing to adopt novel molten alkali compound extracting solvent, dehydrating effect is more obvious, and product purity is higher, and the rate of recovery is higher, and energy consumption is lower.
Simultaneously, because the molten alkali compound extracting of whole process solvent can be recycled, production cost is lower, and can not throw into question to environment.
Description of drawings
Fig. 1 is the technical process of extracting rectifying and solvent reclamation.
Embodiment
Embodiment 1, molten alkali composite extraction and rectification separates the method for butanone and water, with reference to processing parameter shown in technical process shown in Figure 1 and the table 1,1. raw material is the mixed solution of butanone and water, wherein the mass content of butanone and water is respectively 90%, 10%, flow is 5Kg/h, solvent is 9. for dissolving in the molten alkali compound extracting solvent (wherein potassium hydroxide content is the 0.06Kg/Kg solvent) that ethylene glycol forms with potassium hydroxide, flow is 15Kg/h, extractive distillation column T1 tower top temperature is 78-79 ℃, and tower still temperature is 140-150 ℃, and control of reflux ratio is 4～8, cat head production 3. flow is 4.5Kg/h, consists of x
Butanone=0.9961, x
Water=0.0039, tower still discharging 4. flow is 15.5Kg/h, consists of x
Solvent=0.9677, x
Butanone=0.0012, x
Water=0.0311, this part discharging is the charging of solvent regeneration tower T2 simultaneously, and solvent regeneration tower T2 tower top temperature is 99-100 ℃, and tower still temperature is about 180 ℃, and control of reflux ratio is 4～8, and cat head production 7. flow is 0.5Kg/h, consists of x
Butanone=0.0359, x
Water=0.9641, tower still discharging 9. flow is 20Kg/h, and wherein molten alkali compound extracting solvent quality content 〉=99.8% can recycle.1,3 is condenser among the figure, and 2,4 is reboiler.1.-9. be stream burst title (table 2).
Each tower process condition of table 1
| Processing parameter | The T-1 tower | The T-2 tower |
| Theoretical plate number | 50 | 40 |
| The raw material feed entrance point | 10 | 15 |
| The solvent feed position | 35 | |
| Reflux ratio | 4～8 | 4～8 |
| Tower top temperature (℃) | 78～79 | 99～100 |
| Tower still temperature (℃) | 140～150 | 180 |
Burst explanation of table 2 stream
Embodiment 2, and is substantially the same manner as Example 1, but extraction solvent and raw materials quality throughput ratio are: 2.5/1.
Embodiment 3, and is substantially the same manner as Example 1, but extraction solvent and raw materials quality throughput ratio are: 5/1.
Embodiment 4, and is substantially the same manner as Example 1, but extraction solvent and raw materials quality throughput ratio are: 3/1.
Claims (4)
1, a kind of molten alkali composite extraction and rectification separation method of butanone-aqueous systems is characterized in that step is as follows,
With butanone-water mixture is raw material, and dissolving in ethylene glycol with potassium hydroxide is molten alkali compound extracting solvent, and itself and raw material mixed solution are added extractive distillation column with certain proportioning, carries out the extracting rectifying operation;
After the separation, cat head is the butanone of purity 〉=99.5%, and the tower still is molten alkali compound extracting solvent+water;
Tower still material is sent into solvent regeneration tower and is carried out the distillation dehydration operation, and the cat head production is a water, and the tower still is the molten alkali compound extracting solvent after regenerating;
The compound extracting solvent is sent extractive distillation column back to and is recycled.
2, the molten alkali composite extraction and rectification separation method of butanone-aqueous systems according to claim 1 is characterized in that, described compound extracting solvent with the ratio of the mass rate of raw material is: 2.5/1～5/1.
3, the molten alkali composite extraction and rectification separation method of butanone-aqueous systems according to claim 1 and 2 is characterized in that, described compound extracting solvent with the ratio of the mass rate of raw material is: 3/1.
4, the molten alkali composite extraction and rectification separation method of butanone-aqueous systems according to claim 3 is characterized in that the processing condition of described each tower are shown in following form:
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| CN2008100254638A CN101284770B (en) | 2008-07-01 | 2008-07-01 | Extraction and rectification separation method for alkali solution in butanone-water system |
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| CN2008100254638A CN101284770B (en) | 2008-07-01 | 2008-07-01 | Extraction and rectification separation method for alkali solution in butanone-water system |
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| CN101284770A true CN101284770A (en) | 2008-10-15 |
| CN101284770B CN101284770B (en) | 2011-03-30 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641700A (en) * | 2013-11-22 | 2014-03-19 | 天津大学 | Method for separating butanone-water azeotrope through extraction distillation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103641700A (en) * | 2013-11-22 | 2014-03-19 | 天津大学 | Method for separating butanone-water azeotrope through extraction distillation |
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