CN1621399A - Method for separating tert-butyl alcohol and water by extraction and rectification - Google Patents
Method for separating tert-butyl alcohol and water by extraction and rectification Download PDFInfo
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- CN1621399A CN1621399A CN 200310115075 CN200310115075A CN1621399A CN 1621399 A CN1621399 A CN 1621399A CN 200310115075 CN200310115075 CN 200310115075 CN 200310115075 A CN200310115075 A CN 200310115075A CN 1621399 A CN1621399 A CN 1621399A
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Abstract
The present invention relates to method of separating tert-butanol from water, and is especially extraction and rectification process of separating tert-butanol from water. The present invention adopts alcohol or the mixture of alcohol and salt or strong alkali as the extractant for extraction and rectification to obtain tert-butanol across azeotropic point, and this lays the foundation for further purifying tert-butanol and makes it possible to obtain anhydrous tert-butanol containing no dimer and other impurities.
Description
Technical field
The present invention relates to the method for a kind of separating tert-butanol and water, particularly adopt the method separating tert-butanol and the water of extracting rectifying.
Technical background
Anhydrous tertiary butanol (massfraction of the trimethyl carbinol is greater than 99.5%) is a kind of important Fine Organic Chemical product, uses very extensive.For example, be used for gasoline dope, to improve the octane value of gasoline; Be used for synthetic pesticide, weedicide, essence and methylated spirits etc.; The solvent and the thinner that are used for soluble cotton and synthetic resins; Be used for the important oxidation inhibitor of synthetic plastics industry and the intermediate of stablizer and soluble phenolic resin; Be used to make high-purity isobutylene etc.And in the production process of the trimethyl carbinol, because the trimethyl carbinol and water form azeotrope, therefore adopt the method for conventional distillation to be lower than and obtain the mixture (massfraction that is the trimethyl carbinol and water is respectively 88.2% and 11.8%) formed near azeotropic the trimethyl carbinol aqueous solution that azeotropic forms, can't produce high purity tert-butyl alcohol from concentration.Therefore how from azeotrope, the trimethyl carbinol further put forward the dense difficult problem that needs to be resolved hurrily that becomes.
" petrochemical complex ", nineteen eighty-two the 11st rolls up, and 404-409 has reported that a kind of method separation concentration of extractive distillation with salt that adopts is lower than the trimethyl carbinol aqueous solution that azeotropic is formed.Though adopt this method to obtain crossing over the trimethyl carbinol (massfraction is greater than 88.2%) that azeotropic is formed in the extracting rectifying column overhead, but owing to contain acidic substance in the salt that is added, cause the dehydration and the condensation reaction of the trimethyl carbinol easily, make in the trimethyl carbinol that obtains except that moisture, also contain the impurity such as dipolymer that chemical reaction generates.And the salt that the present invention added does not contain acidic substance, and initiating chamical reaction does not have impurity such as dipolymer in the trimethyl carbinol.Because the existence of impurity such as dipolymer, make the trimethyl carbinol that leap azeotropic that cat head obtains forms in the follow-up technology of producing anhydrous tertiary butanol, must make anhydrous tertiary butanol (remove water respectively, remove dipolymer) by a plurality of common rectifying towers, thereby make sepn process complicated.
Summary of the invention
The purpose of this invention is to provide a kind of extracting rectifying separating tert-butanol and water method, adopt alcohol or alcohol and salt or alkaline mixture to 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 present invention is the method for the refining trimethyl carbinol of a kind of extracting rectifying, the extracting rectifying process is the double-column process that comprises extractive distillation column and solvent recovery tower, it is characterized in that: adopt the mixture of A or A and B to carry out extracting rectifying, and the mass percent of B component in the mixture of A and B is 0-30% as extraction agent.
A is ethylene glycol, propylene glycol, butyleneglycol or glycerol, or the mixture of above-mentioned alcohol;
B is sodium-chlor, calcium chloride, nitrocalcite, sodium sulfate, yellow soda ash, Potassium ethanoate, potassiumiodide, sodium hydroxide or potassium hydroxide, or the mixture of above-mentioned substance.
The operational condition of extractive distillation column is a normal pressure, the extraction agent volumetric flow rate is 1.0-5.0 with the ratio of raw material volumetric flow rate, reflux ratio is 1.0-3.0, tower top temperature is controlled at 81.0-83.0 ℃, tower still temperature is controlled at 95.4-140.0 ℃, but cat head extraction massfraction is greater than 88.2% trimethyl carbinol product.
The tower still is the mixture that contains extraction agent, the trimethyl carbinol and water.The tower bottoms of extractive distillation column is introduced solvent recovery tower and is reclaimed, the operational condition of solvent recovery tower is normal pressure or decompression, and the scope of working pressure is absolute pressure 0.10-1atm, reflux ratio 0.5-5.0, tower top temperature is controlled at 40.0-100.0 ℃, and tower still temperature is controlled at 104.7-196.0 ℃.Tower still product returns extractive distillation column and recycles.
Method of the present invention does not have particular requirement to extractive distillation column and solvent recovery tower, and rectifying tower commonly used in the chemical process gets final product.The theoretical plate number of extractive distillation column usually should be more than 25, (stage number is many more to be preferably 25-50, separating effect is good more, but investment cost increases), the theoretical plate number of solvent recovery tower usually should be more than 20, be preferably 20-40 (stage number is many more, and separating effect is good more, but investment cost increases).
The raw material that method of the present invention is suitable for is the azeotrope of the trimethyl carbinol and water composition or the mixture of forming near azeotropic, and promptly the content of the trimethyl carbinol is usually about 85%.
The trimethyl carbinol that the present invention obtains can be produced anhydrous tertiary butanol by another conventional distillation.
The effect of invention: the present invention is directed to the tertiary butanol and water system, proposed a kind of method that adopts extracting rectifying separating tert-butanol and water, by selecting suitable extraction agent, thereby improve separating power significantly.As shown by the data in the table, relative volatility approaches 1 when not adding extraction agent, and when adding extraction agent, between the 1.28-2.63, thereby can cross over constant boiling point during relative volatility can improve.Because product of the present invention does not contain impurity such as dipolymer, subsequent technique only need adopt a common rectifying tower to remove water can produce anhydrous tertiary butanol.
Table: various extraction agents are to the separating power of the trimethyl carbinol and water
| Sequence number | Extraction agent | Proportioning | Relative volatility |
| ????1 | Do not have | ????- | ????1.014 |
| ????2 | Ethylene glycol | ????- | ????1.510 |
| ????3 | Ethylene glycol+sodium-chlor (NaCl) | Saturated (＜0.1g) NaCl/g ethylene glycol | ????1.774 |
| ????3 | Ethylene glycol+sodium-chlor (NaCl) | Saturated (＜0.1g) NaCl/g ethylene glycol | ????1.774 |
| ????4 | Ethylene glycol+calcium chloride (CaCl 2) | ????0.1g?CaCl 2/ g ethylene glycol | ????1.930 |
| ????5 | Ethylene glycol+yellow soda ash (NaCO 3) | Saturated (＜0.1g) NaCO 3/ g ethylene glycol | ????1.539 |
| ????6 | Ethylene glycol+Potassium ethanoate (KAc) | 0.1gKAc/g ethylene glycol | ????1.713 |
| ????7 | Ethylene glycol+Potassium ethanoate (KAc) | 0.2gKAc/g ethylene glycol | ????1.979 |
| ????8 | Ethylene glycol+sodium hydroxide (NaOH) | 0.1gNaOH/g ethylene glycol | ????1.741 |
| ????9 | Ethylene glycol+KAc+NaOH | (0.2gKAc+0.1gNaOH)/g ethylene glycol | ????2.629 |
| ????10 | Ethylene glycol+1, the 2-propylene glycol | 1.0g1,2-propylene glycol/g ethylene glycol | ????1.412 |
| ????11 | Glycerol | ????- | ????1.456 |
| ????12 | 1, the 2-propylene glycol | ????- | ????1.392 |
| ????13 | 1, the 4-butyleneglycol | ????- | ????1.282 |
Description of drawings
Fig. 1 is the separating technology that the present invention includes extractive distillation column and solvent recovery tower.Among the figure:
1 is the extraction agent charging opening;
2 is raw material (azeotrope or the mixture of forming near azeotropic) charging opening;
3 is the outlet of extractive distillation column (mixture of being made up of extraction agent and rare trimethyl carbinol aqueous solution) tower bottoms;
4 are extraction agent recovery mouth;
5 is the mixture outlet of rare trimethyl carbinol water;
6 is trimethyl carbinol product (massfraction is greater than 88.2%) discharge port.
Extractive distillation column (stage number from top to bottom count) as shown in Figure 1, extraction agent enters from extractive distillation column top, raw material (trimethyl carbinol and water) enters from the extractive distillation column middle part, at normal pressure, the solvent ratio ratio of raw material volumetric flow rate (the extraction agent volumetric flow rate with) 1.0-5.0, reflux ratio 1.0-3.0, tower top temperature is controlled at 81.0-83.0 ℃, and tower still temperature is controlled at 95.4-140.0 ℃.Under this condition, the recoverable trimethyl carbinol mass percent of cat head is greater than 88.2% product, and do not contain the dewatered product of the dipolymer or the trimethyl carbinol.The tower bottoms that comes out from extracting rectifying Tata still (mixture of being made up of extraction agent and rare trimethyl carbinol aqueous solution) enters the solvent recovery tower middle part, the working pressure of solvent recovery tower is 0.10-1atm (absolute pressure), reflux ratio 0.5-5.0, tower top temperature is controlled at 40.0-100.0 ℃, and tower still temperature is controlled at 104.7-196.0 ℃.Under this condition, the extraction agent that reclaims from the tower still recycles.
Embodiment
Embodiment 1
Extractive distillation column as shown in Figure 1.Extractive distillation column has 25 blocks of theoretical trays and (utilizes normal heptane and methylcyclohexane system to demarcate, stage number is counted from top to bottom), with ethylene glycol as extraction agent, add from the 4th theoretical stage, flow is 4ml/min, and the mixture of the trimethyl carbinol and water adds from the 10th theoretical stage, consists of trimethyl carbinol 85.9wt%, water 14.1wt%, flow are 4ml/min.Extractive distillation column is operated under normal pressure, and trim the top of column is than being 1.0-3.0,81.3 ℃ of tower top temperatures, 95.4-104.0 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 95.9wt% through gas chromatographic analysis, and water 4.1wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 42.7-56.8 ℃, 104.7-140.6 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 2
Other condition is with embodiment 1, and changing the extraction agent flow that enters extractive distillation column is 8ml/min, and this moment, tower top temperature was 82.4 ℃, 96.8-101.4 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 98.4wt% through gas chromatographic analysis, and water 1.6wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 42.7-56.8 ℃, 104.7-140.6 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 3
Other condition is with embodiment 1, and changing the extraction agent flow that enters extractive distillation column is 20ml/min, and this moment, tower top temperature was 82.6 ℃, 105.0-108.0 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 98.7wt% through gas chromatographic analysis, and water 1.3wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 42.7-56.8 ℃, 104.7-140.6 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 4
Extractive distillation column as shown in Figure 1.Extractive distillation column has 25 blocks of theoretical trays and (utilizes normal heptane and methylcyclohexane system to demarcate, stage number is counted from top to bottom), with ethylene glycol and 1, the mixture of 2-propylene glycol (mass ratio is 1: 1) adds from the 4th theoretical stage as extraction agent, and flow is 4ml/min, the mixture of the trimethyl carbinol and water adds from the 10th theoretical stage, consist of trimethyl carbinol 85.9wt%, water 14.1wt%, flow are 4ml/min.Extractive distillation column is operated under normal pressure, and trim the top of column is than being 1.0-3.0,81.0 ℃ of tower top temperatures, 96.4-104.5 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 95.1wt% through gas chromatographic analysis, and water 4.9wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 42.7-56.8 ℃, 104.4-150.6 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 5
Other condition is with embodiment 4, and changing the extraction agent flow that enters extractive distillation column is 8ml/min, and this moment, tower top temperature was 81.4 ℃, 97.8-106.5 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 96.2wt% through gas chromatographic analysis, and water 3.8wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 42.7-56.8 ℃, 104.4-150.6 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 6
Extractive distillation column as shown in Figure 1.Extractive distillation column has 25 blocks of theoretical trays and (utilizes normal heptane and methylcyclohexane system to demarcate, stage number is counted from top to bottom), with the mixture (massfraction of Potassium ethanoate is 0.20) of ethylene glycol and Potassium ethanoate (KAc) as extraction agent, add from the 4th theoretical stage, flow is 4ml/min, and the mixture of the trimethyl carbinol and water adds from the 10th theoretical stage, consists of trimethyl carbinol 85.9wt%, water 14.1wt%, flow are 4ml/min.Extractive distillation column is operated under normal pressure, and trim the top of column is than being 1.0-3.0,81.2 ℃ of tower top temperatures, 102.0-104.3 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 98.5wt% through gas chromatographic analysis, and water 1.5wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: normal pressure, reflux ratio 0.5-5.0, tower top temperature 82.7-99.8 ℃, 106.7-196.0 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 7
Other condition is with embodiment 6, and changing the extraction agent flow that enters extractive distillation column is 8ml/min, and this moment, tower top temperature was 82.0-82.5 ℃, 103.9-106.0 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 99.0wt% through gas chromatographic analysis, and water 1.0wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: normal pressure, reflux ratio 0.5-5.0, tower top temperature 82.7-99.8 ℃, 106.7-196.0 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 8
Extractive distillation column as shown in Figure 1.Extractive distillation column has 25 blocks of theoretical trays and (utilizes normal heptane and methylcyclohexane system to demarcate, stage number is counted from top to bottom), with the mixture (massfraction of KAc and NaOH is respectively 0.20 and 0.10) of ethylene glycol, Potassium ethanoate (KAc) and sodium hydroxide (NaOH) as extraction agent, add from the 4th theoretical stage, flow is 4ml/min, and the mixture of the trimethyl carbinol and water adds from the 10th theoretical stage, consists of trimethyl carbinol 85.9wt%, water 14.1wt%, flow are 4ml/min.Extractive distillation column is operated under normal pressure, and trim the top of column is than being 1.0-3.0, tower top temperature 81.9-82.2 ℃, 122.0-136.3 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 97.4wt% through gas chromatographic analysis, and water 2.6wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 44.4-61.6 ℃, 72.8-146.2 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 9
Other condition is with embodiment 8, and changing the extraction agent flow that enters extractive distillation column is 8ml/min, and this moment, tower top temperature was 81.1-81.2 ℃, 123.9-140.0 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 97.5wt% through gas chromatographic analysis, and water 2.5wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 44.4-61.6 ℃, 72.8-146.2 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 10
Extractive distillation column as shown in Figure 1.Extractive distillation column has 25 blocks of theoretical trays (utilize normal heptane and methylcyclohexane system to demarcate, stage number is counted from top to bottom), with ethylene glycol and calcium chloride (CaCl
2) mixture (CaCl wherein
2Massfraction be 0.10) as extraction agent, add from the 4th theoretical stage, flow is 4ml/min, the mixture of the trimethyl carbinol and water adds from the 10th theoretical stage, consists of trimethyl carbinol 85.9wt%, water 14.1wt%, flow are 4ml/min.Extractive distillation column is operated under normal pressure, and trim the top of column is than being 1.0-3.0, tower top temperature 82.0-82.2 ℃, 124.5-137.4 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 98.5wt% through gas chromatographic analysis, and water 1.5wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 43.8-61.6 ℃, 82.4-145.6 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 11
Extractive distillation column as shown in Figure 1.Extractive distillation column has 25 blocks of theoretical trays and (utilizes normal heptane and methylcyclohexane system to demarcate, stage number is counted from top to bottom), (wherein the massfraction of NaOH is 0.10 with the mixture of ethylene glycol and sodium hydroxide,) as extraction agent, add from the 4th theoretical stage, flow is 4ml/min, the mixture of the trimethyl carbinol and water adds from the 10th theoretical stage, consist of trimethyl carbinol 85.9wt%, water 14.1wt%, flow are 4ml/min.Extractive distillation column is operated under normal pressure, and trim the top of column is than being 1.0-3.0, tower top temperature 81.8-82.1 ℃, 125.2-137.0 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 96.1wt% through gas chromatographic analysis, and water 3.9wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 44.2-61.6 ℃, 85.5-145.5 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Embodiment 12
Extractive distillation column as shown in Figure 1.Extractive distillation column has 25 blocks of theoretical trays and (utilizes normal heptane and methylcyclohexane system to demarcate, stage number is counted from top to bottom), with 1, the 4-butyleneglycol adds from the 4th theoretical stage as extraction agent, and flow is 4ml/min, the mixture of the trimethyl carbinol and water adds from the 10th theoretical stage, consist of trimethyl carbinol 85.9wt%, water 14.1wt%, flow are 4ml/min.Extractive distillation column is operated under normal pressure, and trim the top of column is than being 1.0-3.0, tower top temperature 81.8-82.0 ℃, 115.7-136.0 ℃ of tower still temperature.Overhead product consists of trimethyl carbinol 90.8wt% through gas chromatographic analysis, and water 9.2wt% does not contain the dewatered product of the dipolymer or the trimethyl carbinol.
The tower still logistics of extractive distillation column enters and has 20 theoretical stages the solvent recovery tower of (utilizing normal heptane and methylcyclohexane system to demarcate).The operational condition of solvent recovery tower is: vacuum tightness 0.086MPa, reflux ratio 0.5-5.0, tower top temperature 43.8-61.6 ℃, 87.2-166.8 ℃ of tower still temperature.Tower still product returns extractive distillation column and recycles.
Claims (6)
1. the method for extracting rectifying separating tert-butanol and water, the extracting rectifying process is the double-column process that comprises extractive distillation column and solvent recovery tower, it is characterized in that: adopt the mixture of A or A and B to carry out extracting rectifying, and the mass percent of B component in the mixture of A and B is 0-30% as extraction agent;
A is ethylene glycol, propylene glycol, butyleneglycol or glycerol, or the mixture of above-mentioned alcohol;
B is sodium-chlor, calcium chloride, nitrocalcite, sodium sulfate, yellow soda ash, Potassium ethanoate, potassiumiodide, sodium hydroxide or potassium hydroxide, or the mixture of above-mentioned substance.
2. according to the method for claim 1, it is characterized in that: the operational condition of extractive distillation column is a normal pressure, the extraction agent volumetric flow rate is 1.0-5.0 with the ratio of raw material volumetric flow rate, reflux ratio is 1.0-3.0, tower top temperature is controlled at 81.0-83.0 ℃, tower still temperature is controlled at 95.4-140.0 ℃, and cat head can obtain crossing over the trimethyl carbinol that azeotropic is formed.
3. according to the method for claim 1, it is characterized in that: the tower bottoms of extractive distillation column enters solvent recovery tower and reclaims, the operational condition of solvent recovery tower is normal pressure or decompression, the scope of working pressure is absolute pressure 0.10-1atm, reflux ratio 0.5-5.0, tower top temperature is controlled at 40.0-100.0 ℃, and tower still temperature is controlled at 104.7-196.0 ℃.
4. according to the method for claim 1 or 2 or 3, it is characterized in that: said raw material is the azeotrope of the trimethyl carbinol and water composition or the mixture of forming near azeotropic.
5. according to the method for claim 1 or 2 or 3, it is characterized in that: the theoretical plate number of extractive distillation column is more than 25, and the theoretical plate number of solvent recovery tower is more than 20.
6. according to the method for claim 5, it is characterized in that: the theoretical plate number of extractive distillation column is 25-50, and the theoretical plate number of solvent recovery tower is 20-40.
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| CN109134198A (en) * | 2018-11-08 | 2019-01-04 | 山东科技大学 | A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture |
| CN109761769A (en) * | 2019-01-28 | 2019-05-17 | 宝鸡文理学院 | A kind of technique refining methyl phenyl ethers anisole |
| CN109678679A (en) * | 2019-01-28 | 2019-04-26 | 宝鸡文理学院 | A kind of technique purifying methyl phenyl ethers anisole |
| CN109851482A (en) * | 2019-01-28 | 2019-06-07 | 宝鸡文理学院 | A kind of technique purifying phenetole |
| CN109678679B (en) * | 2019-01-28 | 2021-05-28 | 宝鸡文理学院 | Process for purifying anisole |
| CN109851482B (en) * | 2019-01-28 | 2021-06-25 | 宝鸡文理学院 | Process for purifying phenetole |
| CN109761769B (en) * | 2019-01-28 | 2021-06-29 | 宝鸡文理学院 | Process for refining anisole |
| CN111138240A (en) * | 2019-12-28 | 2020-05-12 | 中国船舶重工集团公司第七一八研究所 | Water removal device and water removal method for hexafluorobutadiene |
| CN111138240B (en) * | 2019-12-28 | 2022-11-25 | 中国船舶重工集团公司第七一八研究所 | Water removal device and water removal method for hexafluorobutadiene |
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