CN102633597A - Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture - Google Patents
Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture Download PDFInfo
- Publication number
- CN102633597A CN102633597A CN2012100776028A CN201210077602A CN102633597A CN 102633597 A CN102633597 A CN 102633597A CN 2012100776028 A CN2012100776028 A CN 2012100776028A CN 201210077602 A CN201210077602 A CN 201210077602A CN 102633597 A CN102633597 A CN 102633597A
- Authority
- CN
- China
- Prior art keywords
- extraction
- tower
- alcohol
- ethanol
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention relates to a novel process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture. By means of extraction and salting out, separation coefficient of water and mixed alcohol is increased and water content in extract phase is greatly reduced, and energy consumption is greatly reduced by means of subsequent azeotropic rectification. An extractant serves as an entrainer during azeotropic rectification, the extractant, water and ethanol form a ternary azeotropic mixture to enter an ethanol tower for separation of the ethanol, and the defect of difficulty in separation of the ethanol and the propyl alcohol. Energy consumption in treatment of high-water-content alcohol-water mixture can be greatly reduced while high purity of the alcohols (the ethanol being higher than 95%, the propyl alcohol being higher than 99% and the isobutyl alcohol being higher than 97% in purity) can be guaranteed. The process is especially applicable to high-water-content mixed alcohol hydrodissection systems, and has remarkable practicality and economic benefit.
Description
Technical field
The present invention relates to a kind of novel process that from polyvalent alcohol-water mixture, reclaims ethanol, n-propyl alcohol and isopropylcarbinol, specifically be utilize that extraction is saltoutd, azeotropic distillation and variable-pressure rectification combination technology are realized several kinds alcohol and water separates and reclaim the pure process method of high purity.
Technical background
The polyvalent alcohol water mixture also is referred to as potato spirit, and potato spirit is the by product of fermentative Production alcohol and liquor, is one of main flavour ingredient that constitutes liquor.If the potato spirit too high levels can be to toxic elements in human body evil effect, be 8.5 times of alcoholic acid like the toxicity of n-propyl alcohol, the toxicity of isopropylcarbinol is 8 times of alcoholic acid.Along with comprehensive startup of China's use vehicle-use alcohol gasoline work, the ethanol demand amount is cumulative year after year trend, by the present edible ethanol of China and 4,000,000 tons of calculating of alcohol fuel YO, and nearly about 1.5 ten thousand tons of year by-product potato spirit.Make full use of the potato spirit resource, produce high value-added product, eliminate the direct environmental pollution caused by discharge of potato spirit, will create nearly hundred million yuan direct economic benefit for Chinese alcohol enterprise.
In the polyvalent alcohol water mixture; Ethanol is a kind of water white transparency, the liquid of special aromatising flavour is arranged; 78.32 ℃ of boiling points (101.3kPa); Can with immiscible organic solvents such as water, ether, chloroform, ester, hydrocarbon derivative, can be used as the manufacturing raw material of agricultural chemicals, medicine, rubber, plastics, regenerated fiber, washing composition etc.; N-propyl alcohol is a kind of colourless, liquid with aromatising flavour; 97.2 ℃ of boiling points (101.3kPa); Can with multiple immiscible organic solvents such as water, alcohol, ether, hydrocarbon, can be used as the solvent of plant oil, tree elastomer and resene, some synthetic resins and TKK 021, polyvinyl butyral; Isopropylcarbinol is a kind of water white transparency, the liquid of special odor is arranged; 107.9 ℃ of boiling points (101.3kPa); Can with immiscible organic solvents such as alcohol, ether; As the solubility promoter of Nitrocellulose, the solvent of TKK 021, polyvinyl butyral acetal, multiple oils, rubber, natural resin, petroleum additive, oxidation inhibitor, softening agent etc.Ethanol and water form azeotrope (78.17 ℃ of azeotropic temperatures; Ethanol quality: quality=96: 4); N-propyl alcohol and water form azeotrope (87.7 ℃ of azeotropic temperatures; The n-propyl alcohol quality: quality=71.7: 28: 3), isopropylcarbinol and water form azeotrope (89.92 ℃ of azeotropic temperatures, isopropylcarbinol quality: quality=66.8: 33.2).And, causing difficulty to separation because ethanol is close with n-propyl alcohol character, n-propyl alcohol has also increased difficulty to separating with the isopropylcarbinol relative volatility is too small.
Owing to form azeotrope between fusel W/O and the alcohol, become a difficult problem in the industry so from potato spirit, remove water and extract high purity alcohol.The method of industrial treatment potato spirit roughly has three kinds at present: first kind; Add the NaCl branch water of saltouing, this method divides the water effect undesirable, is inappropriate for handling water cut about 20% even lower system; And, follow-up equipment is caused certain corrosion because the Cl ionic is introduced; Second kind, adopt extractive distillation with salt to handle, the cat head extraction is the mixture of ethanol and n-propyl alcohol; Because ethanol, n-propyl alcohol character are approaching, can not get highly purified single alcohol, the water cut about 5% of alcohol; Along with the rising of n-propyl alcohol content, water-content also rises thereupon, does not realize alcohol-water, alcohol-pure isolating purpose; And the extraction agent consumption is very big, for the subsequent recovery extraction agent has caused difficulty; The third adopts simple azeotropic distillation to handle, and entrainer is a benzene, and the toxicity of benzene is very big, can cause environmental pollution, and this technology entrainer consumption is big simultaneously, energy consumption is high, recovery cost is high, exist between alcohol and the alcohol and separate problems such as not thorough.
Summary of the invention
The purpose of this invention is to provide a kind of novel process that from polyvalent alcohol-water mixture, reclaims ethanol, n-propyl alcohol and isopropylcarbinol, adopt the method for saltout abstraction combined azeotropy distillation, variable-pressure rectification,, and obtain the single alcohol product of high density effectively with alcohol-water sepn.The entrainer of being selected for use is a hexanaphthene; Toxicity is low, and azeotropic band water is effective, has reduced and has reclaimed the energy consumption that alcohol is brought; The single alcohol product purity that obtains simultaneously is high; Be specially adapted to the high pure water sepn system of water cut, improve alcohol and separate halfway problem, have significant practicality and economy with alcohol.
Technical scheme of the present invention is:
A kind of technology that from polyvalent alcohol-water mixture, reclaims ethanol, n-propyl alcohol and isopropylcarbinol, the step that comprises is following:
1) alcohol-water mixture raw material F is from extraction tower 103 middle part chargings, and extraction agent S1 injects from extraction tower 103 bottoms, and salting-out agent S2 injects from extraction tower 103 tops.
2) through extraction tower 103 salt separation extractings, rich aqueous extracting phase R gets into evaporating pot 102 from extraction tower 103 tower still extraction, and the alcohol-water mixture of evaporating pot 102 top extraction gets into concentration tower 101 and carries and densely get into extraction tower 103 with raw material F again.Evaporating pot 102 bottoms obtain the solution identical with the initial salting-out agent S2 mass concentration that adds and inject extraction tower 103 top recycles.
3) through extraction tower 103 salt separation extractings; The extraction phase E that is rich in alcohol mixture and extraction agent gets into azeotropy rectification column 104 from extraction tower 103 cat head extraction; Extraction agent S1 plays the effect of entrainer again in azeotrope column 104, get into first phase separation tank 105 at azeotrope column 104 cat head productions, and oil phase part H refluxes; Another part HS turns back to and gets into extraction tower 103 among the extraction agent S1, and the water extraction gets into ethanol treating tower 107.Azeotrope column 104 tower still productions get into n-propyl alcohol, isobutanol separation column 106.
4) can obtain ethanol at ethanol treating tower 107 tower stills, the cat head production gets into second phase separation tank 108, and oil phase refluxes, and water gets into evaporating pot 102 recycles.
5) n-propyl alcohol, isobutanol separation column 106 adopt rectification under vacuum, and the cat head extraction can obtain n-propyl alcohol, and the extraction of tower still can obtain isopropylcarbinol.
Described alcohol-water mixture raw material F consists of water: ethanol: n-propyl alcohol: isopropylcarbinol=20%～24%: 38%～40%: 26%～30%: 10% (mass percent);
Described concentration tower 101 stage number 40, feed entrance point 20～23, cat head extraction position 2～4, tower still extraction position 37～39,85～90 ℃ of tower top temperatures, 100～105 ℃ of tower still temperature, reflux ratio 2～3, working pressure is 101.3kPa;
90 ℃～100 ℃ of described evaporating pot 102 temperature, working pressure is 101.3kPa;
Described extraction tower 103 stage number 40, raw material feed entrance point 20～23, extractant feed position 36～38; Salting-out agent feed entrance point 2～4, extraction phase extraction position 6～8, extracting phase extraction position 39～40; 20～30 ℃ of service temperatures, working pressure are 101.3kPa;
Described azeotrope column 104 stage number 40, feed entrance point 20～23, oil phase backflow position 4～6, cat head extraction position 2～4, tower still extraction position 37～39,60～65 ℃ of tower top temperatures, 95～100 ℃ of tower still temperature, reflux ratio 2～3, working pressure is 101.3kPa;
Described n-propyl alcohol, isobutanol separation column 106 stage number 40, feed entrance point 20～23, cat head extraction position 2～4, tower still extraction position 37～39, reflux ratio 2～3, working pressure 10～40kPa;
Described ethanol treating tower 107 stage number 40, feed entrance point 20～23, cat head extraction position 2～4, tower still extraction position 37～39,60～65 ℃ of tower top temperatures, 80～90 ℃ of tower still temperature, reflux ratio 2～3, working pressure is 101.3kPa;
Described extraction agent S1 is a hexanaphthene, 20～30 ℃ of temperature, and the two volume ratio of extraction agent S1/ raw material F is 1.1～3;
Described salting-out agent S2 is the Potassium ethanoate aqueous solution, 20～30 ℃ of temperature, and its solution quality concentration is 50%～70%, two phase mass ratio=1～3.3 of salting-out agent S2/ raw material F.
The present invention adopts a kind of novel process that from polyvalent alcohol-water mixture, reclaims ethanol, n-propyl alcohol and isopropylcarbinol, makes mass percent>=99%, isopropylcarbinol mass percent>=97% of aqueous mass percent≤0.3%, alcoholic acid mass percent>=95%, n-propyl alcohol.Through extraction tower 103 salt separation extractings, make water and alcohol mixture separation factor improve, the water cut among the extraction phase E greatly reduces, and follow-up azeotropic distillation energy consumption is significantly reduced; Extraction agent S1 plays the effect of entrainer again in the azeotropic distillation process, extraction agent S1, water, ethanol ternary azeotropic get into ethanol treating tower 107 refining ethanol, can overcome the not segregative shortcoming of ethanol and n-propyl alcohol.Extracting phase R obtains getting into extraction tower 103 recycles with the initial salting-out agent S2 mass concentration same solution that adds through evaporation process.In n-propyl alcohol, isobutanol separation column 106, adopt rectification under vacuum, improve the relative volatility of n-propyl alcohol and isopropylcarbinol, improve product purity.
This technology has characteristics such as less energy-consumption, low pollution, high-recovery, high product purity, has broad application prospects, and is particularly suitable for high alcohol mixture of water cut and water sepn system.Make water cut (mass percent) be reduced to 1～2% through the present invention's processing the alcohol-water mixture of moisture (mass percent) 20～30%; Handle through azeotropic distillation again; Water-content (mass percent) is minimum in the high purity alcohol that reclaims reduces to 0.1%; Handle the high-moisture alcohol-water mixture than direct use azeotropic distillation, the present invention has saved energy consumption for the polyvalent alcohol recovery stage of chemical process, is recovered to high purity alcohol product simultaneously.
Description of drawings
Fig. 1 is a kind of schema that from polyvalent alcohol-water mixture, reclaims the technology of ethanol, n-propyl alcohol and isopropylcarbinol of the present invention.
Embodiment
The present invention specifies as follows with reference to accompanying drawing, but for illustrative purposes only rather than limit the present invention.
Among Fig. 1,101-concentration tower, 102-evaporating pot, 103-extraction tower; The 104-azeotrope column, 105-first phase separation tank, 106-n-propyl alcohol, isobutanol separation column, 107-ethanol treating tower; 108-second phase separation tank, F-raw material, S1-extraction agent, S2-salting-out agent; E-is rich in the extraction phase of alcohol mixture and extraction agent, the rich aqueous extracting phase of R-, and H-azeotrope column cat head oil phase is back to the part of azeotrope column, and HS-azeotrope column cat head oil phase is back to the part in the extraction agent
The step that a kind of novel process that from polyvalent alcohol-water mixture, reclaims ethanol, n-propyl alcohol and isopropylcarbinol provided by the invention comprises is described in detail as follows:
1) extraction tower 103 stage number are 40, and working pressure is 101.3kPa, 20～30 ℃ of service temperatures.Alcohol-water mixture raw material F is from the 20th～23 plate charging of extraction tower 103,20～30 ℃ of liquid stock F temperature.Extraction agent S1 is a hexanaphthene, 20～30 ℃ of temperature, and extraction agent S1 gets into from the 36th～38 block of plate of extraction tower 103; Salting-out agent S2 is the Potassium ethanoate aqueous solution, 20～30 ℃ of temperature, and salting-out agent S2 gets into from the 2nd～4 block of plate of extraction tower 103.Extraction agent S1 and raw material F volume ratio=1.1～3, salting-out agent S2 and raw material F mass ratio=1～3.3, salting-out agent S2 mass percent is 50～70%.
2) through extraction tower 103 salt separation extractings, mass percent≤0.6% of hexanaphthene among the rich aqueous extracting phase R, extracting phase R gets into evaporating pot 102,90～100 ℃ of evaporating pot 102 temperature from the 39th～40 plate extraction of extraction tower 103; Concentration tower 101 stage number are 40, and working pressure is 101.3kPa, 85～90 ℃ of tower top temperatures, 100～105 ℃ of tower still temperature, reflux ratio 2～3.The alcohol-water mixture of evaporating pot 102 top extraction gets into the 20th～23 block of plate of concentration tower 101, and concentration tower 101 gets into the 20th～23 block of plate of extraction tower 103 from the 2nd～4 continuous extraction of plate with raw material F; Mass percent≤0.03% of alcohol has reached emission standard in the waste water of the 37th～39 plate extraction of concentration tower 101.Evaporating pot 102 bottoms obtain the 2nd～4 plate recycle that the solution identical with the initial salting-out agent S2 mass concentration (mass concentration 50～70%) that adds injects extraction tower 103.
3) through extraction tower 103 salt separation extractings, the extraction phase E water cut (mass percent) that is rich in alcohol mixture and extraction agent is 1.1～2%.Azeotrope column 104 stage number are 40, reflux ratio 2～3, and working pressure is 101.3kPa, 60～65 ℃ of tower top temperatures, 95～100 ℃ of tower still temperature.Extraction phase E gets into the 20th～23 block of plate of azeotrope column 104 from the 6th～8 plate extraction of extraction tower 103; The 2nd～4 plate production of azeotrope column 104 gets into first phase separation tank 105; Oil phase part H is back to the 4th～6 block of plate of azeotrope column 104; Another part HS turns back to the 36th～38 block of plate that extraction agent S1 gets into extraction tower 103, and H: HS (volume ratio) is 2: 1; Water gets into the 20th～23 block of plate of ethanol treating tower 107; The 37th～39 plate extraction of azeotrope column 104 gets into the 20th～23 block of plate of n-propyl alcohol, isobutanol separation column 106.
4) ethanol treating tower 107 stage number are 40, reflux ratio 2～3, and working pressure is 101.3kPa, 60～65 ℃ of tower top temperatures, 80～90 ℃ of tower still temperature.The 2nd～4 plate production of ethanol treating tower 107 gets into the 4th～6 block of plate that oil phase after 108 phase-splittings of second phase separation tank is back to ethanol treating tower 107, and water gets into evaporating pot 102 and recycles.It is 95% above ethanol that the 37th～39 plate extraction of ethanol treating tower 107 can obtain mass percent.
5) n-propyl alcohol, isobutanol separation column 106 stage number are 40; Working pressure is 10～40kPa; Reflux ratio 2～3; It is 99% above n-propyl alcohol that n-propyl alcohol, isobutanol separation column 106 can get mass percent from the 2nd～4 plate extraction, and it is 97% above isopropylcarbinol that n-propyl alcohol, the 37th～39 plate extraction of isobutanol separation column 106 can get mass percent.
Application example 1:
It is the θ ring packing post of 30mm that concentration tower 101, extraction tower 103, azeotrope column 104, n-propyl alcohol isobutanol separation column 106, ethanol treating tower 107 all adopt internal diameter, and filler size is φ 3mm * 3mm, tower height 1500mm (filler has been amounted to into stage number through demarcating).Raw material F inlet amount 800g/h; Raw material F forms water: ethanol: n-propyl alcohol: isopropylcarbinol=20%: 40%: 30%: 10% (mass percent), and the temperature that raw material F gets into extraction tower 103 is 20 ℃, extraction agent S1 is a hexanaphthene; Salting-out agent S2 is the Potassium ethanoate aqueous solution of mass percent 50%; Extraction agent S1 and raw material F volume ratio=1.2: 1, salting-out agent S2 and raw material F mass ratio=1.8: 1, it is 20 ℃ that extraction agent S1 and salting-out agent S2 get into extraction tower 103 temperature.After extraction is saltoutd through extraction tower 103, consist of water from the extracting phase R of extraction tower 103 extraction: ethanol: n-propyl alcohol: isopropylcarbinol: hexanaphthene=83.8%: 11.3%: 4.3%: 0.06%: 0.54% (mass percent); Consist of water from the extraction phase E of extraction tower 103 extraction: ethanol: n-propyl alcohol: isopropylcarbinol: hexanaphthene=2%: 22%: 22%: 3%: 51% (mass percent).
Extraction phase E gets into azeotrope column 104, and azeotrope column 104 cat head productions are through 105 phase-splittings of first phase separation tank, and water gets into ethanol treating tower 107, but ethanol treating tower 107 tower still extraction mass percents are 95.5% ethanol.Azeotrope column 104 tower still productions get into n-propyl alcohol, isobutanol separation column 106, and n-propyl alcohol, isobutanol separation column 106 cat head extraction mass percents are 99.9% n-propyl alcohol, and moisture mass percent is 0.10%; Tower still extraction mass percent is 97.4% isopropylcarbinol, and moisture mass percent is 0.1%.
Be the gas chromatographic analysis result with upper reaches thigh concentration.
After extraction tower 103 extractions are saltoutd; Make the water cut (mass percent) of alcohol-water mixture drop to 2% by 20%; The while extraction agent also can be used as entrainer and is used for azeotropic water removing and combines refining polyvalent alcohol to handle; Can make alcohol concn arrive mass percent is 95.5%, and the n-propyl alcohol mass percent is 99.9%, and the isopropylcarbinol mass percent is 97.4%; Water cut (mass percent) is less than 0.2%, and this technology is handled the technology energy efficient 20% of high-moisture alcohol-water mixture than direct use azeotropic distillation (using high toxicity solvent benzene as entrainer).
Application example 2:
It is the θ ring packing post of 30mm that concentration tower 101, extraction tower 103, azeotrope column 104, n-propyl alcohol isobutanol separation column 106, ethanol treating tower 107 all adopt internal diameter, and filler size is φ 3mm * 3mm, tower height 1500mm (filler has been amounted to into stage number through demarcating).Raw material F inlet amount 800g/h; Raw material F forms water: ethanol: n-propyl alcohol: isopropylcarbinol=22%: 38%: 30%: 10% (mass percent), and the temperature that raw material F gets into extraction tower 103 is 25 ℃, extraction agent S1 is a hexanaphthene; Salting-out agent S2 massfraction is 60% wet chemical; Extraction agent S1 and raw material F volume ratio=2: 1, salting-out agent S2 and raw material F mass ratio=1.3: 1, extraction agent S1 and salting-out agent S2 inlet temperature of stabilizer are 25 ℃.After extraction is saltoutd through extraction tower 103, consist of water from the extracting phase R of extraction tower 103 extraction: ethanol: n-propyl alcohol: isopropylcarbinol: hexanaphthene=79.3%: 15.1%: 4.7%: 0.7%: 0.2% (mass percent); Consist of water from the extraction phase E of extraction tower 103 extraction: ethanol: n-propyl alcohol: isopropylcarbinol: hexanaphthene=1.3%: 15%: 12%: 3%: 68.7% (mass percent).
Extraction phase E gets into azeotrope column 104, and azeotrope column 104 cat head productions are through 105 phase-splittings of first phase separation tank, and water gets into ethanol treating tower 107, and ethanol treating tower 107 tower still extraction mass percents are 95.2% ethanol.Azeotrope column 104 tower still productions get into n-propyl alcohol, isobutanol separation column 106, and n-propyl alcohol, isobutanol separation column 106 cat head extraction mass percents are 99.85% n-propyl alcohol, moisture (mass percent) 0.15%; Tower still extraction mass percent is 97.1% isopropylcarbinol, moisture (mass percent) 0.22%.
Be the gas chromatographic analysis result with upper reaches thigh concentration.
After extraction tower 103 extractions are saltoutd; Make the water cut (mass percent) of alcohol-water mixture drop to 1.3% by 22%; The while extraction agent also can be used as entrainer and is used for azeotropic water removing and combines refining polyvalent alcohol to handle; Can make alcohol concn arrive (mass percent) 95.2%, n-propyl alcohol (mass percent) 99.85%, isopropylcarbinol (mass percent) 97.1%; Water cut (mass percent) is less than 0.25%, and this technology is handled the technology energy efficient 22% of high-moisture alcohol-water mixture than direct use azeotropic distillation (using high toxicity solvent benzene as entrainer).
Application example 3:
It is the θ ring packing post of 30mm that concentration tower 101, extraction tower 103, azeotrope column 104, n-propyl alcohol isobutanol separation column 106, ethanol treating tower 107 all adopt internal diameter, and filler size is φ 3mm * 3mm, tower height 1500mm (filler is amounted to into stage number through demarcating oneself).Raw material F inlet amount 800g/h; Raw material F forms water: ethanol: n-propyl alcohol: isopropylcarbinol=24%: 40%: 26%: 10% (mass percent), and the temperature that raw material F gets into extraction tower 103 is 20 ℃, extraction agent S1 is a normal hexane; Salting-out agent S2 is the Potassium ethanoate aqueous solution of massfraction 70%; Extraction agent S1 and raw material F volume ratio=1.5: 1, salting-out agent S2 and raw material F mass ratio=1.5: 1, extraction agent S1 and salting-out agent S2 inlet temperature of stabilizer are 20 ℃.After extraction is saltoutd through extraction tower 103, consist of water from the extracting phase R of extraction tower 103 extraction: ethanol: n-propyl alcohol: isopropylcarbinol: normal hexane=78.1%: 13.8%: 4.9%: 0.7%: 2.5% (mass percent); Consist of water from the extraction phase E of extraction tower 103 extraction: ethanol: n-propyl alcohol: isopropylcarbinol: normal hexane=1.5%: 18%: 16%: 4.5%: 60% (mass percent).
Extraction phase E gets into azeotrope column 104, and azeotrope column 104 cat head productions are through 105 phase-splittings of first phase separation tank, and water gets into ethanol treating tower 107, ethanol treating tower 107 tower still extraction 95.6% (mass percent) ethanol.Azeotrope column 104 tower still productions get into n-propyl alcohol, isobutanol separation column 106, n-propyl alcohol, isobutanol separation column 106 cat head extraction 99.8% (mass percent) n-propyl alcohols, moisture 0.20% (mass percent); Tower still extraction 97.3% (mass percent) isopropylcarbinol, moisture 0.25% (mass percent).
Be the gas chromatographic analysis result with upper reaches thigh concentration.
After extraction tower 103 extractions are saltoutd; Make the water cut of alcohol-water mixture drop to 1.5% by 24%; The while extraction agent also can be used as entrainer and is used for azeotropic water removing and combines refining polyvalent alcohol to handle; Can make alcohol concn arrive 95.6% (mass percent), n-propyl alcohol 99.8% (mass percent), isopropylcarbinol (mass percent) 97.3%; Water cut is less than 0.3% (mass percent), and this technology is handled the technology energy efficient 21% of high-moisture alcohol-water mixture than direct use azeotropic distillation (using high toxicity solvent benzene as entrainer).
It is known technology that the present invention does not state matters.
Claims (10)
1. technology that from polyvalent alcohol-water mixture, reclaims ethanol, n-propyl alcohol and isopropylcarbinol, it is following to it is characterized by the step that comprises:
1) the alcohol-water mixture raw material is from extraction tower (103) middle part charging, and extraction agent injects from extraction tower (103) bottom, and salting-out agent inject from extraction tower (103) top;
2) through extraction tower (103) salt separation extracting, rich aqueous extracting phase gets into evaporating pot (102) from the extraction of extraction tower (103) tower still, and the alcohol-water mixture of evaporating pot (102) top extraction gets into concentration tower (101) and carries and densely get into extraction tower (103) with raw material again.Evaporating pot (102) bottom obtains the solution identical with the initial salting-out agent mass concentration that adds and injects extraction tower (103) top recycle;
3) through extraction tower (103) salt separation extracting; The extraction phase that is rich in alcohol mixture and extraction agent gets into azeotropy rectification column (104) from extraction tower (103) cat head extraction; Extraction agent plays the effect of entrainer again in azeotrope column (104), get into first phase separation tank (105) at azeotrope column (104) cat head production, and an oil phase part refluxes; Another part turns back to and gets into extraction tower (103) in the extraction agent, and the water extraction gets into ethanol treating tower (107).Azeotrope column (104) tower still production gets into n-propyl alcohol, isobutanol separation column (106);
4) can obtain ethanol at ethanol treating tower (107) tower still, the cat head production gets into second phase separation tank (108), and oil phase refluxes, and water gets into evaporating pot (102) recycle;
5) n-propyl alcohol, isobutanol separation column (106) adopt rectification under vacuum, and the cat head extraction can obtain n-propyl alcohol, and the extraction of tower still can obtain isopropylcarbinol.
2. according to the described technology of claim 1, it is characterized in that the water that consists of of described alcohol-water mixture raw material: ethanol: n-propyl alcohol: isopropylcarbinol=20%～24%: 38%～40%: 26%～30%: 10% (mass percent).
3. according to the described technology of claim 1, it is characterized in that described concentration tower (101) stage number 40, feed entrance point 20～23; Cat head extraction position 2～4; Tower still extraction position 37～39,85～90 ℃ of tower top temperatures, 100～105 ℃ of tower still temperature; Reflux ratio 2～3, working pressure are 101.3kPa.
4. according to the described technology of claim 1, it is characterized in that 90 ℃～100 ℃ of described evaporating pot (102) temperature, working pressure is 101.3kPa.
5. according to the described technology of claim 1, it is characterized in that described extraction tower (103) stage number 40, raw material feed entrance point 20～23; Extractant feed position 36～38; Salting-out agent feed entrance point 2～4, extraction phase extraction position 6～8, extracting phase extraction position 39～40; 20～30 ℃ of service temperatures, working pressure are 101.3kPa.
6. according to the described technology of claim 1, it is characterized in that described azeotrope column (104) stage number 40, feed entrance point 20～23; Oil phase backflow position 4～6, cat head extraction position 2～4, tower still extraction position 37～39; 60～65 ℃ of tower top temperatures; 95～100 ℃ of tower still temperature, reflux ratio 2～3, working pressure is 101.3kPa.
7. according to the described technology of claim 1, it is characterized in that described n-propyl alcohol, isobutanol separation column (106) stage number 40, feed entrance point 20～23, cat head extraction position 2～4, tower still extraction position 37～39, reflux ratio 2～3, working pressure 10～40kPa.
8. according to the described technology of claim 1, it is characterized in that described ethanol treating tower (107) stage number 40, feed entrance point 20～23; Cat head extraction position 2～4; Tower still extraction position 37～39,60～65 ℃ of tower top temperatures, 80～90 ℃ of tower still temperature; Reflux ratio 2～3, working pressure are 101.3kPa.
9. according to the described technology of claim 1, it is characterized in that described extraction agent is a hexanaphthene, 20～30 ℃ of temperature, the two volume ratio of extraction agent/raw material is 1.1～3.
10. according to the described technology of claim 1, it is characterized in that described salting-out agent are the Potassium ethanoate aqueous solution, 20～30 ℃ of temperature, its solution quality concentration is 50%～70%, two phase mass ratio=1～3.3 of salting-out agent/raw material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100776028A CN102633597B (en) | 2012-03-22 | 2012-03-22 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100776028A CN102633597B (en) | 2012-03-22 | 2012-03-22 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102633597A true CN102633597A (en) | 2012-08-15 |
| CN102633597B CN102633597B (en) | 2013-11-13 |
Family
ID=46618198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012100776028A Expired - Fee Related CN102633597B (en) | 2012-03-22 | 2012-03-22 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102633597B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044194A (en) * | 2012-12-18 | 2013-04-17 | 沈阳化工大学 | Method for separating alcohol and water mixture through extraction and rectification |
| CN103193590A (en) * | 2013-03-26 | 2013-07-10 | 沈阳化工大学 | Method for continuously extracting, rectifying and separating mixed alcohols from water |
| CN105906488A (en) * | 2014-08-06 | 2016-08-31 | 东营市海科新源化工有限责任公司 | Method applied to refining purification device for by-product diisopropylether during isopropanol production |
| CN109661259A (en) * | 2016-09-08 | 2019-04-19 | 伊士曼化工公司 | For separating the method for being thermally integrated Distallation systm and use it of the ternary composition with heterogeneous azeotrope |
| CN113214039A (en) * | 2021-05-08 | 2021-08-06 | 青岛科技大学 | Extractive distillation process for separating ternary complex azeotropic mixture cyclohexane/normal propyl alcohol/water |
| CN114380662A (en) * | 2020-10-21 | 2022-04-22 | 华东理工大学 | Method for preparing absolute ethanol from ethanol-water azeotrope by adopting dissolved salt extraction rectification mode |
| CN115073270A (en) * | 2022-05-12 | 2022-09-20 | 山东昆达生物科技有限公司 | Continuous azeotropic extraction and rectification method for separating low-carbon polyol-water mixture |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5756866A (en) * | 1994-12-21 | 1998-05-26 | Agip Petroli S.P.A. | Process for obtaining separate streams of methanol and ethanol, n-propanol and isobutanol |
| CN1316410A (en) * | 2001-02-27 | 2001-10-10 | 上海远东香料化学工程研究中心 | Process for separating ternary butanol-propanol-water mixture |
| CN1458260A (en) * | 2003-05-13 | 2003-11-26 | 天津大学 | Fusel oil molecular sieve gas phase dewatering method and separating and purifying method |
| US20100069515A1 (en) * | 2006-04-13 | 2010-03-18 | Tirtowidjojo Max M | Mixed alcohol synthesis with enhanced carbon value use |
-
2012
- 2012-03-22 CN CN2012100776028A patent/CN102633597B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5756866A (en) * | 1994-12-21 | 1998-05-26 | Agip Petroli S.P.A. | Process for obtaining separate streams of methanol and ethanol, n-propanol and isobutanol |
| CN1316410A (en) * | 2001-02-27 | 2001-10-10 | 上海远东香料化学工程研究中心 | Process for separating ternary butanol-propanol-water mixture |
| CN1458260A (en) * | 2003-05-13 | 2003-11-26 | 天津大学 | Fusel oil molecular sieve gas phase dewatering method and separating and purifying method |
| US20100069515A1 (en) * | 2006-04-13 | 2010-03-18 | Tirtowidjojo Max M | Mixed alcohol synthesis with enhanced carbon value use |
Non-Patent Citations (2)
| Title |
|---|
| 熊道陵: "杂醇油提纯分离技术及应用", 《酿酒科技》 * |
| 许新乐: "杂油醇加盐萃取精馏提取低水乙醇的研究", 《青海大学学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044194A (en) * | 2012-12-18 | 2013-04-17 | 沈阳化工大学 | Method for separating alcohol and water mixture through extraction and rectification |
| CN103193590A (en) * | 2013-03-26 | 2013-07-10 | 沈阳化工大学 | Method for continuously extracting, rectifying and separating mixed alcohols from water |
| CN105906488A (en) * | 2014-08-06 | 2016-08-31 | 东营市海科新源化工有限责任公司 | Method applied to refining purification device for by-product diisopropylether during isopropanol production |
| CN105906488B (en) * | 2014-08-06 | 2019-11-15 | 东营市海科新源化工有限责任公司 | A kind of purification purifying plant for by-product diisopropyl ether in isopropyl alcohol production |
| CN109661259A (en) * | 2016-09-08 | 2019-04-19 | 伊士曼化工公司 | For separating the method for being thermally integrated Distallation systm and use it of the ternary composition with heterogeneous azeotrope |
| CN114380662A (en) * | 2020-10-21 | 2022-04-22 | 华东理工大学 | Method for preparing absolute ethanol from ethanol-water azeotrope by adopting dissolved salt extraction rectification mode |
| CN113214039A (en) * | 2021-05-08 | 2021-08-06 | 青岛科技大学 | Extractive distillation process for separating ternary complex azeotropic mixture cyclohexane/normal propyl alcohol/water |
| CN115073270A (en) * | 2022-05-12 | 2022-09-20 | 山东昆达生物科技有限公司 | Continuous azeotropic extraction and rectification method for separating low-carbon polyol-water mixture |
| CN115073270B (en) * | 2022-05-12 | 2024-04-02 | 山东昆达生物科技有限公司 | Continuous azeotropic extractive distillation method for separating low-carbon polyol-water mixture |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102633597B (en) | 2013-11-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102633597B (en) | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture | |
| CN105001056B (en) | A kind of method of variable-pressure rectification separation isobutanol and normal heptane azeotropic system | |
| CN102675265B (en) | Method of refining furfural through six-tower continuous rectification | |
| KR20120039017A (en) | Recovery of butanol from a mixture of butanol, water and an organic extractant | |
| CN105503522B (en) | For the recovery of methylbenzene methanol/ethanol, refining plant and separation method | |
| CN1023799C (en) | Purification and preparation processes for methyl methacrylate | |
| CN101289363B (en) | Process for preparing 1-amylene by separating C5 distillate of petroleum | |
| TW201934525A (en) | Method for separating aromatic hydrocarbon using extractive distillation | |
| CN103664446A (en) | Technology for separating n-hexane-methylcyclopentane through extractive distillation | |
| CN106397252B (en) | Device and method for efficiently recycling DMF (dimethyl formamide) from wastewater | |
| CN101412671B (en) | Method for separating isobutyl acetate, ethanol and water by azeotropic distillation | |
| CN101289362B (en) | Process for preparing 1-amylene by separating C5 distillate of petroleum | |
| CN106478339B (en) | Method for separating cyclopentane and 2, 2-dimethylbutane | |
| CN105111046A (en) | New technology for separating isopropanol-isopropyl ether azeotrope by using ionic liquids | |
| CN104447198A (en) | Novel separation technology for preparation of isopropanol by acetone hydrogenation | |
| CN1956928A (en) | Removal of propylene glycol and propylene glycol ethers from aqueous streams | |
| CN106349107B (en) | A kind of method and device of heterogeneous azeotropic rectification separating acetonitrile-triethylamine mixture | |
| CN111377801B (en) | Method and system for refining low carbon alcohol | |
| CN103936642B (en) | The method of purification of vitamin A isomer in a kind of vitamin A mother solution | |
| CN104693005A (en) | New process for separating methanol-propyl formate azeotrope through extractive distillation | |
| CN109704908B (en) | Method for preparing hexane from aromatic raffinate oil | |
| CN109503360A (en) | A kind of technique for spirit of vinegar recycling | |
| CN104961624A (en) | Butyl octanol production waste liquid recovery and recycle method | |
| CN1226261C (en) | Liquid-liquid extraction process of dioxyethyl methane and water solution of ethanol | |
| CN106187717B (en) | The method for being thermally integrated variable-pressure rectification separation methyl tertiary butyl ether(MTBE) and methanol azeotrope |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131113 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |