CN1760191A - Method for batch extracting rectified purified tetrahydrofuran - Google Patents
Method for batch extracting rectified purified tetrahydrofuran Download PDFInfo
- Publication number
- CN1760191A CN1760191A CN 200510016029 CN200510016029A CN1760191A CN 1760191 A CN1760191 A CN 1760191A CN 200510016029 CN200510016029 CN 200510016029 CN 200510016029 A CN200510016029 A CN 200510016029A CN 1760191 A CN1760191 A CN 1760191A
- Authority
- CN
- China
- Prior art keywords
- tower
- tetrahydrofuran
- water
- thf
- extraction agent
- 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
Images
Landscapes
- Furan Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A process for refining tetraphdrofuran is disclosed. Its system is composed of rectifying tower, pump, extractant storage tank, condenser, reflux tank and product storage tank. Its preparing steps includes adding the azeotrope or azeotrope-similar mixture of tetraphdrofuran and water to rectifying tower, full reflux reaction, adding 1,2-propanediol as extractant, continuous full reflux reaction, tapping high-purity (99.7%) tetrahpdrofuran from tower top, tapping water from tower top at particular temp, and recovering high-purity 1,2-propanediol.
Description
Technical field
The present invention relates to a kind of method of batch extracting rectified purified tetrahydrofuran, belong to the isolation technique of the azeotropic mixture of tetrahydrofuran (THF) and water.
Background technology
Tetrahydrofuran (THF) has another name called 1; 4-oxyethane (being called for short THF); it is a kind of valuable organic solvent of excellent property; has widespread use at chemical industry, medicine in producing; be commonly used for reactive solvents; the title that " menstruum universale " arranged generally is used for the surface treatment of topcoating, protective coating, printing ink, extraction agent and leatheroid.In the medicine industry, can be used for producing pentoxiverin, Progesterone, sharp multiple Lei Su etc.Has good volatility.Can be used for accurate tape industry and be used for the tackiness agent aspect.It also is used for the synthesis material of multiple Chemicals in addition, as nylon 66, polytetrahydrofuran etc.Tetrahydrofuran (THF) and water form minimum azeotrope under the normal pressure, 64 ℃ of azeotropic temperature, and moisture 6.7% (mass fraction), the conventional distillation method can't obtain highly purified tetrahydrofuran (THF).
From the existing literature report, separate THF-H
2The O azeotrope mainly adopts three kinds of methods---extracting rectifying, membrane separation process and general chemical process.But back two kinds of methods also are only limited to the laboratory study stage, and industrialized have only extracting rectifying." chemical industry environmental protection ", 1999 the 19th the 1st phases of volume, 12-16 has reported with the reaction, extraction distillation technology and has removed THF-H
2Moisture among the O, in rectifying to THF-H
2Add ethylene glycol sodium in the O mixture, make it to take place reversible reaction:
In this reversible reaction, ethylene glycol sodium plays " carrier " effect, it and water in the separated system react generation ethylene glycol and sodium hydroxide.And in the solvent recuperation process, ethylene glycol and sodium hydroxide reaction generate ethylene glycol sodium and water, and promptly ethylene glycol sodium constantly goes out the water ballast in the system, and itself does not change.The THF purity that this method obtains can reach 99.4%.
US:Appl.222727 proposes with 1, the 4-butyleneglycol as extraction agent to THF-H
2The O azeotrope carries out extracting rectifying to be separated.Operating temperature range is 40～60 ℃, pressure range is 0.1～9.8bar, tetrahydrofuran (THF) reclaims as one discharging of rectifying tower, one discharging then is 1 in addition, the mixture of 4-butyleneglycol and water, and water can more easily be separated from mixture, thereby make 1, the 4-butyleneglycol recycles, and has avoided existing among the patent EP-A-0255400 danger of blast, and this method is the major industry method of removing moisture in the tetrahydrofuran (THF) at present.
In addition, US:appl.303325 uses the mixture of 1-propylene di-alcohol as extraction agent separation of tetrahydrofuran and water, and the tetrahydrofuran (THF) water content that this method obtains is 140ppm only.Hungarian Dencs, Bela, Mrs. etc. remove water with tetracol phenixin as extraction agent, and the content of water is less than 0.1g/dm
3
All there is certain problem in above the whole bag of tricks, especially extraction agent cost an arm and a leg and usage quantity big, present 1, the 4-butyleneglycol is most economical, the extraction agent that separating effect is best, but bigger solvent ratio has increased the load of extractive distillation column and solvent recovery tower, and energy expenditure and facility investment are all bigger.
Summary of the invention
The method that the purpose of this invention is to provide a kind of batch extracting rectified purified tetrahydrofuran, the tetrahydrofuran (THF) product quality height that this method obtains.
The present invention is realized by the following technical programs: a kind of method of batch extracting rectified purified tetrahydrofuran, this method adopts by rectifying tower, pump, the extraction agent storage tank, condenser, the extracting rectifying device that return tank and product storage tank constitute, realize batch extracting rectified purified tetrahydrofuran, it is characterized in that comprising following process: in the tower still of the disposable adding rectifying tower of mixture of the azeotrope that tetrahydrofuran (THF) and water are formed or tetrahydrofuran (THF) of forming near azeotropic and water, normal pressure was 60～80 ℃ of following total refluxs of tower still temperature 0.5～2 hour, add 1 then, the 2-propylene glycol is an extraction agent, the quality of extraction agent is 1.5～2.5 times of azeotrope quality to be separated, and be controlled at 65～66 ℃ in tower top temperature, tower still temperature is controlled at 70～190 ℃, continue to keep the total reflux state 0.5～2 hour, be 1～5 with reflux ratio then, reach more than the 99.7wt% from cat head extraction purity, the content of water is lower than 0.24wt% tetrahydrofuran (THF) product, when tower top temperature surpasses 66 ℃, stops to add extraction agent.Again with reflux ratio 1～3, tower still temperature is at 100～190 ℃, and behind the cat head recovered water, it is pure 1 that the tower still obtains, the 2-propylene glycol.
Advantage of the present invention is: technology is simple, need not to carry out scrap build, and yield is good, the quality product height.The extraction agent 1 that extraction agent that uses and prior art are used, the 4-butyleneglycol is compared, and has not only significantly reduced the consumption of extraction agent, and has reduced the temperature of tower still, has reduced required energy consumption in the process, and 1, the toxicity of 2-propylene glycol is little, and is cheap, reclaims easily.
Description of drawings
The device synoptic diagram of Fig. 1 for realizing that the present invention adopts.
Among the figure, 1 is the rectifying tower tower body, and 2 is muff, and 3 are rectifying Tata still, and 4 is pump, and 5 is the extraction agent storage tank, and 6 is condenser, and 7 is return tank, and 8 is the product storage tank.
Embodiment
Embodiment
Adopting internal diameter is the effective packed height 1m of 25mm, the rectifying tower of the efficient stainless steel θ ring filler of interior dress 3mm * 3mm, and theoretical plate number is 30, the working pressure of rectifying tower is a normal pressure.The tower still is the 250ml there-necked flask, adds raw material 100ml (tetrahydrofuran (THF) of moisture 12.7wt%) to the tower still.Open the electrically heated cover, keep total reflux 40min, tower top temperature is controlled at 62～64 ℃, and tower still temperature is controlled at 64～70 ℃.Add 1 of 150ml from cat head with the speed of 60ml/h then, 2-propylene glycol extraction agent continues to keep total reflux 0.5h, and tower top temperature is controlled at 66 ℃, and tower still temperature is controlled at 80～190 ℃.Then be 3 speed extraction product, after tower top temperature surpasses 66 ℃, show the extraction of most of tetrahydrofuran (THF), continue heating with reflux ratio, keep reflux ratio constant, from the cat head recovered water, when tower still temperature rises to 185-190 ℃, by tower still extraction 1,2-propylene glycol.
Overhead product consists of tetrahydrofuran (THF) 99.76wt% through gas chromatographic analysis, water 0.24wt%, and the extraction agent 1 of recovery, the 2-content of propylene glycol reaches 99.9wt%.
Claims (1)
1. the method for a batch extracting rectified purified tetrahydrofuran, this method adopts by rectifying tower, pump, the extraction agent storage tank, condenser, the extracting rectifying device that return tank and product storage tank constitute, realize batch extracting rectified purified tetrahydrofuran, it is characterized in that comprising following process: in the tower still of the disposable adding rectifying tower of mixture of the azeotrope that tetrahydrofuran (THF) and water are formed or tetrahydrofuran (THF) of forming near azeotropic and water, normal pressure was 60～80 ℃ of following total refluxs of tower still temperature 0.5～2 hour, add 1 then, the 2-propylene glycol is an extraction agent, the quality of extraction agent is 1.5～2.5 times of azeotrope quality to be separated, and be controlled at 65～66 ℃ in tower top temperature, tower still temperature is controlled at 70～190 ℃, continue to keep the total reflux state 0.5～2 hour, be 1～5 with reflux ratio then, reach more than the 99.7wt% from cat head extraction purity, the content of water is lower than 0.24wt% tetrahydrofuran (THF) product, when tower top temperature surpasses 66 ℃, stop to add extraction agent, again with reflux ratio 1～3, tower still temperature is at 100～190 ℃, behind the cat head recovered water, it is pure 1 that the tower still obtains, the 2-propylene glycol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510016029XA CN1313454C (en) | 2005-11-11 | 2005-11-11 | Method for batch extracting rectified purified tetrahydrofuran |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510016029XA CN1313454C (en) | 2005-11-11 | 2005-11-11 | Method for batch extracting rectified purified tetrahydrofuran |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1760191A true CN1760191A (en) | 2006-04-19 |
| CN1313454C CN1313454C (en) | 2007-05-02 |
Family
ID=36706437
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510016029XA Expired - Fee Related CN1313454C (en) | 2005-11-11 | 2005-11-11 | Method for batch extracting rectified purified tetrahydrofuran |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1313454C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101596371B (en) * | 2009-06-29 | 2011-04-06 | 天津大学 | Device for purifying formic acid solution with interval azeotropic distillation and method thereof |
| CN103435445A (en) * | 2013-08-20 | 2013-12-11 | 天津科林泰克科技有限公司 | Method for separating mixture of ethanol alcohol and water |
| CN103449969A (en) * | 2013-09-05 | 2013-12-18 | 天津科林泰克科技有限公司 | Method and production unit for separating methanol-ethanol-isopropanol-water mixture |
| CN111620843A (en) * | 2019-10-28 | 2020-09-04 | 重庆大学 | Method for separating tetrahydrofuran-ethanol-water ternary azeotropic system by combining reactive distillation with side line extractive distillation |
| CN111892560A (en) * | 2020-07-20 | 2020-11-06 | 湖北华邦化学有限公司 | Recovery processing technology of tetrahydrofuran in step-by-step Grignard method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5464505A (en) * | 1994-05-31 | 1995-11-07 | Texaco Chemical Inc. | Use of propylene oxide adducts in the purification of propylene oxide by extractive distillation |
| US5958192A (en) * | 1997-08-27 | 1999-09-28 | Huntsman Specialty Chemicals Corporation | Purification of propylene oxide using ethylene glycol monomethyl ether as an extractive distillation agent |
| JP2000143652A (en) * | 1998-11-13 | 2000-05-26 | Mitsubishi Chemicals Corp | Purification of crude tetrahydrofuran |
-
2005
- 2005-11-11 CN CNB200510016029XA patent/CN1313454C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101596371B (en) * | 2009-06-29 | 2011-04-06 | 天津大学 | Device for purifying formic acid solution with interval azeotropic distillation and method thereof |
| CN103435445A (en) * | 2013-08-20 | 2013-12-11 | 天津科林泰克科技有限公司 | Method for separating mixture of ethanol alcohol and water |
| CN103449969A (en) * | 2013-09-05 | 2013-12-18 | 天津科林泰克科技有限公司 | Method and production unit for separating methanol-ethanol-isopropanol-water mixture |
| CN111620843A (en) * | 2019-10-28 | 2020-09-04 | 重庆大学 | Method for separating tetrahydrofuran-ethanol-water ternary azeotropic system by combining reactive distillation with side line extractive distillation |
| CN111892560A (en) * | 2020-07-20 | 2020-11-06 | 湖北华邦化学有限公司 | Recovery processing technology of tetrahydrofuran in step-by-step Grignard method |
| CN111892560B (en) * | 2020-07-20 | 2022-08-12 | 湖北华邦化学有限公司 | Recovery processing technology of tetrahydrofuran in step-by-step Grignard method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1313454C (en) | 2007-05-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105175633B (en) | A kind of Combined stone oleoresin hydrotreating method and processing system | |
| US5185481A (en) | Method for the separation of impurities from crude ethanol aqueous solution | |
| CN1760191A (en) | Method for batch extracting rectified purified tetrahydrofuran | |
| CN102816281A (en) | Method for preparing C5 petroleum resin for traffic paint | |
| CN111205248A (en) | Deacidifying method in propylene oxide refining process | |
| CN110304990B (en) | Green process for producing vinyl beta-ionol | |
| EP2573066B1 (en) | Method for preparing a lactate | |
| CN101830788A (en) | Method for separating azeotropic mixture of ethyl methyl ketone and water through variable-pressure rectification | |
| CN106588828A (en) | Separation and purification method of THF (tetrahydrofuran) distillation waste liquid | |
| CN101056841A (en) | Method for preparing asymmetric linear carbonate | |
| CN106478339B (en) | Method for separating cyclopentane and 2, 2-dimethylbutane | |
| CN107556172B (en) | Process method for producing ethylene glycol mono-tert-butyl ether | |
| JP5356455B2 (en) | Method for separating glycol mono-tert-butyl ether and glycol di-tert-butyl ether | |
| CN100445259C (en) | Method for removing heavy hydrocarbon from reaction product of preparation of sec-butyl acetate | |
| CN106866373B (en) | Method for rectifying and refining ethylene glycol | |
| CN113121346A (en) | Purification method of electronic grade dimethyl carbonate | |
| CN1102826A (en) | improved synthetic method of dialkyl carbonate | |
| CN109704919A (en) | Water-methanol-ethanol mixture extractive distillation separation method based on choline chloride eutectic solvent | |
| CN111875469B (en) | Ultra-deep removal method for carbon disulfide in isoprene product | |
| CN110845349B (en) | Purification method of Sacubitril valsartan sodium intermediate | |
| CN218945032U (en) | Preparation facilities of electron level trimethyl silane | |
| CN102219689A (en) | Method for producing dimethyl terephthalate (DMT) | |
| CN102372564B (en) | Method for preparing ethene by ethanol dehydration | |
| CN1660828A (en) | Method for retrieving tetrahydrofuran from waste of pharmacy | |
| CN220513452U (en) | Piperidine separation and purification system |
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 | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |