CN106749115A - A kind of preparation method of anhydrous level tetrahydrofuran - Google Patents
A kind of preparation method of anhydrous level tetrahydrofuran Download PDFInfo
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- CN106749115A CN106749115A CN201610994423.9A CN201610994423A CN106749115A CN 106749115 A CN106749115 A CN 106749115A CN 201610994423 A CN201610994423 A CN 201610994423A CN 106749115 A CN106749115 A CN 106749115A
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- tetrahydrofuran
- anhydrous level
- preparation
- anhydrous
- level tetrahydrofuran
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/04—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D307/06—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D307/08—Preparation of tetrahydrofuran
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- Organic Chemistry (AREA)
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Abstract
The invention belongs to technical field of chemical engineering, and in particular to a kind of preparation method of anhydrous level tetrahydrofuran, it is comprised the following steps：(1) in N2Under protective condition, to magnesium chips is added in industrial tetrahydrofuran, heating and be added dropwise bromoethane carries out grignard reaction；(2) back flow reaction liquid；(3) rectifying obtains high-purity anhydrous level tetrahydrofuran.The method of the present invention first passes through grignard reaction and removes the impurity such as micro alcohol, carbonyls, peroxide, then rectifying obtains high-purity anhydrous level tetrahydrofuran, and the anhydrous level tetrahydrofuran purity of preparation is high.
Description
Technical field
The invention belongs to technical field of chemical engineering, and in particular to a kind of preparation method of anhydrous level tetrahydrofuran.
Background technology
Tetrahydrofuran is a kind of fine solvent, often due to aqueous exceeded and cannot use in practice.Conventional
Tetrahydrofuran dewatering system is generally stationary stream device, because tetrahydrofuran is miscible with water, is directly dehydrated precision with the method for rectifying
It is restricted, only up to takes off to 400 to 500PPm.And its that cannot remove in tetrahydrofuran using the method for adsorption filtration
His impurity.
Preparing the conventional method of anhydrous tetrahydro furan mainly has following two：
(1) tetrahydrofuran is extruded by basin with nitrogen, into distillation still, adds reagent in distillation still, reagent with
Water reacts to form higher-boiling compound, and heating pot temperature is raised to 80-90 DEG C and steams tetrahydrofuran, distillation column out four
After the condensed device condensation of hydrogen furans steam, basin is flowed automatically to.Disadvantage of this method is that：The technique is removed water merely, it is impossible to effectively
Impurities in removal tetrahydrofuran.
(2) tetrahydrofuran waste liquid will be contained by multiple distillation and concentration, progressively the content of tetrahydrofuran will be improved, oxygen will then be used
Change calcium dehydration, filtering, it is characterized in that the filtrate after the dehydration of oxidized calcium, filtering is dehydrated with grignard reagent and removes peroxide again,
Redistillation, isolation moisture collects 65-68 DEG C of cut and obtains that water content is low, tetrahydrofuran without peroxide.This method lack
Put and be：It is cumbersome, it is dehydrated using calcium oxide, post processing cost increases, and the relatively low (moisture of gained content of tetrahydrofuran
＜ 0.1ppm, content ＞ 99.5%).
The content of the invention
Invention broadly provides a kind of preparation method of anhydrous level tetrahydrofuran, grignard reaction removing is first passed through micro
The impurity such as alcohol, carbonyls, peroxide, then rectifying obtains high-purity anhydrous level tetrahydrofuran, the anhydrous level tetrahydrochysene of preparation
Furans purity is high.Its technical scheme is as follows：
A kind of preparation method of anhydrous level tetrahydrofuran, comprises the following steps：
(1) in N2Under protective condition, to magnesium chips is added in industrial tetrahydrofuran, heating and be added dropwise bromoethane, to carry out grignard anti-
Should；
(2) back flow reaction liquid；
(3) rectifying obtains high-purity anhydrous level tetrahydrofuran.
Preferably, 10-20g magnesium chips, 15-30g bromoethanes are added in 1L industry tetrahydrofuran in step (1).
Preferably, back flow reaction liquid 1-2h in step (2).
Preferably, the specific method of rectifying is in step (3), the cut of 8-12% and last 10-15% weight before collecting
Integrate with raw material, the cut for collecting remaining stage is the anhydrous level tetrahydrofuran of product.
Preferably, the overall recovery of anhydrous level tetrahydrofuran is 85-90%, the content of anhydrous level tetrahydrofuran >=
99.99wt%, moisture≤20ppm.
Using the preparation method of above-mentioned anhydrous level tetrahydrofuran, the present invention has advantages below：
The impurity such as micro alcohol, carbonyls, peroxide in industrial tetrahydrofuran can be removed by grignard reaction,
Then high-purity anhydrous tetrahydro furan is obtained by rectifying, its content >=99.99wt%, moisture≤20ppm.
Specific embodiment
Embodiment 1
(1) in N2Under protection, 10g magnesium chips is added in 1L industry tetrahydrofurans, heating and be added dropwise bromoethane 15g carries out grignard
Reaction, is then refluxed for 2 hours；
(2) rectifying：The cut of preceding 12% weight is front-end volatiles, and front-end volatiles are separated as raw material, remain next treatment, middle
73% cut is product, and remaining cut stays recycling next time in the reactor；
(3), through 6 treatment, overall recovery is 88% for front-end volatiles and residual tetrahydrofuran；Obtain the content of anhydrous level product
>=99.99% (wt), moisture≤20ppm.
Embodiment 2
(1) in N2Under protection, 15g magnesium chips is added in 1L industry tetrahydrofurans, heating and be added dropwise bromoethane 25g carries out grignard
Reaction, is then refluxed for 1.5 hours；
(2) rectifying：The cut of preceding 10% weight is front-end volatiles, and front-end volatiles are separated as raw material, remain next treatment, middle
80% cut is product, and remaining cut stays recycling next time in the reactor；
(3), through 6 treatment, overall recovery is 89% for front-end volatiles and residual tetrahydrofuran；Obtain the content of anhydrous level product
>=99.99% (wt), moisture≤20ppm.
Embodiment 3
(1) in N2Under protection, 20g magnesium chips is added in 1L industry tetrahydrofurans, heating and be added dropwise bromoethane 30g carries out grignard
Reaction, is then refluxed for 1 hour；
(2) rectifying：The cut of preceding 8% weight is front-end volatiles, and front-end volatiles are separated as raw material, remain next treatment, middle
82% cut is product, and remaining cut stays recycling next time in the reactor；
(3), through 6 treatment, overall recovery is 89% for front-end volatiles and residual tetrahydrofuran；Obtain the content of anhydrous level product
>=99.99% (wt), moisture≤20ppm.
It will be apparent to those skilled in the art that technical scheme that can be as described above and design, make other various
It is corresponding to change and deformation, and all these change and deformation should all belong to the protection domain of the claims in the present invention
Within.
Claims (5)
1. a kind of preparation method of anhydrous level tetrahydrofuran, it is characterised in that：Comprise the following steps：
(1) in N2Under protective condition, to magnesium chips is added in industrial tetrahydrofuran, heating and be added dropwise bromoethane carries out grignard reaction；
(2) back flow reaction liquid；
(3) rectifying obtains high-purity anhydrous level tetrahydrofuran.
2. the preparation method of anhydrous level tetrahydrofuran according to claim 1, it is characterised in that：1L industry in step (1)
10-20g magnesium chips, 15-30g bromoethanes are added in tetrahydrofuran.
3. the preparation method of anhydrous level tetrahydrofuran according to claim 1, it is characterised in that：Backflow is anti-in step (2)
Answer liquid 1-2h.
4. the preparation method of anhydrous level tetrahydrofuran according to claim 1, it is characterised in that：Rectifying in step (3)
Specific method is during the cut of 8-12% and last 10-15% weight integrates with raw material before collecting, to collect the cut in remaining stage
It is the anhydrous level tetrahydrofuran of product.
5. the preparation method of anhydrous level tetrahydrofuran according to claim 1, it is characterised in that：Anhydrous level tetrahydrofuran
Overall recovery is 85-90%, the content >=99.99wt% of anhydrous level tetrahydrofuran, moisture≤20ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610994423.9A CN106749115A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method of anhydrous level tetrahydrofuran |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610994423.9A CN106749115A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method of anhydrous level tetrahydrofuran |
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| CN106749115A true CN106749115A (en) | 2017-05-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610994423.9A Pending CN106749115A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method of anhydrous level tetrahydrofuran |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5387348A (en) * | 1977-01-10 | 1978-08-01 | Toyo Soda Mfg Co Ltd | Method of purifying tetrahydrofuran |
| CN101555238A (en) * | 2009-05-21 | 2009-10-14 | 广西万德药业股份有限公司 | Method for tetrahydrofuran recycling |
| CN101723922A (en) * | 2009-11-18 | 2010-06-09 | 天津市康科德科技有限公司 | Method for purifying high-purity organic solvent tetrahydrofuran for scientific research |
| CN106187954A (en) * | 2016-07-08 | 2016-12-07 | 上海沃凯生物技术有限公司 | A kind of method preparing anhydrous level oxolane |
-
2016
- 2016-11-11 CN CN201610994423.9A patent/CN106749115A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5387348A (en) * | 1977-01-10 | 1978-08-01 | Toyo Soda Mfg Co Ltd | Method of purifying tetrahydrofuran |
| CN101555238A (en) * | 2009-05-21 | 2009-10-14 | 广西万德药业股份有限公司 | Method for tetrahydrofuran recycling |
| CN101723922A (en) * | 2009-11-18 | 2010-06-09 | 天津市康科德科技有限公司 | Method for purifying high-purity organic solvent tetrahydrofuran for scientific research |
| CN106187954A (en) * | 2016-07-08 | 2016-12-07 | 上海沃凯生物技术有限公司 | A kind of method preparing anhydrous level oxolane |
Non-Patent Citations (2)
| Title |
|---|
| 郑仙珏: "四氢呋喃的回收提纯", 《环境科学与技术》 * |
| 齐润红，乔世璋，朱宝福: "工业级四氢呋喃的精制", 《石油化工》 * |
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Application publication date: 20170531 |