CN106187954A - A kind of method preparing anhydrous level oxolane - Google Patents
A kind of method preparing anhydrous level oxolane Download PDFInfo
- Publication number
- CN106187954A CN106187954A CN201610535251.9A CN201610535251A CN106187954A CN 106187954 A CN106187954 A CN 106187954A CN 201610535251 A CN201610535251 A CN 201610535251A CN 106187954 A CN106187954 A CN 106187954A
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- China
- Prior art keywords
- oxolane
- preparation
- reagent
- anhydrous level
- anhydrous
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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
Abstract
The invention discloses the preparation method of a kind of anhydrous level oxolane reagent, this preparation method comprises the steps: that first passing through grignard reaction is converted into high boiling point or low voc compounds by the trace alcohol in Industrial Grade Tetrahydrofuran, carbonyl compound and peroxide, rectification is further used to obtain anhydrous level oxolane, advantages of the present invention is that the response rate is high, preparation method is simple, efficiently, it is adaptable to the production of high purity reagent.
Description
Technical field
The invention belongs to chemical technology field, disclose a kind of method preparing anhydrous level oxolane.
Background technology
Oxolane is a kind of fine solvent, in practice often due to aqueous exceeding standard and cannot use, conventional
Oxolane dewatering system mostly is stationary stream device, owing to oxolane is miscible with water, is dehydrated precision by the method for rectification and receives
Limit, only up to take off to 400 to 500PPm, and it is miscellaneous to use the method for adsorption filtration cannot remove other in oxolane
Matter.
In the prior art, prepare the conventional method of anhydrous level oxolane and mainly have a following two: (1) with nitrogen by four
Hydrogen furan is extruded by basin, enters in distillating still, adds reagent in distillating still, and reagent and water react formation high boiling point chemical combination
Thing, heating pot temperature is raised to 80-90 DEG C and is steamed by oxolane, and the distillation column condensed device of oxolane steam out is cold
After Ning, flow automatically to basin.Disadvantage of this method is that: this technique is merely except water, it is impossible to effectively remove in oxolane contained miscellaneous
Matter.
(2) oxolane will be contained through repeatedly distillation and concentration, progressively the content of oxolane is improved, then use calcium oxide
Dehydration, filters, and it is characterized in that the filtrate after the dehydration of oxidized calcium, filtration is dehydrated with grignard reagent and removes peroxide, then steams
Evaporating, isolation moisture is collected the fraction of 65-68 DEG C and is obtained that water content is low, oxolane without peroxide.The shortcoming of this method exists
In: complex operation, use calcium oxide dehydration, post processing cost increases, and gained content of tetrahydrofuran is relatively low.
Summary of the invention
In place of it is an object of the invention to according to above-mentioned the deficiencies in the prior art, it is provided that a kind of prepare anhydrous level oxolane
Method, the alcohol of trace, carbonyl compound, peroxide etc. in industry oxolane are converted by this preparation method by grignard reaction
For low boiling or higher-boiling compound, then obtain anhydrous level oxolane through rectification.
The object of the invention realizes being completed by techniques below scheme:
A kind of a kind of method preparing anhydrous level oxolane, it is characterised in that described preparation method is: anhydrous level oxolane
The preparation method of reagent, it is characterised in that described preparation method comprises the steps: to first pass through grignard reaction by industry tetrahydrochysene
Trace alcohol, carbonyl compound and peroxide in furan reagent are converted into low boiling or higher-boiling compound, then pass through rectification
Obtain anhydrous level oxolane.
The step of described grignard reaction is: 1), under N2 protects, and adds 10-20g magnesium in industry oxolane described in 1L
Bits；2), heat described step 1) and in described step 1) drip bromoethane 15-30g carry out grignard reaction；3), backflow 1-2
Hour.
Using by the oxolane after described grignard reaction as rectification raw material, carry out rectification, collecting midbarrel is institute
State anhydrous rank oxolane, front-end volatiles and last residual fraction returned in raw material, process for next time.
Collect described front-end volatiles weight ratio 8-12% and return in described raw material with described residual fraction weight ratio 10-15%,
Process for next time.
Described front-end volatiles and described last residual fraction process through 6 times.
The beneficial effects of the present invention is: the response rate is high, preparation method is simple, efficiently, it is adaptable to the production of high purity reagent.
Detailed description of the invention
By the following examples inventive feature and other correlated characteristic are described in further detail, in order to colleague
The understanding of industry technical staff:
Embodiment 1: the present embodiment is specifically related to a kind of method preparing anhydrous level oxolane, this preparation method specifically include as
Lower step:
(1) under N2 protects, 1L industry oxolane adds 10g magnesium chips, heat and drip bromoethane 15g to carry out grignard anti-
Should, it is then refluxed for 2 hours；
(2) rectification, the fraction of front 12% separates as raw material, remains process next time；Middle 70% fraction is product；Remainder fractionation
Recycling next time in the reactor；
(3) front-end volatiles and residual oxolane process through 6 times, and overall recovery is 88%；Obtain the content of anhydrous level product >=
99.99%(wt), moisture≤20ppm.
Embodiment 2: the present embodiment is specifically related to a kind of method preparing anhydrous tetrahydro furan, this preparation method specifically includes
Following steps:
(1) under N2 protects, 1L industry oxolane adds 15g magnesium chips, heat and drip bromoethane 25g to carry out grignard anti-
Should, it is then refluxed for 1.5 hours；
(2) rectification, the fraction of front 10% separates as raw material, remains process next time；Middle 75% fraction is product；Remainder fractionation
Recycling next time in the reactor；
(3) front-end volatiles and residual oxolane process through 6 times, and overall recovery is 89%；Obtain the content of anhydrous level product >=
99.99%(wt), moisture≤20ppm.
Embodiment 3: the present embodiment is specifically related to a kind of method preparing anhydrous tetrahydro furan, this preparation method specifically includes
Following steps:
(1) under N2 protects, 1L industry oxolane adds 20g magnesium chips, heat and drip bromoethane 30g to carry out grignard anti-
Should, it is then refluxed for 1 hour；
(2) rectification, the fraction of front 8% separates as raw material, remains process next time；Middle 75% fraction is product；Remainder fractionation
Recycling next time in the reactor；
(3) front-end volatiles and residual oxolane process through 6 times, and overall recovery is 89%；Obtain the content of anhydrous level product >=
99.99%(wt), moisture≤20ppm.
Claims (5)
1. the preparation method of an anhydrous level oxolane reagent, it is characterised in that described preparation method comprises the steps: head
First pass through grignard reaction by industry oxolane reagent in trace alcohol, carbonyl compound and peroxide be converted into low boiling or
Higher-boiling compound, then obtain anhydrous level oxolane by rectification.
The preparation method of a kind of anhydrous level oxolane reagent the most according to claim 1, it is characterised in that: described grignard
The step of reaction is:
1), under N2 protects, in industry oxolane described in 1L, 10-20g magnesium chips is added；
2), heat described step 1) and in described step 1) drip bromoethane 15-30g carry out grignard reaction；
3), backflow 12 hours.
The preparation method of a kind of anhydrous level oxolane reagent the most according to claim 1, it is characterised in that: by described lattice
The reacted oxolane of family name, as rectification raw material, carries out rectification, and collecting midbarrel is described anhydrous rank oxolane, will
Front-end volatiles and last residual fraction return in raw material, process for next time.
The preparation method of a kind of anhydrous level oxolane reagent the most according to claim 3, it is characterised in that: collect described
Front-end volatiles weight ratio 8 12% and described residual fraction weight ratio 10-15% return in described raw material, process for next time.
The preparation method of a kind of anhydrous level oxolane reagent the most according to claim 5, it is characterised in that: its feature exists
In, described front-end volatiles and described last residual fraction process through 6 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610535251.9A CN106187954A (en) | 2016-07-08 | 2016-07-08 | A kind of method preparing anhydrous level oxolane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610535251.9A CN106187954A (en) | 2016-07-08 | 2016-07-08 | A kind of method preparing anhydrous level oxolane |
Publications (1)
| Publication Number | Publication Date |
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| CN106187954A true CN106187954A (en) | 2016-12-07 |
Family
ID=57473287
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610535251.9A Pending CN106187954A (en) | 2016-07-08 | 2016-07-08 | A kind of method preparing anhydrous level oxolane |
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| CN (1) | CN106187954A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749115A (en) * | 2016-11-11 | 2017-05-31 | 上海沃凯生物技术有限公司 | A kind of preparation method of anhydrous level tetrahydrofuran |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2016
- 2016-07-08 CN CN201610535251.9A patent/CN106187954A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 荣国斌 主编: "《大学有机化学基础（第二版）上册》", 31 August 2006, 华东理工大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749115A (en) * | 2016-11-11 | 2017-05-31 | 上海沃凯生物技术有限公司 | A kind of preparation method of anhydrous level tetrahydrofuran |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161207 |
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| RJ01 | Rejection of invention patent application after publication |