CN108191795A - The method of purification of chromatographic grade tetrahydrofuran - Google Patents
The method of purification of chromatographic grade tetrahydrofuran Download PDFInfo
- Publication number
- CN108191795A CN108191795A CN201810077958.9A CN201810077958A CN108191795A CN 108191795 A CN108191795 A CN 108191795A CN 201810077958 A CN201810077958 A CN 201810077958A CN 108191795 A CN108191795 A CN 108191795A
- Authority
- CN
- China
- Prior art keywords
- tetrahydrofuran
- purification
- chromatographic grade
- activated carbon
- chromatography
- 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.)
- Pending
Links
Classifications
-
- 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 a kind of methods of purification of chromatographic grade tetrahydrofuran, which is characterized in that includes the following steps：A, raw material tetrahydrofuran is taken, uses oxidation, plant fiber activated carbon adsorption；B, by the rectifying under nitrogen protection of step a resulting products.The method of purification of chromatographic grade tetrahydrofuran provided by the invention, it adsorbs to obtain the tetrahydrofuran of purity >=99.99% (wt) by modified activated carbon, the tetrahydrofuran that purification obtains is made to can be applied to the fields such as chromatography, chromatographic isolation, chromatography preparation, expands application range.
Description
Technical field
The present invention relates to solvent purifications field, more particularly to a kind of method of purification of chromatographic grade tetrahydrofuran.
Background technology
Chromatorgaphy reagent refers to the chemical reagent prepared for chromatography, chromatographic isolation, chromatography.Because chromatography type is more, mistake
Journey is complicated, therefore chromatorgaphy reagent is categorized into a variety of different chromatorgaphy reagents such as again：Gas-chromatography reagent, high pressure liquid chromatography examination
Agent, reagent for thin-layer chromatography, column chromatography chromatogram reagent, ion chromatography reagent, Ion-pair chromalography reagent etc..Tetrahydrofuran is as a kind of
Reagents for high performance liquid chromatography, for liquid-phase chromatographic analysis, in the fields extensive use such as medication chemistry, check analysis, detection.
The preparation method of China's tetrahydrofuran liquid chromatogram reagent seldom has been reported that, and the yield of domestic tetrahydrofuran compared with
It is low, it is not high containing impurity, purity such as aldehydes, benzene class, water.High-purity tetrahydrofuran relies on import mostly, causes cost higher, by
It is larger that foreign technology restrains degree.Tetrahydrofuran is oxidizable, needs to add antioxidant to prevent tetrahydrochysene during transport, storage
Furans aoxidizes.So it is particularly urgent to develop a kind of method of tetrahydrofuran purification.
Invention content
The purpose of the invention is to overcome deficiency of the prior art, a kind of color for improving tetrahydrofuran purity is provided
The method of purification of spectrum level tetrahydrofuran.
In order to achieve the above object, the invention is realized by the following technical scheme：
The method of purification of chromatographic grade tetrahydrofuran, which is characterized in that include the following steps：
A. raw material tetrahydrofuran is taken, uses oxidation, plant fiber activated carbon adsorption ()；
B. by the rectifying under nitrogen protection of step a resulting products.
In the present invention, rectifying can remove the BHT stabilizers in industrial raw material.
According to one embodiment of present invention, the plant fiber activated carbon is after steam, pure water, 180~200
It is reused after drying and processing in step A at DEG C.
According to one embodiment of present invention, the plant fiber activated carbon is coconut husk charcoal.
According to one embodiment of present invention, the nitrogen pressure is 0.05~0.1MPa
The method of purification of chromatographic grade tetrahydrofuran provided by the invention, by modified activated carbon adsorb to obtain purity >=
The tetrahydrofuran of 99.99% (wt), makes the tetrahydrofuran that purification obtains can be applied to chromatography, chromatographic isolation, chromatography system
It is standby to wait fields, expand application range.Method of purification provided by the invention, the production for having filled up domestic high-purity tetrahydrofuran are empty
In vain, cost needed for import is reduced, while alleviates the degree restrained by foreign technology.Method of purification provided by the invention, production
Product yield >=95%, high income, while also have low energy consumption, production process is easy, it is stable, suitable for industrialized production etc.
Advantage.Rectifying is protected using nitrogen, can prevent tetrahydrofuran from aoxidizing and moisture can be isolated.
Specific embodiment
The present invention is described in detail with reference to embodiment：
Embodiment 1
The method of purification of chromatographic grade tetrahydrofuran, includes the following steps：
A. the raw material tetrahydrofuran that purity is 99.5% (wt) is taken, is added in using activated carbon made of aluminium oxide, coconut husk charcoal
Absorption.Activated carbon is for before adsorbing, first using steaming, after dried 4 hours at 180~190 DEG C.
B. rectifying under nitrogen protection, nitrogen pressure 0.05MPa, rectifying up to purity >=99.99% (wt) chromatography
Grade tetrahydrofuran.
Embodiment 2
The method of purification of chromatographic grade tetrahydrofuran, includes the following steps：
A. the raw material tetrahydrofuran that purity is 99.5% (wt) is taken, is added in using activated carbon made of aluminium oxide, coconut husk charcoal
Absorption.Activated carbon is for before adsorbing, first using steaming, after dried 5 hours at 190~200 DEG C.
B. rectifying under nitrogen protection, nitrogen pressure 0.07MPa, rectifying up to purity >=99.99% (wt) chromatography
Grade tetrahydrofuran.
Embodiment 3
The method of purification of chromatographic grade tetrahydrofuran, includes the following steps：
A. the raw material tetrahydrofuran that purity is 99.5% (wt) is taken, is added in using activated carbon made of aluminium oxide, coconut husk charcoal
Absorption.Activated carbon is for before adsorbing, first using steaming, after dried 3 hours at 185~195 DEG C.
B. rectifying under nitrogen protection, nitrogen pressure 0.1MPa, rectifying up to purity >=99.99% (wt) chromatographic grade
Tetrahydrofuran.
Embodiment 4
The method of purification of chromatographic grade tetrahydrofuran, includes the following steps：
A. the raw material tetrahydrofuran that purity is 99.5% (wt) is taken, is added in using activated carbon made of aluminium oxide, coconut husk charcoal
Absorption.
Activated carbon is for before adsorbing, first using steaming, after dried 6 hours at 190~195 DEG C.
B. rectifying under nitrogen protection, nitrogen pressure 0.06MPa, rectifying up to purity >=99.99% (wt) chromatography
Grade tetrahydrofuran.
Raw material data
Product data
After testing, each embodiment can reach above-mentioned technique effect.
The method of purification of chromatographic grade tetrahydrofuran provided by the invention, by modified activated carbon adsorb to obtain purity >=
The tetrahydrofuran of 99.99% (wt), makes the tetrahydrofuran that purification obtains can be applied to chromatography, chromatographic isolation, chromatography system
It is standby to wait fields, expand application range.Method of purification provided by the invention, the production for having filled up domestic high-purity tetrahydrofuran are empty
In vain, cost needed for import is reduced, while alleviates the degree restrained by foreign technology.Method of purification provided by the invention, production
Product yield >=95%, high income, while also have low energy consumption, production process is easy, it is stable, suitable for industrialized production etc.
Advantage.Rectifying is protected using nitrogen, can prevent tetrahydrofuran from aoxidizing and moisture can be isolated.
Embodiment in the present invention is only used for that the present invention will be described, and is not construed as limiting the scope of claims limitation,
Other substantially equivalent replacements that those skilled in that art are contemplated that, all fall in the scope of protection of the present invention.
Claims (4)
1. the method for purification of chromatographic grade tetrahydrofuran, which is characterized in that include the following steps：
A. raw material tetrahydrofuran is taken, uses oxidation, plant fiber activated carbon adsorption；
B. by the rectifying under nitrogen protection of step a resulting products.
2. the method for purification of chromatographic grade tetrahydrofuran according to claim 1, which is characterized in that the plant fiber activity
Charcoal is reused after drying and processing in step A after steam, pure water at 180~200 DEG C.
3. the method for purification of chromatographic grade tetrahydrofuran according to claim 1, which is characterized in that the plant fiber activity
Charcoal is coconut husk charcoal.
4. the method for purification of chromatographic grade tetrahydrofuran according to claim 1, which is characterized in that the nitrogen pressure is
0.05~0.1MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810077958.9A CN108191795A (en) | 2018-01-26 | 2018-01-26 | The method of purification of chromatographic grade tetrahydrofuran |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810077958.9A CN108191795A (en) | 2018-01-26 | 2018-01-26 | The method of purification of chromatographic grade tetrahydrofuran |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108191795A true CN108191795A (en) | 2018-06-22 |
Family
ID=62591329
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810077958.9A Pending CN108191795A (en) | 2018-01-26 | 2018-01-26 | The method of purification of chromatographic grade tetrahydrofuran |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108191795A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06179667A (en) * | 1992-12-14 | 1994-06-28 | Tosoh Corp | Production of tetrahydrofuran |
| CN105085444A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of chromatographic-grade tetrahydrofuran |
| CN106243067A (en) * | 2016-08-17 | 2016-12-21 | 太仓沪试试剂有限公司 | A kind of purification process of oxolane |
| CN107522678A (en) * | 2017-08-29 | 2017-12-29 | 湖北工程学院 | A kind of chromatogram pure tetrahydrofuran and preparation method thereof, production system |
-
2018
- 2018-01-26 CN CN201810077958.9A patent/CN108191795A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06179667A (en) * | 1992-12-14 | 1994-06-28 | Tosoh Corp | Production of tetrahydrofuran |
| CN105085444A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of chromatographic-grade tetrahydrofuran |
| CN106243067A (en) * | 2016-08-17 | 2016-12-21 | 太仓沪试试剂有限公司 | A kind of purification process of oxolane |
| CN107522678A (en) * | 2017-08-29 | 2017-12-29 | 湖北工程学院 | A kind of chromatogram pure tetrahydrofuran and preparation method thereof, production system |
Non-Patent Citations (1)
| Title |
|---|
| 刘自力 主编: "《林产化工生产技术》", 31 March 2005, 江西科学技术出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101570468B (en) | Method for preparing pesticide residue grade chromatographic ethanol | |
| CN101543762A (en) | Carbon dioxide adsorbent and method for preparing same | |
| CN101544551A (en) | Method for purifying high-purity organic solvent-acetone for scientific research | |
| CN103482624B (en) | Preparation method for active carbon with photocatalysis function | |
| CN102965199B (en) | Tea leaf aroma extraction method and application | |
| CN102093160B (en) | Method for preparing chromatographically-pure trichloromethane | |
| CN101570497A (en) | Method for purifying high-purity organic solvent acetonitrile for research | |
| CN101318717B (en) | Method and apparatus for removing and recycling organic phase in wastewater with distillation-free complete-molecular sieve | |
| CN102060674B (en) | Method for purifying high-purity organic solvent diethyl ether | |
| CN108191795A (en) | The method of purification of chromatographic grade tetrahydrofuran | |
| CN100384798C (en) | Prepn process of high purity alcohol reagent | |
| US9108897B2 (en) | Method for desorbing and regenerating butanol-adsorbing hydrophobic macroporous polymer adsorbent | |
| CN105884608A (en) | Method for separating levulinic acid from lignocellulose hydrolysate | |
| CN103159616B (en) | Decoloration method and purification method for solution containing critic acid | |
| CN102093268A (en) | Preparation method of chromatographic grade dimethyl sulfoxide | |
| US8766019B2 (en) | Method for separating butanol | |
| KR101865774B1 (en) | A process of producing bismuth graphene oxide and a process of adsorbing iodine using bismuth graphene oxide | |
| CN102875326B (en) | A kind of azeotropic-absorption method prepares the method for high-pure anhydrous methyl alcohol | |
| CN204952599U (en) | Exhaust treatment device who contains volatile organic compounds | |
| CN104744212B (en) | The method of purification of solvent gradient methanol | |
| CN107365246B (en) | Full-temperature-range adsorption extraction purification method of ultrapure isopropanol | |
| CN113087774A (en) | Method for removing echinocandin B mother nucleus degradation impurities | |
| CN102040496A (en) | Purification method of high-purity organic solvent 4-methyl-2-pentanone | |
| CN102008595B (en) | Method for separating capsaicinoids from chilli extract | |
| CN113563297B (en) | Method for removing zearalenone from natural vitamin E and product obtained by said method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180622 |
|
| RJ01 | Rejection of invention patent application after publication |