CN107746394A - The polishing purification method of water-containing tetrahydrofuran - Google Patents
The polishing purification method of water-containing tetrahydrofuran Download PDFInfo
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- CN107746394A CN107746394A CN201711277667.6A CN201711277667A CN107746394A CN 107746394 A CN107746394 A CN 107746394A CN 201711277667 A CN201711277667 A CN 201711277667A CN 107746394 A CN107746394 A CN 107746394A
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- tetrahydrofuran
- water
- purification method
- thick
- distillation still
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Furan Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the polishing purification method of water-containing tetrahydrofuran, comprise the following steps：Water-containing tetrahydrofuran is contacted with storng-acid cation exchange resin, the dihydrofuran in tetrahydrofuran is converted into hydroxyl tetrahydrofuran, obtains conversion reaction liquid；Step conversion reaction liquid is distilled, the aqueous solution containing hydroxyl tetrahydrofuran is flowed out from bottom of towe, and tetrahydrofuran is distillated together with water from tower top and obtain thick tetrahydrofuran；Thick tetrahydrofuran is added into distillation still, then adds reducing agent to remove the peroxide in thick tetrahydrofuran, heating distillation, the water-containing tetrahydrofuran condensation steamed is collected in storage tank；With nitrogen by the water-containing tetrahydrofuran press-in distillation still in storage tank, into distillation still, addition is dissolved in water and improves the reagent of water boiling point, it is subsequently heated pot temperature and is raised to 80 90 DEG C and steam tetrahydrofuran, collects and condense tetrahydrofuran steam tetrahydrofuran after purification is made.Tetrahydrofuran purity of the present invention is high.
Description
Technical field
The present invention relates to a kind of purification process, and in particular to the polishing purification method of water-containing tetrahydrofuran.
Background technology
Tetrahydrofuran is a kind of important organic chemical industry and fine chemical material, is had to many organic and inorganic matter good
Dissolubility, all compounds in addition to polyethylene, polypropylene and fluororesin can be dissolved, reactive solvents is widely used as, there is " ten thousand
The title of energy solvent ".
Preparation method as tetrahydrofuran, it is known to the catalytic hydrogenation of furans, the cyclodehydration of BDO, two acetic acid fourths
The several methods such as the de- ester cyclisation of alkane, obtain typically containing aldehydes, water of dihydrofuran etc. in tetrahydrofuran using these methods
Impurity, tetrahydrofuran is set to be reused because containing impurity, it is directly discarded, both wasted, and polluted environment again, do not meet energy-conservation
The demand for development of emission reduction.
The content of the invention
The technical problems to be solved by the invention are the impurity such as the aldehydes containing dihydrofuran, water, purpose in tetrahydrofuran
It is the polishing purification method that water-containing tetrahydrofuran is provided, solves tetrahydrofuran and asked because what can not be reused containing impurity
Topic.
The present invention is achieved through the following technical solutions：
The polishing purification method of water-containing tetrahydrofuran, comprises the following steps：
S1, water-containing tetrahydrofuran is contacted with storng-acid cation exchange resin, the dihydrofuran in tetrahydrofuran is turned
Change hydroxyl tetrahydrofuran into, obtain conversion reaction liquid；
It S2, will be distilled conversion reaction solution in step S1, and the aqueous solution containing hydroxyl tetrahydrofuran is flowed out from bottom of towe,
And tetrahydrofuran is distillated together with water from tower top and obtain thick tetrahydrofuran；
S3, the thick tetrahydrofuran in step S2 is added to distillation still, then add reducing agent to remove the peroxide in thick tetrahydrofuran
Compound, heating distillation, the water-containing tetrahydrofuran condensation steamed are collected in storage tank；
S4, with nitrogen by storage tank water-containing tetrahydrofuran press-in distillation still in, into distillation still add be dissolved in water and carry
The reagent of high water boiling point, is subsequently heated pot temperature and is raised to 80-90 DEG C and steam tetrahydrofuran, collects and condenses tetrahydrofuran
Tetrahydrofuran after purification is made in steam.
The present invention first contacts water-containing tetrahydrofuran with storng-acid cation exchange resin, eliminates in tetrahydrofuran
Dihydrofuran, tetrahydrofuran is conveyed using nitrogen, nitrogen envelope can be played a part of；The present invention improves the boiling of tetrahydrofuran reclaimed water
Point, is subsequently heated pot temperature and is raised to 80-90 DEG C and steam tetrahydrofuran, collects and condenses tetrahydrofuran steam purifying is made
Tetrahydrofuran afterwards, tetrahydrofuran water content can be made to reduce to below 100PPm, at the same can also remove peroxide in tetrahydrofuran,
The compositions such as antioxidant, mechanical admixture.
In step S3, before addition of the reducing agent, acid adding or alkali is added to adjust thick tetrahydrofuran to neutrality.
The acid is sulfuric acid, and the alkali is sodium hydroxide or potassium hydroxide.
The heating-up temperature of distillation still is 85 DEG C in step S4.
Reagent is sodium chloride in step S4.Sodium chloride formation salt solution soluble in water, the boiling point of salt solution are higher than the boiling point of pure water.
The present invention compared with prior art, has the following advantages and advantages：
1st, the polishing purification method of water-containing tetrahydrofuran of the present invention can make tetrahydrofuran water content reduce to below 100PPm, together
When can also remove the compositions such as peroxide in tetrahydrofuran, antioxidant, mechanical admixture；
2nd, the polishing purification method of water-containing tetrahydrofuran of the present invention first hands over water-containing tetrahydrofuran and highly acidic cation
Resin contact is changed, eliminates the dihydrofuran in tetrahydrofuran；
3rd, the polishing purification method of water-containing tetrahydrofuran of the present invention can play the work that nitrogen seals using nitrogen conveying tetrahydrofuran
With.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, with reference to embodiment, the present invention is made
Further to describe in detail, exemplary embodiment of the invention and its explanation are only used for explaining the present invention, are not intended as to this
The restriction of invention.
Embodiment 1
The polishing purification method of water-containing tetrahydrofuran of the present invention, comprises the following steps：
S1, water-containing tetrahydrofuran is contacted with storng-acid cation exchange resin, the dihydrofuran in tetrahydrofuran is turned
Change hydroxyl tetrahydrofuran into, obtain conversion reaction liquid；
It S2, will be distilled conversion reaction solution in step S1, and the aqueous solution containing hydroxyl tetrahydrofuran is flowed out from bottom of towe,
And tetrahydrofuran is distillated together with water from tower top and obtain thick tetrahydrofuran；
S3, the thick tetrahydrofuran in step S2 is added to distillation still, then add reducing agent to remove the peroxide in thick tetrahydrofuran
Compound, heating distillation, the water-containing tetrahydrofuran condensation steamed are collected in storage tank；
S4, with nitrogen by storage tank water-containing tetrahydrofuran press-in distillation still in, into distillation still add be dissolved in water and carry
The reagent of high water boiling point, is subsequently heated pot temperature and is raised to 80-90 DEG C and steam tetrahydrofuran, collects and condenses tetrahydrofuran
Tetrahydrofuran after purification is made in steam.In step S3, before addition of the reducing agent, acid adding or plus the thick tetrahydrofuran of alkali regulation
To neutrality.The acid is sulfuric acid, and the alkali is sodium hydroxide or potassium hydroxide.Reagent is sodium chloride in step S4.Sodium chloride is molten
Yu Shuizhong forms salt solution, and the boiling point of salt solution is higher than the boiling point of pure water.
The present invention first contacts water-containing tetrahydrofuran with storng-acid cation exchange resin, eliminates in tetrahydrofuran
Dihydrofuran, tetrahydrofuran is conveyed using nitrogen, nitrogen envelope can be played a part of；The present invention improves the boiling of tetrahydrofuran reclaimed water
Point, is subsequently heated pot temperature and is raised to 80-90 DEG C and steam tetrahydrofuran, collects and condenses tetrahydrofuran steam purifying is made
Tetrahydrofuran afterwards, tetrahydrofuran water content can be made to reduce to below 100PPm, at the same can also remove peroxide in tetrahydrofuran,
The compositions such as antioxidant, mechanical admixture.
Embodiment 2
Based on embodiment 1, the heating-up temperature of distillation still is 85 DEG C in step S4.Tetrahydrofuran purity exists in the present embodiment
More than 95%, the aldehyde of dihydrofuran and carbon number below 3 is all in below 10ppm.
Above-described embodiment, the purpose of the present invention, technical scheme and beneficial effect are carried out further
Describe in detail, should be understood that the embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc., all should include
Within protection scope of the present invention.
Claims (5)
1. the polishing purification method of water-containing tetrahydrofuran, it is characterised in that comprise the following steps：
S1, water-containing tetrahydrofuran is contacted with storng-acid cation exchange resin, the dihydrofuran in tetrahydrofuran is converted into
Hydroxyl tetrahydrofuran, obtain conversion reaction liquid；
It S2, will be distilled conversion reaction solution in step S1, and the aqueous solution containing hydroxyl tetrahydrofuran is flowed out from bottom of towe, and make
Tetrahydrofuran distillates from tower top together with water and obtains thick tetrahydrofuran；
S3, the thick tetrahydrofuran in step S2 is added to distillation still, then adds reducing agent to remove the peroxide in thick tetrahydrofuran,
Heating distillation, the water-containing tetrahydrofuran condensation steamed are collected in storage tank；
S4, with nitrogen by the water-containing tetrahydrofuran press-in distillation still in storage tank, added into distillation still and be dissolved in water and improve water
The reagent of boiling point, is subsequently heated pot temperature and is raised to 80-90 DEG C and steam tetrahydrofuran, collects and condenses tetrahydrofuran steam
Tetrahydrofuran after purification is made.
2. the polishing purification method of water-containing tetrahydrofuran according to claim 1, it is characterised in that in step S3, adding
Before entering reducing agent, acid adding or alkali is added to adjust thick tetrahydrofuran to neutrality.
3. the polishing purification method of water-containing tetrahydrofuran according to claim 2, it is characterised in that the acid is sulfuric acid,
The alkali is sodium hydroxide or potassium hydroxide.
4. the polishing purification method of water-containing tetrahydrofuran according to claim 1, it is characterised in that distillation still in step S4
Heating-up temperature be 85 DEG C.
5. the polishing purification method of water-containing tetrahydrofuran according to claim 1, it is characterised in that reagent is in step S4
Sodium chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711277667.6A CN107746394A (en) | 2017-12-06 | 2017-12-06 | The polishing purification method of water-containing tetrahydrofuran |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711277667.6A CN107746394A (en) | 2017-12-06 | 2017-12-06 | The polishing purification method of water-containing tetrahydrofuran |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438413A (en) * | 2018-12-13 | 2019-03-08 | 天津康科德医药化工有限公司 | A kind of purification process of chromatographically pure 1,4- dioxane |
| CN114315764A (en) * | 2020-09-27 | 2022-04-12 | 太仓沪试试剂有限公司 | Method for refining and purifying tetrahydrofuran containing water |
| CN116041285A (en) * | 2022-12-08 | 2023-05-02 | 杰特(宁夏)科技有限公司 | Novel tetrahydrofuran dehydration process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1386739A (en) * | 2002-06-21 | 2002-12-25 | 东营南开精细化工科技有限公司 | Process for dewatering and prifying tetrahydrofuran |
| CN1398860A (en) * | 2001-07-11 | 2003-02-26 | 三菱化学株式会社 | Tetrahydrofuran refining process |
| CN102596926A (en) * | 2009-10-30 | 2012-07-18 | 株式会社日立工业设备技术 | Process and system for purification of tetrahydrofuran |
| CN103408514A (en) * | 2013-08-20 | 2013-11-27 | 江苏九天高科技股份有限公司 | Technique and device for recovering tetrahydrofuran by pervaporation method |
| 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 |
-
2017
- 2017-12-06 CN CN201711277667.6A patent/CN107746394A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1398860A (en) * | 2001-07-11 | 2003-02-26 | 三菱化学株式会社 | Tetrahydrofuran refining process |
| CN1386739A (en) * | 2002-06-21 | 2002-12-25 | 东营南开精细化工科技有限公司 | Process for dewatering and prifying tetrahydrofuran |
| CN102596926A (en) * | 2009-10-30 | 2012-07-18 | 株式会社日立工业设备技术 | Process and system for purification of tetrahydrofuran |
| CN103408514A (en) * | 2013-08-20 | 2013-11-27 | 江苏九天高科技股份有限公司 | Technique and device for recovering tetrahydrofuran by pervaporation method |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438413A (en) * | 2018-12-13 | 2019-03-08 | 天津康科德医药化工有限公司 | A kind of purification process of chromatographically pure 1,4- dioxane |
| CN114315764A (en) * | 2020-09-27 | 2022-04-12 | 太仓沪试试剂有限公司 | Method for refining and purifying tetrahydrofuran containing water |
| CN116041285A (en) * | 2022-12-08 | 2023-05-02 | 杰特(宁夏)科技有限公司 | Novel tetrahydrofuran dehydration process |
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Application publication date: 20180302 |