CN107596733A - A kind of method for carrying out extract and separate to the blend of organic matter and water using triethylamine - Google Patents
A kind of method for carrying out extract and separate to the blend of organic matter and water using triethylamine Download PDFInfo
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- CN107596733A CN107596733A CN201710810994.7A CN201710810994A CN107596733A CN 107596733 A CN107596733 A CN 107596733A CN 201710810994 A CN201710810994 A CN 201710810994A CN 107596733 A CN107596733 A CN 107596733A
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Abstract
A kind of method for carrying out extract and separate to the blend of organic matter and water using triethylamine, it is related to the separation technology field of green, efficient organic matter and water.Triethylamine is mixed with the blend of organic matter and water, is passed through CO2Reacted, reaction terminate after, upper strata be the organic phase containing organic matter, then by lower floor heat or and N2Reaction, water and triethylamine are obtained respectively.Reacted upper strata is the organic phase containing organic matter above, and wherein the mass fraction of organic matter is up to 75~95%.Lower floor it is heated or further with N2Reaction, can be recycled to obtain triethylamine, can recycle.The present invention can replace volatile organic solvent and current inorganic salts saltout the inorganic salts used in technique, be the direction of green chemistry chemical technology development.
Description
Technical field
The present invention relates to green, efficient organic matter and the separation technology field of water.
Background technology
It is that the common method of organic substance is reclaimed from product and the aqueous solution to saltout with rectifying.But saltouing can produce largely
Salt-containing organic wastewater, and rectifying need to consume substantial amounts of energy and cause partial solvent volatilization loss and pollution environment.
The target of Green Chemistry is more more efficient than traditional chemical process, the few waste of development, the process and skill of few environmental pollution
Art, in 12 basic principles of Green Chemistry, one of which requires that chemical process does not have to solvent as far as possible, if can not keep away
Exempt from, also will be as far as possible with harmless solvent.If adding a kind of additive into water, make the ionic strength of the system and/or hydrophilic
Property can switch and control interior in a big way, and this water containing additive can be recycled easier.Such additive
Volatile solvent can be substituted active ingredient is extracted from solid material, and substitute the inorganic salts in technique of saltouing at present, it is molten
Agent can recycle at any time, greatly reduce energy consumption and the material consumption of production process, meet current green chemical industry development
Direction.And the discovery of ionic strength intelligent switch solvent can solve this problem.
The content of the invention
, being capable of green, efficient extract and separate it is an object of the invention to provide a kind of extracting process using triethylamine
The blend of organic matter and water, and can easily reclaim extractant.
The technical scheme is that：Triethylamine is mixed with the blend of organic matter and water, is passed through CO2Reacted, instead
After should terminating, upper strata is the organic phase containing organic matter, then by lower floor heating or and N2Reaction, water and triethylamine are obtained respectively.
The present invention is extractant with triethylamine, passes through CO2With being mixed after triethylamine react generation triethylamine-bicarbonate with water
It is molten, to reach the purpose of separation organic matter.Reacted upper strata is the matter of the organic phase containing organic matter, wherein organic matter above
Fraction is measured up to 75~95%.Lower floor it is heated or further with N2Reaction, can be recycled to obtain triethylamine, can recycle.This
Invention can replace volatile organic solvent and current inorganic salts saltout the inorganic salts used in technique, be green chemistry chemical technology hair
The direction of exhibition.
Triethylamine-bicarbonate solution can extract the organic matter in water outlet in the present invention, and with triethylamine-bicarbonate
The increase of salting liquid mass fraction and the increase of concentration, the mass fraction of organic matter constantly increases in organic phase.It is real by application
Example is understood, when the volume ratio of triethylamine and water is 3:When 1, you can carry out extract and separate well, obtain organic more than 80%
Thing.Amine proton type ionic liquid extractant used by the process, have dissolubility is good, operating condition is gentle, steam forces down,
The advantages that structure can design.And environment is not polluted, be it is a kind of efficiently, the extracting process of green, while extractant can be with
Recycling so that extraction cost is greatly lowered.
Further, content of organics is 20~90w% in the blend of organic matter and water of the present invention.When using this
The proportioning of triethylamine and water can extract the organic matter in blend well in invention, simple to operate, less toxic, efficient, together
When extractant can be by simply heating or being passed through N2Recycle, meet the theory of Green Chemistry.
When the mixed material feeding volume ratio of organic matter in the blend of the triethylamine and the organic matter and water is 2~4: 1
When, extraction yield is good, reaches more than 80%.
It is passed through CO2Reaction carried out under the K of 283.15 K~303.15 temperature conditionss.Because favors low temperature is in extraction,
When the temperature is too low, consuming cost is excessive, and when temperature is too high, extraction yield is low.
Embodiment
Example 1：
（1）20mL water, 40mL triethylamines, 20mL tetrahydrofurans are taken with graduated cylinder correct amount.
（2）The solution measured is poured into the beaker of cleaning, and sealed with preservative film, be put into 283.1K thermostatted water
It is stand-by in bath.
（3）By high-purity CO2It is passed into beaker, takes upper solution and lower floor's solution to carry out gas-chromatography respectively every 0.5h
Analysis, until the composition no longer reacting condition of solution obtains upper solution respectively and lower floor is molten i.e. up to balance.
（4）Upper solution and each 1mL of lower floor's solution is taken to be placed in 25mL volumetric flask, toluene is settled to as internal standard compound
25mL, promoting the circulation of qi analysis of hplc of going forward side by side.Analysis condition is as follows：Detector：Hydrogen flame ionization detector (fid detector)；Heating
Device：493.15K；Detect room temperature：523.15K；Post case initial temperature is 343.15K, with 20Kmin-1Speed be warming up to
493.15K；Carrier gas：Nitrogen；H2Flow：60ml·min-1；Air mass flow：400ml·min-1；Tail wind drift amount：10ml·min-1；Dottle pin purge flow rate：3ml·min-1；Split ratio：50∶1.
（5）Learn that the mass fraction of tetrahydrofuran in upper organic phase is 85~90% by analysis.
Example 2：
（1）20mL water, 40mL triethylamines, 20mL 1,3- dioxolanes are taken with graduated cylinder correct amount.
（2）The solution measured is poured into the beaker of cleaning, and sealed with preservative film, be put into 283.1K thermostatted water
It is stand-by in bath.
（3）By high-purity CO2It is passed into beaker, takes upper solution and lower floor's solution to carry out gas-chromatography respectively every 0.5h
Analysis, until the composition no longer reacting condition of solution obtains upper solution respectively and lower floor is molten i.e. up to balance.
（4）Upper solution and each 1mL of lower floor's solution is taken to be placed in 25mL volumetric flask, toluene is settled to as internal standard compound
25mL, promoting the circulation of qi analysis of hplc of going forward side by side.Analysis condition is as follows：Detector：Hydrogen flame ionization detector (fid detector)；Heating
Device：493.15K；Detect room temperature：523.15K；Post case initial temperature is 343.15K, with 20Kmin-1Speed be warming up to
493.15K；Carrier gas：Nitrogen；H2Flow：60ml· min-1；Air mass flow：400ml·min-1；Tail wind drift amount：10ml·min-1；Dottle pin purge flow rate：3ml·min-1；Split ratio：50∶1.
（5）Learn that the mass fraction of 1,3- dioxolanes in upper organic phase is 80~90% by analysis.
Example 3：
（1）20mL water, 40mL triethylamines, 20mL 1,4- dioxane are taken with graduated cylinder correct amount.
（2）The solution measured is poured into the beaker of cleaning, and sealed with preservative film, be put into 283.1K thermostatted water
It is stand-by in bath.
（3）By high-purity CO2It is passed into beaker, takes upper solution and lower floor's solution to carry out gas-chromatography respectively every 0.5h
Analysis, until the composition no longer reacting condition of solution obtains upper solution respectively and lower floor is molten i.e. up to balance.
（4）Upper solution and each 1mL of lower floor's solution is taken to be placed in 25mL volumetric flask, toluene is settled to as internal standard compound
25mL, promoting the circulation of qi analysis of hplc of going forward side by side.Analysis condition is as follows：Detector：Hydrogen flame ionization detector (fid detector)；Heating
Device：493.15K；Detect room temperature：523.15K；Post case initial temperature is 343.15K, with 20Kmin-1Speed be warming up to
493.15K；Carrier gas：Nitrogen；H2Flow：60ml·min-1；Air mass flow：400ml·min-1；Tail wind drift amount：10ml·min-1；Dottle pin purge flow rate：3ml·min-1；Split ratio：50:1；
（5）Learn that the mass fraction of 1,4- dioxane in upper organic phase is 78~87% by analysis.
Example 4：
（1）80mL water, 40mL triethylamines, 20mL 1,3- dioxolanes are taken with graduated cylinder correct amount.
（2）The solution measured is poured into the beaker of cleaning, and sealed with preservative film, be put into 283.1K thermostatted water
It is stand-by in bath.
（3）By high-purity CO2It is passed into beaker, takes upper solution and lower floor's solution to carry out gas-chromatography respectively every 0.5h
Analysis, until the composition no longer reacting condition of solution obtains upper solution respectively and lower floor is molten i.e. up to balance.
（4）Upper solution and each 1mL of lower floor's solution is taken to be placed in 25mL volumetric flask, toluene is settled to as internal standard compound
25mL, promoting the circulation of qi analysis of hplc of going forward side by side.Analysis condition is as follows：Detector：Hydrogen flame ionization detector (fid detector)；Heating
Device：493.15K；Detect room temperature：523.15K；Post case initial temperature is 343.15K, with 20Kmin-1Speed be warming up to
493.15K；Carrier gas：Nitrogen；H2Flow：60ml· min-1；Air mass flow：400ml·min-1；Tail wind drift amount：10ml·min-1；Dottle pin purge flow rate：3ml·min-1；Split ratio：50∶1.
（5）Learn that the mass fraction of 1,3- dioxolanes in upper organic phase is 82.5~90% by analysis.
Example 5：
（1）90mL water, 40mL triethylamines, 10mL 1,3- dioxolanes are taken with graduated cylinder correct amount.
（2）The solution measured is poured into the beaker of cleaning, and sealed with preservative film, be put into 283.1K thermostatted water
It is stand-by in bath.
（3）By high-purity CO2It is passed into beaker, takes upper solution and lower floor's solution to carry out gas-chromatography respectively every 0.5h
Analysis, until the composition no longer reacting condition of solution obtains upper solution respectively and lower floor is molten i.e. up to balance.
（4）Upper solution and each 1mL of lower floor's solution is taken to be placed in 25mL volumetric flask, toluene is settled to as internal standard compound
25mL, promoting the circulation of qi analysis of hplc of going forward side by side.Analysis condition is as follows：Detector：Hydrogen flame ionization detector (fid detector)；Heating
Device：493.15K；Detect room temperature：523.15K；Post case initial temperature is 343.15K, with 20Kmin-1Speed be warming up to
493.15K；Carrier gas：Nitrogen；H2Flow：60ml· min-1；Air mass flow：400ml·min-1；Tail wind drift amount：10ml·min-1；Dottle pin purge flow rate：3ml·min-1；Split ratio：50∶1.
（5）Learn that the mass fraction of 1,3- dioxolanes in upper organic phase is 88~95% by analysis.
Lower floor's solution is further separated obtained by each example by more than：Specific method is as follows：
Heating：By lower floor's solution at a temperature of the K of 323.15 K~333.15 or so two hours of continuous heating, until lower floor
Solution is thoroughly layered, and upper strata is triethylamine, and lower floor is water, and water and triethylamine are obtained after separation, and triethylamine can iterative cycles utilization.
N2Reaction method：Lower floor's solution is continually fed into high-purity N2Two hours or so, triethylamine-bicarbonate solution and N2Instead
Should, solution is gradually layered, and is transformed into triethylamine and water again, until solution is thoroughly layered, acquirement water and triethylamine after separation, three
Ethamine can iterative cycles utilization.
Claims (4)
- A kind of 1. method for carrying out extract and separate to the blend of organic matter and water using triethylamine, it is characterised in that：By three second Amine mixes with the blend of organic matter and water, is passed through CO2Reacted, after reaction terminates, upper strata is to contain the organic of organic matter Phase, then by lower floor heating or and N2Reaction, water and triethylamine are obtained respectively.
- 2. according to the method for claim 1, it is characterised in that：Content of organics is in the blend of the organic matter and water 20~90w%.
- 3. method according to claim 1 or 2, it is characterised in that：The blending of the triethylamine and the organic matter and water The mixed material feeding volume ratio of organic matter is 2~4: 1 in thing.
- 4. according to the method for claim 1, it is characterised in that：It is passed through CO2Reaction the K's of 283.15 K~303.15 Carried out under temperature conditionss.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111203006A (en) * | 2020-01-21 | 2020-05-29 | 西南石油大学 | Separation agent for emulsifying oily wastewater, preparation method and separation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102892713A (en) * | 2010-02-10 | 2013-01-23 | 金斯顿女王大学 | Water with switchable ionic strength |
| CN105498280A (en) * | 2015-12-25 | 2016-04-20 | 天津大学 | Hydrophilic reversible solvent assisted oil-sand separation method |
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2017
- 2017-09-11 CN CN201710810994.7A patent/CN107596733A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102892713A (en) * | 2010-02-10 | 2013-01-23 | 金斯顿女王大学 | Water with switchable ionic strength |
| CN105498280A (en) * | 2015-12-25 | 2016-04-20 | 天津大学 | Hydrophilic reversible solvent assisted oil-sand separation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111203006A (en) * | 2020-01-21 | 2020-05-29 | 西南石油大学 | Separation agent for emulsifying oily wastewater, preparation method and separation method |
| CN111203006B (en) * | 2020-01-21 | 2022-08-02 | 西南石油大学 | Separation agent for emulsifying oily wastewater, preparation method and separation method |
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Application publication date: 20180119 |