CN107376421A - A kind of method for carrying out extract and separate to the blend of organic matter and water using N methyl diethanolamines - Google Patents
A kind of method for carrying out extract and separate to the blend of organic matter and water using N methyl diethanolamines Download PDFInfo
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- CN107376421A CN107376421A CN201710810995.1A CN201710810995A CN107376421A CN 107376421 A CN107376421 A CN 107376421A CN 201710810995 A CN201710810995 A CN 201710810995A CN 107376421 A CN107376421 A CN 107376421A
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- organic matter
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- methyl diethanolamine
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
One kind utilizesNThe method that methyl diethanolamine carries out extract and separate to the blend of organic matter and water, is related to organic matter and water separation technology field.The present invention usesNMethyl diethanolamine is extractant, passes through CO2WithNMethyl diethanolamine reaction generationNSeparated after methyl diethanolamine bicarbonate with organic matter, to reach the purpose of separation organic matter.Reacted upper strata is the organic phase containing organic matter above, and wherein the mass fraction of organic matter is up to 80~95%.After lower floor's aqueous phase rectifyingNMethyl diethanolamine reusable edible.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 organic matter and water separation technology field.
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 in a big way
Interior to switch and control, this water containing additive can be recycled relatively easily.Such additive can substitute
Volatile solvent extracts active ingredient from solid material, and substitutes the inorganic salts in technique of saltouing at present, and solvent can be at any time
Recycling, greatly reduces energy consumption and the material consumption of production process, meets the direction of current green chemical industry development.And
The discovery of ionic strength intelligent switch solvent can solve this problem.
The content of the invention
It is an object of the invention to provide a kind of extracting process, is capable of green, efficiently extract and separate organic matter and water
Blend, and can easily reclaim extractant.
The technical scheme is that：WillN- methyl diethanolamine mixes with the blend of organic matter and water, is passed through CO2Carry out
Reaction, after reaction terminates, upper strata be the organic phase containing organic matter, lower floor be water withNThe water of-methyl diethanolamine mixing composition
Phase, then by water andN- methyl diethanolamine mixing composition aqueous phase rectifying, respectively obtain water andN- methyl diethanolamine.
The present invention usesN- methyl diethanolamine is extractant, passes through CO2WithNThe reaction generation of-methyl diethanolamineN- methyl
Separated after diethanol amine-bicarbonate with organic matter, to reach the purpose of separation organic matter.More than reacted upper strata be containing
The mass fraction of the organic phase of organic matter, wherein organic matter is up to 80~95%.After lower floor's aqueous phase rectifyingN- methyl diethanolamine
Reusable edible.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.
In the present inventionN- methyl diethanolamine-bicarbonate solution can extract the organic matter in water outlet, and withN- first
Base diethanol amine-increase of bicarbonate solution mass fraction and the increase of concentration, the mass fraction of organic matter in organic phase
Constantly increase.From application example, whenNThe volume ratio of-methyl diethanolamine and water is 4:When 1, you can extracted well
Separation is taken, obtains the organic matter more than 85%.Amine proton type ionic liquid extractant used by the process, there is dissolubility
The advantages that good, operating condition is gently, steam forces down, structure can design.And environment is not polluted, it is a kind of efficient, green
Extracting process, while extractant can be recycled so that extraction cost is greatly lowered.
Further, it is of the invention：Content of organics is 20~90w% in the blend of the organic matter and water.When using this
In inventionNThe proportioning of-methyl diethanolamine and water can extract the organic matter in blend well, simple to operate, low toxicity,
Efficiently, while extractant can be recycled by distillation operation, meet the theory of Green Chemistry.
It is describedNThe mixed material feeding volume ratio of-methyl diethanolamine and organic matter in the blend of the organic matter and water is 2
~4: 1.Extraction yield is good, reaches more than 80%.
It is highly preferred that reaction of the present invention is carried out under the K of 283.15 K~303.15 temperature conditionss.Due to low temperature
Be advantageous to extract, 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 are taken with graduated cylinder correct amountN- methyl diethanolamine, 20mL tetrahydrofurans.
（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 and lower floor's solution respectively 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,N,NIn-dimethyl acetamide is used as
Thing is marked, is settled to 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)；Heater：493.15K；Sensing chamber
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 86~92% by analysis.
Example 2：
（1）20mL water, 40mL are taken with graduated cylinder correct amountN- methyl diethanolamine, 20mL 1,3- dioxolanes.
（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 and lower floor's solution respectively 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,N,NIn-dimethyl acetamide is used as
Thing is marked, is settled to 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)；Heater：493.15K；Sensing chamber
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 85~90% by analysis.
Example 3：
（1）20mL water, 40mL are taken with graduated cylinder correct amountN- methyl diethanolamine, 20mL 1,4- dioxane.
（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 reaches balance, upper solution and lower floor's solution are obtained respectively.
（4）Upper solution and each 1ml of lower floor's solution is taken to be placed in 25ml volumetric flask,N,NIn-dimethyl acetamide is used as
Thing is marked, is settled to 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)；Heater：493.15K；Sensing chamber
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 80~90% by analysis.
Example 4：
（1）10mL water, 40mL are taken with graduated cylinder correct amountN- methyl diethanolamine, 20mL 1,4- dioxane.
（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 reaches balance, upper solution and lower floor's solution are obtained respectively.
（4）Upper solution and each 1ml of lower floor's solution is taken to be placed in 25ml volumetric flask,N,NIn-dimethyl acetamide is used as
Thing is marked, is settled to 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)；Heater：493.15K；Sensing chamber
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 90~95% by analysis.
Example 5：
（1）10mL water, 40mL are taken with graduated cylinder correct amountN- methyl diethanolamine, 30mL 1,4- dioxane.
（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 reaches balance, upper solution and lower floor's solution are obtained respectively.
（4）Upper solution and each 1mL of lower floor's solution is taken to be placed in 25ml volumetric flask,N,NIn-dimethyl acetamide is used as
Thing is marked, is settled to 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)；Heater：493.15K；Sensing chamber
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 91.5~95% by analysis.
Rectifying will be carried out by each example gained lower floor solution above, specific method is as follows：
Solution is added in tower reactor, tower reactor heating, 95~110 DEG C of tower top temperature during distillation, 243~260 DEG C of bottom temperature,N- first
The yield of base diethanol amine is more than 96%.
Claims (4)
1. one kind utilizesNThe method that-methyl diethanolamine carries out extract and separate to the blend of organic matter and water, its feature exist
In：WillN- methyl diethanolamine mixes with the blend of organic matter and water, is passed through CO2Reacted, after reaction terminates, upper strata is
Organic phase containing organic matter, lower floor be water andNThe aqueous phase of-methyl diethanolamine mixing composition, then by water andN- methyl diethyl
Hydramine mixing composition aqueous phase rectifying, respectively obtain water andN- methyl diethanolamine.
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：It is describedN- methyl diethanolamine and the organic matter and
The mixed material feeding volume ratio of organic matter is 2~4: 1 in the blend of water.
4. according to the method for claim 1, it is characterised in that：Temperature of the reaction in the K of 283.15 K~303.15
Under the conditions of carry out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710810995.1A CN107376421A (en) | 2017-09-11 | 2017-09-11 | A kind of method for carrying out extract and separate to the blend of organic matter and water using N methyl diethanolamines |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710810995.1A CN107376421A (en) | 2017-09-11 | 2017-09-11 | A kind of method for carrying out extract and separate to the blend of organic matter and water using N methyl diethanolamines |
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| Publication Number | Publication Date |
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| CN107376421A true CN107376421A (en) | 2017-11-24 |
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| CN201710810995.1A Pending CN107376421A (en) | 2017-09-11 | 2017-09-11 | A kind of method for carrying out extract and separate to the blend of organic matter and water using N methyl diethanolamines |
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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 |
| CN114539081A (en) * | 2022-03-07 | 2022-05-27 | 扬州大学 | Method for separating and purifying glycine by using N, N-dibutylethanolamine |
Citations (3)
| 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 |
| CN103694482A (en) * | 2012-09-27 | 2014-04-02 | 中国科学院大连化学物理研究所 | Cellulose solution, cellulose dissolution method and regenerated cellulose |
| CN105925300A (en) * | 2016-05-11 | 2016-09-07 | 西南石油大学 | Recovering method for CO2 switch type solvent for treating oil-based drilling cuttings |
-
2017
- 2017-09-11 CN CN201710810995.1A patent/CN107376421A/en active Pending
Patent Citations (3)
| 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 |
| CN103694482A (en) * | 2012-09-27 | 2014-04-02 | 中国科学院大连化学物理研究所 | Cellulose solution, cellulose dissolution method and regenerated cellulose |
| CN105925300A (en) * | 2016-05-11 | 2016-09-07 | 西南石油大学 | Recovering method for CO2 switch type solvent for treating oil-based drilling cuttings |
Cited By (4)
| 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 |
| CN114539081A (en) * | 2022-03-07 | 2022-05-27 | 扬州大学 | Method for separating and purifying glycine by using N, N-dibutylethanolamine |
| CN114539081B (en) * | 2022-03-07 | 2024-04-02 | 扬州大学 | Method for separating and purifying glycine by utilizing N, N-dibutyl ethanolamine |
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Application publication date: 20171124 |
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