CN109179838A - The processing method of DMF waste water containing triethylamine - Google Patents
The processing method of DMF waste water containing triethylamine Download PDFInfo
- Publication number
- CN109179838A CN109179838A CN201811184840.2A CN201811184840A CN109179838A CN 109179838 A CN109179838 A CN 109179838A CN 201811184840 A CN201811184840 A CN 201811184840A CN 109179838 A CN109179838 A CN 109179838A
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- Prior art keywords
- triethylamine
- dmf
- processing method
- waste water
- organic solvent
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Classifications
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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
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The processing method of the present invention provides a kind of DMF waste water containing triethylamine.The processing method includes: to be extracted using organic solvent to the DMF waste water containing triethylamine, obtains the extract liquor and raffinate containing DMF;It is distilled after being adjusted to the pH value of raffinate, obtains triethylamine.The processing method is passed through after being extracted using organic solvent to the DMF waste water containing triethylamine, DMF organic phase is separated with the triethylamine in water phase, it is distilled after further adjusting pH value to raffinate water phase extracted in turn, it can be further separated out triethylamine organic matter, so that the COD content in the waste water that makes that treated reduces.The above method of the application is only related to extract and be distilled, easy to operate, and used equipment is common device, small investment, it is at low cost, and not only reduced the content of the organic matter after processing in water, but also isolated triethylamine organic matter can be realized and recycle.
Description
Technical field
The present invention relates to the field of waste water treatment containing organic matter, in particular to a kind of DMF waste water containing triethylamine
Processing method.
Background technique
Currently, industrial processing containing DMF (dimethylformamide) waste water method mainly have bioanalysis, physical method (absorption,
Extraction), chemical method (catalysis oxidation, basic hydrolysis), electrolytic oxidation etc..The Biochemical method DMF wastewater treatment time is long, degradation
It is not thorough and DMF can make microorganism be poisoned, extreme shock is caused to biological treatment.The reproducibility of absorption method in physical method
Difference;Extraction is only used for nonpolar organic matter, and the organic matter being extracted and waste water extracted needs are further processed, organic
Solvent may also result in secondary pollution.Chemical method, that is, DMF is decomposed into dimethylamine and formates under alkali effect, but this method consumes alkali
Amount is big, and the dimethylamine that stripping goes out also needs subsequent processing, easily causes secondary pollution.Electrolytic oxidation need many oxidising agents or
Oxidant, and the equipment for needing investment buying to be much electrolysed, it is not easy to operate.
It can be seen that physical extraction method application range is smaller, and processing is not thorough.The organic phase extracted is mutually needed with waste water
It continues with, is generally required after extraction and carry out rectifying again using rectifying column, equipment investment is big.
Summary of the invention
The processing method of the main purpose of the present invention is to provide a kind of DMF waste water containing triethylamine, to solve existing skill
Cardia problem at high cost.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of place of the DMF waste water containing triethylamine
Reason method, processing method include: to be extracted using organic solvent to the DMF waste water containing triethylamine, obtain the extract liquor containing DMF
And raffinate;It is distilled after being adjusted to the pH value of raffinate, obtains triethylamine.
Further, processing method further include: the extract liquor containing DMF is distilled, respectively obtain extractant and
DMF。
Further, before being extracted using organic solvent to the DMF waste water containing triethylamine, processing method is also wrapped
It includes:
The pH for adjusting the DMF waste water containing triethylamine is 7~10.
Further, it is distilled after the pH of raffinate being adjusted to 12~14, obtains triethylamine.
Further, the step of distilling after adjusting to the pH value of raffinate, obtain triethylamine includes: to raffinate
PH value is distilled after adjusting, and obtains distillation head product;Moisture in removal distillation head product, obtains triethylamine.
Further, using one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, magnesium sulfate and sodium sulphate or
Moisture in a variety of removal distillation head products, obtains triethylamine.
Further, it is used to extract the DMF waste water containing triethylamine using extractant as organic solvent.
Further, organic solvent is selected from CHCl3、CH2Cl2, any one of ethyl acetate and toluene.
Further, the volume ratio of organic solvent and the DMF waste water containing triethylamine is 1~5:1.
It applies the technical scheme of the present invention, the processing method of the above-mentioned waste water of the application, by using organic solvent pair
After DMF waste water containing triethylamine is extracted, DMF organic phase is separated with the triethylamine in water phase, Jin Erjin
One step is distilled after adjusting pH value to raffinate water phase extracted, can be further separated out triethylamine organic matter, thus
COD content in the waste water that makes that treated reduces.The above method of the application is only related to extract and be distilled, easy to operate, and institute
The equipment used is common device, and small investment is at low cost, and has not only reduced the content of the organic matter after processing in water, but also make
Isolated triethylamine organic matter can be realized and recycle.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
As background technique is previously mentioned, when handling in the prior art the DMF waste water containing organic matter, there are secondary dirts
Dye or problem at high cost provide one in a kind of typical embodiment of the application to improve this status of the prior art
The processing method of kind of the DMF waste water containing triethylamine, the processing method include using organic solvent to the DMF waste water containing triethylamine into
Row extraction, obtains the extract liquor and raffinate containing DMF;It is distilled after adjusting pH value to raffinate, obtains triethylamine.
The processing method of the above-mentioned waste water of the application, by being carried out using organic solvent to the DMF waste water containing triethylamine
After extraction, DMF organic phase is separated with the triethylamine in water phase, and then further to raffinate water extracted
It is mutually distilled, triethylamine organic matter can be further separated out, so that the COD content in the waste water that makes that treated reduces.This
The above method of application is only related to extract and be distilled, easy to operate, and used equipment is common device, small investment, at
This is low, and has not only reduced the content of the organic matter after processing in water, but also isolated triethylamine organic matter can be realized
It recycles.
It is above-mentioned in a kind of preferred embodiment in order to further be recycled to organic matters such as DMF in waste water
Processing method further includes distilling to the extract liquor containing DMF, respectively obtains extractant and DMF.Organic solvent is extracted
The organic phase arrived separates organic solvent and DMF by distillation, and following for the extractant obtained to recycling both may be implemented
Ring utilizes, and may be implemented to recycle DMF.
In order to further increase organic solvent to the extraction yield of the DMF in waste water, in a kind of preferred embodiment, adopting
Before being extracted with organic solvent to the DMF waste water containing triethylamine, above-mentioned processing method further includes adjusting the DMF containing triethylamine
The pH of waste water is 7~10.In the range by pH control, the extraction yield of organic solvent can be made relatively higher.
In a kind of preferred embodiment, is distilled after adjusting pH to raffinate and being 12~14, obtain triethylamine.?
After going out to DMF extraction and separation, the organic matter in remaining water phase is triethylamine, and in alkalinity, triethylamine is organic base, thus,
The pH value of remaining water phase is adjusted between 12~14, the alkalinity of triethylamine is made to keep stablizing.If pH is outside the range, three second
Amine distillation does not come out, or the triethylamine steamed is very little, and impurity content is more.
In a kind of preferred embodiment, the step of raffinate is distilled, triethylamine is obtained include to raffinate into
Row distillation obtains distillation head product;To the moisture removal in distillation head product, triethylamine is obtained.Due to the boiling point of triethylamine
(89.5 DEG C) are lower than the boiling point of water, thus can be separated triethylamine from waste water by distillation, in order to further increase
The purity of the triethylamine recycled, thus removed water.
Specific water-eliminating method uses existing dewatering, for example dried over anhydrous agent can be added and removed water, desiccant
The including but not limited to alkaline desiccant of the neutral desiccant or calcium chloride etc. such as sodium sulphate.In a kind of preferred embodiment of the application
In, it is distilled just using removals any one or more in sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, magnesium sulfate and sodium sulphate
Moisture in product, obtains triethylamine, and the purity for the triethylamine that this method obtains is higher.
The above-mentioned organic solvent extracted to DMF uses existing organic solvent.In a kind of preferred embodiment
In, organic solvent is selected from CHCl3、CH2Cl2, any one of ethyl acetate and toluene.More hold using these organic solvents are subsequent
Easily separated, the purity of the organic solvent recycled is also higher, thus reduces the risk of secondary pollution.
In a kind of preferred embodiment, using extractant as organic solvent be used for the DMF waste water containing triethylamine into
Row extraction, recycles organic solvent.
In the step of above-mentioned organic solvent extracts the DMF waste water containing triethylamine, organic solvent with containing triethylamine
The volume ratio of DMF waste water can according in specific waste water DMF content height and used organic solvent type and
Rationally determined.In a preferred embodiment of the present application, the volume of above-mentioned organic solvent and the DMF waste water containing triethylamine
Than for 1~5:1.
The beneficial effect of the application is further illustrated below in conjunction with specific embodiments.
Embodiment 1
Certain DMF waste liquid main component containing triethylamine: DMF, triethylamine, unknown inorganic salts etc.;COD is about 800,000 in waste liquid
mg/L。
The pH to 7 that sodium hydroxide adjusts waste liquid is added in water phase waste liquid, uses organic solvent CHCl3It will be in waste liquid (water phase)
DMF extract (volume ratio of organic solvent and waste water be 3:1), organic phase further progress distillation extracted obtains
CHCl3It can apply, obtained DMF purity is very high (purity reaches 97%), can be recycled.
Adjust pH to 12 alkali (sodium hydroxide) in remaining water phase, is added again after extraction, then to water phase into
Row distillation obtains triethylamine, and triethylamine removes moisture using sodium hydroxide, and (purity is up to available high-purity triethylamine
97%) it, is recycled and applies.
Water phase after being disposed is faint yellow as clear as crystal solution, is 190,000 mg/L through detection COD.Extraction
CHCl3The rate of recovery is 95%, DMF recovery rate 90%, and the triethylamine rate of recovery is 92%.
Embodiment 2
Certain DMF waste liquid main component containing triethylamine: DMF, triethylamine, unknown inorganic salts etc.;COD is about 800,000 in waste liquid
mg/L。
The pH to 10 that sodium hydroxide adjusts waste liquid is added in water phase waste liquid, uses organic solvent CHCl3By the DMF in water phase
It extracts (volume ratio of organic solvent and waste water is 3:1), organic phase further progress distillation extracted obtains
CHCl3It can apply, obtained DMF purity is very high (purity reaches 97%), can be recycled.
Alkali is added again and adjusts pH to 14, this water phase distills available triethylamine, three second again after extraction for water phase
Amine removes moisture using sodium hydroxide, and available high-purity triethylamine (purity is up to 97%) is recyclable to apply.
Water phase is faint yellow as clear as crystal solution after being disposed, and COD is 180,000 mg/L.The CHCl of extraction3Recycling
Rate is 95.5%, DMF recovery rate 90.1%, the triethylamine rate of recovery 93.2%.
Embodiment 3
Certain DMF waste liquid main component containing triethylamine: DMF, triethylamine, unknown inorganic salts etc.;COD is about 800,000 in waste liquid
mg/L。
The pH to 8 that sodium hydroxide adjusts waste liquid is added in water phase waste liquid, uses organic solvent CHCl3By the DMF in water phase
It extracts (volume ratio of organic solvent and waste water is 2:1), organic phase distillation extracted, obtained CHCl3It can apply,
Obtained DMF purity is very high (purity reaches 97%), can be recycled.
Alkali is added again and adjusts pH to 13, this water phase distills available triethylamine, three second again after extraction for water phase
Amine removes moisture using sodium hydroxide, and available high-purity triethylamine (purity is up to 96%.) is recyclable to apply.
Water phase is faint yellow as clear as crystal solution after being disposed, and COD is 17.8 ten thousand mg/L.The CHCl of extraction3It returns
Yield is 96%, DMF recovery rate 91%, the triethylamine rate of recovery 93%.
Embodiment 4
Certain DMF waste liquid main component containing triethylamine: DMF, triethylamine, unknown inorganic salts etc.;COD is about 800,000 in waste liquid
mg/L。
The pH to 11 that sodium hydroxide adjusts waste liquid is added in water phase waste liquid, uses organic solvent CHCl3By the DMF in water phase
It extracts (volume ratio of organic solvent and waste water is 2:1), organic phase distillation extracted, obtained CHCl3It can apply,
Obtained DMF purity is very high (purity reaches 95%), can be recycled.
Alkali is added again and adjusts pH to 13, this water phase distills available triethylamine, three second again after extraction for water phase
Amine removes moisture using sodium hydroxide, and available high-purity triethylamine (purity is up to 94%) is recyclable to apply.
Water phase is faint yellow as clear as crystal solution after being disposed, and COD is 21.5 ten thousand mg/L.The CHCl of extraction3It returns
Yield is 92.5%, DMF recovery rate 87.0%, the triethylamine rate of recovery 88.2%.
Embodiment 5
Certain DMF waste liquid main component containing triethylamine: DMF, triethylamine, unknown inorganic salts etc.;COD is about 800,000 in waste liquid
mg/L。
The pH to 8 that sodium hydroxide adjusts waste liquid is added in water phase waste liquid, uses organic solvent CHCl3By the DMF in water phase
It extracts (volume ratio of organic solvent and waste water is 4:1), organic phase distillation extracted, obtained CHCl3It can apply,
Obtained DMF purity is very high (purity reaches 95%), can be recycled.
Alkali is added again and adjusts pH to 11, this water phase distills available triethylamine, three second again after extraction for water phase
Amine removes moisture using sodium hydroxide, and available high-purity triethylamine (purity is up to 95%) is recyclable to apply.
Water phase is faint yellow as clear as crystal solution after being disposed, and COD is 240,000 mg/L.The CHCl of extraction3Recycling
Rate is 90%, DMF recovery rate 84.0%, the triethylamine rate of recovery 85%.
Embodiment 6
Certain DMF waste liquid main component containing triethylamine: DMF, triethylamine, unknown inorganic salts etc.;COD is about 800,000 in waste liquid
mg/L。
The pH to 11 that sodium hydroxide adjusts waste liquid is added in water phase waste liquid, uses organic solvent CHCl3By the DMF in water phase
It extracts (volume ratio of organic solvent and waste water is 3:1), organic phase distillation extracted, obtained CHCl3It can apply,
Obtained DMF purity is very high (purity reaches 94%), can be recycled.
Alkali is added again and adjusts pH to 11, this water phase distills available triethylamine, three second again after extraction for water phase
Amine removes moisture using sodium hydroxide, and available high-purity triethylamine (purity is up to 93%) is recyclable to apply.
Water phase is faint yellow as clear as crystal solution after being disposed, and COD is 300,000 mg/L.The CHCl of extraction3Recycling
Rate is 88%, DMF recovery rate 82.0%, the triethylamine rate of recovery 83%.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements: the present invention is logical
It crosses using the DMF in organic solvent extraction wastewater phase, extractant and DMF can be obtained by single flash in extract liquor, extracts
Solvent can be with recycled, and obtained DMF can also be recycled.And still contain triethylamine by water phase extracted,
Alkali adjusting pH to 12~14 is added in this water phase can steam triethylamine using single flash, can obtain after drying
To the triethylamine of high-purity, can be recycled.This method is not only easy to operate, and equipment investment is low, and can will be in waste water
Triethylamine and DMF recycling and reusing substantially reduce the COD content in waste water.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of processing method of the DMF waste water containing triethylamine, which is characterized in that the treating method comprises:
The DMF waste water containing triethylamine is extracted using organic solvent, obtains the extract liquor and raffinate containing DMF;
It is distilled after being adjusted to the pH value of the raffinate, obtains triethylamine.
2. processing method according to claim 1, which is characterized in that the processing method further include: to described containing DMF's
Extract liquor is distilled, and extractant and DMF are respectively obtained.
3. processing method according to claim 1, which is characterized in that containing triethylamine to described using the organic solvent
DMF waste water extracted before, the processing method further include:
The pH for adjusting the DMF waste water containing triethylamine is 7~10.
4. processing method according to claim 1, which is characterized in that it is laggard that the pH of the raffinate is adjusted to 12~14
Row distillation, obtains the triethylamine.
5. processing method according to claim 1, which is characterized in that steamed after being adjusted to the pH value of the raffinate
The step of evaporating, obtaining the triethylamine include:
It is distilled after being adjusted to the pH value of the raffinate, obtains distillation head product;
The moisture in the distillation head product is removed, the triethylamine is obtained.
6. processing method according to claim 5, which is characterized in that use sodium hydroxide, potassium hydroxide, sodium carbonate, carbon
Moisture in one of sour potassium, magnesium sulfate and sodium sulphate or a variety of removals distillation head product, obtains the triethylamine.
7. processing method according to claim 1, which is characterized in that used the extractant as the organic solvent
It is extracted in the DMF waste water containing triethylamine.
8. processing method according to any one of claim 1 to 7, which is characterized in that the organic solvent is selected from CHCl3、
CH2Cl2, any one of ethyl acetate and toluene.
9. processing method according to any one of claim 1 to 7, which is characterized in that the organic solvent contains with described
The volume ratio of the DMF waste water of triethylamine is 1~5:1.
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