CN105712427A - Extracting agent with high partition coefficient for polyphenol in phenol wastewater and extracting method - Google Patents
Extracting agent with high partition coefficient for polyphenol in phenol wastewater and extracting method Download PDFInfo
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- CN105712427A CN105712427A CN201610210420.1A CN201610210420A CN105712427A CN 105712427 A CN105712427 A CN 105712427A CN 201610210420 A CN201610210420 A CN 201610210420A CN 105712427 A CN105712427 A CN 105712427A
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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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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Abstract
The invention belongs to the technical field of sewage treatment and discloses an extracting agent with high partition coefficient for polyphenol in phenol wastewater and an extracting method. The method comprises the following steps: MIBK (methyl isobutyl ketone) is taken as a main extracting agent, toluene is taken as a synergic extracting agent, the volume fraction of MIBK is 90%-95%, the volume fraction of toluene is 5%-10%, then the phenol wastewater is subjected to multi-stage countercurrent extraction with the composite extracting agent at the temperature of 25-70 DEG C, and an extraction phase and a raffinate phase are obtained. The extracting effect of the composite extracting agent on polyphenol is improved greatly, the polarity of toluene and the polarity of MIBK in the composite extracting agent are close, the boiling point of toluene and the boiling point of MIBK in the composite extracting agent are close, so that less solvent loss is caused, recycling is facilitated, and the extracting agent has good prospect in practical industrial application.
Description
Technical field
The invention belongs to technical field of sewage, be specifically related to a kind of extractant and extracting process that polyhydric phenols in phenol wastewater is had high partition coefficient.
Background technology
Producing highly concentrated phenol wastewater in the techniques such as cooling, washing and purification in the processes such as Lu Qi gasification, BGL gasification, coal low temperature distillation, coal tar hydrogenating, its water quality components content is complicated, and unit phenol, polyphenol content are high, biochemical treatment difficulty.At present, when this kind of phenol wastewater is processed, it is generally adopted the solvent extraction aldehydes matter to remove in waste water, what coal gasification waste water extracting and dephenolizing can be implemented it is critical only that first chooses applicable extractant, extraction conditions and extracts progression, thus determining that rational removing phenol in waste water technological process, Organic substance reclaim and extractant regeneration method and extraction equipment etc. again.At present, carrying out the extractant of aldehydes matter extraction process for this kind of waste water mainly has Di Iso Propyl Ether, hexone, a middle wet goods, and industrial application more be Di Iso Propyl Ether and hexone.Comparing other extractants such as Di Iso Propyl Ether, hexone is higher to the extraction partition coefficient of unit phenol, application existing very ripe in the industry, but it is relatively low to the extraction partition coefficient of polyhydric phenols, and the effect of extracting of polyhydric phenols is not good.For highly concentrated phenol wastewater, the extractant that polyhydric phenols is had high partition coefficient by exploitation is necessary.
Summary of the invention
In order to solve the shortcoming and defect part of prior art, the primary and foremost purpose of the present invention is in that to provide a kind of extractant that polyhydric phenols in phenol wastewater has high partition coefficient.
Another object of the present invention is to provide a kind of method adopting above-mentioned extractant that phenol wastewater is extracted.
The object of the invention is achieved through the following technical solutions:
A kind of extractant that polyhydric phenols in phenol wastewater has high partition coefficient, described extractant is made up of the main body extractant hexone that volume fraction is 90%～95% and the synergic reagent toluene that volume fraction is 5%～10%.
A kind of method adopting above-mentioned extractant that phenol wastewater is extracted, comprises the steps:
With hexone for main body extractant, toluene is synergic reagent, wherein hexone volume fraction is 90%～95%, volume of toluene mark is 5%～10%, then phenol wastewater is carried out multi-stage counter current extraction with this composite extractant at 25～70 DEG C of temperature, be extracted mutually and raffinate phase.
Preferably, described phenol wastewater refers to that polyphenol content is not less than the highly concentrated phenol wastewater of 5000mg/L；But consider and can be directly used in order to ensure dephenolize water outlet next step biochemical treatment from the source of waste water, in described phenol wastewater, total phenol content is more preferably 8000～18000mg/L.
Preferably, described phenol wastewater is containing phenol coal chemical industrial waste water；Described is 5000～10000mg/L containing polyphenol content in phenol coal chemical industrial waste water, and unit phenol content is 3000～8000mg/L.
Preferably, described composite extractant is 1:(2～7 with the volume ratio of phenol wastewater).
Preferably, described extraction refers to the extraction carried out when pH is 6～9；The extraction carried out when being 6～7 more preferably in pH.
Preferably, in described multi-stage counter current extraction process, incorporation time is 30min, and time of repose is 15min.
Before phenol wastewater is extracted by the compound extractant of above-mentioned employing, also include the process that phenol wastewater is carried out oil removing oil removal, deacidification deamination pretreatment.
After phenol wastewater is extracted by the compound extractant of above-mentioned employing, after also including raffinate phase entrance solvent stripper stripping recovery extractant, water purification sends into biochemical treatment；Extraction phase enters rectifying column rectification and reclaims crude phenols and extractant, and the extractant after recovery recycles.
Principles of the invention is: containing gas chromatography in coal gasification waste water, in order to determine the various organic existence impact (playing a driving role or inhibitory action) on extractant separating phenols material, useless Organic substance in water has been carried out qualitative analysis, determine several typical Organic substances in waste water, and measure these organic existence by experiment to hexone separating phenols material with or without impact.Found that the effect that hexone is extracted polyhydric phenols by toluene in suitable concentration range increases significantly, further by experiment test repeatedly, determine under certain extraction conditions (temperature, pH), toluene and hexone are under suitable concentration proportioning, it is possible to the significant effect improving the many polyhydric phenols of extractant.The boiling point (111 DEG C) of toluene and the boiling point (116 DEG C) of hexone are close simultaneously, and they dissolubility in water are close, it is easy to recycling use simultaneously.
Preparation method and the obtained product of the present invention have the advantage that and beneficial effect:
(1) effect of extracting of polyhydric phenols is greatly improved by the more original extractant of the composite extractant of the present invention, provides better environment for follow-up biochemical treatment.
(2) in the composite extractant of the present invention, toluene is close with the polarity of hexone, and the dissolubility in water is less, and solvent loss is less.
(3) in the composite extractant of the present invention, toluene is close with the boiling point of hexone, recycling use simultaneously.
(4) coal chemical industrial waste water containing phenol contains toluene, the coal chemical industrial waste water containing phenol is processed by the composite extractant adopting the present invention, the a part of toluene in waste water can be utilized, so can gather materials on the spot and reduce the consumption of extractant, simultaneously facilitate follow-up to the utilization of toluene centralized recovery.
(5) present invention composite extractant based on hexone, in actual industrial is used, the change of the operating condition of equipment is little, be conducive to quickly being used in extracting and dephenolizing flow process.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Phenol content in following example measures by the following method:
Adopt gas chromatograph, carry out each component analysis with the DB-5MS capillary column of 30m × 0.32mm × 0.25 μm and hydrogen flame ionization detector (FID).Adopting internal standard method, the internal standard substance of MIBK is ethanol, and the internal standard substance of aldehydes matter is capryl alcohol.The temperature of injector and detector respectively 270 DEG C and 230 DEG C.Post case initial temperature is set as 110 DEG C, after keeping 2min, rises to 160 DEG C with 10 DEG C/min.Carrier gas used is nitrogen, flow velocity 30ml/min.
Embodiment 1
By volume the hexone of 90% and the toluene of 10% are configured to compound extractant；Being 8000mg/L by total phenol content, wherein unit phenol content is 3000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 5000mg/L controls at 25 DEG C, and regulates pH value to 6；Then above-mentioned compound extractant and phenol wastewater are carried out four-stage counter-current extraction for 1:4 by volume in 4 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 144mg/L and the 365mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 11425mg/L and 18538mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 95.21% and the polyhydric phenols of 92.69% can be removed by single extraction.
Embodiment 2
By volume the hexone of 95% and the toluene of 5% are configured to compound extractant；Being 18000mg/L by total phenol content, wherein unit phenol content is 8000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 10000mg/L controls at 25 DEG C, and regulates pH value to 6；Then above-mentioned compound extractant and phenol wastewater are carried out four-stage counter-current extraction for 1:4 by volume in 4 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 331mg/L and the 605mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 19172mg/L and 37580mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 95.86% and the polyhydric phenols of 93.95% can be removed by single extraction.
Embodiment 3
By volume the hexone of 95% and the toluene of 5% are configured to compound extractant；Being 8000mg/L by total phenol content, wherein unit phenol content is 3000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 5000mg/L controls at 25 DEG C, and regulates pH value to 6；Then above-mentioned compound extractant and phenol wastewater are carried out four-stage counter-current extraction for 1:4 by volume in 4 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 123mg/L and the 319mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 11506mg/L and 18722mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 95.89% and the polyhydric phenols of 93.61% can be removed by single extraction.
Embodiment 4
By volume the hexone of 90% and the toluene of 10% are configured to compound extractant；Being 10000mg/L by total phenol content, wherein unit phenol content is 4000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 6000mg/L controls at 25 DEG C, and regulates pH value to 7；Then above-mentioned compound extractant and phenol wastewater are carried out four-stage counter-current extraction for 1:2 by volume in 4 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 118mg/L and the 280mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 7763mg/L and 11439mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 97.04% and the polyhydric phenols of 95.33% can be removed by single extraction.
Embodiment 5
By volume the hexone of 95% and the toluene of 5% are configured to compound extractant；Being 14000mg/L by total phenol content, wherein unit phenol content is 6000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 8000mg/L controls at 70 DEG C, and regulates pH value to 7；Then above-mentioned compound extractant and phenol wastewater are carried out four-stage counter-current extraction for 1:7 by volume in 4 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 375mg/L and the 678mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 39370mg/L and 51307mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 93.74% and the polyhydric phenols of 91.62% can be removed by single extraction.
Embodiment 6
By volume the hexone of 90% and the toluene of 10% are configured to compound extractant；Being 8000mg/L by total phenol content, wherein unit phenol content is 3000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 5000mg/L controls at 25 DEG C, and regulates pH value to 9；Then above-mentioned compound extractant and phenol wastewater are carried out four-stage counter-current extraction for 1:4 by volume in 4 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 380mg/L and the 7321mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 10477mg/L and 17072mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 87.31% and the polyhydric phenols of 85.36% can be removed by single extraction.
Embodiment 7
By volume the hexone of 90% and the toluene of 10% are configured to compound extractant；Being 10000mg/L by total phenol content, wherein unit phenol content is 4000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 6000mg/L controls at 50 DEG C, and regulates pH value to 9；Then above-mentioned compound extractant and phenol wastewater are carried out four-stage counter-current extraction for 1:4 by volume in 4 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 199mg/L and the 473.4mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 15203mg/L and 22106mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 95.02% and the polyhydric phenols of 92.11% can be removed by single extraction.
Embodiment 8
By volume the hexone of 92% and the toluene of 8% are configured to compound extractant；Being 12000mg/L by total phenol content, wherein unit phenol content is 5000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 7000mg/L controls at 25 DEG C, and regulates pH value to 7；Then above-mentioned compound extractant and phenol wastewater are carried out six stage countercurrent extractions for 1:4 by volume in 6 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 198mg/L and the 437mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 19208mg/L and 26250mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 96.04% and the polyhydric phenols of 93.75% can be removed by single extraction.
Comparative example
Being 8000mg/L by total phenol content, wherein unit phenol content is 3000mg/L, and the coal chemical industrial waste water temperature containing phenol that polyphenol content is 5000mg/L controls at 25 DEG C, and regulates pH value to 7；Then above-mentioned hexone and phenol wastewater are carried out four-stage counter-current extraction for 1:4 by volume in 4 separatory funnels, wherein mix 30min, stand 15min, be extracted mutually and raffinate phase.
Content respectively 176mg/L and the 1090mg/L of unit phenol and polyhydric phenols, the content of unit phenol and polyhydric phenols respectively 11294mg/L and 15642mg/L in described extraction phase in described raffinate phase after testing.Thus can calculate, the unit phenol of in highly concentrated phenol wastewater 94.12% and the polyhydric phenols of 78.21% can be removed by single extraction.
From the result of above example it can be seen that adopt compound extractant provided by the invention can be greatly improved the extractant extraction efficiency to polyhydric phenols.From the contrast of embodiment 1 and embodiment 7 it can be seen that when the pH value of described highly concentrated phenol wastewater is not higher than 7, extractant can significantly more reduce the content of unit phenol and polyhydric phenols in described phenol wastewater.From the contrast of embodiment 1 and comparative example it can be seen that the partition coefficient of compound extractant polyhydric phenols is higher than hexone.Show the composite extractant of the present invention effect of extracting to unit phenol not second in hexone situation, it is possible to be greatly improved the extraction efficiency to polyhydric phenols, great prospects for commercial application.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted to the described embodiments; the change made under other any spirit without departing from the present invention and principle, modification, replacement, combination, simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the extractant that polyhydric phenols in phenol wastewater is had high partition coefficient, it is characterised in that: described extractant is made up of the main body extractant hexone that volume fraction is 90%～95% and the synergic reagent toluene that volume fraction is 5%～10%.
2. the method that phenol wastewater is extracted by the extractant adopted described in claim 1, it is characterised in that comprise the steps:
With hexone for main body extractant, toluene is synergic reagent, wherein hexone volume fraction is 90%～95%, volume of toluene mark is 5%～10%, then phenol wastewater is carried out multi-stage counter current extraction with this composite extractant at 25～70 DEG C of temperature, be extracted mutually and raffinate phase.
3. a kind of method that phenol wastewater is extracted according to claim 2, it is characterised in that: described phenol wastewater refers to that polyphenol content is not less than 5000mg/L, and total phenol content is the highly concentrated phenol wastewater of 8000～18000mg/L.
4. a kind of method that phenol wastewater is extracted according to Claims 2 or 3, it is characterised in that: described phenol wastewater is containing phenol coal chemical industrial waste water；Described is 5000～10000mg/L containing polyphenol content in phenol coal chemical industrial waste water, and unit phenol content is 3000～8000mg/L.
5. a kind of method that phenol wastewater is extracted according to Claims 2 or 3, it is characterised in that: the volume ratio of described composite extractant and phenol wastewater is 1:(2～7).
6. a kind of method that phenol wastewater is extracted according to Claims 2 or 3, it is characterised in that: described extraction refers to the extraction carried out when pH is 6～9.
7. a kind of method that phenol wastewater is extracted according to claim 6, it is characterised in that: described extraction refers to the extraction carried out when pH is 6～7.
8. a kind of method that phenol wastewater is extracted according to Claims 2 or 3, it is characterised in that: in described multi-stage counter current extraction process, incorporation time is 30min, and time of repose is 15min.
9. a kind of method that phenol wastewater is extracted according to Claims 2 or 3, it is characterised in that: before adopting compound extractant that phenol wastewater is extracted, also include the process that phenol wastewater is carried out oil removing oil removal, deacidification deamination pretreatment.
10. a kind of method that phenol wastewater is extracted according to Claims 2 or 3, it is characterized in that: after adopting compound extractant that phenol wastewater is extracted, after also including raffinate phase entrance solvent stripper stripping recovery extractant, water purification sends into biochemical treatment；Extraction phase enters rectifying column rectification and reclaims crude phenols and extractant, the process that the extractant after recovery recycles.
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| CN106044916A (en) * | 2016-07-12 | 2016-10-26 | 华南理工大学 | Application of methyl isopropyl methylketone to treatment of high-concentration phenolic wastewater |
| CN106145234A (en) * | 2016-07-12 | 2016-11-23 | 华南理工大学 | A kind of processing method of highly concentrated phenol wastewater |
| CN106745901A (en) * | 2016-12-30 | 2017-05-31 | 安徽时联特种溶剂股份有限公司 | A kind of processing method containing high-concentration phenolic wastewater |
| CN106854006A (en) * | 2016-12-21 | 2017-06-16 | 华南理工大学 | The extractant and extracting process of a kind of efficient removal COD and polyhydric phenols |
| CN106865674A (en) * | 2017-03-01 | 2017-06-20 | 煤炭科学技术研究院有限公司 | A kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation |
| CN106865675A (en) * | 2017-03-27 | 2017-06-20 | 中国矿业大学(北京) | A kind of method for extracting and dephenolizing of phenol wastewater |
| CN107739299A (en) * | 2017-11-23 | 2018-02-27 | 魏艳娟 | The refining spearation combined dehydration method and device of mixed phenol |
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| ES2112095B1 (en) * | 1994-01-26 | 1999-07-16 | Bakelite Iberica S A | PROCEDURE FOR THE RECOVERY OF PHENOL PRESENT IN AQUEOUS EFFLUENTS CONTAINING IT AND FOR THE PURIFICATION OF SUCH EFFLUENTS. |
| CN102674608A (en) * | 2012-05-11 | 2012-09-19 | 华南理工大学 | Method for recycling and treating high-concentration phenol/ammonia wastewater |
| CN104276618B (en) * | 2014-10-30 | 2015-11-18 | 河南龙成煤高效技术应用有限公司 | The dephenolization method of a kind of coal chemical industrial waste water dephenolize extraction agent and uses thereof and coal chemical industrial waste water |
| CN105176556A (en) * | 2015-09-11 | 2015-12-23 | 波露明（北京）科技有限公司 | Method for separating phenol from coal tar phenol-containing distillate oil |
| CN105399174B (en) * | 2015-12-17 | 2018-08-03 | 王伟东 | Low energy consumption extracting and dephenolizing coal chemical industry wastewater and phenol recycling complete set of equipments and processing method |
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| CN106044916A (en) * | 2016-07-12 | 2016-10-26 | 华南理工大学 | Application of methyl isopropyl methylketone to treatment of high-concentration phenolic wastewater |
| CN106145234A (en) * | 2016-07-12 | 2016-11-23 | 华南理工大学 | A kind of processing method of highly concentrated phenol wastewater |
| CN106854006A (en) * | 2016-12-21 | 2017-06-16 | 华南理工大学 | The extractant and extracting process of a kind of efficient removal COD and polyhydric phenols |
| CN106854006B (en) * | 2016-12-21 | 2020-08-18 | 华南理工大学 | Extracting agent for efficiently removing COD (chemical oxygen demand) and polyphenol and extracting method |
| CN106745901A (en) * | 2016-12-30 | 2017-05-31 | 安徽时联特种溶剂股份有限公司 | A kind of processing method containing high-concentration phenolic wastewater |
| CN106865674A (en) * | 2017-03-01 | 2017-06-20 | 煤炭科学技术研究院有限公司 | A kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation |
| CN106865675A (en) * | 2017-03-27 | 2017-06-20 | 中国矿业大学(北京) | A kind of method for extracting and dephenolizing of phenol wastewater |
| CN107739299A (en) * | 2017-11-23 | 2018-02-27 | 魏艳娟 | The refining spearation combined dehydration method and device of mixed phenol |
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