CN110117034A - A kind of method of Centrifugical extraction high-concentration phenolic wastewater and its recycling - Google Patents
A kind of method of Centrifugical extraction high-concentration phenolic wastewater and its recycling Download PDFInfo
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- CN110117034A CN110117034A CN201810117239.5A CN201810117239A CN110117034A CN 110117034 A CN110117034 A CN 110117034A CN 201810117239 A CN201810117239 A CN 201810117239A CN 110117034 A CN110117034 A CN 110117034A
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- extraction
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- phenolic wastewater
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- concentration phenolic
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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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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physical Water Treatments (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention belongs to technical field of sewage, a kind of method of Centrifugical extraction high-concentration phenolic wastewater and its recycling is disclosed.Multiple concatenated centrifugal extractors are successively flowed into method includes the following steps: high-concentration phenolic wastewater is pumped, when waste water is flowed out from the discharge port of end centrifugal extractor, extractant is inversely successively flowed into multiple concatenated centrifugal extractors for filling with phenol wastewater through pump, to be extracted dose from first centrifugal extractor when discharge port outflow, Centrifugical extraction, by extraction phase it is washed after through pump enter back extraction centrifugal extractor in, raffinate phase waste water enters aftertreatment device or direct emission；Method of the invention except phenol effect it is good, extraction yield >=98%, phenol in wastewater content drop to 970mg/L hereinafter, reduce subsequent biochemical processing pressure；Cost is relatively low for extractant system, and extractant loss is small after back extraction；Phenolic resin raw materials for production are used as after the phenates recycling of back extraction recycling, realize resource utilization.
Description
Technical field
The invention belongs to technical field of sewage, in particular to a kind of Centrifugical extraction high-concentration phenolic wastewater and its resource
The method of change.
Background technique
Phenol is common raw material and intermediate in a kind of chemical industry, and phenol wastewater source is wider, endangers extremely serious.Phenol
Class compound is a kind of prototype poisonous substance, has certain damaging effect to all biological plastids.Meanwhile phenolic compound is again
A kind of important raw material of industry, phenolic compound purposes is very extensive, such as insecticide, explosive, drug and dyestuff etc..
In the prior art, processing wastewater from chemical industry is generally used biochemical method, physical method, chemical method three categories, wherein with life
Change method is the most cheap, and pollution is small, but phenolic compound is toxic, and excessive concentration can inhibit the degradation of microorganism,
This method is not suitable for handling high-concentration phenolic wastewater.Extraction is with equipment investment is few, occupied area is small, easy to operate, energy consumption
It is low, have many advantages, such as industry park plan experience abundant, and major pollutants energy effective recycling, be valued by people.
In physical extraction dephenolize technology, the higher extractant of Pyrogentisinic Acid's distribution coefficient, solubility in water is also bigger, this is bound to
It will cause secondary pollution, biggish solvent is lost or aggravates the load for being easy recycling in raffinate.Complexometric extraction is a kind of based on can
The new method of inverse complex reaction separating polar organic matter, it had both been absorbed, and physical extraction is easy to operate, processing capacity is strong, it is real to be easy
The advantages of now automating, and the high efficiency, highly selective of chemical extraction is remained, while it is poorly reversible to also overcome chemical extraction
Deficiency.
For the processing of industrial phenol wastewater, common complexing agent mainly has neutral containing phosphorus extractant and amine extracted
Agent.Using the mixture conduct of tributyl phosphate, middle oil and aminated compounds in Chinese disclosure CN201510590378.6
Extractant carries out complexometric extraction polyphenol to semi-coke phenol wastewater, and extraction yield is higher.But extractant higher cost, in addition, three
Octylame tends not to dissolve extracted species well, and emulsification or third phase are easy to appear in extraction process, and it is appropriate to need to be added
Cosolvent, extractant system is relatively complicated, and industrial applications are limited, and the back extraction of extractant is not directed in disclosure
And resource utilization.
In addition, the extracting power of complexing extractant is limited by concentration is complexed in solvent, for weak solution, equilibrium assignmen system
Number is higher, and for highly concentrated solution, coefficient of balance can decline.The present invention forefathers study on the basis of, use it is lower at
This complexing extractant system and Centrifugical extraction method, the modifying agent that higher distribution coefficient is added handle high-concentration phenolic wastewater
For general concentration waste water, complexing extractant plays a role phenolic wastewater treatment, improves dephenolize rate by Centrifugical extraction, reduces
The pressure of successive depths processing waste water, the standard that is even up to expelled directly out.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of phenolic resin
High-concentration phenolic wastewater preprocess method in production or resin grease production, can be improved dephenolize rate by Centrifugical extraction, with
Reduce the pressure of biochemical treatment or subsequent processing.
The purpose of the present invention is realized by following proposal:
A kind of method of Centrifugical extraction high-concentration phenolic wastewater and its recycling, comprising the following steps:
(1) high-concentration phenolic wastewater is pumped and successively flows into multiple concatenated centrifugal extractors；
(2) when high-concentration phenolic wastewater from the discharge port of end centrifugal extractor flow out when, by extractant pumped inversely according to
It is secondary to flow into multiple concatenated centrifugal extractors for filling with phenol wastewater；
(3) to be extracted dose when discharge port flows out from first centrifugal extractor, Centrifugical extraction, extraction phase enters anti-through pump
Extract in section centrifugal extractor, raffinate phase waste water enters aftertreatment device or direct emission；
(4) strip liquor flows into the centrifugal extractor full of extraction phase step by step through pump adverse current, carries out under certain technique anti-
Extraction, multiplexing extractant and phenates after recycling back extraction；
(5) the multiplexing extractant after back extraction is reused, high-concentration phenolic wastewater is extracted again；
(6) CO is passed through into the phenates after back extraction2Gas recycles phenol, for producing；
High-concentration phenolic wastewater described in step (1) be phenolic resin produce or resin grease factory it is useless containing phenol
Water, 40000~88300mg/L of phenol content, COD are 200000~250000mg/L, pH value is 0.6~2；
Multiple concatenated centrifugal extractors described in step (1) refer to 1~3 centrifugal extractor series connection；
Extractant described in step (2) is made of complexing agent≤30%, modifying agent≤70%, diluent≤70%,
In percentage refer to percentage by volume, the sum of complexing agent, percentage by volume of modifying agent and diluent are 100%；The network
Mixture refers to that tributyl phosphate, the modifying agent criticize octanol；The diluent refers to kerosene.
Centrifugal extractor described in step (1) and step (2) be annulus type centrifugal extractor, the range of speeds be 2500~
7000r/min, separation factor are as follows: 200~1100, it flows than 1:100~100:1；
The process conditions of Centrifugical extraction described in step (3) are as follows: extraction series n are as follows: 1~3 grade, extraction time be (3~
5) min*n (n is extraction series), centrifugal extractor revolving speed are as follows: 3000~5000r/min, extractant and high-concentration phenolic wastewater
Two-phase compares (volume ratio) are as follows: 1:1~1:6 (preferably 1:1~1:2), two-phase flux (flow)≤70mL/min；
Subsequent processing in step (3) can be photocatalysis treatment；
The NaOH aqueous solution, ammonium hydroxide or KOH that strip liquor described in step (4) refers to that mass fraction is 5%~20% are water-soluble
Liquid；
The process conditions of back extraction described in step (4) are as follows: the volume ratio of strip liquor and extraction phase is 1:10~15, back extraction
Series is 1~2 grade, and the revolving speed of centrifugal extractor is 3000~5000r/min, the flux of strip liquor and extraction phase≤70mL/
min。
The process flow chart of above-mentioned Centrifugical extraction high-concentration phenolic wastewater and its recycling is as shown in Figure 1.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) except phenol effect it is good, processing method through the invention, high concentration phenol wastewater (phenol content 40000~
88300mg/L) after 1 grade of extraction, after the extraction of phenol extraction yield >=98%, 2 grade, after the extraction of phenol extraction yield >=99%, 3 grade,
Phenol extraction yield >=99.8%, extraction efficiency are high；
(2) by means of the present invention, the phenol wastewater (40000~88300mg/L) of high concentration gives up after 1 grade of extraction
Phenol content drops to 970mg/L hereinafter, after 2 grades of extractions in water, and phenol in wastewater content drops to 455mg/L hereinafter, 3 grades of extractions
Afterwards, phenol in wastewater content drops to 73mg/L hereinafter, reducing the pressure of subsequent biochemical processing；
(3) tributyl phosphate, the n-octyl alcohol, kerosene complexing extractant system of lower cost are used, n-octyl alcohol plays collaboration extraction
Take with hydrotropy double action, by high concentration highly acid phenolic wastewater treatment to general concentration phenol wastewater solution, while extraction is complexed
The general concentration phenol wastewater of processing is taken, without adjusting the pH value of phenol wastewater, is reduced sour, alkali chemical reagent in experimentation
Dosage and experimental implementation；
(4) cost is relatively low for extractant system, and extractant loss is small after back extraction, and when number >=10 is recycled, extraction
Agent extraction efficiency is still preferably >=97%；
(5) phenolic resin raw materials for production are used as after the phenates recycling of back extraction recycling, realize resource utilization.
Detailed description of the invention
Fig. 1 is the process flow chart of the method for Centrifugical extraction high-concentration phenolic wastewater and its recycling of the invention.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Handled high-concentration phenolic wastewater is the phenolic aldehyde tree for building surging (Fanyu Nansha) Chemical Co., Ltd. in embodiment
Rouge factory waste water, phenol content 50453mg/L, COD content 234000mg/L, pH=0.6；Centrifugical extraction used in embodiment
Device is the HL-20D type centrifugal extractor of Beijing extraction application technical research institute.
The method of Centrifugical extraction high-concentration phenolic wastewater in the present invention and its recycling specifically includes the following steps:
(1) high-concentration phenolic wastewater is pumped and successively flows into multiple concatenated centrifugal extractors；
(2) when high-concentration phenolic wastewater from the discharge port of end centrifugal extractor flow out when, by extractant pumped inversely according to
It is secondary to flow into multiple concatenated centrifugal extractors for filling with phenol wastewater；
(3) to be extracted dose from first centrifugal extractor discharge port flow out when, Centrifugical extraction, by extraction phase it is washed after
Enter in back extraction centrifugal extractor through pump, raffinate phase waste water enters aftertreatment device or direct emission；
(4) strip liquor flows into the centrifugal extractor full of extraction phase step by step through pump adverse current, carries out under certain technique anti-
Extraction, extractant and phenates after recycling back extraction；
(5) extractant after back extraction is reused, high-concentration phenolic wastewater is extracted again；
(6) CO is passed through into the phenates after back extraction2Gas recycles phenol, for producing；
Embodiment 1:
Main technologic parameters are as follows for embodiment 1:
Extractant: tributyl phosphate 30%, n-octyl alcohol 35%, kerosene 35%；
Extractant compares 1:2 with high-concentration phenolic wastewater, and the flow velocity of extractant is 10mL/min, high-concentration phenolic wastewater
Flow velocity is 20mL/min；
Centrifugal extractor: revolving speed 3500r/min, extraction series are respectively 1 grade, 2 grades, 3 grades；Extraction time is respectively
3min,6min,9min；
Photocatalysis treatment is carried out to the raffinate after 3 grades of Centrifugical extractions, its phenol content < 0.5mg/L, COD content can be made
< 60mg/L.
Phenol content in raffinate and COD concentration after Centrifugical extraction is as shown in table 1 below:
The extraction yield and COD removal rate in raffinate after 1 multitple extraction of table
Embodiment 2:
Extractant: tributyl phosphate 30%, n-octyl alcohol 35%, kerosene 35%；
Extractant compares 1:1 with high-concentration phenolic wastewater, and the flow velocity of extractant is 10mL/min, high-concentration phenolic wastewater
Flow velocity is 10mL/min；
Centrifugal extractor: revolving speed 4000r/min, extraction series are 3 grades, extraction time 9min；
Phenol content in raffinate and COD concentration after Centrifugical extraction is as shown in table 2 below:
Extraction yield and COD removal rate in 2 grades of raffinates extracted of table
Embodiment 3:
Extractant three-level extraction phase extracted in embodiment 1 is stripped using 20wt%NaOH, 20wt%NaOH
Flow velocity be 6mL/min, load organic phases (extraction reaction after extraction phase) flow velocity is 60mL/min；Back extraction series: 2 grades, instead
Extraction centrifugal extractor revolving speed is 3200r/min, obtains sodium phenate and multiplexing extractant；After 10 back extraction, extractant loss late≤
0.2‰；
The repeated experiment that the extractant for being recycled 10 times is extracted, the results are shown in Table 3:
Extraction yield and COD removal rate in 3 repeated experiment of table in raffinate
It can be seen that extraction yield >=98% of method of the invention from table 1~2, and the phenol wastewater of high concentration is through this
After the method processing of invention, phenol in wastewater content also drops to 100mg/L hereinafter, reducing successive depths processing after 3 grades of extractions
Pressure.
From table 3 it is observed that extraction yield is still higher when extractant extracted is after stripping agent is stripped, 3 grades of extraction yields
>=99.6%；CO is passed through into the phenates of back extraction recycling2, phenol is obtained, phenolic resin raw materials for production is can be used as, realizes resource
Change and utilizes.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of method of Centrifugical extraction high-concentration phenolic wastewater and its recycling, it is characterised in that the following steps are included:
(1) high-concentration phenolic wastewater is pumped and successively flows into multiple concatenated centrifugal extractors；
(2) when high-concentration phenolic wastewater is flowed out from the discharge port of end centrifugal extractor, extractant is inversely successively flowed through pump
Enter in multiple concatenated centrifugal extractors for filling with phenol wastewater；
(3) to be extracted dose from first centrifugal extractor discharge port flow out when, Centrifugical extraction, extraction phase through pump enter stripping section
In centrifugal extractor, raffinate phase waste water enters aftertreatment device or direct emission；
(4) strip liquor flows into the centrifugal extractor full of extraction phase step by step through pump adverse current, is stripped under certain technique, returns
Multiplexing extractant and phenates after receiving back extraction；
(5) the multiplexing extractant after back extraction is reused, high-concentration phenolic wastewater is extracted again；
(6) CO is passed through into the phenates after back extraction2Gas recycles phenol, for producing.
2. the method for Centrifugical extraction high-concentration phenolic wastewater according to claim 1 and its recycling, it is characterised in that:
High-concentration phenolic wastewater described in step (1) is the phenol wastewater of phenolic resin production or resin grease factory, benzene
40000~88300mg/L of phenol content, COD are 200000~250000mg/L, pH value is 0.6~2.
3. the method for Centrifugical extraction high-concentration phenolic wastewater according to claim 1 and its recycling, it is characterised in that:
Multiple concatenated centrifugal extractors described in step (1) refer to 1~3 centrifugal extractor series connection.
4. the method for Centrifugical extraction high-concentration phenolic wastewater according to claim 1 and its recycling, it is characterised in that:
Extractant described in step (2) is made of complexing agent≤30%, modifying agent≤70%, diluent≤70%, therein
Percentage refers to percentage by volume, and the sum of complexing agent, percentage by volume of modifying agent and diluent are 100%；The complexing agent
Refer to that tributyl phosphate, the modifying agent criticize octanol；The diluent refers to kerosene.
5. the method for Centrifugical extraction high-concentration phenolic wastewater according to claim 1 and its recycling, it is characterised in that:
Centrifugal extractor described in step (1) and step (2) be annulus type centrifugal extractor, the range of speeds be 2500~
7000r/min, separation factor are as follows: 200~1100, it flows than 1:100~100:1.
6. the method for Centrifugical extraction high-concentration phenolic wastewater according to claim 1 and its recycling, it is characterised in that:
The process conditions of Centrifugical extraction described in step (3) are as follows: extraction series n are as follows: 1~3 grade, extraction time is (3~5)
Min*n, centrifugal extractor revolving speed are as follows: 3000~5000r/min, extractant are compared with high-concentration phenolic wastewater two-phase are as follows: 1:1~
1:6, two-phase flux≤70mL/min.
7. the method for Centrifugical extraction high-concentration phenolic wastewater according to claim 1 and its recycling, it is characterised in that:
Strip liquor described in step (4) refers to that mass fraction is 5%~20% NaOH aqueous solution, ammonium hydroxide or KOH aqueous solution.
8. the method for Centrifugical extraction high-concentration phenolic wastewater according to claim 1 and its recycling, it is characterised in that:
The process conditions of back extraction described in step (4) are as follows: the volume ratio of strip liquor and extraction phase is 1:10~15, is stripped series
Be 1~2 grade, the revolving speed of centrifugal extractor is 3000~5000r/min, the flux of strip liquor and extraction phase≤70mL/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314726A (en) * | 2020-09-27 | 2022-04-12 | 广州中国科学院沈阳自动化研究所分所 | Hydrophobic eutectic solvent and application thereof in extraction of industrial phenol-containing wastewater |
| CN114956395A (en) * | 2021-02-24 | 2022-08-30 | 广州中国科学院沈阳自动化研究所分所 | Device and method for treating high-concentration phenol-containing wastewater by combining centrifugal extraction and electrocatalysis |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314726A (en) * | 2020-09-27 | 2022-04-12 | 广州中国科学院沈阳自动化研究所分所 | Hydrophobic eutectic solvent and application thereof in extraction of industrial phenol-containing wastewater |
| CN114956395A (en) * | 2021-02-24 | 2022-08-30 | 广州中国科学院沈阳自动化研究所分所 | Device and method for treating high-concentration phenol-containing wastewater by combining centrifugal extraction and electrocatalysis |
| CN114956395B (en) * | 2021-02-24 | 2023-08-11 | 广州中国科学院沈阳自动化研究所分所 | Device and method for treating high-concentration phenol-containing wastewater by centrifugal extraction and electrocatalytic combination |
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Application publication date: 20190813 |