CN108545849A - A method of phenol wastewater produced by processing needle coke production technology - Google Patents

A method of phenol wastewater produced by processing needle coke production technology Download PDF

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Publication number
CN108545849A
CN108545849A CN201810441836.3A CN201810441836A CN108545849A CN 108545849 A CN108545849 A CN 108545849A CN 201810441836 A CN201810441836 A CN 201810441836A CN 108545849 A CN108545849 A CN 108545849A
Authority
CN
China
Prior art keywords
phenol
production technology
needle coke
waste water
coke production
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810441836.3A
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Chinese (zh)
Inventor
张麟
张维冰
钟志华
赵雅梦
王守凯
安路阳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing Win Point Chromatographic Separation Technology Co Ltd
East China University of Science and Technology
Sinosteel Anshan Research Institute of Thermo Energy Co Ltd
Original Assignee
Nanjing Win Point Chromatographic Separation Technology Co Ltd
East China University of Science and Technology
Sinosteel Anshan Research Institute of Thermo Energy Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing Win Point Chromatographic Separation Technology Co Ltd, East China University of Science and Technology, Sinosteel Anshan Research Institute of Thermo Energy Co Ltd filed Critical Nanjing Win Point Chromatographic Separation Technology Co Ltd
Priority to CN201810441836.3A priority Critical patent/CN108545849A/en
Publication of CN108545849A publication Critical patent/CN108545849A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/16Nitrogen compounds, e.g. ammonia
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • C02F2101/345Phenols
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32

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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)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The present invention relates to a kind of methods of phenol wastewater produced by processing needle coke production technology.Waste water caused by needle coke production technology mainly contains phenol and nitrogen amide, and concentration is higher, and pH is close to 10.Such waste water nature determines that conventional method is difficult to realize detach except phenol condition is harsher.The present invention innovatively uses the mixed fillers of the macroporous absorbent resin that skeleton is polystyrene and the strong-base anion-exchange resin that skeleton is polystyrene to adsorb the aldehydes matter in waste water.Since the resin of aldehydes matter and polystyrene all has benzene ring structure, specific binding can be formed by π π interactions between the two, in addition, the ion exchange between phenol ion and anion exchange resin so that this mixed fillers can reach removes phenol effect well.Discharge standard is fully achieved in waste water after this flow processing, and present invention process flow is simple, at low cost, effect is good and environmentally protective.

Description

A method of phenol wastewater produced by processing needle coke production technology
Technical field
The present invention relates to technical field of waste water processing, and specifically, being that a kind of processing needle coke production technology is produced contains phenol The method of waste water.
Background technology
Needle coke is a kind of good carbon raw materials, and surface is in apparent strip lines, mostly strip needle when being crushed Fibrous structure, thus referred to as needle coke can be observed in shape fragment under the microscope.Needle coke is production high power graphite electrode With the raw material of ultra high power graphite electrode, the graphite electrode made of needle coke have thermal shock resistance strong, high mechanical strength, The advantages that current density that oxidation susceptibility is good, consumption of electrode is low and allows is big.Needle coke with oil refinery's heavy distillate or Person's coal tar, pitch are raw material, will produce volatile phenol and the amic waste water of nitrogen containing higher concentration, and its pH in production process It is higher, close to 10.
Phenol wastewater is extremely serious to environmental disruption, and phenolic compound is a kind of strong neurotoxic substance again, has corrosion Property, it is harmful to biology, therefore the hot spot that people study sewage disposal is had become to the processing of phenol wastewater.Locate both at home and abroad at present The method of reason phenol wastewater mainly has:Leather follows the example of, biochemical process, liquid-film method and active carbon adsorption, but all there are some defects, than Such as the problems such as complicated for operation, energy consumption is big, of high cost, and handle the ineffective of this kind of needle coke waste water.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide contain produced by a kind of processing needle coke production technology The method of phenol waste water.
The purpose of the present invention is achieved through the following technical solutions:
A method of phenol wastewater produced by processing needle coke production technology, the specific steps are:
(1) filtered wastewater removes suspended matter and solid impurity therein;
(2) by the mixed fillers after activation loaded in glass column or stainless steel column;
(1) with constant flow pump control waste water flow through resin column carry out absorption remove phenol;
(3) resin column is impregnated with eluant, eluent, is reused after zeolite regeneration.
As an optimization, in above-mentioned steps (2), using the macroporous absorbent resin and polystyrene skeleton of polystyrene skeleton The mixed fillers of strong-base anion-exchange resin.
As an optimization, in above-mentioned steps (2), volume ratio shared by macroporous absorbent resin is 70~85%.
As an optimization, in above-mentioned steps (3), it is 4~6 times of column volume/hours that constant flow pump, which controls waste water flow velocity,.
As an optimization, in above-mentioned steps (4), eluant, eluent is absolute ethyl alcohol, and soaking time is 1~3 hour, is impregnated twice.
This method is suitable for processing and contains phenol and nitrogen amide, and concentration is higher, waste water of the pH close to 10.
Compared with prior art, the positive effect of the present invention is:
In the processing scheme for the phenol wastewater that needle coke production technology provided by the present invention generates, used macropore is inhaled Attached resin and strong-base anion-exchange resin are using styrenic as skeleton.Aldehydes matter and styrene skeleton it Between π-π interaction and the electrostatic interaction between phenol and anion exchange resin so that mixed fillers are this severe There is fabulous adsorption effect under conditions of quarter to aldehydes matter office.Mixed fillers regenerating easily can follow bad utilization, and elute Agent dosage is only 0.5 times of column volume, and the organic contamination of generation is few.Present invention process is simple, economical and efficient, environmentally protective.
Description of the drawings
Fig. 1 is the liquid chromatogram before waste water absorption;
Fig. 2 is the liquid chromatogram after waste water absorption;
Fig. 3 is to adsorb breakthrough curve for the first time;
Fig. 4 is second of absorption breakthrough curve;
Fig. 5 is third time absorption breakthrough curve;
Specific implementation mode
The specific embodiment party of the method for phenol wastewater produced by a kind of processing needle coke production technology of the present invention presented below Formula.
Embodiment 1
A method of phenol wastewater produced by processing needle coke production technology, the specific steps are:
(1) filtered wastewater removes suspended matter and solid impurity therein;
(2) by the mixed fillers after activation loaded in glass column or stainless steel column;
(1) with constant flow pump control waste water flow through resin column carry out absorption remove phenol;
(3) resin column is impregnated with eluant, eluent, is reused after zeolite regeneration.
It is cloudy using the macroporous absorbent resin of polystyrene skeleton and the strong basicity of polystyrene skeleton in above-mentioned steps (2) The mixed fillers of ion exchange resin.
In above-mentioned steps (2), volume ratio shared by macroporous absorbent resin is 70~85%.
In above-mentioned steps (3), it is 4~6 times of column volume/hours that constant flow pump, which controls waste water flow velocity,.
In above-mentioned steps (4), eluant, eluent is absolute ethyl alcohol, and soaking time is 1~3 hour, is impregnated twice.
This method is suitable for processing and contains phenol and nitrogen amide, and concentration is higher, waste water of the pH close to 10.
The method of Phenol-Containing Wastewater Treatment of the present invention, specific experiment process are as follows:
Refer to attached drawing 1,2,3,4,5, waste water is extracted with constant flow pump, 5 μm of filter plate is flowed it through, it is miscellaneous to be filtered to remove solid Matter.By the mixed fillers after activation, (macroporous absorbent resin selects HZ-16 type resins, strong-base anion-exchange resin to select D201 type resins;It is 20%) to fill column in diameter that wherein volume shared by HZ-16 types resin, which is volume shared by 80%, D201 type resins, 15mm, in the glass column of height 360mm.It is adsorbed by resin column with the flow velocity of 5mL/min with constant flow pump control waste water, often Adsorption liquid is collected every 10min, the content of phenol in adsorption liquid is measured by high performance liquid chromatography.
Etc. resin adsorptions saturation after, i.e. when the phenol changes of contents of liquid chromatogram measuring is little stop absorption, made with constant flow pump Absolute ethyl alcohol is pumped into glass column, until glass column bottom stops when having liquid outflow, closes valve, absolute ethyl alcohol is made to be impregnated in column Then 1h is blown out whole liquid with air pump.This step 1 time is repeated, resin regeneration is completed.The eluting agent that the process uses 30mL (0.5 times of column volume) is only needed, organic contamination that is simple for process, generating is small, environmentally protective.
It repeats the above adsorption and desorption step twice, draws breakthrough curve.Breakthrough curve is according in different time adsorption liquid The concentration of object is drawn.Can visually see the adsorption capacity and adsorption effect of mixed fillers from breakthrough curve.
This experiment carries out identification and with high performance liquid chromatography to phenol using gas chromatography combined with mass spectrometry to waste component Content carries out quantitative calculating.
Gas chromatography combined with mass spectrometry is the results show that mainly contain phenol, 2- methylphenols, 2-aminotoluene, 4- in waste water Methylphenol.
The front and back liquid chromatogram of comparison absorption can be seen that by the way that after mixed fillers column, Phenol for Waste Water substance is almost It is adsorbed completely.
The present invention is fine to the adsorption effect of Phenol for Waste Water it can be seen from three breakthrough curve figures, and adsorption capacity is big, and And there is no weaken for the effect after resin zeolite regeneration.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art Member, without departing from the inventive concept of the premise, can also make several improvements and modifications, these improvements and modifications also should be regarded as In protection scope of the present invention.

Claims (6)

1. a kind of method of phenol wastewater produced by processing needle coke production technology, which is characterized in that use polystyrene skeleton Macroporous absorbent resin and polystyrene skeleton strong-base anion-exchange resin mixed fillers absorption remove phenol.
2. the method for phenol wastewater, feature produced by a kind of processing needle coke production technology according to claim 1 exist In, the specific steps are:
(1) filtered wastewater removes suspended matter and solid impurity therein;
(2) by the mixed fillers after activation loaded in glass column or stainless steel column;
Mixed fillers are the strong-base anion-exchange resin of the macroporous absorbent resin and polystyrene skeleton of polystyrene skeleton;
(3) with constant flow pump control waste water flow through resin column carry out absorption remove phenol;
(4) resin column is impregnated with eluant, eluent, is reused after zeolite regeneration.
3. the method for phenol wastewater, feature produced by a kind of processing needle coke production technology according to claim 2 exist In volume ratio shared by macroporous absorbent resin is 70~85%.
4. the method for phenol wastewater, feature produced by a kind of processing needle coke production technology according to claim 2 exist In in above-mentioned steps (3), it is 4~6 times of column volume/hours that constant flow pump, which controls waste water flow velocity,.
5. the method for phenol wastewater, feature produced by a kind of processing needle coke production technology according to claim 2 exist In in above-mentioned steps (4), eluant, eluent is absolute ethyl alcohol, and soaking time is 1~3 hour, is impregnated twice.
6. the method for phenol wastewater, feature produced by a kind of processing needle coke production technology according to claim 1 exist It is suitable for processing in, this method and contains phenol and nitrogen amide, concentration is higher, waste water of the pH close to 10.
CN201810441836.3A 2018-05-10 2018-05-10 A method of phenol wastewater produced by processing needle coke production technology Pending CN108545849A (en)

Priority Applications (1)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100263689A1 (en) * 2009-04-21 2010-10-21 Ecolab Usa Inc. Methods and apparatus for controlling water hardness
CN104024168A (en) * 2011-11-30 2014-09-03 罗门哈斯公司 Coking wastewater treatment
CN106732447A (en) * 2016-12-03 2017-05-31 华莉君 A kind of macroporous absorbent resin for containing phenol industrial wastewater for processing and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100263689A1 (en) * 2009-04-21 2010-10-21 Ecolab Usa Inc. Methods and apparatus for controlling water hardness
CN104024168A (en) * 2011-11-30 2014-09-03 罗门哈斯公司 Coking wastewater treatment
CN106732447A (en) * 2016-12-03 2017-05-31 华莉君 A kind of macroporous absorbent resin for containing phenol industrial wastewater for processing and preparation method thereof

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Application publication date: 20180918