CN107697978A - The processing method of carbon fibre precursor finish waste liquid - Google Patents
The processing method of carbon fibre precursor finish waste liquid Download PDFInfo
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- CN107697978A CN107697978A CN201710997000.7A CN201710997000A CN107697978A CN 107697978 A CN107697978 A CN 107697978A CN 201710997000 A CN201710997000 A CN 201710997000A CN 107697978 A CN107697978 A CN 107697978A
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- waste liquid
- finish
- flocculant
- carbon fibre
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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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Water Treatment By Sorption (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The present invention provides a kind of processing method of carbon fibre precursor finish waste liquid, combinational demulsifier is obtained using the method by polyoxyethylene polyoxypropylene block copolymer compound, flocculant, alkali and solvent complex, then combinational demulsifier is mixed with finish waste liquid, it is demulsified under certain technique and separates waste liquid and upper surface oil slick, waste liquid is directly discharged after adsorption cleaning；Present invention process is simple, and power consumption and cost are relatively low, have extremely strong practicality, and effect is fabulous, and the COD ranges of decrease are up to 95%~99.5%.
Description
Technical field
A kind of processing method the present invention relates to carbon fibre precursor with finish waste liquid, belong to carbon fibre precursor finish waste liquid
The technical field of processing, it is intended to which being changed into caused finish waste liquid in precursor production process by the method can be with qualified discharge
Industrial wastewater.
Background technology
Finish is auxiliary agent essential in polyacrylonitrile (PAN) base carbon fibre production process, carbon fibre precursor finish
Effect be to reduce the coefficient of friction of filament surfaces, so that the precursor produced has the characteristics such as soft, smooth, boundling, ensure
PAN base yarn spinning each operations smoothly complete, and ensure finally produce the measured carbon fiber production of mechanical performance height, matter
Product.It may be said that just there is no carbon fiber without spinning oil, without high performance spinning oil, high performance carbon is not just manufactured yet
Fiber.High performance carbon fibre precursor finish should possess excellent resistance to elevated temperatures, antistatic property, greasy property and boundling
With anti-adhesion performance.
Substantial amounts of finish waste liquid can be produced in carbon fibre precursor production process, after being handled by finish precursor,
Because main component concentration is too low, requirement is not reached.The main component of finish waste liquid is surfactant and organic
Silicon class compound, because its COD COD value is high, degradability is poor and can not directly discharge, and otherwise will bring serious environment
Problem.Therefore, it need to carry out after demulsification processing that adsorption cleaning could discharge again to finish waste liquid.And domestic now used processing
The method of finish waste liquid is based on the method for high-temperature calcination, and the presence power consumption of this method is high, efficiency is low and the drawbacks such as processing cost is high, more
For the serious is will cause atmosphere pollution.
The content of the invention
Solve to deposit in the prior art with the processing method of finish waste liquid it is an object of the invention to provide a kind of carbon fibre precursor
The method with high-temperature calcination based on have that power consumption is high, efficiency is low and the drawbacks such as processing cost is high, will more seriously make
Into the problem of atmosphere pollution.
The present invention technical solution be：
The processing method of a kind of carbon fibre precursor finish waste liquid, using by polyoxyethylene polyoxypropylene block copolymerization chemical combination
Thing, flocculant, the method for alkali and solvent complex obtain combinational demulsifier, then mix combinational demulsifier with finish waste liquid,
It is demulsified under certain technique and separates waste liquid and upper surface oil slick, waste liquid is directly discharged after adsorption cleaning；Specifically
For,
1) based on combinational demulsifier gross weight 100%, wherein polyoxyethylene polyoxypropylene block copolymer compound account for 20%~
50%, flocculant accounts for 1%~10%, and alkali accounts for 20%~45%, and solvent accounts for 20%~40%；
2) demulsifier of compounding and finish waste liquid are added in reactor, the mass ratio that combinational demulsifier accounts for finish waste liquid is
5%~40%, temperature range is at 40 DEG C~90 DEG C, and rotating speed of agitator scope is in 40r/min~120r/min, through after a while
Reaction after, upper surface floating oil collecting is got up, then then the waste liquid after processing is emitted into specified containers by discharging opening
Discharged after adsorption cleaning.
Further, polyoxyethylene polyoxypropylene block copolymer compound account for the mass fraction of combinational demulsifier for 30%~
40%, its molecular structure is as follows,
Wherein, the scope that the scope that m scope is 0~20, n is 5~30, p is 0~20.
Further, flocculant uses inorganic flocculant, organic flocculant or microorganism flocculant.
Further, inorganic flocculant is using iron chloride, polyaluminium sulfate, and organic flocculant is using polyacrylamide, benzene
Vinyl sulfonate, microorganism flocculant use glycoprotein, cellulose caused by microorganism.
Further, the mass fraction that alkali accounts for combinational demulsifier is 20%~35%, and alkali uses inorganic base or organic base.
Further, inorganic base is using sodium hydroxide, potassium hydroxide, and organic base is using ethylenediamine, choline.
Further, the mass fraction that solvent accounts for combinational demulsifier is 20%~24%, and solvent for use is water.
The beneficial effects of the invention are as follows：The processing method of this kind of carbon fibre precursor finish waste liquid, being capable of efficient process oil
Agent waste liquid, and consume energy less, the method that processing cost is low, it can reach discharge standard after making the purification of waste water after processing, then circulate
Using or directly discharge.This method realizes water-oil separating by using polyether demulsification agent and flocculant compounding.The present invention uses
Combinational demulsifier is obtained by the method for polyoxyethylene polyoxypropylene block copolymer compound, flocculant, alkali and solvent complex, then
Combinational demulsifier is mixed with finish waste liquid, is demulsified under certain technique and separates waste liquid and upper surface oil slick, will be useless
Liquid can be discharged directly after adsorption cleaning.Present invention process is simple, and power consumption and cost are relatively low, have extremely strong practicality,
And effect is fabulous, the COD ranges of decrease are up to 95%~99.5%.
Embodiment
The following detailed description of the preferred embodiments of the present invention.
In order to accomplish that high-efficiency low energy consumption handles finish waste liquid at low cost, embodiment is added in finish waste liquid and broken by polyethers
Emulsion, flocculant, alkali, solvent composition combinational demulsifier come cause water-oil phase separate, reduction finish waste liquid COD value.
The processing method of this kind of carbon fibre precursor finish waste liquid, using by polyoxyethylene polyoxypropylene block copolymerization chemical combination
Thing, flocculant, the method for alkali and solvent complex obtain combinational demulsifier, then mix combinational demulsifier with finish waste liquid,
It is demulsified under certain technique and separates waste liquid and upper surface oil slick, waste liquid is directly discharged after adsorption cleaning；Specifically
For,
1) based on combinational demulsifier gross weight 100%, wherein polyoxyethylene polyoxypropylene block copolymer compound account for 20%~
50%, flocculant accounts for 1%~10%, and alkali accounts for 20%~45%, and solvent accounts for 20%~40%；
2) demulsifier of compounding and finish waste liquid are added in reactor, the mass ratio that combinational demulsifier accounts for finish waste liquid is
5%~40%, temperature range is at 40 DEG C~90 DEG C, and rotating speed of agitator scope is in 40r/min~120r/min, through after a while
Reaction after, upper surface floating oil collecting is got up, then then the waste liquid after processing is emitted into specified containers by discharging opening
Discharged after adsorption cleaning.
Embodiment 1
First combinational demulsifier, wherein polyoxyethylene polyoxypropylene block copolymer compound mass fraction are 20%, and m, n, p divide
Wei 0,15,10；Flocculant selective chlorination iron, mass fraction 5%；Alkali selects sodium hydroxide, mass fraction 10%；It is used
Solvent is water, mass fraction 40%.Above-mentioned raw materials are made into demulsifier, add 1 in a kettle#Finish waste liquid, measures 1#Oil
Agent waste liquid COD value is 92400mg/L, and the amount for adding combinational demulsifier is the 5% of finish waste liquid quality, and handling process is protected for temperature
40 DEG C are held, rotating speed of agitator 40r/min, upper surface floating oil collecting is got up after reaction, then by the waste liquid after processing by going out
Material mouth is discharged after being emitted into specified containers then adsorption cleaning.Waste liquid COD value is 950mg/L after measuring processing, and COD is decreased by
99%, by waste liquid after processing after adsorption cleaning, it is 400mg/L to measure waste liquid COD value, reaches discharge standard.
Embodiment 2
First combinational demulsifier, wherein polyoxyethylene polyoxypropylene block copolymer compound mass fraction are 30%, and m, n, p divide
Wei 5,5,0；Flocculant selective polymerization aluminum sulfate, mass fraction 1%；Alkali selects potassium hydroxide, mass fraction 45%；Institute
It is water with solvent, mass fraction 24%.Above-mentioned raw materials are made into demulsifier, add 2 in a kettle#Finish waste liquid, measures 2#
Finish waste liquid COD value is 97300mg/L, and the amount for adding combinational demulsifier is the 10% of finish waste liquid quality, and handling process is temperature
Degree is kept for 60 DEG C, rotating speed of agitator 70r/min, upper surface floating oil collecting is got up after reaction, then the waste liquid after processing is led to
Cross after discharging opening is emitted into specified containers then adsorption cleaning and discharge.Waste liquid COD value is 890mg/L after measuring processing, and COD drops
Width is up to 99.1%, and by waste liquid after processing after adsorption cleaning, it is 380mg/L to measure waste liquid COD value, reaches discharge standard.
Embodiment 3
First combinational demulsifier, wherein polyoxyethylene polyoxypropylene block copolymer compound mass fraction are 40%, and m, n, p divide
Wei 20,30,5；Flocculant selects polyacrylamide, mass fraction 5%；Alkali selects ethylenediamine, mass fraction 35%；Institute
It is water with solvent, mass fraction 20%.Above-mentioned raw materials are made into demulsifier, add 3 in a kettle#Finish waste liquid, measures 3#
Finish waste liquid COD value is 90100mg/L, and the amount for adding combinational demulsifier is the 20% of finish waste liquid quality, and handling process is temperature
Degree is kept for 90 DEG C, rotating speed of agitator 100r/min, upper surface floating oil collecting is got up after reaction, then the waste liquid after processing is led to
Cross after discharging opening is emitted into specified containers then adsorption cleaning and discharge.It is 730mg/L to measure liquor C OD values, and COD is decreased by
99.2%, by waste liquid after processing after adsorption cleaning, it is 330mg/L to measure waste liquid COD value, reaches discharge standard.
Embodiment 4
First combinational demulsifier, wherein polyoxyethylene polyoxypropylene block copolymer compound mass fraction are 50%, and m, n, p divide
Wei 15,20,20；Flocculant selects styrene sulfonate, mass fraction 10%；Alkali selects choline, mass fraction 20%；
Solvent for use is water, mass fraction 15%.Above-mentioned raw materials are made into demulsifier, add 4 in a kettle#Finish waste liquid, survey
Obtain 4#Finish waste liquid COD value is 97800mg/L, and the amount for adding combinational demulsifier is the 40% of finish waste liquid quality, handling process
Kept for 90 DEG C for temperature, rotating speed of agitator 120r/min, upper surface floating oil collecting got up after reaction, then will be useless after processing
Liquid discharges after being emitted into specified containers then adsorption cleaning by discharging opening.It is 970mg/L to measure liquor C OD values, the COD ranges of decrease
Up to 99%, by waste liquid after processing after adsorption cleaning, it is 450mg/L to measure waste liquid COD value, reaches discharge standard.
The concentration (mass fraction) of carbon fibre precursor finish is in the range of 3%~10%, and finish liquid waste concentration
1.5%~3%, COD COD value reaches mg/L up to ten thousand, and liquid waste concentration is low after the processing of the method for embodiment 1,2,3,4
In 0.2%, COD COD value is less than 1000mg/L, and the COD ranges of decrease are handled up to 95%~99.5%, then through adsorption cleaning
COD value of waste water is less than 500mg/L afterwards, reaches discharge index.
Claims (7)
- A kind of 1. carbon fibre precursor processing method of finish waste liquid, it is characterised in that：Using embedding by polyoxyethylene polyoxypropylene Section copolymerization, flocculant, the method for alkali and solvent complex obtain combinational demulsifier, and then combinational demulsifier and finish give up Liquid mixes, and is demulsified under certain technique and separates waste liquid and upper surface oil slick, by waste liquid after adsorption cleaning directly Discharge；Specifically,1) based on combinational demulsifier gross weight 100%, wherein polyoxyethylene polyoxypropylene block copolymer compound accounts for 20%~50%, Flocculant accounts for 1%~10%, and alkali accounts for 20%~45%, and solvent accounts for 20%~40%；2) demulsifier of compounding and finish waste liquid are added in reactor, the mass ratio that combinational demulsifier accounts for finish waste liquid is 5% ~40%, temperature range is at 40 DEG C~90 DEG C, and rotating speed of agitator scope is in 40r/min~120r/min, through after a while After reaction, upper surface floating oil collecting is got up, then the waste liquid after processing is emitted into specified containers and then inhaled by discharging opening Discharged after attached purification.
- 2. the carbon fibre precursor as claimed in claim 1 processing method of finish waste liquid, it is characterised in that：Polyoxyethylene polyoxy The mass fraction that polypropylene block copolymerization accounts for combinational demulsifier is 30%~40%, and its molecular structure is as follows,Wherein, the scope that the scope that m scope is 0~20, n is 5~30, p is 0~20.
- 3. the carbon fibre precursor as claimed in claim 1 processing method of finish waste liquid, it is characterised in that：Flocculant uses nothing Machine flocculant, organic flocculant or microorganism flocculant.
- 4. the carbon fibre precursor as claimed in claim 3 processing method of finish waste liquid, it is characterised in that：Inorganic flocculant is adopted With iron chloride, polyaluminium sulfate, organic flocculant is using polyacrylamide, styrene sulfonate, and microorganism flocculant is using micro- Biogenic glycoprotein, cellulose.
- 5. the processing method of the carbon fibre precursor finish waste liquid as described in claim any one of 1-4, it is characterised in that：Alkali accounts for The mass fraction of combinational demulsifier is 20%~35%, and alkali uses inorganic base or organic base.
- 6. the carbon fibre precursor as claimed in claim 5 processing method of finish waste liquid, it is characterised in that：Inorganic base uses hydrogen Sodium oxide molybdena, potassium hydroxide, organic base is using ethylenediamine, choline.
- 7. the carbon fibre precursor as claimed in claim 1 processing method of finish waste liquid, it is characterised in that：It is broken that solvent accounts for compounding The mass fraction of emulsion is 20%~24%, and solvent for use is water.
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| CN201710997000.7A CN107697978A (en) | 2017-10-20 | 2017-10-20 | The processing method of carbon fibre precursor finish waste liquid |
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| CN201710997000.7A CN107697978A (en) | 2017-10-20 | 2017-10-20 | The processing method of carbon fibre precursor finish waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113026149A (en) * | 2021-04-27 | 2021-06-25 | 山西钢科碳材料有限公司 | Method for treating polyacrylonitrile precursor waste oil agent |
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| CN105800827A (en) * | 2016-04-18 | 2016-07-27 | 中国科学院山西煤炭化学研究所扬州碳纤维工程技术中心 | Demulsification treatment method for waste oil agent for acrylic fiber spinning |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5154831A (en) * | 1988-12-22 | 1992-10-13 | Ensr Corporation | Solvent extraction process employing comminuting and dispersing surfactants |
| JPH0796284A (en) * | 1993-09-29 | 1995-04-11 | Kurita Water Ind Ltd | Treatment of oil-containing waste water |
| CN1958735A (en) * | 2005-10-31 | 2007-05-09 | 中国石油化工股份有限公司 | Method for removing powder of catalyst in catalytic cracking oil slurry |
| JP2015229158A (en) * | 2014-06-06 | 2015-12-21 | 栗田工業株式会社 | Oil water separation method |
| JP2016052623A (en) * | 2014-09-03 | 2016-04-14 | 栗田工業株式会社 | Oil-water separation method for o/w type emulsion and oil-water separation agent for the o/w type emulsion |
| CN105800827A (en) * | 2016-04-18 | 2016-07-27 | 中国科学院山西煤炭化学研究所扬州碳纤维工程技术中心 | Demulsification treatment method for waste oil agent for acrylic fiber spinning |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113026149A (en) * | 2021-04-27 | 2021-06-25 | 山西钢科碳材料有限公司 | Method for treating polyacrylonitrile precursor waste oil agent |
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Application publication date: 20180216 |