CN109574120A - A kind of graphene doping textile dyestuff Wastewater purification material and preparation method thereof - Google Patents

A kind of graphene doping textile dyestuff Wastewater purification material and preparation method thereof Download PDF

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Publication number
CN109574120A
CN109574120A CN201811537939.6A CN201811537939A CN109574120A CN 109574120 A CN109574120 A CN 109574120A CN 201811537939 A CN201811537939 A CN 201811537939A CN 109574120 A CN109574120 A CN 109574120A
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graphene
textile dyestuff
wastewater purification
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陈绪涛
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/261Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • 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
    • 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

Abstract

The invention discloses a kind of graphenes to adulterate textile dyestuff Wastewater purification material, it is composed of the following raw materials by weight: nano dispersion fluid 180-200, graphene 5-7, aluminum sulfate 10-14, fatty diglycollic amide 1-2, sorbitan monooleate 0.6-1, methyl methacrylate 30-40, initiator 1-2.The wastewater treatment of scavenging material of the invention especially suitable for textile dyestuff, good purification, high recycling rate.

Description

A kind of graphene doping textile dyestuff Wastewater purification material and preparation method thereof
Technical field
The invention belongs to Water warfare fields, and in particular to a kind of graphene doping textile dyestuff Wastewater purification material and its system Preparation Method.
Background technique
Waste water from dyestuff has the features such as high organic content, coloration is deep, and biodegradability is poor, belongs to difficult waste water.Especially It is that used dyestuff is more stable in recent years, the degree of biodegradability further decreases.Currently, the method for administering waste water from dyestuff Have: physisorphtion, chemical oxidization method, microorganism treatment etc..There is low efficiencys for these conventional methods, and energy consumption is high, cannot Thorough decomposing pollutant, the disadvantages of being also easy to produce secondary pollution.Although all will be useless even in a period of time in the future now in the past The predominant methods of water process.But with continuous nervous and continuous improvement of the China to sewage drainage standard of water resource, new dirt Water treatment technology must and be continuously available development.Wherein, photocatalysis technology is a kind of novel and promising method, and current The development of photochemical catalyst is concentrated mainly on about the research of this respect;Titanium dioxide optical catalyst is stablized with chemical property, nothing The advantages that poison ring is protected, cheap.But the titanium dioxide that prior synthesizing method obtains haves the shortcomings that larger: titanium-dioxide photo is urged That there is specific surface areas is not high for agent, and porosity is small and pore-size distribution is not concentrated, this is unfavorable for Wastewater Dyes macromolecular in hole Absorption and mass transport process in road.
Summary of the invention
The object of the present invention is to provide a kind of graphene doping textile dyestuff Wastewater purification materials and preparation method thereof.
To achieve the above object, the invention adopts the following technical scheme:
A kind of graphene doping textile dyestuff Wastewater purification material, it is composed of the following raw materials by weight:
The smooth single oleic acid of nano dispersion fluid 180-200, graphene 5-7, aluminum sulfate 10-14, fatty diglycollic amide 1-2, sorb Ester 0.6-1, methyl methacrylate 30-40, initiator 1-2.
The initiator is one of ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
The nano dispersion fluid is made of the raw material of following weight parts:
Nano-carbon powder 70-80, N-Methyl pyrrolidone 1-3, polyacrylamide 10-16, alkenyl succinic anhydride 3-5, dodecyl Primary amine 2-4.
The preparation method of the nano dispersion fluid, comprising the following steps:
(1) dodecyl primary amine is taken, is added in the dehydrated alcohol of 10-17 times of its weight, stirs evenly, nano-carbon powder is added, Increasing temperature is 50-55 DEG C, and insulated and stirred 1-2 hours, ethyl alcohol is distilled off, obtains modified carbon dust;
(2) N-Methyl pyrrolidone, polyacrylamide mixing are taken, is added in the deionized water of 65-70 times of mixture weight, Insulated and stirred 30-40 minutes at 60-65 DEG C, aqueous dispersions are obtained;
(3) alkenyl succinic anhydride is taken, is added in the chloroform of 18-20 times of its weight, stirs evenly, above-mentioned modified carbon dust is added, Insulated and stirred 50-70 minutes at 70-75 DEG C, chloroform is distilled off, is added in above-mentioned aqueous dispersions, it is 10-20 minutes ultrasonic, Up to the nano dispersion fluid.
A kind of preparation method of graphene doping textile dyestuff Wastewater purification material, comprising the following steps:
(1) initiator is taken, is added in the deionized water of 30-40 times of its weight, stirs evenly;
(2) graphene, aluminum sulfate, fatty diglycollic amide mixing are taken, the deionized water of 17-20 times of mixture weight is added to In, it stirs evenly, methyl methacrylate is added, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjust reaction kettle temperature Degree is 70-75 DEG C, and insulated and stirred 4-6 hours, discharging cooling obtained polymer emulsion;
(3) nano dispersion fluid is taken, mixes, stirs evenly with above-mentioned polymer emulsion, sorbitan monooleate, ultrasonic 10- is added It 20 minutes, filters, filter cake is washed, is sent in baking oven, it is dry to adulterate textile dyestuff purification of waste water material to get the graphene Material.
Drying temperature described in step (3) is 85-90 DEG C, and drying time is 100-140 minutes.
Advantages of the present invention:
The present invention uses dodecyl primary amine to handle nano-carbon powder first, then is blended instead with the chloroformic solution of alkenyl succinic anhydride It answers, obtains the carbon dust of amide modifications, be subsequently dispersed in the aqueous solution of polyacrylamide, obtain nano dispersion fluid, the present invention is logical It crosses and is modified carbon dust progress amidation, can effectively improve the dispersion performance of carbon dust in aqueous solution, the present invention is with methyl-prop E pioic acid methyl ester is monomer, is blended with graphene, aluminum sulfate, polymerize under initiator effect, obtains polymer emulsion;Divide again with nanometer Dispersion liquid is blended, and obtains finished product scavenging material, material strong adsorption of the invention, is blended with polyacrylamide, aluminum sulfate etc., also has There is good flocculability, good synergistic purification water effect can be played;Scavenging material of the invention is contaminated especially suitable for weaving The wastewater treatment of material, good purification, high recycling rate.
Specific embodiment
Embodiment 1
A kind of graphene doping textile dyestuff Wastewater purification material, it is composed of the following raw materials by weight:
Nano dispersion fluid 180, graphene 5, aluminum sulfate 10, fatty diglycollic amide 1, sorbitan monooleate 0.6, methyl-prop E pioic acid methyl ester 30, initiator 1.
The initiator is ammonium persulfate.
The nano dispersion fluid is made of the raw material of following weight parts:
Nano-carbon powder 70, N-Methyl pyrrolidone 1, polyacrylamide 10, alkenyl succinic anhydride 3, dodecyl primary amine 2.
The preparation method of the nano dispersion fluid, comprising the following steps:
(1) dodecyl primary amine is taken, is added in the dehydrated alcohol of 10 times of its weight, stirs evenly, nano-carbon powder is added, is increased Temperature is 50 DEG C, and insulated and stirred 1 hour, ethyl alcohol is distilled off, obtains modified carbon dust;
(2) N-Methyl pyrrolidone, polyacrylamide mixing are taken, is added in 65 times of mixture weight of deionized water, 60 Insulated and stirred 30 minutes, obtain aqueous dispersions at DEG C;
(3) alkenyl succinic anhydride is taken, is added in the chloroform of 18 times of its weight, stirs evenly, above-mentioned modified carbon dust is added, 70 Insulated and stirred 50 minutes, are distilled off chloroform at DEG C, are added in above-mentioned aqueous dispersions, and ultrasound 10 minutes to get the nanometer Dispersion liquid.
A kind of preparation method of graphene doping textile dyestuff Wastewater purification material, comprising the following steps:
(1) initiator is taken, is added in the deionized water of 30 times of its weight, stirs evenly;
(2) graphene, aluminum sulfate, fatty diglycollic amide mixing are taken, is added in 17 times of mixture weight of deionized water, It stirs evenly, methyl methacrylate is added, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 70 DEG C, insulated and stirred 4 hours, discharging cooling obtained polymer emulsion;
(3) nano dispersion fluid is taken, mixes, stirs evenly with above-mentioned polymer emulsion, sorbitan monooleate, 10 points of ultrasound is added Clock filters, filter cake is washed, is sent in baking oven, dry to adulterate textile dyestuff Wastewater purification material to get the graphene.
Drying temperature described in step (3) is 85 DEG C, and drying time is 100 minutes.
Embodiment 2
A kind of graphene doping textile dyestuff Wastewater purification material, it is composed of the following raw materials by weight:
Nano dispersion fluid 200, graphene 7, aluminum sulfate 14, fatty diglycollic amide 2, sorbitan monooleate 1, metering system Sour methyl esters 40, initiator 2.
The initiator is potassium peroxydisulfate.
The nano dispersion fluid is made of the raw material of following weight parts:
Nano-carbon powder 80, N-Methyl pyrrolidone 3, polyacrylamide 16, alkenyl succinic anhydride 5, dodecyl primary amine 4.
The preparation method of the nano dispersion fluid, comprising the following steps:
(1) dodecyl primary amine is taken, is added in the dehydrated alcohol of 17 times of its weight, stirs evenly, nano-carbon powder is added, is increased Temperature is 55 DEG C, and insulated and stirred 2 hours, ethyl alcohol is distilled off, obtains modified carbon dust;
(2) N-Methyl pyrrolidone, polyacrylamide mixing are taken, is added in 70 times of mixture weight of deionized water, 65 Insulated and stirred 40 minutes, obtain aqueous dispersions at DEG C;
(3) alkenyl succinic anhydride is taken, is added in the chloroform of 20 times of its weight, stirs evenly, above-mentioned modified carbon dust is added, 75 Insulated and stirred 70 minutes, are distilled off chloroform at DEG C, are added in above-mentioned aqueous dispersions, and ultrasound 20 minutes to get the nanometer Dispersion liquid.
A kind of preparation method of graphene doping textile dyestuff Wastewater purification material, comprising the following steps:
(1) initiator is taken, is added in the deionized water of 40 times of its weight, stirs evenly;
(2) graphene, aluminum sulfate, fatty diglycollic amide mixing are taken, is added in 20 times of mixture weight of deionized water, It stirs evenly, methyl methacrylate is added, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 75 DEG C, insulated and stirred 6 hours, discharging cooling obtained polymer emulsion;
(3) nano dispersion fluid is taken, mixes, stirs evenly with above-mentioned polymer emulsion, sorbitan monooleate, 20 points of ultrasound is added Clock filters, filter cake is washed, is sent in baking oven, dry to adulterate textile dyestuff Wastewater purification material to get the graphene.
Drying temperature described in step (3) is 90 DEG C, and drying time is 140 minutes.
Performance test:
The graphene of the graphene doping textile dyestuff Wastewater purification material of the 10g embodiment of the present invention 1, embodiment 2 is adulterated and is spun Knit waste water from dyestuff scavenging material, commercially available carbon dust is respectively placed in the methylene blue solution that 500ml concentration is 200mg/l;
After concussion processing 30 minutes, the methylene of the graphene doping textile dyestuff Wastewater purification material by the embodiment of the present invention 1 The concentration of base indigo plant solution becomes 20.1mg/l;
The concentration of the methylene blue solution of graphene doping textile dyestuff Wastewater purification material by the embodiment of the present invention 2 becomes 19.0mg/l;
The concentration of the methylene blue solution handled by commercially available carbon dust becomes 88.4mg/l.

Claims (6)

1. a kind of graphene adulterates textile dyestuff Wastewater purification material, which is characterized in that it is the raw material group by following weight parts At:
The smooth single oleic acid of nano dispersion fluid 180-200, graphene 5-7, aluminum sulfate 10-14, fatty diglycollic amide 1-2, sorb Ester 0.6-1, methyl methacrylate 30-40, initiator 1-2.
2. a kind of graphene according to claim 1 adulterates textile dyestuff Wastewater purification material, which is characterized in that described Initiator is one of ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
3. a kind of graphene according to claim 1 adulterates textile dyestuff Wastewater purification material, which is characterized in that described Nano dispersion fluid is made of the raw material of following weight parts:
Nano-carbon powder 70-80, N-Methyl pyrrolidone 1-3, polyacrylamide 10-16, alkenyl succinic anhydride 3-5, dodecyl Primary amine 2-4.
4. a kind of graphene according to claim 3 adulterates textile dyestuff Wastewater purification material, which is characterized in that described The preparation method of nano dispersion fluid, comprising the following steps:
(1) dodecyl primary amine is taken, is added in the dehydrated alcohol of 10-17 times of its weight, stirs evenly, nano-carbon powder is added, Increasing temperature is 50-55 DEG C, and insulated and stirred 1-2 hours, ethyl alcohol is distilled off, obtains modified carbon dust;
(2) N-Methyl pyrrolidone, polyacrylamide mixing are taken, is added in the deionized water of 65-70 times of mixture weight, Insulated and stirred 30-40 minutes at 60-65 DEG C, aqueous dispersions are obtained;
(3) alkenyl succinic anhydride is taken, is added in the chloroform of 18-20 times of its weight, stirs evenly, above-mentioned modified carbon dust is added, Insulated and stirred 50-70 minutes at 70-75 DEG C, chloroform is distilled off, is added in above-mentioned aqueous dispersions, it is 10-20 minutes ultrasonic, Up to the nano dispersion fluid.
5. a kind of preparation method of graphene doping textile dyestuff Wastewater purification material as described in claim 1, which is characterized in that The following steps are included:
(1) initiator is taken, is added in the deionized water of 30-40 times of its weight, stirs evenly;
(2) graphene, aluminum sulfate, fatty diglycollic amide mixing are taken, the deionized water of 17-20 times of mixture weight is added to In, it stirs evenly, methyl methacrylate is added, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjust reaction kettle temperature Degree is 70-75 DEG C, and insulated and stirred 4-6 hours, discharging cooling obtained polymer emulsion;
(3) nano dispersion fluid is taken, mixes, stirs evenly with above-mentioned polymer emulsion, sorbitan monooleate, ultrasonic 10- is added It 20 minutes, filters, filter cake is washed, is sent in baking oven, it is dry to adulterate textile dyestuff purification of waste water material to get the graphene Material.
6. a kind of preparation method of graphene doping textile dyestuff Wastewater purification material according to claim 5, feature It is, drying temperature described in step (3) is 85-90 DEG C, and drying time is 100-140 minutes.
CN201811537939.6A 2018-12-16 2018-12-16 A kind of graphene doping textile dyestuff Wastewater purification material and preparation method thereof Withdrawn CN109574120A (en)

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CN105080512A (en) * 2015-08-25 2015-11-25 江苏大学 Preparation method and application of oxidized graphene based cadmium ion imprinted polymer
US20160175814A1 (en) * 2014-12-23 2016-06-23 King Fahd University Of Petroleum And Minerals Activated carbon/aluminum oxide/polyethylenimine composites and methods thereof
CN106519407A (en) * 2016-10-14 2017-03-22 宁波爱克创威新材料科技有限公司 Automatic temperature-control heating polymer and filled carbon powder composite material and preparation method thereof
CN108772046A (en) * 2018-05-28 2018-11-09 安徽中弘科技发展有限公司 A kind of polyester active carbon adsorption material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160175814A1 (en) * 2014-12-23 2016-06-23 King Fahd University Of Petroleum And Minerals Activated carbon/aluminum oxide/polyethylenimine composites and methods thereof
CN105080512A (en) * 2015-08-25 2015-11-25 江苏大学 Preparation method and application of oxidized graphene based cadmium ion imprinted polymer
CN106519407A (en) * 2016-10-14 2017-03-22 宁波爱克创威新材料科技有限公司 Automatic temperature-control heating polymer and filled carbon powder composite material and preparation method thereof
CN108772046A (en) * 2018-05-28 2018-11-09 安徽中弘科技发展有限公司 A kind of polyester active carbon adsorption material and preparation method thereof

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Title
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