CN110508247A - A kind of preparation method of the graphene oxide composite material for Industrial Waste Water Treatments - Google Patents

A kind of preparation method of the graphene oxide composite material for Industrial Waste Water Treatments Download PDF

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CN110508247A
CN110508247A CN201910816021.3A CN201910816021A CN110508247A CN 110508247 A CN110508247 A CN 110508247A CN 201910816021 A CN201910816021 A CN 201910816021A CN 110508247 A CN110508247 A CN 110508247A
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composite material
graphene oxide
polyacrylamide
reaction vessel
oxide composite
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李启龙
李虓
李圆
蔺文
冯加民
张丽萍
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Fangda Carbon New Materials Technology Co Ltd
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Fangda Carbon New Materials Technology Co Ltd
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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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/198Graphene oxide
    • 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
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • C02F2101/20Heavy metals or heavy metal compounds
    • 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
    • C02F2101/36Organic compounds containing halogen
    • 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
    • C02F2101/38Organic compounds containing nitrogen
    • 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
    • C02F2101/40Organic compounds containing sulfur
    • 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
    • C02F2103/007Contaminated open waterways, rivers, lakes or ponds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention is a kind of preparation method of graphene oxide composite material for Industrial Waste Water Treatments, expanded graphite used, the concentrated sulfuric acid, potassium permanganate, polyacrylamide, hydrogen peroxide mass ratio be 1:(180 ~ 250): (7 ~ 9): (1 ~ 2): (4 ~ 5), the concentrated sulfuric acid, expanded graphite are added in reaction vessel, stir 10-20min, again in powdered potassium permanganate reaction vessel, reaction vessel, is placed in 2 DEG C -4 DEG C of low temperature environment later and continues to make material reaction by stirring;Reaction vessel is taken out from low temperature environment, is warming up to 35 DEG C, constant temperature 30-40min, polyacrylamide is added reaction vessel, stirs 2-3h, is warming up to 95 degrees Celsius, insulated and stirred 15-20min, hydrogen peroxide is added dropwise, until in solution no longer until bubbling;Reaction product washing, filtering, filter residue and drying obtain graphene oxide composite material.Advantage: composite material is inexpensively practical, adsorbs methylene blue and lead ion effect is especially prominent.

Description

A kind of preparation method of the graphene oxide composite material for Industrial Waste Water Treatments
Technical field
The invention belongs to technical field of sewage, are related to the grapheme material of Industrial Waste Water Treatments.
Background technique
The high speed development of industry is that mankind's social progress brings many conveniences, and simultaneous manufactures the work generated Industry waste water also causes serious pollution to earth environment, how to remove the harmful substance in sewage, is problem urgently to be resolved.Work Industry waste water flows directly into channel, rivers and lake, polluted surface water;If be more toxic will lead to aquatic animals and plants it is dead very To disappearance.Industrial wastewater is also possible to penetrate into underground, polluted underground water, and then pollutes crops.Industrial wastewater penetrates into soil, makes At soil pollution or heavy metal pollution, the growth of plant and Soil Microorganism is influenced.Venomous injurant in industrial wastewater Matter can be ingested by animals and plants and absorb and remain in vivo, then reached in human body, done harm to huamn body by food chain.
Polluting caused by industrial wastewater mainly has: organic aerobic substance pollution, chemical toxicant pollution, inoganic solids suspended matter Pollution, heavy metal pollution, acid pollution, alkali pollution, pollution of plant nutritions, thermal pollution and pathogen contamination etc..
Graphene oxide (GO) be it is a kind of modified on the surface of graphene with edge various oxygen-containing functional groups (hydroxyl, carboxyl, Epoxy group and carbonyl) atomic thickness ultra-thin two-dimension nanometer sheet.GO has been proved to possess pleated structure thus has larger Specific surface area, the oxygen-containing functional group on surface has negative electricity, can be used to adsorb the harmful components in water, so that it is dirty to reach purification The effect of water.
Existing trade effluent adsorbent material largely uses organic matter to prepare, and the pollutant for handling trade effluent is possible to draw Enter new organic pollutant, causes secondary pollution, and the preparation cost of existing trade effluent adsorbent material is relatively high.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation sides of graphene oxide composite material for Industrial Waste Water Treatments Method.
Technical scheme is as follows: be ready in proportion expanded graphite, the concentrated sulfuric acid, potassium permanganate, polyacrylamide, Hydrogen peroxide, the expanded graphite, the concentrated sulfuric acid, potassium permanganate, polyacrylamide, hydrogen peroxide mass ratio be 1:(180 ~ 250): (7 ~ 9): (1 ~ 2): (4 ~ 5), the concentrated sulfuric acid are mass fraction 98%, and hydrogen peroxide is volume fraction 30%, first the concentrated sulfuric acid are added anti- It answers container, then expanded graphite is added in reaction vessel, stir 10-20min, then in powdered potassium permanganate reaction vessel, 10-20min is stirred, reaction vessel is placed in later in 2 DEG C -4 DEG C of low temperature environment and continues to make material reaction, cold preservation time 8- 24h;Reaction vessel is taken out from low temperature environment, is warming up to 35 DEG C, constant temperature 30-40min, reaction is added in polyacrylamide and is held Device stirs 2-3h, is warming up to 95 degrees Celsius, insulated and stirred 15-20min, and hydrogen peroxide is added dropwise, until no longer bubbling is in solution Only;Washing reaction product after completion of the reaction, wash Shi Xianyong hydrochloric acid washing by soaking, then use deionized water centrifuge washing, filtering, filter Slag is finally dried to obtain graphene oxide composite material.
Preferably, the mesh number of the expanded graphite is 50 mesh ~ 100 mesh.
Preferably, the polyacrylamide is cationic polyacrylamide or anionic polyacrylamide.
Preferably, the Molecular Weight for Polyacrylamide is 5,000,000 ~ 20,000,000.
Preferably, the drying temperature range after reactant washing is 30-50 DEG C.
Preferably, it when washing reaction product, first with hydrochloric acid washing by soaking 2 times of 5%, is then washed again with deionized water centrifugation It washs 5 times, revolving speed 3000r/min.
Compared with prior art, the present invention having the advantage that (1) composite material prepared by the present invention has cracking suction Attached effect, adsorbs methylene blue and lead ion effect is especially prominent.(2) composite material additive amount prepared by the present invention is few, absorption Mode is simple, economic and practical.(3) composite material of the present invention uses and composite material simply (is packed into nothing when use by way of recycling Put into waste water and adsorbed in woven fabric bag, take out bag after absorption), it is easy to operate.(4) present invention preparation Composite material non-toxic efficient, and it is cheap practical, can the dye of positive ion, heavy metal ion etc. effectively in absorption effluent.
Detailed description of the invention
Fig. 1 is the test result that composite material adsorbs ylidene methyl indigo plant solution;
Fig. 2 is the ICP test result of composite material adsorpting lead ion;
Fig. 3 is the XRD characterization result of 1 composite material of embodiment;
Fig. 4 is the microscopic characterization result of 1 composite material of embodiment;
Fig. 5 is the SEM characterization result of 1 composite material of embodiment.
Specific embodiment
A kind of preparation method of the graphene oxide composite material for Industrial Waste Water Treatments, the composite material be by than Example addition expanded graphite, the concentrated sulfuric acid, potassium permanganate, polyacrylamide, hydrogen peroxide are prepared by way of heating oxidation, are washed It is dried to obtain composite material powder after washing.
In above-mentioned technical proposal, composite material is to add expanded graphite, the concentrated sulfuric acid, potassium permanganate in proportion in 3 DEG C of conditions Lower reaction a period of time, then addition polyacrylamide, hydrogen peroxide are prepared by way of heating oxidation, after washing It is dried to obtain composite material powder.
Preferably, the mesh number of expanded graphite is 50 mesh ~ 100 mesh.
Preferably, the Molecular Weight for Polyacrylamide is 5,000,000 ~ 20,000,000.
Preferably, the polyacrylamide can be cationic polyacrylamide, or anionic polyacrylamide.
Preferably, expanded graphite, the concentrated sulfuric acid, potassium permanganate, polyacrylamide, hydrogen peroxide weight ratio be 1:(180 ~ 250): (7 ~ 9): (1 ~ 2): (4 ~ 5).
Preferably, 3 DEG C of reaction time are 8-24h.
Preferably, the oxidizing temperature range is 35-95 DEG C.
Preferably, the drying temperature range is 30-50 DEG C.
More specifically steps are as follows:
1) it cold stage: weighs the 180-250g concentrated sulfuric acid and pours into beaker and stir, then place the beaker 2-4 DEG C of low temperature environment In;It weighs 1g expanded graphite to be slowly added in beaker, stirs 10-20min;The grinding of 7-9g potassium permanganate is weighed uniformly to be slowly added to In beaker, 10-20min is stirred;Beaker is placed in 3 DEG C of low temperature environments and refrigerates 8-24h.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30- 40min;It weighs 1-2g polyacrylamide and is added thereto stirring 2-3h, be warming up to 95 degrees Celsius, insulated and stirred 15-20min, be added dropwise 4-5g volume fraction is 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and in 30-50 DEG C of item Drying for 24 hours, obtains graphene oxide composite material under part.
The present invention is described further with reference to the accompanying drawings and examples.
Experimental method used in following embodiments is conventional method unless otherwise specified;Institute in following embodiments Material, reagent etc., are commercially available unless otherwise specified.The medicine and reagent used in the present invention can be from Commercial sources obtain.
Enumerate several specific embodiments below to further understand specific implementation of the invention.
Embodiment 1
1) it cold stage: weighs the 180g concentrated sulfuric acid and pours into beaker and stir, then place the beaker in 2 DEG C of low temperature environments;It weighs 50 mesh expanded graphite of 1g is slowly added in beaker, stirs 10min;The grinding of 7g potassium permanganate is weighed uniformly to be slowly added in beaker, Stir 10min;Beaker is placed in 3 DEG C of low temperature environments and refrigerates 8h.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30min;1g cationic polyacrylamide is weighed, molecular weight is added thereto stirring 2h for 5,000,000, is warming up to 95 degrees Celsius, heat preservation 15min is stirred, dropwises addition 4g volume fraction is 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and under the conditions of 30 DEG C Drying for 24 hours, obtains graphene oxide composite material.
As shown in figure 3, the XRD characterization of 1 composite material of embodiment, characteristic peak integrally also complies with oxidation stone at 10 degree or so The form of black alkene XRD spectra.
As shown in figure 4, the microscopic characterization of 1 composite material of embodiment, laminated structure are visible.
Fig. 5 is the SEM characterization result of 1 composite material of embodiment, and film-form lamellar structure is relatively sharp in figure.The above characterization Illustrate that product prepared by the present invention is graphene oxide.
Embodiment 2:
1) it cold stage: weighs the 200g concentrated sulfuric acid and pours into beaker and stir, then place the beaker in 3 DEG C of low temperature environments;It weighs 50 mesh expanded graphite of 1g is slowly added in beaker, stirs 20min;The grinding of 7g potassium permanganate is weighed uniformly to be slowly added in beaker, Stir 20min;Beaker is placed in 3 DEG C of low temperature environments and refrigerates 8h.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30min;1g cationic polyacrylamide is weighed, molecular weight is added thereto stirring 2h for 5,000,000, is warming up to 95 degrees Celsius, heat preservation 15min is stirred, dropwises addition 4g volume fraction is 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and under the conditions of 30 DEG C Drying for 24 hours, obtains graphene oxide composite material.
Embodiment 3:
1) it cold stage: weighs the 200g concentrated sulfuric acid and pours into beaker and stir, then place the beaker in 3 DEG C of low temperature environments;It weighs 80 mesh expanded graphite of 1g is slowly added in beaker, stirs 10min;The grinding of 9g potassium permanganate is weighed uniformly to be slowly added in beaker, Stir 10min;Beaker is placed in 3 DEG C of low temperature environments and refrigerates 12h.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30min;1g cationic ion polyacrylamide is weighed, molecular weight is added thereto stirring 2h for 10,000,000, is warming up to 95 degrees Celsius, Insulated and stirred 15min, dropwise addition 4g volume fraction are 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and under the conditions of 40 DEG C Drying for 24 hours, obtains graphene oxide composite material.
Embodiment 4:
1) it cold stage: weighs the 250g concentrated sulfuric acid and pours into beaker and stir, then place the beaker in 4 DEG C of low temperature environments;It weighs 50 mesh expanded graphite of 1g is slowly added in beaker, stirs 20min;The grinding of 7g potassium permanganate is weighed uniformly to be slowly added in beaker, Stir 20min;Beaker is placed in 3 DEG C of low temperature environments and is refrigerated for 24 hours.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30min;1g anionic ion polyacrylamide is weighed, molecular weight is added thereto stirring 2h for 12,000,000, is warming up to 95 degrees Celsius, Insulated and stirred 15min, dropwise addition 4g volume fraction are 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and under the conditions of 50 DEG C Drying for 24 hours, obtains graphene oxide composite material.
Embodiment 5:
1) it cold stage: weighs the 230g concentrated sulfuric acid and pours into beaker and stir, then place the beaker in 2 DEG C of low temperature environments;It weighs 80 mesh expanded graphite of 1g is slowly added in beaker, stirs 10min;The grinding of 8g potassium permanganate is weighed uniformly to be slowly added in beaker, Stir 10min;Beaker is placed in 3 DEG C of low temperature environments and is refrigerated for 24 hours.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30min;1g cationic ion polyacrylamide is weighed, molecular weight is added thereto stirring 2h for 15,000,000, is warming up to 95 degrees Celsius, Insulated and stirred 15min, dropwise addition 4g volume fraction are 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and under the conditions of 50 DEG C Drying for 24 hours, obtains graphene oxide composite material.
Embodiment 6:
1) it cold stage: weighs the 240g concentrated sulfuric acid and pours into beaker and stir, then place the beaker in 4 DEG C of low temperature environments;It weighs 80 mesh expanded graphite of 1g is slowly added in beaker, stirs 10min;The grinding of 9g potassium permanganate is weighed uniformly to be slowly added in beaker, Stir 10min;Beaker is placed in 3 DEG C of low temperature environments and is refrigerated for 24 hours.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30min;1g anionic ion polyacrylamide is weighed, molecular weight is added thereto stirring 2h for 20,000,000, is warming up to 95 degrees Celsius, Insulated and stirred 15min, dropwise addition 5g volume fraction are 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and under the conditions of 40 DEG C Drying for 24 hours, obtains graphene oxide composite material.
Embodiment 7:
1) it cold stage: weighs the 240g concentrated sulfuric acid and pours into beaker and stir, then place the beaker in 3 DEG C of low temperature environments;It weighs 80 mesh expanded graphite of 1g is slowly added in beaker, stirs 10min;The grinding of 9g potassium permanganate is weighed uniformly to be slowly added in beaker, Stir 10min;Beaker is placed in 3 DEG C of low temperature environments and is refrigerated for 24 hours.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30min;1g anionic ion polyacrylamide is weighed, molecular weight is added thereto stirring 2h for 25,000,000, is warming up to 95 degrees Celsius, Insulated and stirred 15min, dropwise addition 5g volume fraction are 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and under the conditions of 40 DEG C Drying for 24 hours, obtains graphene oxide composite material.
Embodiment 8:
1) it cold stage: weighs the 240g concentrated sulfuric acid and pours into beaker and stir, then place the beaker in 3 DEG C of low temperature environments;It weighs 80 mesh expanded graphite of 1g is slowly added in beaker, stirs 10min;The grinding of 9g potassium permanganate is weighed uniformly to be slowly added in beaker, Stir 10min;Beaker is placed in 3 DEG C of low temperature environments and is refrigerated for 24 hours.;
2) oxidation stage: beaker is taken out from low temperature environment, is placed water-bath stirring, is warming up to 35 degrees Celsius, constant temperature 30min;1g cationic ion polyacrylamide is weighed, molecular weight is added thereto stirring 2h for 25,000,000, is warming up to 95 degrees Celsius, Insulated and stirred 15min, dropwise addition 5g volume fraction are 30% hydrogen peroxide, until in solution no longer until bubbling.
3) drying stage is washed: by above-mentioned hydrochloric acid washing by soaking 2 times for preparing sample and first using 5%, every time with 5% hydrochloric acid 1L, Then it uses deionized water centrifuge washing 5 times again, revolving speed 3000r/min.Above-mentioned sample is filtered with filter paper, and under the conditions of 40 DEG C Drying for 24 hours, obtains graphene oxide composite material.
Characterization and performance test
The composite material that above-described embodiment 1-4 is obtained has carried out methylene blue solution adsorption experiment respectively, and test result is as schemed 1;Lead ion solution adsorption experiment, test result such as Fig. 2 are carried out.As shown in Figure 1, abscissa is sample label in figure, indulges and sit It is designated as the concentration of methylene blue;No. 1 sample is initial ylidene methyl indigo plant solution, No. 2, No. 3, No. 4, No. 5 samples respectively correspond reality Example 1,2,3,4 is applied as solution after composite material absorption is added, adsorption time is for 24 hours.As shown in Fig. 2, abscissa is sample in figure Label, ordinate are the concentration of chlorination lead solution;No. 1 sample is the plumbum ion concentration of initial chlorination lead solution, No. 2, No. 3,4 Number, No. 5 samples respectively correspond embodiment 1,2,3,4 for be added composite material absorption after solution, adsorption time be for 24 hours.From Fig. 1, It is obvious for methylenum careuleum and lead chloride adsorption effect that Fig. 2 can be seen that composite material, and by adsorbing for 24 hours, solution pollutant is residual It stays concentration very low, illustrates that composite material adsorption effect is good.

Claims (6)

1. a kind of preparation method of the graphene oxide composite material for Industrial Waste Water Treatments, which is characterized in that quasi- in proportion Get expanded graphite, the concentrated sulfuric acid, potassium permanganate, polyacrylamide, hydrogen peroxide ready, the expanded graphite, the concentrated sulfuric acid, potassium permanganate, Polyacrylamide, hydrogen peroxide mass ratio be 1:(180 ~ 250): (7 ~ 9): (1 ~ 2): (4 ~ 5), the concentrated sulfuric acid be mass fraction 98% , hydrogen peroxide is volume fraction 30%, reaction vessel first is added in the concentrated sulfuric acid, then expanded graphite is added in reaction vessel, stirred 10-20min is mixed, then in powdered potassium permanganate reaction vessel, stirs 10-20min, reaction vessel is placed in 2 DEG C -4 later DEG C low temperature environment in continue to make material reaction, cold preservation time 8-24h;Reaction vessel is taken out from low temperature environment, is warming up to 35 DEG C, polyacrylamide is added reaction vessel, stirs 2-3h, be warming up to 95 degrees Celsius, insulated and stirred 15- by constant temperature 30-40min Hydrogen peroxide is added dropwise in 20min, until in solution no longer until bubbling;Washing reaction product after completion of the reaction washs Shi Xianyong hydrochloric acid Washing by soaking, then with deionized water centrifuge washing, filtering, filter residue is finally dried to obtain graphene oxide composite material.
2. a kind of preparation method of graphene oxide composite material for Industrial Waste Water Treatments according to claim 1, It is characterized in that, the mesh number of the expanded graphite is 50 mesh ~ 100 mesh.
3. a kind of preparation method of graphene oxide composite material for Industrial Waste Water Treatments according to claim 1, It is characterized in that, the polyacrylamide is cationic polyacrylamide or anionic polyacrylamide.
4. a kind of preparation method of graphene oxide composite material for Industrial Waste Water Treatments according to claim 1, It is characterized in that, the Molecular Weight for Polyacrylamide is 5,000,000 ~ 20,000,000.
5. a kind of preparation method of graphene oxide composite material for Industrial Waste Water Treatments according to claim 1, It is characterized in that, the drying temperature range after reactant washing is 30-50 DEG C.
6. a kind of preparation method of graphene oxide composite material for Industrial Waste Water Treatments according to claim 1, It is characterized in that, when washing reaction product, first with hydrochloric acid washing by soaking 2 times of 5%, deionized water centrifuge washing 5 is then used again Time, revolving speed 3000r/min.
CN201910816021.3A 2019-08-30 2019-08-30 A kind of preparation method of the graphene oxide composite material for Industrial Waste Water Treatments Pending CN110508247A (en)

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