CN106865713A - A kind of graphene-based water purifying flocculating agent and preparation method and application - Google Patents
A kind of graphene-based water purifying flocculating agent and preparation method and application Download PDFInfo
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- CN106865713A CN106865713A CN201710156666.XA CN201710156666A CN106865713A CN 106865713 A CN106865713 A CN 106865713A CN 201710156666 A CN201710156666 A CN 201710156666A CN 106865713 A CN106865713 A CN 106865713A
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
Abstract
The invention discloses a kind of graphene-based water purifying flocculating agent and preparation method and application.The graphene-based water purifying flocculating agent is made up of anionic polymer polymer, graphene oxide compound, amphoteric metal salt polymer, plant type high molecular polymer and pH adjusting agent；The mass fraction of each component is：Anionic polymer polymer：1~20；Graphene oxide compound：2~10；Amphoteric metal salt polymer：10~70；Plant type high molecular polymer：3~25；PH adjusting agent：1~10.Extensively, preparation process is simple, use cost is low for the raw material sources of Quick purifying flocculant of the present invention.Quick purifying flocculant of the present invention is applied in sewage, particularly rivers and lakes, and application method is simple, convenient, can quickly remove the heavy metal in water, and wawter bloom removes the black smelly phenomenon of water body, improves water body environment.Graphene oxide compound of the present invention can control the surface nature and pore structure of graphene sponge by controlling the addition of thiocarbamide and the size of graphene oxide.
Description
Technical field
The present invention relates to a kind of graphene-based water purifying flocculating agent and preparation method and application, belong to field of waste water treatment.
Background technology
In recent years, with the fast development of economy and society, the battalion such as trade effluent source, urban life source and agricultural area source
Foster material largely enters surface water environment, causes body eutrophication phenomenon serious and content of beary metal exceeded.It is nutritious
Water body amount reproduction grow algae so that Blue-green Algae Fast Growth simultaneously forms the offscum of one layer of blue-green with bad smell in the water surface, claims
It is " wawter bloom ".Large-scale Blue-green Algae Fast Growth, causes water quality deterioration, ecosystem of lake regions balance heavy damage, the diversity of aquatile
A large amount of decay, serious threat is constituted to drinking water safety.Five big freshwater lakes of China come into wawter bloom state, fresh water
The eutrophication problem in lake spreads the whole world.On the other hand, the discharge capacity of heavy metal wastewater thereby constantly increases, and heavy metal can pass through
The mode of water body enrichment causes harm to water environment and the whole ecosystem, and can be by contact or through food in human body cohesion
Collection, induces various diseases, endangers the health of the mankind.Spreading unchecked for heavy metal and harmful, poisonous algae is how removed and controlled, is recovered
The aquatic ecosystem of health is one of international great environmental scientific research forward position in water body in lake.
At present, administering surface water environment can substantially be divided into physics, chemistry and biological three kinds of methods.Although physical method effect
It is good, but quantities is big, operation period is long, and disposable input cost is higher, it is impossible to tackle the problem at its root；Though chemical method
So have speed fast, effect clear advantage, but easily cause secondary pollution；Biological method non-secondary pollution, but technology is in itself
And it is immature.
For above mentioned problem, the side that algae removing heavy metals are settled with inorganic composite floculant is generally believed in the world at present
Method is one of optimal selection.Inorganic organic composite coagulator has reaction speed fast, and flocculating result is good, is difficult anti-molten generation secondary
The problem of pollution.However, limited sorption capacity of the above-mentioned flocculant for heavy metal.
The content of the invention
It is an object of the invention to provide a kind of graphene-based Quick purifying flocculant and its preparation method and application, the present invention
Flocculant can solve the problem that traditional flocculant reaction speed in waste water control is slow, and flocculating effect is poor, Yi Fanrong, removes removing heavy metals energy
The limited problem of power, is that Graphene is laid a good foundation in the application of sewage treatment area.
Present invention firstly provides a kind of preparation method of graphene oxide compound, comprise the following steps：
(1) oligomeric 3- aminopropyl triethoxysilanes are added into the aqueous dispersions of graphene oxide and obtains flocculating heavy
Form sediment, the graphene oxide of as oligomeric 3- aminopropyl triethoxysilanes modification；
The oligomeric 3- aminopropyl triethoxysilanes are obtained by 3- aminopropyl triethoxysilanes through hydrolysis, its number
Average molecular weight can be 221~20000, such as 10000；
(2) under the catalysis of carbodiimides, the graphene oxide of the oligomeric 3- aminopropyl triethoxysilanes modification
With polyacrylamide react and obtain acrylamide oligomers graphene oxide；
The number-average molecular weight of the polyacrylamide can be 2,000,000~30,000,000, such as 2,000,000；
(3) to thiocarbamide is added in the aqueous solution of the acrylamide oligomers graphene oxide, obtained by hydrothermal method
Graphene sponge, as described graphene oxide compound, then through washing, freeze-drying the step of.
In above-mentioned preparation method, in step (1), the particle diameter of the graphene oxide can be 10~1000nm, such as 40~
80nm；
The temperature of the hydrolysis can be 40~50 DEG C, and the time can be 2~8 hours, and 6 are such as carried out under conditions of 45 DEG C
Hour；
In step (2), the reaction can normal condition such as raw material proportioning, catalyst amount, temperature, enter under the time
OK；
In step (3), the graphene oxide can be 1 with the mol ratio of the thiocarbamide：0.1~10, such as 1：0.2.
The hydrothermal method can be carried out under normal conditions.
On the basis of the graphene oxide compound prepared in the above method, the present invention still further provides wadding
Solidifying agent, by anionic polymer polymer, the graphene oxide compound, amphoteric metal salt polymer, plant type macromolecule
Polymer and pH adjusting agent are constituted.
The mass fraction of each component is in described flocculant：
Anionic polymer polymer：1~20；
Graphene oxide compound：2~10；
Amphoteric metal salt polymer：10~70；
Plant type high molecular polymer：3~25；
PH adjusting agent：1~10.
The mass fraction of each component concretely 1) -5 in the flocculant) in any one：
1) anionic polymer polymer：10~20；
Graphene oxide compound：2~8；
Amphoteric metal salt polymer：50~70；
Plant type high molecular polymer：10~20；
PH adjusting agent：4~8；
2) anionic polymer polymer：20；
Graphene oxide compound：2；
Amphoteric metal salt polymer：50；
Plant type high molecular polymer：20；
PH adjusting agent：8；
3) anionic polymer polymer：10；
Graphene oxide compound：6；
Amphoteric metal salt polymer：70；
Plant type high molecular polymer：10；
PH adjusting agent：4；
4) anionic polymer polymer：15；
Graphene oxide compound：8；
Amphoteric metal salt polymer：50；
Plant type high molecular polymer：20；
PH adjusting agent：7；
5) anionic polymer polymer：18；
Graphene oxide compound：7；
Amphoteric metal salt polymer：60；
Plant type high molecular polymer：10；
PH adjusting agent：5.
In described flocculant, the number-average molecular weight of the anionic polymer polymer can be 2,000,000~30,000,000；
The anionic polymer polymer is chosen in particular from PAMA, Sodium Polyacrylate and polyvinyl sulfonic acid
At least one of sodium；
The amphoteric metal salt polymer is polyaluminium thing, polyaluminum sulfate thing and the polymerization silicate of following metallic elements
At least one of：Iron, aluminium and magnesium；
The mass fraction of metallic element is calculated as 10%~50% with its oxide described in the amphoteric metal salt polymer,
Concretely 25%~30%, 25%, 26% or 30%；
The plant type high molecular polymer can be anionic starch or anionic cellulose；
The pH adjusting agent may be selected from least one of calcium oxide, sodium carbonate, potassium carbonate and sodium acid carbonate.
In described flocculant, the flocculant is in granular form, and its mesh number can be 300~400 mesh.
Flocculant of the present invention can be prepared by the following method：By the anionic polymer polymer, the oxidation
Graphene complex, the amphoteric metal salt polymer, the plant type high molecular polymer and the pH adjusting agent are mixed, powder
It is broken, that is, obtain the flocculant.
Flocculant of the present invention can be used for heavy metal and improvement wawter bloom in wastewater treatment, removing water.
The present invention has following features compared with prior art：
Extensively, preparation process is simple, use cost is low for the raw material sources of Quick purifying flocculant of the present invention.
Quick purifying flocculant of the present invention is applied in sewage, particularly rivers and lakes, and application method is simple, convenient, can
The quick heavy metal removed in water, wawter bloom removes the black smelly phenomenon of water body, improves water body environment.
Graphene oxide compound of the present invention can be by controlling the addition of thiocarbamide and the size of graphene oxide to control
The surface nature and pore structure of graphene sponge processed.
Quick purifying flocculant alumen ustum of the present invention is big, sedimentation is fast, flocculation decoloration and COD clearance effects are obvious.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of graphene oxide compound prepared by the embodiment of the present invention 1.
Fig. 2 is the electromicroscopic photograph of different size graphene oxide compound prepared by the embodiment of the present invention 1.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute
State method and be conventional method unless otherwise instructed.The raw material can be obtained from open commercial sources unless otherwise instructed.
Embodiment 1, graphene oxide compound
(1) 3- aminopropyl triethoxysilanes are hydrolyzed 6 hours under conditions of 45 DEG C and obtain oligomeric 3- aminopropyls three
Ethoxysilane, its number-average molecular weight is 10000Da.Oligomeric 3- aminopropyl triethoxysilanes are added to graphene oxide
Flocculation sediment is obtained in aqueous dispersions (wherein the particle diameter of graphene oxide can be 40~80nm), the as oligomeric second of 3- aminopropyls three
The graphene oxide of TMOS modification；
(2) under the catalysis of carbodiimides, the graphene oxide of oligomeric 3- aminopropyl triethoxysilanes modification with it is poly-
Acrylamide (number-average molecular weight is 2,000,000) react and obtains acrylamide oligomers graphene oxide；
(3) to adding thiocarbamide, wherein graphene oxide and thiocarbamide in the aqueous solution of acrylamide oligomers graphene oxide
Mol ratio be 1：0.2, graphene sponge is obtained by hydrothermal method, as graphene oxide compound, then through washing, cold
Lyophilized dry step.
The infrared spectrum of graphene oxide compound manufactured in the present embodiment is as shown in Figure 1, it can be seen that acrylamide is low
Polymers is already attached to surface of graphene oxide, forms acrylamide oligomers graphene oxide.
Shown in electromicroscopic photograph such as Fig. 2 (a) of graphene oxide compound manufactured in the present embodiment.
Use the graphene oxide of above-mentioned size and Different adding amount thiocarbamide (mol ratio of graphene oxide and thiocarbamide for
1：0.1) graphene oxide compound is prepared according to the method described above, obtains electromicroscopic photograph such as Fig. 2 (b) of graphene oxide compound
It is shown.
As seen from Figure 2, with the change of thiocarbamide and the ratio of graphene oxide, the aperture of its graphene sponge and chi
The very little change that also there occurs response, therefore can be by controlling the addition of thiocarbamide and the size of graphene oxide to control stone
The surface nature and pore structure of black alkene sponge.
The preparation and its application of embodiment 2, flocculant
Take the raw material of following weight：It is PAMA (10,000,000) 20Kg, graphene oxide compound 2Kg, poly-
Close aluminium iron silicate (mass content of aluminium is calculated as 25% with aluminum oxide) 40Kg, aluminum sulfate 10Kg, anionic cellulose sodium 20Kg, carbon
Sour sodium 8Kg, after being well mixed, after ball milling, crosses 200~300 mesh sieves, both obtains Quick purifying flocculant.
200mL rivers are taken, experimental group 1 and experimental group 2 are set：Experimental group 1 adds the present embodiment flocculant 200mg, experiment
Commercially available flocculant (aluminium polychloride, five Star, the Licheng District five-pointed star chemical industry sales department) 200mg of the addition of group 2, stirs and evenly mixs respectively,
Clarification is precipitated to, then is detected.
Wherein the treatment water pH value of experimental group 1 is 7.2, COD clearances 88%, BOD clearances 73%, total tp removal rate
90.2%, nitrogen removal rate 44.6%, 20 microns of solid content residual rates 20%, flocculant residual rate 8.9%
The treatment water pH value of experimental group 2 is 7.5, COD clearances 52%, and BOD clearances are 36%, total tp removal rate
52%, nitrogen removal rate 12%, 20 microns of solid content residual rates 66%, flocculant residual rate 55%.
The preparation and its application of embodiment 3, flocculant
Take the raw material of following weight：Anionic acrylic receives (8,000,000) 10Kg, graphene oxide compound 6Kg, polymerised sulphur
Sour ferro-aluminum (mass content of aluminium is calculated as 25% by aluminum oxide) 45Kg, (mass content of aluminium is in terms of aluminum oxide for PAFC
Be 20%) 25Kg, anionic starch 10Kg, calcium oxide 4Kg, after being well mixed, after ball milling, cross 200-300 mesh sieves, both quickly
Water purifying flocculating agent.
200mL rivers are taken, experimental group 1 and experimental group 2 are set：Experimental group 1 adds the present embodiment flocculant 200mg, experiment
The commercially available flocculant 200mg of the addition of group 2, stirs and evenly mixs respectively, is precipitated to clarification, then detected.
Wherein the treatment water pH value of experimental group 1 is 7.2, COD clearances 89%, BOD clearances 74%, total tp removal rate
91.3%, nitrogen removal rate 47.2%, 20 microns of solid content residual rates 18.1%, flocculant residual rate 9.6%
The treatment water pH value of experimental group 2 is 7.5, COD clearances 50%, and BOD clearances are 39%, total tp removal rate
51%, nitrogen removal rate 14%, 20 microns of solid content residual rates 67%, flocculant residual rate 56%.
The preparation and its application of embodiment 4, flocculant
Take the raw material of following weight：It is anion sodium apolate (2,000,000) 15Kg, graphene oxide compound 8Kg, poly-
(mass content of aluminium is to aoxidize to close aluminium iron sulfate (mass content of aluminium is calculated as 26% with aluminum oxide) 35Kg, polymeric aluminium ferrum silicate
Aluminium is calculated as 25%) 15Kg, anionic cellulose sodium 20Kg, sodium acid carbonate 7Kg, after being well mixed, after ball milling, crosses 200~300 mesh
Sieve, both the Quick purifying flocculant.
200mL rivers are taken, experimental group 1 and experimental group 2 are set：Experimental group 1 adds the present embodiment flocculant 200mg, experiment
The commercially available flocculant 200mg of the addition of group 2, stirs and evenly mixs respectively, is precipitated to clarification, then detected.
Wherein the treatment water pH value of experimental group 1 is 7.2, COD clearances 87.8%, BOD clearances 72.6%, total phosphorus ligands
Rate 89.7%, nitrogen removal rate 45.9%, 20 microns of solid content residual rates 19.4%, flocculant residual rate 9.2%
The treatment water pH value of experimental group 2 is 7.5, COD clearances 48.8%, and BOD clearances are 39.8%, total tp removal rate
53%, nitrogen removal rate 12%, 20 microns of solid content residual rates 65%, flocculant residual rate 57%.
The preparation and its application of embodiment 5, flocculant
Take the raw material of following weight：Anionic acrylic sodium (20,000,000) 18Kg, graphene oxide compound 7Kg, polymerization
Ferric sulfate (mass content of iron is calculated as 30% with aluminum oxide) 35Kg, magnesium chloride 25Kg, anionic cellulose sodium 10Kg, potassium carbonate
5Kg, be well mixed after, after ball milling, cross 200~300 mesh sieves, both the Quick purifying flocculant.
200mL rivers are taken, experimental group 1 and experimental group 2 are set：Experimental group 1 adds the present embodiment flocculant 200mg, experiment
(polyaluminium sulfate, lotus board calculate content 15.6% to the commercially available flocculant of the addition of group 2 with aluminium, and Hengyang City builds the weighing apparatus limited public affairs of industry
Department) 200mg, stir and evenly mix respectively, clarification is precipitated to, then detected.
Wherein the treatment water pH value of experimental group 1 is 7.1, COD clearances 89.8%, BOD clearances 73.6%, total phosphorus ligands
Rate 90.5%, nitrogen removal rate 46.7%, 20 microns of solid content residual rates 19.7%, flocculant residual rate 9.4%.
The treatment water pH value of experimental group 2 is 7.5, COD clearances 47.9%, and BOD clearances are 38.1%, total tp removal rate
50.2%, nitrogen removal rate 11.4%, 20 microns of solid content residual rates 63.1%, flocculant residual rate 57.2%.
After addition graphene oxide compound being can be seen that by above-described embodiment 2-5, flocculant removal COD, BOD, total nitrogen
It is obviously improved than common flocculant with total phosphorus and other effects.
Embodiment 6, flocculant is used to remove heavy metal
Flocculant prepared by testing example 5 removes the ability of heavy metal, comprises the following steps that：
1. the leaded simulated wastewaters of 10mg/L are configured, Pb (NO are weighed3)20.799g is dissolved in water and constant volume is in 100mL, then
Weigh 2mL solution and be dissolved to 1000mL, shake up rear standby.
2. the configuration of the mercurous simulated wastewaters of 8mg/L is configured：Weigh 1.3669g Hg (NO3)2·H2O in beaker, plus in right amount
After water dissolves, add the digestion of 3.5mL concentrated nitric acids and be dissolved to 100mL with water.Then solution 10mL is weighed, is dissolved to water
1000mL, shakes up rear standby.
3. the configuration of 10mg/L cadmium wastewater is configured：Weigh 5.485g Cd (NO3)2·4H2O, is dissolved to after dissolving
100mL, then goes the 1mL solution to be dissolved to 2L, is labelled after shaking up standby.
4. 3 20mL test tubes are taken, 10mL solution after above-mentioned dilution is separately added into, the flocculation of the embodiment 5 of 10mg is added
Agent, aluminium polychloride and polymeric aluminium ferrum silicate, after shaking up concussion 15 minutes, the Pd (detection methods in detection supernatant solution：GB/
T7475-1987), Cd (detection methods：GB/T30157-2013), Hg (detection methods：GB/T 7468-1987) content.Survey
Examination structure is as shown in table 1,
Flocculant removing Pb prepared by embodiment 5 is can be seen that by the data in table 12+、Cd3+、Hg2+Amount can reach
More than 98%.
The flocculant of the present invention of table 1 removes heavy metal (unit is ppm)
| Sample | 10 | 10 | 8 |
| The flocculant of embodiment 5 | 0.01 | 0.02 | 0.01 |
| Aluminium polychloride | 3.0 | 4.1 | 3.2 |
| Polymeric aluminium ferrum silicate | 2.7 | 3.1 | 2.5 |
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements done etc. should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene oxide compound, comprises the following steps：
(1) oligomeric 3- aminopropyl triethoxysilanes are added into the aqueous dispersions of graphene oxide and obtains flocculation sediment, i.e.,
It is the graphene oxide of oligomeric 3- aminopropyl triethoxysilanes modification；
The oligomeric 3- aminopropyl triethoxysilanes are obtained by 3- aminopropyl triethoxysilanes through hydrolysis；
(2) under the catalysis of carbodiimides, the graphene oxide of the oligomeric 3- aminopropyl triethoxysilanes modification with it is poly-
Acrylamide react and obtains acrylamide oligomers graphene oxide；
The number-average molecular weight of the polyacrylamide is 2,000,000~30,000,000；
(3) to thiocarbamide is added in the aqueous solution of the acrylamide oligomers graphene oxide, graphite is obtained by hydrothermal method
Alkene sponge, as described graphene oxide compound.
2. preparation method according to claim 1, it is characterised in that：In step (1), the particle diameter of the graphene oxide is
10~1000nm；
The temperature of the hydrolysis is 40~50 DEG C, and the time is 2~8 hours；
In step (3), the graphene oxide is 1 with the mol ratio of the thiocarbamide：0.1~10.
3. the graphene oxide compound that prepared by the methods described of claim 1 or 2.
4. application of the graphene oxide compound in water purifying flocculating agent is prepared described in claim 3.
5. a kind of flocculant, graphene oxide compound, amphoteric metal as described in anionic polymer polymer, claim 3
Salt polymer, plant type high molecular polymer and pH adjusting agent composition.
6. flocculant according to claim 5, it is characterised in that：In the flocculant, the mass fraction of each component is：
Anionic polymer polymer：1~20；
Graphene oxide compound：2~10；
Amphoteric metal salt polymer：10~70；
Plant type high molecular polymer：3~25；
PH adjusting agent：1~10.
7. the flocculant according to claim 5 or 6, it is characterised in that：The number of the anionic polymer polymer is divided equally
Son amount is 2,000,000~30,000,000；
The anionic polymer polymer is chosen in particular from PAMA, Sodium Polyacrylate and sodium apolate
It is at least one；
The amphoteric metal salt polymer be following metallic elements polyaluminium thing, polyaluminum sulfate thing and polymerization silicate in extremely
Few one kind：Iron, aluminium and magnesium；
The mass fraction of metallic element is calculated as 10%~50% with its oxide described in the amphoteric metal salt polymer；
The plant type high molecular polymer is anionic starch or anionic cellulose；
The pH adjusting agent is selected from least one of calcium oxide, sodium carbonate, potassium carbonate and sodium acid carbonate.
8. the flocculant according to any one of claim 5-7, it is characterised in that：The flocculant is in granular form, its mesh
Number is 300~400 mesh.
9. the preparation method of flocculant any one of claim 5-8, comprises the following steps：By the anionic polymer
Polymer, the graphene oxide compound, the amphoteric metal salt polymer, the plant type high molecular polymer and described
PH adjusting agent is mixed, and is crushed, that is, obtain the flocculant.
10. flocculant any one of claim 5-8 wastewater treatment, remove in water in heavy metal and/or wawter bloom should
With.
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| CN107983307A (en) * | 2017-12-03 | 2018-05-04 | 凯思普科技有限责任公司 | A kind of efficiently water purification nano-graphene material |
| CN108658195A (en) * | 2018-06-21 | 2018-10-16 | 宁波沸柴机器人科技有限公司 | A kind of composite flocculation agent and its preparation method and application |
| CN109133456A (en) * | 2018-09-30 | 2019-01-04 | 贺州市骏鑫矿产品有限责任公司 | A kind of circulation utilization method of feldspar in powder production waste |
| CN109629226A (en) * | 2018-11-27 | 2019-04-16 | 洪春 | The preparation process and application of polymer fiber graphene composition |
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