CN103861565A - Preparation of linear amino modified graphene oxide adsorption material - Google Patents
Preparation of linear amino modified graphene oxide adsorption material Download PDFInfo
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- CN103861565A CN103861565A CN201210539883.4A CN201210539883A CN103861565A CN 103861565 A CN103861565 A CN 103861565A CN 201210539883 A CN201210539883 A CN 201210539883A CN 103861565 A CN103861565 A CN 103861565A
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Abstract
The invention provides a preparation method of an adsorbent for removal of lead ions, cadmium ions, manganese ions, copper ions and other heavy metal ions in wastewater. The method is as follows: first using graphite powder as a raw material to prepare graphene oxide by concentrated sulfuric acid, potassium permanganate and hydrogen peroxide oxidation, dissolving the graphene oxide in ethanol to disperse the graphene oxide in the ethanol by means of ultrasonic, then adding a certain amount of an ammonia-functional-group-containing linear molecule, reacting in water bath at 50-80 DEG C for 12-24 hours, performing vacuum suction filtration of an obtained product, then washing with the ethanol, and then drying at 50-100 DEG C to obtain the heavy metal adsorption material. SEM (scanning electron microscope) pictures show that the adsorbent has a loose surface, and the adsorbent has a good application prospect in adsorption field. Adsorption experiments show that, under the condition of normal temperature, the adsorbent has a good adsorption capacity to the lead ions, cadmium ions, manganese ions and copper ions, and especially has a strong adsorption capacity to the lead ions, and the maximum adsorption amount can reach 370mg/g above.
Description
Technical field
The present invention relates to the technical field that Heavy-metal Polluted Environment is repaired, be specifically related to preparation method and the application thereof of a class adsorbent for heavy metal.
Background technology
Along with developing rapidly of modern industrial technology, heavy metal is on the rise to water pollution problem.Heavy metal ion is mainly that urban domestic wastewater discharges in natural environment, and enters animal and plant body by the enrichment of food chain, and then threatens human health by industrial wastewaters such as smelting, plating.Traditional process for treating heavy-metal waste water mainly contains chemical precipitation, ion-exchange, counter-infiltration, membrane technology, distillation, electrochemical treatments and electrodialysis etc., these methods have good effect to a certain extent, but ubiquity cost is high, clearance is lower, easily produce secondary pollution problems.Wherein absorption method cost is low, and technique is simple, is to remove very effective method of heavy metal ions in wastewater.
Graphene oxide contains a large amount of hydroxyls and the acid active group of carboxyl, has larger specific area simultaneously, has potential using value aspect heavy metal adsorption.Met especially the different demand of people through processing the graphene oxide of modification, when adsorbing the heavy metal ion of removing waste water, conventionally revised graphene oxide with amido functional group, this class sorbing material has larger load capacity to heavy metal ion.The present invention uses the graphene oxide sorbing material that makes the linear amino molecular modification of a class containing the graphene oxide of amino-compound and ethanol dissolving under gentle condition.There are again many carboxyl functional groups in the existing polyamino of the adsorbent functional group that adopts the method to make, and the heavy metal ion in waste water is had to good absorption property.
Summary of the invention
The present invention proposes one and is used for removing lead ion, cadmium ion, the preparation method of the graphene oxide sorbing material containing amino molecular modification of the heavy metal ion such as manganese ion and copper ion.The method is by first take graphite powder as raw material, and under 0 ~ 120 ℃ of temperature conditions, through the concentrated sulfuric acid, the oxidant oxidations such as hydrogen peroxide and potassium permanganate obtain graphene oxide, and sulfuric acid mass fraction used is 50 ~ 98%, and hydrogen peroxide mass fraction is 5 ~ 30%; Process graphene oxide is dissolved in ethanol through ultrasonic wave again, with amino-contained molecule, graphene oxide is modified, under 50 ~ 80 ℃ of water-baths, reacted 12 ~ 24 hours, the product obtaining washs with ethanol after decompress filter, dry at 50 ~ 100 ℃, can obtain heavy metal adsorption material; Described is polyacrylamide, ethylenediamine, poly-propylamine or poly-butylamine containing amino compound.
Feature of the present invention is that adsorbent is to lead ion, cadmium ion, and manganese ion and copper ion have good absorption property, and adopting process is simple.
Chemical relationship described in synthesis step is graphene oxide: the mass ratio of ethanol in the scope of 1:10 ~ 150, graphene oxide: containing the mass ratio of amino linear molecule in the scope of 1:2 ~ 20; Described ethanol is to analyze straight alcohol; Described temperature is 50 ~ 80 ℃; The described reaction time is 6 ~ 48 hours; The graphene oxide solution that described ethanol dissolves is, after graphene oxide is mixed with ethanol, to obtain through ultrasonic wave processing; Described product is the graphene oxide sorbing material containing amino molecular modification.
Compared with prior art, sorbing material prepared by the present invention, has carboxyl and amino two kinds of groups on its strand, and its outstanding feature is:
(1) can pass through the electrostatic attraction effect Adsorption of Heavy Metal Ions of carboxylic group, increase adsorption capacity; Make heavy metal ion be easy to desorb from adsorbent by the repulsive interaction of basic group, improve its power of regeneration; Overcome adsorbent prepared by prior art and only contained simple function group, the shortcoming that adsorption capacity is weak, desorption is difficult;
(2) can regulate the absorption of ABSORBENTS ABSORPTION metal ion to select by the content of carboxyl and amino group in adjusting adsorbent, overcome the shortcoming that adsorbent group kind is unadjustable, applicability is poor prepared by prior art.
That reports with Chinese patent 200810246170.2 carries out epoxy addition by silane coupler and acid anhydrides and reacts, carrying out quaterisation synthetic same with halogenated alkane is again to contain carboxyl to compare with the method that the organic/inorganic hybridization material of amino two kinds of groups carrys out Adsorption of Heavy Metal Ions, preparation technology of the present invention is simple, strong to heavy metal ion adsorbed ability.
Accompanying drawing explanation
Fig. 1 is the SEM figure of graphene oxide-ethylenediamine sorbing material; SEM figure shows that this adsorbent has more fluffy surface, and this adsorbent may have good application prospect in adsorbing domain.
Fig. 2 is during take graphene oxide-ethylenediamine as sorbing material, lead ion, cadmium ion, manganese ion and the concentration of copper ion ion and the relation curve of adsorbance; Show by adsorption experiment, under normal temperature condition, this adsorbent is to lead ion, cadmium ion, and manganese ion, copper ion all have good absorption, especially lead ion are had to larger adsorption capacity, more than maximal absorptive capacity reaches 370mg/g.
The specific embodiment
The present invention can describe in detail by embodiment, but they are not that the present invention is done to any restriction.
These embodiment have illustrated the building-up process of graphene oxide-ethylenediamine, illustrate in greater detail graphene oxide-ethylenediamine absorption property good to lead ion, cadmium ion, manganese ion and copper ion simultaneously.
Embodiment 1
First at room temperature graphene oxide is dissolved in ethanol, it was mixed in ultrasonic 1 hour, join in 500ml there-necked flask, the ethylenediamine that adds again a certain amount of ethanol to dissolve, the mass ratio of reactant is, graphene oxide: ethylenediamine: ethanol=1:1 ~ 10:10 ~ 120, in the process that adds ethylenediamine, can find the two vigorous reaction, show to react, and ethylenediamine dissolves very soon.Whole reaction is continuous mechanical agitation in 80 ℃ of water-baths, reaction is carried out after 24h, to react gained material and wash 3 times with ethanol after decompress filter, at 80 ℃, after dry 12h, obtain having graphene oxide-ethylenediamine sorbing material of carboxyl and amino group simultaneously.For guaranteeing the ability of the complete of reaction and raising adsorbent Adsorption of Heavy Metal Ions, in the preparation process of the present embodiment adsorbent, make ethylenediamine keep excessive.
The present invention adopts static adsorptive method to measure adsorbent to lead ion, cadmium ion, the adsorbance of manganese ion and copper ion.Concrete steps are as follows:
Take respectively the adsorbent preparing in 0.1g experimental example 1 and be placed in the round-bottomed flask that 250ml is dry, adding respectively 100ml initial concentration is 2.0mmol/L, pH=2.0,2.5,3.0,3.5,4.0,4.5 and 5.0 Pb (NO
3)
2solution, sonic oscillation 1 hour, adsorbent is disperseed better in solution, then be placed in 25 ℃ of waters bath with thermostatic control, sealing round-bottomed flask, constant temperature stirs, and the solution funnel of getting after 3h after absorption filters, measure the concentration of lead ion residual in filtrate by atomic absorption spectrophotometer, then calculate the adsorbance of adsorbent according to (1).
Experimental result shows: under 25 ℃ of temperature conditions, and pH=2.0,2.5,3.0,3.5,4.0,4.5 and 5.0 pairs of lead ion adsorbances are 27.19 ~ 197.33mg/g, wherein, under pH=4.5 condition, the adsorbance maximum of the adsorbent preparing in experimental example 1 to lead ion, is 197.33mg/g.
Experimental example 2
Take respectively the adsorbent preparing in 0.1g experimental example 1 and be placed in the round-bottomed flask that 250ml is dry, adding respectively 100ml initial concentration is pH=4.5, concentration C
0=0.5,1,1.5,2.0,2.5,3.0,3.5,4,4.5 and Pb (the NO of 5mmol/L
3)
2solution, sonic oscillation 1 hour, adsorbent is disperseed better in solution, then be placed in 25 ℃ of waters bath with thermostatic control, sealing round-bottomed flask, constant temperature stirs, and the solution funnel of getting after 3h after absorption filters, measure the concentration of lead ion residual in filtrate by atomic absorption spectrophotometer, then calculate the adsorbance of adsorbent according to (1).
Experimental result shows: be 25 ℃ in temperature, under pH=4.5 condition, the adsorbent preparing in experimental example 1 is 379.62mg/g to lead ion adsorbance.
Experimental example 3
Take respectively the adsorbent preparing in 0.1g experimental example 1 and be placed in the round-bottomed flask that 250ml is dry, adding respectively 100ml initial concentration is 2mmol/L, pH=2.0,2.5,3.0,3.5,4.0,4.5 and 5.0 Cd (NO
3)
2solution, sonic oscillation 1 hour, adsorbent is disperseed better in solution, then be placed in 25 ℃ of waters bath with thermostatic control, sealing round-bottomed flask, constant temperature stirs, and the solution funnel of getting after 3h after absorption filters, measure the concentration of cadmium ion residual in filtrate by atomic absorption spectrophotometer, then calculate the adsorbance of adsorbent according to (1).
Experimental result shows: under 25 ℃ of temperature conditions, and pH=2.0,2.5,3.0,3.5,4.0,4.5 and 5.0 pairs of cadmium sorption amounts are 14.56 ~ 113.6mg/g, wherein, under pH=5.0 condition, the adsorbance maximum of the adsorbent preparing in experimental example 1 to cadmium ion, is 113.6mg/g.
Experimental example 4
Take respectively the adsorbent preparing in 0.1g experimental example 1 and be placed in the round-bottomed flask that 250ml is dry, adding respectively 50ml initial concentration is pH=5, concentration C
0=0.5,1,1.5,2.0,2.5,3.0 and Cd (the NO of 4mmol/L
3)
2solution, sonic oscillation 1 hour, adsorbent is disperseed better in solution, then be placed in 25 ℃ of waters bath with thermostatic control, sealing round-bottomed flask, constant temperature stirs, and the solution funnel of getting after 3h after absorption filters, measure the concentration of cadmium ion residual in filtrate by atomic absorption spectrophotometer, then calculate the adsorbance of adsorbent according to (1).
Experimental result shows: be 25 ℃ in temperature, under pH=4.5 condition, the adsorbent preparing in experimental example 1 is 33.59mg/g to cadmium sorption amount.
Experimental example 5
Take respectively the adsorbent preparing in 0.1g experimental example 1 and be placed in the round-bottomed flask that 250ml is dry, adding respectively 100ml initial concentration is 2mmol/L, pH=3.0,4.0,5.0,5.5,6.0 and 6.5 MnSO
4solution, sonic oscillation 1 hour, adsorbent is disperseed better in solution, then be placed in 25 ℃ of waters bath with thermostatic control, sealing round-bottomed flask, constant temperature stirs, and the solution funnel of getting after 3h after absorption filters, measure the concentration of manganese ion residual in filtrate by atomic absorption spectrophotometer, then calculate the adsorbance of adsorbent according to (1).
Experimental result shows: under 25 ℃ of temperature conditions, and pH=3.0,4.0,5.0,5.5,6.0 and 6.5 pairs of manganese ion adsorbances are 9.695 ~ 26.135mg/g, wherein, under pH=5.0 condition, the adsorbance maximum of the adsorbent preparing in experimental example 1 to manganese ion, is 26.135mg/g.
Claims (3)
1. this sorbing material is a kind of graphene oxide based on the amino molecular modification of linearity, can effectively remove Pb In Exhausted Water ion, cadmium ion, the heavy metal ion such as manganese ion, copper ion; The amino molecule of described linearity comprises containing of the different chain length such as ammonia ethylenediamine, propane diamine, butanediamine, hexamethylene diamine of two amino micromolecular linear molecules, also wrap in molecule the little molecule of linearity or large molecule containing more than 2 functional group, as the large molecule of polyacrylamide of different molecular weight etc.
2. according in chemical relationship claimed in claim 1, graphene oxide: the mass ratio of ethanol in the scope of 1:10 ~ 150, graphene oxide: containing amino linear molecule in the scope of 1:2 ~ 20; It is 30 ~ 80 ℃ according to the preparation temperature of adsorbent claimed in claim 1; According to the reaction time claimed in claim 1 be 6 ~ 48 hours.
3. the product obtaining according to the preparation method described in claim 1
forthere is the heavy metal adsorption material of amino and carboxyl.
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Cited By (10)
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| CN104525126A (en) * | 2014-12-18 | 2015-04-22 | 湖北中烟工业有限责任公司 | Bio-polyamines-modified graphene adsorption material as well as preparation method and application thereof |
| CN104759268A (en) * | 2015-04-15 | 2015-07-08 | 长沙学院 | Preparation method of ACF/GO/PEI composite material capable of efficiently adsorbing heavy metal |
| CN105148867A (en) * | 2015-09-15 | 2015-12-16 | 李云峰 | Graphene oxide-recombined streptococcal protein G non-covalent composite material as well as preparation method and application thereof |
| CN105645392A (en) * | 2016-01-11 | 2016-06-08 | 天津师范大学 | Preparation method and application of aminated graphene |
| CN105886001A (en) * | 2014-12-15 | 2016-08-24 | 闫立群 | Lubricating oil based on nitrogen containing surface modifier modified graphene and preparation method thereof |
| CN106241783A (en) * | 2016-07-29 | 2016-12-21 | 新乡学院 | A kind of synthetic method of amido Graphene sewage-treating agent |
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| WO2017206579A1 (en) * | 2016-05-31 | 2017-12-07 | 成都新柯力化工科技有限公司 | Graphene micro-sheet having mesh structure and preparation method therefor |
| RU2659285C1 (en) * | 2017-10-25 | 2018-06-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Тамбовский государственный технический университет" (ФГБОУ ВО "ТГТУ") | Sorbent based on modified graphene oxide and method of its production |
| CN112958056A (en) * | 2021-02-03 | 2021-06-15 | 中南大学 | Three-dimensional graphene oxide composite material and preparation method and application thereof |
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| CN105886001B (en) * | 2014-12-15 | 2020-04-07 | 闫立群 | Lubricating oil based on nitrogen-containing surface modifier modified graphene and preparation method thereof |
| CN105886001A (en) * | 2014-12-15 | 2016-08-24 | 闫立群 | Lubricating oil based on nitrogen containing surface modifier modified graphene and preparation method thereof |
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| CN104759268B (en) * | 2015-04-15 | 2017-05-03 | 长沙学院 | Preparation method of ACF/GO/PEI composite material capable of efficiently adsorbing heavy metal |
| CN104759268A (en) * | 2015-04-15 | 2015-07-08 | 长沙学院 | Preparation method of ACF/GO/PEI composite material capable of efficiently adsorbing heavy metal |
| CN107265529A (en) * | 2015-06-27 | 2017-10-20 | 合肥龙精灵信息技术有限公司 | A kind of multiple-effect water treatment agent and preparation method thereof and method for treating water |
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| CN107337297A (en) * | 2015-06-27 | 2017-11-10 | 合肥龙精灵信息技术有限公司 | A kind of multiple-effect water treatment agent and preparation method thereof and method for treating water |
| CN107487820A (en) * | 2015-06-27 | 2017-12-19 | 合肥龙精灵信息技术有限公司 | A kind of multiple-effect water treatment agent and preparation method thereof and method for treating water |
| CN107487821A (en) * | 2015-06-27 | 2017-12-19 | 合肥龙精灵信息技术有限公司 | A kind of multiple-effect water treatment agent and preparation method thereof and method for treating water |
| CN105148867A (en) * | 2015-09-15 | 2015-12-16 | 李云峰 | Graphene oxide-recombined streptococcal protein G non-covalent composite material as well as preparation method and application thereof |
| CN105645392A (en) * | 2016-01-11 | 2016-06-08 | 天津师范大学 | Preparation method and application of aminated graphene |
| WO2017206579A1 (en) * | 2016-05-31 | 2017-12-07 | 成都新柯力化工科技有限公司 | Graphene micro-sheet having mesh structure and preparation method therefor |
| CN106241783A (en) * | 2016-07-29 | 2016-12-21 | 新乡学院 | A kind of synthetic method of amido Graphene sewage-treating agent |
| RU2659285C1 (en) * | 2017-10-25 | 2018-06-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Тамбовский государственный технический университет" (ФГБОУ ВО "ТГТУ") | Sorbent based on modified graphene oxide and method of its production |
| CN112958056A (en) * | 2021-02-03 | 2021-06-15 | 中南大学 | Three-dimensional graphene oxide composite material and preparation method and application thereof |
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