CN113000032A - Preparation method of graphene oxide-biomass composite adsorbent - Google Patents
Preparation method of graphene oxide-biomass composite adsorbent Download PDFInfo
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- CN113000032A CN113000032A CN202110387469.5A CN202110387469A CN113000032A CN 113000032 A CN113000032 A CN 113000032A CN 202110387469 A CN202110387469 A CN 202110387469A CN 113000032 A CN113000032 A CN 113000032A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
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Abstract
The invention relates to the technical field of sewage treatment and discloses a graphene oxide-biomass composite adsorbent, which is prepared by mixing graphene oxide and biomass into a composite material with good stability and rich functional groups on the surface, so that the adsorption capacity and stability of the adsorbent are enhanced, and active groups containing lone pair electrons, such as hydroxyl, carboxyl and the like in the graphene oxide-biomass composite adsorbent are typical electron donors and can react with heavy metal ions in sewage, such as Pb (lead) ions2+The empty orbit forms a stable complex compound through coordination bonds, and the complex compound is adsorbed on the surface of the adsorbent, so that heavy metal ions in the sewage are adsorbed and removed, and an excellent adsorption effect is achievedAnd sewage treatment effect.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a preparation method of a graphene oxide-biomass composite adsorbent.
Background
The heavy metal pollution of the water body refers to serious pollution of ionic heavy metal or compound heavy metal to the water environment, and generally refers to zinc, mercury, nickel, cadmium, manganese, lead, copper, silver, gold and the like. With the rapid development of the industry, agriculture and manufacturing industry in China, the phenomenon of heavy metal pollution of water bodies is increasingly aggravated. The method is extremely important for pollution control of lead in water, lead can be remained in human bodies and animal tissues, and if the lead exceeds the standard, the toxicity of the lead is shown as follows: anemia, nervous system disorders, and impaired reproductive system.
At present, the adsorption method is considered to be one of the most effective methods for treating sewage containing heavy metal ions. By utilizing the characteristics of high comparative area and high porosity of the adsorption material, heavy metal ions in the solution are accumulated on the surface or in the adsorbent to complete the removal of pollutants. The method has the advantages of low use cost, simple operation, wide source of adsorbent materials, good adsorption effect and the like.
Graphene oxide is a derivative of graphene, contains oxygen-containing functional groups such as hydroxyl, carboxyl, epoxy, carbonyl and the like, has polarity, has good dispersibility in an aqueous solution, and is very suitable for sewage treatment. The existence of the groups also enables the surface modification treatment of the graphene oxide to be feasible, and the graphene oxide can be compounded with other polar substances to prepare a composite material. The reports of various graphene oxide composite materials are infinite nowadays, and a good way is provided for preparing a novel adsorption material which is more efficient and environment-friendly.
The natural biomass materials comprise bagasse, straws, mulberry stems, peanut shells, orange peels and the like, are wide in source and low in price, can treat metal ions in wastewater, and has the effects of changing waste into valuable and recycling resources. Compared with other crops, the bagasse has higher cellulose content, higher lignification degree and higher fiber yield, is a natural high polymer material, contains hydrophilic functional groups such as hydroxyl and the like, has the characteristics of porosity, large specific surface area, abundant resources, low cost, low density, easiness in processing and good hydrophilicity, and can be used as an adsorbing material.
According to the invention, the graphene oxide is compounded with the bagasse and the grass meal, and the advantages of the bagasse and the grass meal are combined, so that the defect that the graphene oxide is easy to disperse in a solution is reduced, the operability of the adsorbing material is improved, the recovery and separation of the adsorbent are realized, and the adsorption efficiency of the adsorbing material is improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a graphene oxide-biomass composite adsorbent, which is used for treating heavy metal ions in sewage, such as Pb2+Etc., having a strong adsorption effect.
In order to achieve the purpose, the invention provides the following technical scheme: a graphene oxide-biomass composite adsorbent is prepared by a method comprising the following steps:
(1) under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid;
(2) respectively adding bagasse and grass meal into a mixed solution of sodium hydroxide and urea, stirring, and performing freeze preservation to prepare a biomass solution;
(3) adding the graphene oxide dispersion liquid and the biomass solution into a reaction kettle, reacting for 2 hours at 90 ℃, washing with deionized water to be neutral, centrifugally separating, and freeze-drying to prepare the graphene oxide-biomass composite adsorbent.
Preferably, the concentration of the graphene oxide dispersion liquid in the step (1) is 2 mg/L.
Preferably, the mass ratio of sodium hydroxide to urea in the mixed solution in the step (2) is 3: 4.
preferably, the mass ratio of the graphene oxide to the biomass in the step (3) is 3-1: 1-3.
Preferably, no biomass solution is added in the step (3), and the mass ratio of the graphene oxide dispersion liquid to the ascorbic acid is 1: 10, obtaining reduced graphene oxide through reaction, and comparing the reduced graphene oxide with the graphene oxide-biomass composite adsorbent.
Preferably, the mass ratio of the graphene oxide to the biomass to the ascorbic acid in the step (3) is 1: 1: 10, reacting to obtain the reduced graphene oxide-biomass composite adsorbent, and comparing the reduced graphene oxide-biomass composite adsorbent with the graphene oxide-biomass composite adsorbent.
Preferably, the graphene oxide is compared to the graphene oxide-biomass composite adsorbent.
Preferably, the biomass is compared to the graphene oxide-biomass composite adsorbent.
Preferably, in the above technical solution, the sewage is Pb2+And (3) solution.
Preferably, in the above technical solution, in the adsorption method, after adding different weights of adsorbents into the pollutant solution with corresponding concentrations, shaking the table at constant temperature.
Preferably, in the above technical solution, the absorbance test is performed by an atomic absorption spectrophotometer.
Advantageous technical effects
Compared with the prior art, the invention has the following chemical experiment principle and beneficial technical effects:
according to the graphene oxide-biomass composite material adsorbent, graphite is subjected to intercalation oxidation reaction in three stages of low temperature, medium temperature and high temperature under the action of an oxidant, graphene oxide is obtained through ultrasonic stripping, the graphene oxide is combined with bagasse and grass meal, the graphene oxide and biomass are stably combined together through the interaction of surface functional groups of the graphene oxide and biomass, the adsorption performance of the graphene oxide and the biomass is maintained to a certain extent, and meanwhile the problem that the graphene oxide is difficult to separate from a solution after adsorption is finished can be avoided. Active groups containing lone pair electrons, such as hydroxyl, carboxyl and the like in the graphene oxide-biomass composite material adsorbent are typical electron donors and can react with Pb2+The empty orbit forms a stable complex compound through coordination bonds, and the complex compound is adsorbed on the surface of the adsorbent, so that heavy metal ions in the sewage are adsorbed and removed, and an excellent adsorption effect and a sewage treatment effect are achieved.
Drawings
FIG. 1 shows adsorbents prepared from graphene oxide and bagasse in different proportions according to examples and comparative examples of the present application for different concentrations of Pb2+Adsorption capacity ofCompare the figures.
FIG. 2 shows different adsorbents for different concentrations of Pb, which are provided in examples and comparative examples of the present application2+Adsorption capacity of (c) versus (d).
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a graphene oxide-biomass composite adsorbent is prepared by the following steps:
(1) under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding bagasse and grass meal into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of the sodium hydroxide to the urea is 3: 4, stirring, freezing and storing to prepare a biomass solution;
(3) adding a graphene oxide dispersion liquid and a biomass solution into a reaction kettle, wherein the mass ratio of graphene oxide to biomass is 3-1: reacting for 2 hours at the temperature of 90 ℃ for 1-3, washing with deionized water to be neutral, centrifugally separating, cooling to be dry, and preparing the graphene oxide-biomass composite adsorbent.
Example 1
(1) Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding bagasse into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of sodium hydroxide to urea is 3: 4, stirring, freezing and storing to prepare bagasse solution;
(3) adding a graphene oxide dispersion solution and a bagasse solution into a reaction kettle, wherein the mass ratio of the graphene oxide to the bagasse is 3: reacting for 2 hours at the temperature of 1 and 90 ℃, washing to be neutral by deionized water, centrifugally separating, cooling to be dry, and preparing the graphene oxide-biomass composite adsorbent for Pb2+The maximum adsorption amount of (2) is 224.2 mg/g。
Example 2
(1) Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding bagasse into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of sodium hydroxide to urea is 3: 4, stirring, freezing and storing to prepare bagasse solution;
(3) adding a graphene oxide dispersion solution and a bagasse solution into a reaction kettle, wherein the mass ratio of the graphene oxide to the bagasse is 2: reacting for 2 hours at the temperature of 1 and 90 ℃, washing to be neutral by deionized water, centrifugally separating, cooling to be dry, and preparing the graphene oxide-biomass composite adsorbent for Pb2+The maximum adsorption amount of (a) was 239.5 mg/g.
Example 3
(1) Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding bagasse into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of sodium hydroxide to urea is 3: 4, stirring, freezing and storing to prepare bagasse solution;
(3) adding a graphene oxide dispersion solution and a bagasse solution into a reaction kettle, wherein the mass ratio of the graphene oxide to the bagasse is 1: reacting for 2 hours at the temperature of 1 and 90 ℃, washing to be neutral by deionized water, centrifugally separating, cooling to be dry, and preparing the graphene oxide-biomass composite adsorbent for Pb2+The maximum adsorption amount of (a) was 245.3 mg/g.
Example 4
(1) Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding bagasse into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of sodium hydroxide to urea is 3: 4, stirring, freezing and storing to prepare bagasse solution;
(3) adding a graphene oxide dispersion solution and a bagasse solution into a reaction kettle, wherein the mass ratio of graphene oxide to bagasse is 1: reacting for 2 hours at the temperature of 2 and 90 ℃, washing to be neutral by deionized water, centrifugally separating, cooling to be dry, and preparing the graphene oxide-biomass composite adsorbent for Pb2+The maximum adsorption amount of (a) was 222.7 mg/g.
Example 5
(1) Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding bagasse into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of sodium hydroxide to urea is 3: 4, stirring, freezing and storing to prepare bagasse solution;
(3) adding a graphene oxide dispersion solution and a bagasse solution into a reaction kettle, wherein the mass ratio of the graphene oxide to the bagasse is 1: reacting for 2 hours at the temperature of 3 and 90 ℃, washing to be neutral by deionized water, centrifugally separating, cooling to be dry, and preparing the graphene oxide-biomass composite adsorbent for Pb2+The maximum adsorption amount of (a) was 230.5 mg/g.
Example 6
(1) Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding grass meal into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of the sodium hydroxide to the urea is 3: 4, stirring, freezing and storing to prepare a grass meal solution;
(3) adding graphene oxide dispersion liquid and grass meal solution into a reaction kettle, wherein the graphene oxide and the grass meal are in the same qualityThe quantity ratio is 1: reacting for 2 hours at the temperature of 1 and 90 ℃, washing to be neutral by deionized water, centrifugally separating, cooling to be dry, and preparing the graphene oxide-biomass composite adsorbent for Pb2+The maximum adsorption amount of (A) was 183.7 mg/g.
Comparative example 1
(1) Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding a graphene oxide dispersion liquid and ascorbic acid into a reaction kettle, wherein the mass ratio of the graphene oxide to the ascorbic acid is 1: reacting at 10 and 90 ℃ for 2h, washing with deionized water to be neutral, centrifugally separating, cooling to be dry to obtain reduced graphene oxide, namely Pb2+Maximum adsorption of 79.9 mg/g.
Comparative example 2
(1) Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid with the concentration of 2 mg/L;
(2) adding bagasse into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of sodium hydroxide to urea is 3: 4, stirring, freezing and storing to prepare bagasse solution;
(3) adding a graphene oxide dispersion solution, a bagasse solution and ascorbic acid into a reaction kettle, wherein the mass ratio of the graphene oxide to the bagasse to the ascorbic acid is 1: 1: reacting for 2 hours at 10 and 90 ℃, washing with deionized water to be neutral, centrifugally separating, cooling to be dry to obtain the reduced graphene oxide-biomass composite adsorbent for treating Pb2+The maximum adsorption amount of (2) was 105.3 mg/g.
Comparative example 3
Under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to neutrality, ultrasonically stripping to prepare graphene oxide dispersion liquid with the concentration of 2mg/L, wherein the graphene oxide dispersion liquid is graphene oxideFor Pb2+The maximum adsorption amount of (A) was 121.2 mg/g.
Comparative example 4
Adding bagasse into a mixed solution of sodium hydroxide and urea, wherein the mass ratio of sodium hydroxide to urea is 3: 4, stirring, freezing and storing to prepare bagasse solution, wherein the bagasse is opposite to Pb2+The maximum adsorption amount of (A) was 59.2 mg/g.
Claims (11)
1. The graphene oxide-biomass composite adsorbent is characterized in that: the preparation method of the graphene oxide-biomass composite adsorbent comprises the following steps:
under the condition of stirring, sequentially adding graphite, concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide into a three-necked bottle, washing with deionized water, centrifuging to be neutral, and ultrasonically stripping to prepare a graphene oxide dispersion liquid;
adding bagasse and grass meal into a mixed solution of sodium hydroxide and urea, stirring, and freezing and storing to prepare a biomass solution;
adding the graphene oxide dispersion liquid and the biomass solution into a reaction kettle, reacting for 2 hours at 90 ℃, washing with deionized water to be neutral, centrifugally separating, cooling to be dry, and preparing to obtain the graphene oxide-biomass composite adsorbent.
2. The graphene oxide-biomass composite adsorbent of claim 1, wherein: the concentration of the graphene oxide dispersion liquid in the step (1) is 2 mg/L.
3. The graphene oxide-biomass composite adsorbent of claim 1, wherein: the mass ratio of sodium hydroxide to urea in the mixed solution in the step (2) is 3: 4.
4. the graphene oxide-biomass composite adsorbent of claim 1, wherein: the mass ratio of the graphene oxide to the bagasse in the step (3) is 3-1: 1-3.
5. The graphene oxide-biomass composite adsorbent of claim 1, wherein: in the step (3), no biomass solution is added, and the mass ratio of the graphene oxide dispersion liquid to the ascorbic acid is 1: 10, obtaining reduced graphene oxide through reaction, and comparing the reduced graphene oxide with the graphene oxide-biomass composite adsorbent.
6. The graphene oxide-biomass composite adsorbent of claim 1, wherein: in the step (3), the mass ratio of the graphene oxide to the biomass to the ascorbic acid is 1: 1: 10, reacting to obtain the reduced graphene oxide-biomass composite adsorbent, and comparing the reduced graphene oxide-biomass composite adsorbent with the graphene oxide-biomass composite adsorbent.
7. The graphene oxide-biomass composite adsorbent of claim 1, wherein: and comparing the graphene oxide with the graphene oxide-biomass composite adsorbent.
8. The graphene oxide-biomass composite adsorbent of claim 1, wherein: biomass is compared with the graphene oxide-biomass composite adsorbent.
9. The graphene oxide-biomass composite adsorbent of claim 1, wherein: the sewage is Pb2+ And (3) solution.
10. The graphene oxide-biomass composite adsorbent of claim 1, wherein: according to the adsorption method, after adsorbents with different weights are added and put into pollutant solutions with corresponding concentrations, shaking tables are subjected to constant-temperature oscillation.
11. The graphene oxide-biomass composite adsorbent of claim 1, wherein: the absorbance test is carried out on an atomic absorption spectrophotometer.
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| CN113617342A (en) * | 2021-09-24 | 2021-11-09 | 长春工业大学 | Preparation method of aminated bagasse/graphene composite aerogel and application of aminated bagasse/graphene composite aerogel in wastewater treatment |
| CN113648974A (en) * | 2021-09-29 | 2021-11-16 | 长春工业大学 | Preparation of magnetic charcoal adsorbent |
| CN115178224A (en) * | 2022-05-06 | 2022-10-14 | 河南工程学院 | Nitrogen-doped hydrothermal carbon/graphene composite membrane and preparation method and application thereof |
| CN115518615A (en) * | 2022-09-11 | 2022-12-27 | 新疆农业大学 | Graphene aerogel prepared by taking Gansu pedicularis as biomass and application thereof |
| CN116272887A (en) * | 2023-03-17 | 2023-06-23 | 长春工业大学 | Preparation method of corn stalk/graphene oxide composite material adsorbent |
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