CN113908806B - Graphene/inorganic polymer composite adsorption material, preparation method and application thereof - Google Patents
Graphene/inorganic polymer composite adsorption material, preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a graphene/inorganic polymer composite adsorption material, a preparation method and application thereof, wherein the adsorption material is complete in spherical shape, the particle size distribution is 50-2000 mu m, the phase is mainly amorphous, and the adsorption characteristic is better. The preparation method comprises the steps of preparing an alkali excitation solution, preparing an ultrasonic-assisted graphene/alkali excitation solution, preparing graphene/inorganic polymer slurry, spheroidizing an adsorption material and removing alkali from the spherical adsorption material. According to the method, graphene is dispersed in alkali-activated inorganic polymer slurry by utilizing the reaction characteristic of solid waste powder and the assistance of ultrasonic, and the graphene/inorganic polymer composite spherical adsorbing material is obtained by the mode of assisting mechanical stirring by using an organic solvent, so that the adsorption performance of the spherical adsorbing material is improved, the recycling of typical industrial solid waste is realized, and the high-efficiency treatment of industrial wastewater is realized.
Description
Technical Field
The invention relates to a preparation method of a graphene/inorganic polymer composite spherical adsorbing material, in particular to a method for improving the adsorption efficiency of the inorganic polymer spherical adsorbing material by introducing a graphene nano material under the assistance of ultrasonic waves, and realizing a low-temperature spheroidization process and controlling the spherical particle size of the adsorbing material.
The prepared graphene/inorganic polymer composite spherical adsorbing material belongs to the technical field of green preparation of graphene/inorganic composite adsorbing materials.
Background
While the rapid development of industrial technology, certain industrial solid waste is generated, and in addition, a large amount of toxic and harmful waste water is generated, so that the environment is polluted and the health is harmed. The common wastewater treatment methods comprise various modes such as chemistry, flocculation and the like, but industrial wastewater contains a large amount of toxic and harmful heavy metals and the like, is harmful to the environment and is difficult to treat. The adsorption method is a simple and efficient mode for treating toxic and harmful wastewater, and the principle of the adsorption method is that the adsorption reaction can occur when the adsorption agent is mixed with wastewater by utilizing the characteristic of large specific surface area of the adsorbent so as to achieve the aim of cleaning water. Industrially, carbon nanotubes, activated carbon, ion exchange resins, and the like are mainly used as adsorbents. Wherein, the carbon material has the characteristics of high specific surface area, porous structure, simple and convenient production and the like, and has wide market in the field of industrial wastewater treatment. However, the adsorption characteristics are different from the materials and the quality, so that the development of the efficient adsorbent is still problematic. The graphene is composed of carbon atoms, in sp 2 The two-dimensional planar network structure which is formed by hybridization and arranged in a honeycomb shape. Due to the special two-dimensional structure, graphene also has a good adsorption property.
The inorganic polymer is a novel material which is usually prepared by taking materials such as fly ash, metakaolin, slag and the like as raw materials and reacting under the low-temperature curing condition, and has the advantages of simple process, wide raw material source, environmental protection, difficult generation of secondary pollution, good stability and mechanical property in aqueous solution and the like. In addition, it also has a unique three-dimensional pore structure and thus can be used as an adsorbent in wastewater treatment.
Therefore, the composite adsorbent is obtained by introducing the graphene into the inorganic polymer, and the introduction of the graphene greatly improves the adsorption efficiency, adsorption capacity and recycling performance of the traditional adsorbent, and shows huge commercial potential and application prospect.
Therefore, under the assistance of ultrasound, graphene is introduced into an inorganic polymer and solidified into spheres under the synergistic effect of mechanical stirring and an organic solvent, so that the preparation of the graphene/inorganic polymer composite spherical adsorbing material is realized, the graphene/inorganic polymer composite spherical adsorbing material with uniform spheres and controllable particle size is obtained, and the toxic and harmful wastes in industrial wastewater are quickly removed. The raw materials of the composite spherical adsorbing material are from industrial solid wastes, the source is wide, the balling process is realized in a low-temperature state for a short time, the operation is convenient, and the composite spherical adsorbing material is suitable for industrial production and deep sewage treatment.
Disclosure of Invention
The invention provides a novel process for dispersing graphene and subsequent spheroidization by ultrasonic assistance, aiming at the problems of difficult preparation of a graphene/inorganic polymer composite spherical adsorbing material and spheroidization of a composite material. By utilizing the reaction characteristic of typical solid waste fly ash and slag and the low-temperature preparation advantage of inorganic polymer slurry, graphene is directly introduced into the reaction process of the inorganic polymer under the assistance of ultrasound, and is pelletized and cured under the assistance of stirring action and an organic solvent, so that the preparation and the spherical control of the graphene/inorganic polymer composite spherical adsorption material are realized. Provides a preparation method of a graphene/inorganic polymer composite spherical adsorbing material, and aims to solve the problems in the background technology. The invention adopts the following technical scheme:
the invention provides a preparation method of a graphene/inorganic polymer composite spherical adsorbing material and a method thereof, and the preparation method is characterized by comprising the following steps: by utilizing the reaction characteristics of solid waste powder, graphene is dispersed in inorganic polymer slurry with the aid of ultrasonic assistance, and the graphene/inorganic polymer composite slurry is molded in an organic solvent assisted mechanical stirring manner to obtain a spherical adsorbing material, wherein the obtained graphene/inorganic polymer spherical adsorbing material has controllable particle size, complete sphere and particle size of 50-2000 micrometers, and is mainly amorphous in phase and adjustable in pore space, so that the graphene/inorganic polymer spherical adsorbing material is suitable for large-scale production.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a graphene/inorganic polymer composite spherical adsorption material comprises the following steps:
step one, preparing an alkali-activated solution: adding potassium hydroxide into 30-50% of silica gel solution according to a molar ratio (0.8-1.2) to (0.8-1.2), and stirring by using a magnetic stirrer to obtain an alkali-activated solution;
step two, preparing an ultrasonic-assisted graphene/alkali excitation solution: slowly adding graphene into the alkali-activated solution prepared in the first step, wherein the mass ratio of graphene to the alkali-activated solution is (1-30) to (80-90), stirring by magnetic force, and then performing ultrasonic-assisted oscillation treatment to uniformly disperse the flaky graphene in the alkali-activated solution to obtain a well-dispersed graphene/alkali-activated solution;
step three, preparing graphene/inorganic polymer slurry: mixing and grinding silicon-aluminum-containing solid waste powder, namely fly ash and slag, and mechanically stirring and mixing according to a certain mass ratio, wherein the mass ratio of the fly ash to the slag is (1-2): 1; and (3) adding the mixed powder into the graphene/alkali excitation solution obtained in the step two, wherein the mass ratio of the mixed powder to the graphene/alkali excitation solution is (3-6): (4-5) adding a certain mass of deionized water in the stirring process to adjust the viscosity, wherein the mass ratio of the deionized water to the alkali-activated solution obtained in the step (1) is (1-10): (4-5), mechanically stirring by using an electric stirrer to obtain graphene/inorganic polymer slurry;
step four, spheroidizing the adsorbing material: slowly dripping the graphene/inorganic polymer slurry obtained in the third step into a polyethylene glycol solution for multiple times under the high-temperature condition of 60-90 ℃ and with the aid of mechanical stirring, solidifying the graphene/inorganic polymer slurry obtained in the third step into a small spherical shape in organic liquid and with the aid of mechanical stirring, continuously stirring for 2-10min, taking out, placing in an oven at 60-80 ℃, drying and solidifying for 1-3 days, cleaning with deionized water and absolute ethyl alcohol, and continuously placing in the oven at 60-80 ℃, drying and solidifying for 3-14 days to obtain a graphene/inorganic polymer composite spherical adsorbing material blank;
step five, removing alkali from the spherical adsorbing material: and (3) placing the graphene/inorganic polymer composite spherical adsorbing material obtained in the fourth step into deionized water, dropwise adding a hydrochloric acid solution to neutralize redundant alkali, soaking for 5-14 days until the pH value reaches 7, taking out, washing for 1-3 times by using absolute ethyl alcohol, and then placing at 50-80 ℃ for drying for 0.5-2 days to obtain the graphene/inorganic polymer composite spherical adsorbing material.
In the first step, the stirring time of the magnetic stirrer is 20-240min.
In the second step, the thickness of the graphene sheet layer is 1-10 layers, and the size is 1-50 microns; the magnetic stirring time is 1-10 minutes, the ultrasonic-assisted oscillation treatment time is 10-100 minutes, and the ultrasonic-assisted oscillation power is 100-240W.
In the third step, the grinding particle size of the silicon-aluminum-containing solid waste powder is 1-10 μm, the mechanical stirring and mixing time after grinding is 1-10min, and the mechanical stirring time of the electric stirrer is 10-40min.
In the fourth step, the mass of the graphene/inorganic polymer slurry added each time is 1-30g, the mixture is stirred for 2-10min after each addition, the mixture is taken out after being solidified into small balls, the next graphene/inorganic polymer slurry is continuously added, and the solidification is repeated; polyethylene glycol is liquid, and has molecular weight of 400-600; the addition ratio of the graphene/inorganic polymer slurry to the polyethylene glycol is (2-3): 10.
a graphene/inorganic polymer composite spherical adsorbing material is prepared by the preparation method.
A graphene/inorganic polymer composite spherical adsorption material is used for adsorbing pollutants and heavy metal ions in the fields of metallurgical industry and organic chemical wastewater treatment.
Compared with the prior art, the invention has the advantages that: according to the invention, the graphene/inorganic polymer composite spherical adsorption material is obtained by ultrasonic-assisted dispersion and preparation, the nano functional material is uniformly dispersed in the inorganic polymer and compounded into spheres at low temperature, the special sheet structure of the graphene is utilized, the specific surface area is large, the mechanical property is good, the surface has rich functional groups, the dispersed graphene has excellent adsorption property, and the adsorption property is compounded in the inorganic polymer, so that the adsorption efficiency of the composite material is improved. The method uses industrial solid wastes such as fly ash, slag and the like to replace pure powder materials as raw materials, realizes the utilization of silicon-rich aluminum in the solid wastes, and has rich raw material sources and very low cost. In the spheroidization process, under the low-temperature condition and the action of an organic solvent, the composite slurry is spheroidized in a short time, due to the stability and the good heat transfer property of the organic solvent, the slurry can be solidified into micrometer-centimeter-level spherical particles in a short time, the organic solvent does not participate in the reaction of the graphene/inorganic polymer composite slurry, and the formation of an adsorption material product is not influenced, so that the spheroidization process with short time, short flow and high efficiency can be realized, and the preparation of the graphene/inorganic polymer composite spherical adsorption material is realized.
The graphene/inorganic polymer composite spherical adsorbing material obtained by the invention can be used for treating toxic and harmful components such as heavy metals and the like which are difficult to treat in sewage; the treatment process is simple, the addition amount is small, the treatment efficiency is high, the environment-friendly effect is achieved, the preparation is simple, and the method has wide application prospects in the fields of metallurgical industry and organic chemical wastewater treatment.
Drawings
Fig. 1 is an XRD chart of the graphene/inorganic polymer composite spherical adsorbing material obtained in example 1 of the present invention.
Fig. 2 is an SEM image of the graphene/inorganic polymer composite spherical adsorbent material obtained in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
According to the invention, the graphene flakes are introduced into the inorganic polymer slurry in an ultrasonic dispersion mode, and are pelletized under the assistance of an organic solvent, so that the graphene/inorganic polymer composite spherical adsorbing material is obtained. The preparation process comprises the following steps:
step one, preparing an alkali-activated solution: adding potassium hydroxide into a silica gel solution with the mass fraction of 40% according to a molar ratio of 1.
Step two, preparing an ultrasonic-assisted graphene/alkali excitation solution: slowly adding graphene into the alkali-activated solution prepared in the first step, wherein the thickness of graphene sheets is 5-10 layers, the size is about 5-50 micrometers, the mass ratio of graphene to the alkali-activated solution is 4.
Step three, preparing graphene/inorganic polymer slurry: grinding typical solid waste powder containing silicon and aluminum to the particle size of 5 mu m, and mechanically stirring and mixing for 3min according to a certain mass ratio, wherein the mass ratio of the fly ash to the slag is 1.5. And (2) adding the mixed powder into the graphene/alkali-activated solution obtained in the step (II), wherein the mass ratio of the mixed powder to the graphene/alkali-activated solution is 100.
Step four, spheroidizing the adsorbing material: slowly dripping the graphene/inorganic polymer slurry obtained in the third step into a polyethylene glycol (with the molecular weight of 400, liquid) solution for multiple times by using a medicine spoon under the high-temperature condition of 80 ℃ and with the assistance of mechanical stirring, fishing out 5g of composite slurry by using the medicine spoon each time, solidifying the composite slurry obtained in the third step into a small spherical shape in organic liquid and with the assistance of mechanical stirring, continuously stirring for 3min, taking out, placing in a 60 ℃ drying oven for drying and solidifying for 2 days, washing with deionized water and absolute ethyl alcohol, and continuously placing in the 60 ℃ drying oven for drying and solidifying for 3 days to obtain the graphene/inorganic polymer composite spherical blank adsorbing material.
Step five, removing alkali from the spherical adsorbing material: and (3) placing the graphene/inorganic polymer composite spherical adsorbing material obtained in the fourth step into deionized water, dropwise adding a hydrochloric acid solution to neutralize redundant alkali, soaking for 7 days until the pH value reaches 7, taking out, washing for 3 times by using absolute ethyl alcohol, and then placing in a 60 ℃ drying oven to dry for 1 day to obtain the graphene/inorganic polymer composite spherical adsorbing material.
Fig. 1 is a phase XRD spectrum of the graphene/inorganic polymer composite spherical adsorbing material obtained after the fifth step of example 1. As can be seen from the figure, the phase of the graphene/inorganic polymer composite spherical adsorbing material is mainly of an amorphous structure, and also has some mullite and other peaks, which are derived from the fly ash raw material.
FIG. 2 is an SEM photograph of a graphene/inorganic polymer composite spherical adsorbing material obtained in example 1; the figure shows that the composite spherical adsorbing material has complete sphere and good sphere forming, and micro-level and nano-level pores can be seen on the surface of the sphere, which are beneficial to the exertion of the adsorption effect.
The graphene/inorganic polymer composite spherical adsorbing material obtained by the embodiment has good adsorption performance and adjustable and controllable size, when the dosage of the spherical adsorbent is 4g/L, the adsorption capacity of the spherical adsorbent to 100mg/L lead ion solution reaches 25mg/g, and the removal rate reaches about 100%. When the dosage of the spherical adsorbent is 4g/L, the adsorption capacity of the spherical adsorbent to 100mg/L zinc ion solution reaches 15mg/g, and the removal rate reaches about 59 percent. When the dosage of the spherical adsorbent is 4g/L, the adsorption capacity of the spherical adsorbent to 100mg/L copper ion solution reaches 14mg/g, and the removal rate reaches about 56 percent.
Example 2
The difference from example 1 is that the mass ratio of graphene to alkali-activated solution in step two is 3.
According to the embodiment, the graphene/inorganic polymer composite spherical adsorbing material with a micron and nanometer pore structure can be obtained, when the dosage of the spherical adsorbent is 2g/L, the adsorption capacity of the spherical adsorbent to 100mg/L lead solution reaches 47mg/g, and the removal rate reaches about 93%.
Example 3
The difference from example 1 is that the mass ratio of graphene to alkali-activated solution in step two is 2.
The carbon nano tube reinforced inorganic polymer spherical adsorbent with a micron and nano pore structure can be obtained, when the dosage of the spherical adsorbent is 2g/L, the adsorption capacity of the spherical adsorbent to 100mg/L lead solution reaches 45mg/g, and the removal rate reaches about 91%.
By combining the data analysis, the method can successfully prepare the graphene/inorganic polymer composite spherical adsorbing material.
Claims (7)
1. A preparation method of a graphene/inorganic polymer composite adsorption material is characterized by comprising the following steps: the method comprises the following steps:
step one, preparing an alkali-activated solution: adding potassium hydroxide into 30-50% of silica gel solution according to a molar ratio of (0.8-1.2) to (0.8-1.2), and stirring by using a magnetic stirrer to obtain an alkali-activated solution;
step two, preparing an ultrasonic-assisted graphene/alkali excitation solution: slowly adding graphene into the alkali-activated solution prepared in the first step, wherein the mass ratio of graphene to the alkali-activated solution is (1-30) to (80-90), stirring by magnetic force, and then performing ultrasonic-assisted oscillation treatment to uniformly disperse the flaky graphene in the alkali-activated solution to obtain a well-dispersed graphene/alkali-activated solution; the thickness of the graphene sheet layer is 1-10 layers, and the size is 1-50 micrometers;
step three, preparing graphene/inorganic polymer slurry: mixing and grinding silicon-aluminum-containing solid waste powder, namely fly ash and slag, and mechanically stirring and mixing according to a certain mass ratio, wherein the mass ratio of the fly ash to the slag is (1-2): 1; and (3) adding the mixed powder into the graphene/alkali excitation solution obtained in the step two, wherein the mass ratio of the mixed powder to the graphene/alkali excitation solution is (3-6): (4-5) adding a certain mass of deionized water in the stirring process to adjust the viscosity, wherein the mass ratio of the deionized water to the alkali-activated solution obtained in the step (1) is (1-10): (4-5) mechanically stirring by using an electric stirrer to obtain graphene/inorganic polymer slurry; the grinding particle size of the silicon-aluminum-containing solid waste powder is 1-10 mu m;
step four, spheroidizing the adsorbing material: slowly dripping the graphene/inorganic polymer slurry obtained in the third step into a polyethylene glycol solution for multiple times under the high-temperature condition of 60-90 ℃ and with the aid of mechanical stirring, solidifying the graphene/inorganic polymer slurry obtained in the third step into a small spherical shape in organic liquid and with the aid of mechanical stirring, continuously stirring for 2-10min, taking out, placing in an oven at 60-80 ℃, drying and solidifying for 1-3 days, cleaning with deionized water and absolute ethyl alcohol, and continuously placing in the oven at 60-80 ℃, drying and solidifying for 3-14 days to obtain a graphene/inorganic polymer composite spherical adsorbing material blank;
step five, removing alkali from the spherical adsorbing material: and (3) placing the graphene/inorganic polymer composite spherical adsorbing material obtained in the fourth step into deionized water, dropwise adding a hydrochloric acid solution to neutralize redundant alkali, soaking for 5-14 days until the pH value reaches 7, taking out, washing for 1-3 times by using absolute ethyl alcohol, and then placing at 50-80 ℃ for drying for 0.5-2 days to obtain the graphene/inorganic polymer composite spherical adsorbing material.
2. The method for preparing the graphene/inorganic polymer composite adsorbing material according to claim 1, wherein in the first step, the stirring time of a magnetic stirrer is 20-240min.
3. The preparation method of the graphene/inorganic polymer composite adsorption material according to claim 1, wherein in the second step, the magnetic stirring time is 1-10 minutes, the ultrasonic-assisted oscillation treatment time is 10-100 minutes, and the power of the ultrasonic-assisted oscillation is 100-240W.
4. The method for preparing the graphene/inorganic polymer composite adsorbing material according to claim 1, wherein in the third step, the mechanical stirring and mixing time after grinding is 1-10min, and the mechanical stirring time of an electric stirrer is 10-40min.
5. The method for preparing the graphene/inorganic polymer composite adsorbing material according to claim 1, wherein in the fourth step, the mass of the graphene/inorganic polymer slurry added each time is 1-30g, the slurry is stirred for 2-10min after each addition, the slurry is taken out after being solidified into small balls, the graphene/inorganic polymer slurry is further added next time, and the solidification is repeated; polyethylene glycol is liquid, and has molecular weight of 400-600; the addition ratio of the graphene/inorganic polymer slurry to the polyethylene glycol is (2-3): 10.
6. a graphene/inorganic polymer composite adsorption material, which is prepared by the preparation method of any one of claims 1 to 5.
7. The application of the graphene/inorganic polymer composite adsorbing material prepared by the preparation method of any one of claims 1 to 5 is characterized in that the graphene/inorganic polymer composite adsorbing material is used for adsorbing pollutants and heavy metal ions in the fields of metallurgical industry and organic chemical wastewater treatment.
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