CN111482159A - Preparation method of porous carbon-loaded analcite composite material - Google Patents

Preparation method of porous carbon-loaded analcite composite material Download PDF

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CN111482159A
CN111482159A CN202010311311.5A CN202010311311A CN111482159A CN 111482159 A CN111482159 A CN 111482159A CN 202010311311 A CN202010311311 A CN 202010311311A CN 111482159 A CN111482159 A CN 111482159A
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coal
solid waste
based solid
analcime
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CN111482159B (en
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刘泽
金宇玄
韩乐
李丽
王栋民
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China University of Mining and Technology Beijing CUMTB
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character

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Abstract

The invention provides a preparation method of a porous carbon-loaded analcime composite material, which comprises the following steps: and mixing a silicon source, a sodium hydroxide solution and coal-based solid waste, and carrying out hydrothermal reaction to obtain the porous carbon supported analcime composite material. According to the invention, aluminosilicate components in the coal-based solid waste are directly converted into the analcime by using a hydrothermal method, and carbon components in the coal-based solid waste are loaded on the surface of the analcime, so that the adsorption performance of the composite material is improved. And the recycling of the coal-based solid waste can be realized without the processes of calcining, acid leaching and the like by controlling the pressure and time of the hydrothermal reaction. The results of the examples show that the preparation method provided by the invention can be used for obtaining the porous carbon supported analcime composite material only requiring 1-8 hours of hydrothermal reaction time.

Description

Preparation method of porous carbon-loaded analcite composite material
Technical Field
The invention relates to the technical field of industrial solid waste recycling treatment, in particular to a preparation method of a porous carbon-loaded analcite composite material.
Background
China is a big coal producing country, coal is used as a basic fuel for power production, and with the rapid development of the power industry, the mining amount and the using amount of the coal are increased, so that solid wastes generated in the coal mining and coal washing processes and discharged by combustion are increased year by year. And a large amount of solid wastes which are not reasonably utilized not only cause serious land resource waste, destroy the ecological environment, but also pollute the air. Therefore, the search for further utilization of coal-based solid waste is a problem to be solved urgently by researchers.
The analcime has strong stability, and has a pore diameter of only 2.6A, but has heavy metal ions such as Cu2+、Pb2+、Zn2+、Ag+、Fe2+And the adsorption effect is obvious, and the method can be used for treating industrial wastewater. Although the prior art discloses a hydrothermal method for preparing analcime, for example, patent CN106745027A discloses a method for synthesizing analcime from fly ash, in which the fly ash is ground and calcined at 550-850 ℃, and then soaked in a hydrochloric acid solution, and then subjected to hydrothermal reaction for 10-24 hours. However, when the above patent uses a hydrothermal method to prepare analcite, the reaction time is long, and the analcite can be obtained only by roasting, acid leaching and other processes.
Disclosure of Invention
The invention aims to provide a preparation method of a porous carbon supported analcime composite material, which has short reaction time and does not need roasting, acid leaching and other processes.
In order to achieve the above object, the present invention provides the following technical solutions:
a preparation method of a porous carbon-supported analcime composite material comprises the following steps:
mixing a silicon source, a sodium hydroxide solution and coal-based solid waste, and carrying out hydrothermal reaction to obtain a porous carbon supported analcime composite material;
the pressure of the hydrothermal reaction is 0.5-2.0 MPa, and the time of the hydrothermal reaction is 1-8 hours.
Preferably, the silicon source comprises silica fume or a sodium silicate solution.
Preferably, the coal-series solid waste comprises, by mass percent,comprises the following components: SiO 22:45～60％，Al2O3:25～35％，Fe2O3:0～10％，CaO:0～5％，K2O:0～5％，TiO 20 to 2%, 8 to 30% loss on ignition, and 1 to 3% others.
Preferably, the sodium hydroxide solution is mixed with Na2O as Al in coal-based solid waste2O3The mass ratio of the sodium hydroxide solution to the coal-based solid waste is (8-12): 1.
Preferably, the silicon source is SiO2Measurement of Al in coal-based solid waste2O3The amount ratio of the substance(s) is (3.5-4.5): 1.
Preferably, the granularity of the coal-based solid waste is 100-200 meshes.
Preferably, the hydrothermal reaction further comprises filtering, washing and drying the product of the hydrothermal reaction.
Preferably, the washing is: and washing the hydrothermal reaction product with water until the pH value of the washing liquid is 7-8.
Preferably, the drying temperature is 60-100 ℃, and the drying time is 6-12 hours.
The invention provides a preparation method of a porous carbon-loaded analcime composite material, which comprises the following steps: and mixing a silicon source, a sodium hydroxide solution and coal-based solid waste, and carrying out hydrothermal reaction to obtain the porous carbon supported analcime composite material. According to the invention, aluminosilicate components in the coal-based solid waste are directly converted into the analcime by using a hydrothermal method, and carbon components in the coal-based solid waste are loaded on the surface of the analcime, so that the adsorption performance of the composite material is improved. And the recycling of the coal-based solid waste can be realized without the processes of calcining, acid leaching and the like by controlling the pressure and time of the hydrothermal reaction. The results of the examples show that the preparation method provided by the invention can be used for obtaining the porous carbon supported analcime composite material only requiring 1-8 hours of hydrothermal reaction time.
In addition, the analcime in the porous carbon-supported analcime composite material prepared by the invention shows a tetragonal trioctahedral shape, and the degree of crystallization of the analcime isHigh purity, uniform granularity (20-25 microns), and high Pb content2+The adsorption capacity of (A) was 451 mg/g.
Drawings
FIG. 1 is an XRD pattern of a porous carbon-supported analcime composite prepared according to example 1 of the present invention;
FIG. 2 is an SEM image of a porous carbon-supported analcime composite prepared according to example 1 of the present invention;
FIG. 3 is an SEM image of a porous carbon-supported analcime composite prepared according to example 1 of the present invention;
FIG. 4 is an EDS diagram of a porous carbon-supported analcime composite prepared according to example 1 of the present invention;
FIG. 5 is an adsorption curve of the porous carbon-supported analcime composite prepared in example 1 of the present invention;
fig. 6 is an adsorption curve of analcite prepared from a conventional calcined coal-based solid waste.
Detailed Description
The invention provides a preparation method of a porous carbon-loaded analcime composite material, which comprises the following steps:
mixing a silicon source, a sodium hydroxide solution and coal-based solid waste, and carrying out hydrothermal reaction to obtain a porous carbon supported analcime composite material;
the pressure of the hydrothermal reaction is 0.5-2.0 MPa, and the time of the hydrothermal reaction is 1-8 hours.
According to the invention, a silicon source, a sodium hydroxide solution and coal-series solid waste are mixed to obtain a mixture. In the present invention, the silicon source preferably comprises silica fume or a sodium silicate solution, more preferably a sodium silicate solution. The preparation method of the sodium silicate solution is not particularly limited in the present invention, and the sodium silicate solution can be prepared by a preparation method known to those skilled in the art.
In the invention, the silicon source is SiO2Measurement of Al in coal-based solid waste2O3The ratio of the amounts of the substances (1) to (3.5) is preferably (3.5 to 4.5), and more preferably (4 to 4.5). In the present invention, the amount of the silicon source is preferably controlled within the above range, which is advantageous for the formation of analcite having high crystallinity and for shortening the hydrothermal reaction time.
In the invention, the sodium hydroxide solution is mixed with Na2O as Al in coal-based solid waste2O3The ratio of the amounts of the substances (1) to (0.75) is preferably 1. In the invention, the mass ratio of the sodium hydroxide solution to the coal-based solid waste is preferably (8-12): 1, and more preferably (10-12): 1. In the present invention, the concentration and amount of the sodium hydroxide solution are preferably controlled within the above-mentioned ranges, which is advantageous for the formation of analcite having high crystallinity and for shortening the hydrothermal reaction time. When Na is contained in sodium hydroxide solution2O and Al in coal-based solid waste2O3When the mass ratio of the sodium hydroxide solution to the coal-based solid waste is less than 0.75:1 and the mass ratio of the sodium hydroxide solution to the coal-based solid waste is less than 8:1, the mixture of the analcime and the NaP zeolite with low crystallization degree is obtained by the hydrothermal reaction, the NaP zeolite is an intermediate for synthesizing the analcime from the coal-based solid waste, the reaction time needs to be prolonged for converting the intermediate into the analcime, and the concentration and the dosage of the sodium hydroxide solution are too high, so that unnecessary waste is caused.
The preparation method of the sodium hydroxide solution is not particularly limited in the present invention, and the sodium hydroxide solution may be prepared by a preparation method known to those skilled in the art.
The present invention is not particularly limited in the kind of the coal-based solid waste, and the coal-based solid waste known to those skilled in the art may be used.
In the invention, the coal-based solid waste comprises the following components in percentage by mass: SiO 22:45～60％，Al2O3:25～35％，Fe2O3:0～10％，CaO:0～5％，K2O:0～5％，TiO 20 to 2%, 8 to 30% loss on ignition, and 1 to 3% others. The invention preferably uses coal-based solid waste with the content of each component within the range, which is beneficial to synthesizing analcime with high crystallinity, avoids the generation of NaP zeolite and further shortens the time of hydrothermal reaction.
In the invention, the granularity of the coal-based solid waste is preferably 100-200 meshes. In the present invention, when the particle size of the coal-based solid waste does not meet the above-mentioned conditions, it is preferable that the coal-based solid waste is pulverized and then ground. The crushing and grinding method of the coal-based solid waste is not particularly limited, and the crushing and grinding method well known to those skilled in the art can be adopted. The invention preferably controls the particle size of the coal-based solid waste within the range, which is beneficial to accelerating the hydrothermal reaction process and shortening the reaction time.
The operation of mixing the silicon source, the sodium hydroxide solution and the coal-based solid waste is not particularly limited in the present invention, and a mixing technical scheme well known to those skilled in the art may be adopted. In the present invention, the mixing of the silicon source, the sodium hydroxide solution and the coal-based solid waste is preferably stirring. In the present invention, the rotation speed of the stirring is preferably 300 to 600rpm, more preferably 350 to 550rpm, and most preferably 400 to 500 rpm. In the invention, the stirring time is preferably 20-30 min, and more preferably 25-30 min. In the present invention, the stirring device is preferably a magnetic stirrer.
After the mixture is obtained, hydrothermal reaction is carried out to prepare the porous carbon supported analcime composite material. The apparatus for the hydrothermal reaction is not particularly limited in the present invention, and apparatuses known to those skilled in the art and usable for the hydrothermal reaction may be used. In the present invention, the hydrothermal reaction apparatus is preferably a saturated steam autoclave.
In the present invention, the pressure of the hydrothermal reaction is preferably 0.5 to 2.0MPa, more preferably 0.75 to 2MPa, and most preferably 1 to 2 MPa. The pressure of the hydrothermal reaction is preferably controlled within the range, so that the method is favorable for generating the analcime with high crystallinity, avoids the coal-based solid waste from being converted into the intermediate NaP zeolite to appear in a reaction product, and further accelerates the reaction process.
In the present invention, the time of the hydrothermal reaction is preferably 1 to 8 hours, and more preferably 2 to 6 hours.
After the hydrothermal reaction is finished, the product of the hydrothermal reaction is preferably filtered, washed and dried to obtain the porous carbon supported analcime composite material. The operation of filtering, washing and drying is not particularly limited in the present invention, and the technical scheme of filtering, washing and drying known to those skilled in the art can be adopted. In the present invention, the filtration is preferably suction filtration. In the invention, the washing is preferably carried out by washing the hydrothermal reaction product with water until the pH of the washing solution is 7-8. In the invention, the drying temperature is preferably 60-100 ℃, and more preferably 65-80 ℃. In the invention, the drying time is preferably 6-12 hours, and more preferably 6-8 hours.
The analcime in the porous carbon loaded analcime composite material prepared by the preparation method provided by the invention shows a tetragonal trioctahedral shape, and has the advantages of high crystallization degree, high purity, uniform granularity of about 20-25 mu m, and Pb-supported analcime composite material2+The adsorption capacity of (A) was 451 mg/g.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
5g of coal-derived solid waste (containing SiO)2:53.9wt％，Al2O3:25.7wt％，Fe2O3:4.31wt％，K2O:1.91wt％，TiO21.23 wt%, loss on ignition 11.75 wt%, and the other 1.2 wt%) were pulverized to 200 mesh, and Na was added to the sodium hydroxide solution2O as Al in coal-based solid waste2O3The amount of the substance(s) in (b) was 0.75:1 to prepare a sodium hydroxide solution. Adding the prepared sodium hydroxide solution into the coal-based solid waste according to the mass ratio of the prepared sodium hydroxide solution to the coal-based solid waste of 10:1 (namely the dosage of the sodium hydroxide solution is 50g), and then adding the sodium hydroxide solution into the coal-based solid waste according to the SiO in the sodium silicate solution2Al in coal-based solid waste2O3The amount of substance(s) was added to the sodium silicate solution in a ratio of 4:1 to obtain a mixture. And (3) stirring the mixture in a magnetic stirrer at the rotating speed of 500rpm for 25min, transferring the mixture into a flask, placing the flask in a saturated steam autoclave, reacting for 3h under the saturated steam pressure of 1MPa, and naturally cooling to the normal temperature. Carrying out suction filtration on the obtained product, then washing with water until the pH value of the washing liquid is 7, and finally drying in a 65 ℃ oven for 8h to obtain the porous carbon supported blockA zeolite composite material.
Fig. 1 is an XRD pattern of the porous carbon-supported analcime composite material prepared in example 1, and it can be seen from fig. 1 that the diffraction peak of analcime in the synthesized composite material is strong and there is no hetero-peak, indicating that the synthesized analcime has a high degree of crystallization and a high purity.
Fig. 2 and 3 are SEM images of the porous carbon-supported analcime composite prepared in example 1, wherein fig. 3 is an enlarged view of fig. 2, and it can be seen from fig. 2 and 3 that the composite has a uniform particle size of about 20 to 25 μm, analcime exhibits a tetragonal trioctahedral shape, and the degree of crystallinity is high.
FIG. 4 is an EDS diagram of a porous carbon-supported analcime composite material prepared in example 1, which is obtained by EDS elemental analysis of at least ten micro-domains selected from FIG. 3, and it can be seen from FIG. 4 that the composite material contains 13.28% of carbon atoms, the ratio of Na, Al and Si elements is 1:1:2, and the chemical formula of analcime Na (AlSi)2O6)·H2O is consistent, and it can be determined that the synthesized analcite is analcite.
Adsorption Performance test
Firstly, 500 mg/L of Pb-containing material is prepared2+Then 250m of L solution was put in a 500m L container, 0.25g of the composite material prepared in example 1 was added, the pH of the solution was adjusted to 3, the container was placed in a 30 ℃ water bath and stirred at a speed of 200r/min, and after 120min, the composite material was measured for Pb vs2+The adsorption capacity of (A) was 486 mg/g.
Example 2
By adopting the same raw materials and preparation method as in example 1, the pressure of the hydrothermal reaction is replaced by 2MPa, the corresponding temperature is 212 ℃, and the porous carbon-supported analcite composite material is obtained after 1h of reaction.
Example 3
By adopting the same raw materials and preparation method in the embodiment 1, the pressure of the hydrothermal reaction is replaced by 1.5MPa, the corresponding temperature is 200 ℃, and the porous carbon supported analcime composite material is obtained after 2h reaction.
Example 4
The same raw materials and preparation method as in example 1 are adopted, the pressure of the hydrothermal reaction is changed to 0.75MPa, the corresponding temperature is 168 ℃, and the porous carbon supported analcime composite material is obtained after 4h reaction.
Example 5
By adopting the same raw materials and preparation method in the embodiment 1, the pressure of the hydrothermal reaction is replaced by 0.5MPa, the corresponding temperature is 150 ℃, and the porous carbon supported analcime composite material is obtained after 8 hours of reaction.
Comparative example 1
The same raw materials and preparation method as in example 5 were used, and the composite material containing analcime, quartz and NaP zeolite was obtained after 6 hours of reaction. And the same adsorption performance test method as that of example 5 is adopted to test the Pb pair of the composite material2+The adsorption capacity of (A) was 365 mg/g.
Example 6
The same raw materials and preparation method as in example 1 were used, and the sodium hydroxide solution was replaced with Na2O as Al in coal-based solid waste2O3The mass ratio of the (A) to (B) is 1:1, and the porous carbon supported analcime composite material is obtained after 3 hours of reaction.
Comparative example 2
The same raw materials and preparation method as in example 6 were used, and the sodium hydroxide solution was replaced with Na2O as Al in coal-based solid waste2O3The mass ratio of (A) to (B) is 0.5:1, and the composite material obtained after 3h reaction contains analcime, quartz and NaP zeolite. And the same adsorption performance test method as that of example 6 is adopted to test the Pb pair of the composite material2+The adsorption capacity of (A) was 336 mg/g.
Example 7
By adopting the same raw materials and preparation method as in example 1, the mass ratio of the sodium hydroxide solution to the coal-based solid waste is replaced by 12:1, and the porous carbon-supported analcite composite material is obtained after 3h reaction.
Example 8
By adopting the same raw materials and preparation method as in example 1, the mass ratio of the sodium hydroxide solution to the coal-based solid waste is replaced by 8:1, and the porous carbon-supported analcite composite material is obtained after 3h reaction.
Example 9
The same materials and preparation methods as in example 1 were used to prepare SiO in the silicon source2Al in coal-based solid waste2O3The mass ratio of the substances is replaced by 3.5:1, and the porous carbon supported analcime composite material is obtained after 3 hours of reaction.
Example 10
The same materials and preparation methods as in example 1 were used to prepare SiO in the silicon source2Al in coal-based solid waste2O3The mass ratio of the substances is replaced by 4.5:1, and the porous carbon supported analcime composite material is obtained after 3 hours of reaction.
TABLE 1 Experimental parameters and adsorption Properties for examples 1-10 and comparative examples 1-2
Figure BDA0002457693620000071
Figure BDA0002457693620000081
Note: n (Na)2O) represents Na in sodium hydroxide solution2Amount of substance of O, n (SiO)2) Indicating SiO in the silicon source2Amount of substance(s), n (Al)2O3) Representing Al in coal-based solid wastes2O3The amount of substance(s) of (c).
Comparative example 3
First preparing Pb2+，Cr2+，Ni2+And Cu2+The heavy metal ion adsorption test method comprises the steps of (1) taking a heavy metal mixed solution with the concentration of 500 mg/L, then respectively placing 250m of L heavy metal mixed solution into 500m of L containers, adjusting the pH value of the solution to be 3, respectively adding 0.25g of the porous carbon-supported analcite composite material prepared in example 1 and analcite prepared by taking calcined coal-based solid waste as a raw material into the mixed solution, then placing the containers into a water bath kettle at the temperature of 30 ℃, stirring at the speed of 200r/min, and testing the adsorption performance of two materials with different adsorption times on heavy metal ions.
Fig. 5 and fig. 6 are adsorption curves of the two materials in the multi-ion mixed solution for 10min, 30min, 60min, 120min and 180 min. Can be used forIt is shown that the porous carbon-supported analcime composite material prepared by the invention has obviously improved adsorption capacity to heavy metal ions compared with analcime prepared by taking coal-based solid waste after carbon removal through calcination as a raw material. Wherein for Pb2+The adsorption capacity is improved by 20 percent, and the Cr content is improved2+The adsorption capacity is improved by 43 percent, and the Ni is absorbed2+The adsorption capacity is improved by 204 percent for Cu2+The adsorption capacity is improved by 406%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A preparation method of a porous carbon-supported analcime composite material comprises the following steps:
mixing a silicon source, a sodium hydroxide solution and coal-based solid waste, and carrying out hydrothermal reaction to obtain a porous carbon supported analcime composite material;
the pressure of the hydrothermal reaction is 0.5-2.0 MPa, and the time of the hydrothermal reaction is 1-8 hours.
2. The method of claim 1, wherein the silicon source comprises silica fume or a sodium silicate solution.
3. The preparation method of claim 1, wherein the coal-based solid waste comprises the following components in percentage by mass: SiO 22:45～60％，Al2O3:25～35％，Fe2O3:0～10％，CaO:0～5％，K2O:0～5％，TiO20 to 2%, 8 to 30% loss on ignition, and 1 to 3% others.
4. The method of claim 1, wherein the sodium hydroxide solution is prepared with Na2O as Al in coal-based solid waste2O3The ratio of the amount of the substance(s) is (0.75-1): 1, the hydrogen and oxygenThe mass ratio of the sodium sulfide solution to the coal-based solid waste is (8-12): 1.
5. The method of claim 1, wherein the silicon source is SiO2Measurement of Al in coal-based solid waste2O3The amount ratio of the substance(s) is (3.5-4.5): 1.
6. The preparation method according to claim 1, wherein the particle size of the coal-based solid waste is 100 to 200 mesh.
7. The method according to claim 1, wherein the hydrothermal reaction is followed by filtering, washing and drying the product of the hydrothermal reaction.
8. The method of claim 7, wherein the washing is: and washing the hydrothermal reaction product with water until the pH value of the washing liquid is 7-8.
9. The method according to claim 7, wherein the drying temperature is 60 to 100 ℃ and the drying time is 6 to 12 hours.
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CN115818659A (en) * 2022-12-29 2023-03-21 武汉大学(肇庆)资源与环境技术研究院 Method for preparing analcite from silicon-aluminum tailings

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