CN114849643A - Coal gangue-based porous material taking actinomycetes as template and preparation method thereof - Google Patents
Coal gangue-based porous material taking actinomycetes as template and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a coal gangue-based porous material taking actinomycetes as a template and a preparation method thereof, and the method comprises the following specific steps: preparing actinomycete liquid with the mass concentration of 1 g/L-1.2 g/L; pretreating coal gangue to obtain a silicon-aluminum source precursor solution, adding a silicon source and/or an aluminum source to adjust the silicon-aluminum ratio in the silicon-aluminum source precursor solution, and preparing n (silicon source): n (aluminum source): n (deionized water) ═ 2-20: 1:3000 of synthetic mother liquor; the method solves the problem that the prior microbial template agent which is more applied has limited guiding and supporting functions on the porous material pore channel structure, has simpler process of obtaining and culturing the microbial template agent, effectively shortens the preparation period of the material, and improves the production efficiency.
Description
Technical Field
The invention belongs to the field of porous materials, and particularly relates to a coal gangue-based porous material taking actinomycetes as a template and a preparation method thereof.
Background
Coal gangue is one of the largest large solid wastes discharged in the world at present. Utilizes the main component S1O in coal gangue 2 、Al 2 O 3 The porous silicon-aluminum adsorption material with high added value prepared by using the porous silicon-aluminum adsorption material as a silicon source and an aluminum source can achieve the purpose of treating wastes with processes of wastes against one another.
However, CaCO is generally used in the preparation of porous materials 3 The hard template agents and the soft template agents such as TEAOH surface active substances have certain limitations. The hard template agent reduces the orderliness of the pore structure of the molecular sieve, has higher cost and limits the large-scale production of the molecular sieve. Although the soft template agent can effectively realize the regulation and control of the molecular sieve pore passage, the environmental pollution is caused by the large amount of use and discharge of the organic reagent in the production, and the concept of 'green synthesis' is violated. The self-assembly and space confinement effect of the microorganisms can replace the traditional template agent, and the characteristics of reproducibility, easy removal and zero emission can also realize the sustainable development of the preparation of the molecular sieve.
The microbial templates for preparing the porous materials disclosed at present comprise staphylococcus albus, yeast DNA, escherichia coli flagella and the like, but the microbial templates have limited structure guiding and pore supporting effects on the porous materials, a certain amount of organic amine template agent still needs to be added, and extraction of microbial active macromolecules and microbial structures in the preparation process is troublesome.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a coal gangue-based porous material taking actinomycetes as a template and a preparation method thereof, which are used for solving the problem that the guide and support effects of a microbial template agent which is frequently applied to the pore structure of the porous material are limited, and the process of obtaining and culturing the microbial template agent is simpler, so that the preparation period of the material is effectively shortened, and the production efficiency is improved.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a coal gangue-based porous material taking actinomycetes as a template comprises the following specific steps:
s1, preparing actinomycete liquid with the mass concentration of 1 g/L-1.2 g/L;
s2, pretreating coal gangue to obtain a silicon-aluminum source precursor solution, and adding a silicon source and/or an aluminum source to adjust the silicon-aluminum ratio in the silicon-aluminum source precursor solution to obtain n (silicon source): n (aluminum source): n (deionized water) ═ 2-20: 1:3000 of synthetic mother liquor;
s3, mixing the actinomycete liquid with the synthetic mother liquid to obtain a mixed liquid, adjusting the pH value of the mixed liquid, and crystallizing, washing, drying and calcining the mixed liquid to obtain the porous material.
Further, in step S2, the preprocessing specifically includes:
s2.1, calcining the coal gangue powder with the particle size of 240-300 meshes at 800-880 ℃ for 3-8 h to obtain a first precursor;
s2.2, mixing the first precursor with 1.8-2 mol/L HCl solution, stirring for 2-3 h at 70-80 ℃, washing, filtering and drying to obtain a second precursor,
s2.3 reacting the second precursor with Na 2 CO 3 Mixing and calcining for 1-1.8 h at 780-880 ℃, dissolving the calcined product in deionized water according to the solid-to-liquid ratio of 1:4, stirring for 1-1.8 h, and filtering out coal gangue powder to obtain the silicon-aluminum source precursor solution.
Furthermore, in step S3, the volume ratio of the actinomycete liquid to the synthetic mother liquid is 1 (4-6).
Further, in step S3, the pH value of the mixed solution is adjusted to 9.8-10.8 by using 3-6 mol/L HCl solution, and then the mixed solution is stirred for 1 hour.
Further, in step S3, the mixed solution is placed in a hydrothermal crystallization kettle with a teflon liner, and the hydrothermal crystallization kettle is placed in an oven for crystallization.
Further, in step S3, the crystallization temperature is 160 ℃ to 180 ℃, and the crystallization time is 18h to 28 h.
Further, in step S3, the calcination is performed by heating to 180-200 ℃ at a heating rate of 1 ℃/m1n for 1-1.8 h.
Further, in step S2, the silicon source is tetraethoxysilane or silica sol, and the aluminum source is sodium metaaluminate or sodium aluminate.
The invention also provides a coal gangue-based porous material taking actinomycetes as a template, and the preparation method is adopted.
Furthermore, the particle size of the coal gangue-based porous material is 2.8-3.8 μm, and the pore size is 0.7-0.9 μm.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a method for preparing a coal gangue-based porous material by taking actinomycetes as a template, which takes actinomycetes mycelium as a microbial template, wherein nutrient mycelium has certain support property on a pore structure of the porous material, and the natural morphological structure of the actinomycetes mycelium and functional groups such as hydroxyl, amino and the like attached to the surface of the natural morphological structure of the actinomycetes mycelium can effectively adsorb silicon-aluminum ions in silicon-aluminum precursor liquid, so that the formation of the pore structure of the porous material has higher guidance property, and the coal gangue-based porous material can be efficiently prepared by utilizing the natural morphological structure of the actinomycetes mycelium.
The invention adopts actinomycete mycelium as template agent, and does not need additional chemical guiding agent or template agent. On one hand, the preparation cost of the porous material is reduced, and on the other hand, green synthesis is realized to a certain extent, namely, longer environmental and economic benefits are generated.
The invention adopts actinomycete mycelium as template agent, and the preparation effect is superior to rod-shaped and spherical microbial template agent. The method is characterized in that a bacterial liquid with the mass concentration of 1-1.2 g/L and a silicon-aluminum precursor liquid are mixed according to the volume ratio of 1: 4-1: 6, a coal gangue-based porous material with the best crystallization effect and the best adsorption performance can be obtained, and the process of culturing and extracting the actinomycete mycelium is simple to other microbial tissues and biomacromolecule structures.
The invention adopts actinomycete mycelium as template agent, which has no aerial mycelium and no spore, and the nutritious mycelium can be broken into V-shaped or Y-shaped body with diameter smaller than 1 micron.
Drawings
FIG. 1 is a scanning electron microscope image of a gangue-based porous material using actinomycete mycelium as a template agent.
FIG. 2 is an adsorption contrast diagram of the porous material and the raw coal gangue to the rhodamine B solution in example 1 of the present invention.
FIG. 3 is an adsorption contrast diagram of the porous material and the raw coal gangue to the rhodamine B solution in example 2 of the present invention.
FIG. 4 is an adsorption contrast diagram of the porous material and the raw coal gangue to the rhodamine B solution in example 3 of the present invention.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
The invention provides a preparation method of a coal gangue-based porous material taking actinomycetes as a template, which comprises the following specific steps:
(1) culturing the actinomycete strain for 24 hours, centrifuging at the rotating speed of 4000r/m1n for 8m1m to separate bacteria, preparing actinomycete liquid with the mass concentration of 1-1.2 g/L, and ultrasonically oscillating for 10m1n for later use.
(2) Crushing and grinding the coal gangue to prepare coal gangue powder with the granularity of 240-300 meshes;
(3) calcining the coal gangue powder in a tubular furnace at 800-880 ℃ for 3-8 h, and taking out after natural cooling;
(4) mixing the calcined coal gangue powder with 1.8-2 mol/L HCl solution according to the solid-to-liquid ratio of 1 (2-3), stirring for 2-3 h at 70-80 ℃, washing, filtering and drying the coal gangue powder;
(8) mixing the acid-leached coal gangue powder with Na 2 CO 3 Mixing and mixing the raw materials according to a mass ratio of 1 (0.8-1.2), calcining the mixture in a tubular furnace at the temperature of 780-880 ℃ for 1-1.8 h, dissolving the calcined product in deionized water according to a solid-to-liquid ratio of 1:4, stirring the mixture for 1-1.8 h, and filtering coal gangue powder to obtain a silica-alumina source precursor solution;
(6) and (3) adding a silicon source and/or an aluminum source to adjust the silicon-aluminum ratio in the silicon-aluminum source precursor solution to prepare n (silicon source): n (aluminum source): mixing the actinomycete liquid obtained in the step (1) with the mixed mother liquor according to the volume ratio of 1 (4-6), adjusting the pH value of the mixed mother liquor to 9.8-10.8 by using 3-6 mol/L HCl solution, and stirring for 1 h;
(7) and (3) transferring the mother solution to a hydrothermal crystallization kettle with a polytetrafluoroethylene lining, placing the hydrothermal crystallization kettle in an oven at 160-180 ℃, wherein the crystallization time is 18-28 h, taking out the hydrothermal crystallization kettle after crystallization is finished and natural cooling, washing, drying, heating to 180-200 ℃ at the heating rate of 1 ℃/m1n, and calcining for 1-1.8 h to carbonize and gasify the mycelia of the actinomycetes, thereby obtaining the porous material.
Preferably, in the step (6), the silicon source is tetraethoxysilane or silica sol, and the aluminum source is sodium metaaluminate or sodium aluminate.
FIG. 1 is a scanning electron microscope image of a gangue-based porous material with actinomycete mycelium as a template agent, and shows that the crystals of the porous material are regularly spherical and have uniform sizes, the particle size is 2.8-3.8 mu m, the pore diameter is 0.7-0.9 mu m, and the actinomycete mycelium structure provides uniform pore channels for the porous material, so that the porous material has good adsorption capacity, and the problems of environmental pollution and the like caused by the large use of organic template agents in the traditional process are solved.
Example 1
The embodiment discloses a preparation method of a coal gangue-based porous material by taking actinomycetes as a template, which specifically comprises the following steps:
culturing actinomycete strains for 24h, centrifuging at the rotating speed of 4000r/m1n for 8m1n to separate bacteria, preparing 10mL actinomycete liquid with the mass concentration of 1g/L, and ultrasonically oscillating for 10m1n for later use.
18g of coal gangue is crushed, ground and sieved to obtain 240-mesh coal gangue powder. Putting the coal gangue powder into a tubular furnace, heating to 800 ℃ within 2h, calcining for 3h, and naturally cooling. Mixing the cooled coal gangue powder with 1.8mol/L HCl solution according to the mass ratio of 1:3, stirring for 2h at 70 ℃, filtering the coal gangue powder, washing with deionized water and absolute ethyl alcohol for three times, and drying for 1.8h at 78 ℃. Mixing the dried coal gangue powder with Na 2 CO 3 Mixing the components according to the mass ratio of 1:0.8, placing the mixture in a tubular furnace for 1h, heating the mixture to 780 ℃ and calcining the mixture for 1h, dissolving the calcined product in 60ml of deionized water, stirring the mixture for 1h, and filtering coal gangue powder to obtain the silicon-aluminum source precursor solution. With the addition of a certain amount of biasSodium aluminate solution to n (silicon source): n (aluminum source): n (deionized water) ═ 2:1: 3000.
10ml of actinomycete liquid prepared in the previous stage is mixed with 40ml of synthetic mother liquor, the pH value of the mother liquor is adjusted to 9.8 by using 3mol/L HCl solution, and the mixture is stirred for 1 hour. And transferring the mother liquor to a hydrothermal crystallization kettle with a polytetrafluoroethylene lining and a specification of 100ml, placing the hydrothermal crystallization kettle in an oven for crystallization at 160 ℃ for 18h, naturally cooling the crystallization kettle, taking out the crystallization kettle, washing the crystallization kettle for 3 times respectively by using deionized water and absolute ethyl alcohol, drying the crystallization kettle, heating the crystallization kettle to 180 ℃ at a heating rate of 1 ℃/m1n, and calcining the gasification actinomycete mycelium for 1h to obtain the coal gangue-based porous material.
The crystal grains of the porous material are in a spherical structure, the granularity is 2.8-3 mu m, and the aperture diameter is 700 nm. Specific surface area 268.84m 2 ·g -1 Total pore volume 0.139cm 3 ·g -1 . As shown in FIG. 2, at room temperature, the adsorption rate of 28mg of the porous material to 20mg/L rhodamine B solution is as shown in FIG. 2, namely the removal rate of 78m1n reaches 89.8 percent, which is improved by about 30 percent compared with the removal rate of raw coal gangue;
example 2
The embodiment discloses a preparation method of a coal gangue-based porous material by taking actinomycetes as a template, which specifically comprises the following steps:
culturing actinomycete strains for 24h, centrifuging at the rotating speed of 4000r/m1n for 8m1n to separate bacteria, preparing 12mL actinomycete liquid with the mass concentration of 1.1g/L, and ultrasonically oscillating for 10m1n for later use.
Crushing and grinding 18g of coal gangue, and screening to obtain 300-mesh coal gangue powder. And (3) putting the coal gangue powder into a tubular furnace, heating to 830 ℃ within 2h, calcining for 4h, and naturally cooling. Mixing the cooled coal gangue powder with 1.8mol/L HCl solution according to the mass ratio of 1:2.8, stirring for 2.8h at 78 ℃, filtering the coal gangue powder, washing with deionized water and absolute ethyl alcohol for three times, and drying the coal gangue powder for 1.8h at 78 ℃. Mixing the dried coal gangue powder with Na 2 CO 3 Mixing according to the mass ratio of 1:1, placing the mixture in a tubular furnace for 1h, heating to 800 ℃ and calcining for 1.2h, dissolving the calcined product in 60ml of deionized water, stirring for 1.2h, and filtering coal gangue powder to obtain the precursor solution of the silicon-aluminum source. Adding sodium aluminate to prepare n (silicon source): n (aluminum source): n (deionization)Daughter water) to a synthesis mother liquor of 10:1: 3000.
12ml of the previously prepared cell suspension was mixed with 60ml of the complex. The pH value of the mother liquor is adjusted to 10 by using 8mol/L HCl solution, and the mother liquor is stirred for 1 hour. And transferring the mother liquor to a hydrothermal crystallization kettle with a polytetrafluoroethylene lining and a specification of 100ml, placing the hydrothermal crystallization kettle in an oven for crystallization at 170 ℃ for 24h, naturally cooling the crystallization kettle, taking out the crystallization kettle, washing the crystallization kettle for 3 times respectively by using deionized water and absolute ethyl alcohol, drying the crystallization kettle, heating the crystallization kettle to 190 ℃ at a heating speed of 1 ℃/m1n, and calcining the gasification actinomycete mycelium for 1.3h to obtain the coal gangue-based porous material.
The grain of the porous material is in a spherical structure, the granularity is 2.8-3 mu m, and the diameter of the pore diameter is 880 nm. Specific surface area 288.21m 2 ·g -1 Total pore volume 0.183cm 3 ·g -1 . At room temperature, the adsorption rate of 28mg of the porous material to 20mg/L rhodamine B solution is shown in figure 3, namely the removal rate of 78m1n reaches 79.8 percent, and is improved by nearly 80 percent compared with the removal rate of raw coal gangue;
example 3
The embodiment discloses a preparation method of a coal gangue-based porous material by taking actinomycetes as a template, which specifically comprises the following steps:
culturing actinomycete strains for 24h, centrifuging at the rotating speed of 4000r/m1n for 8m1n to separate bacteria, preparing 18mL of bacterial solution with the mass concentration of 1.2g/L, and ultrasonically oscillating for 10m1n for later use.
18g of coal gangue is crushed, ground and sieved to obtain coal gangue powder of 260 meshes. And (3) putting the coal gangue powder into a tubular furnace, heating to 880 ℃ within 2h, calcining for 8h, and naturally cooling. Mixing the cooled coal gangue powder with 2mol/L HCl solution according to the mass ratio of 1:3, stirring for 3h at 80 ℃, filtering the coal gangue powder, washing with deionized water and absolute ethyl alcohol for three times, and drying for 1.8h at 78 ℃. Mixing the dried coal gangue powder with Na 2 CO 3 Mixing according to the mass ratio of 1:1.2, placing the mixture in a tubular furnace for 1h, heating to 880 ℃, calcining for 1.8h, dissolving the calcined product in 60ml of deionized water, stirring for 1.8h, and filtering coal gangue powder to obtain the precursor liquid of the silicon-aluminum source. Adding tetraethoxysilane to prepare n (silicon source): n (aluminum source): n (deionized water) ═ 20:1: 3000. 18ml of the previously prepared bacterial suspension was mixed with the mother liquor.The pH value of the mother liquor is adjusted to 10.8 by 6mol/L HCl solution, and the mother liquor is stirred for 1 hour. And transferring the mother liquor to a hydrothermal crystallization kettle with a polytetrafluoroethylene lining and a specification of 100ml, placing the hydrothermal crystallization kettle in an oven for crystallization at 180 ℃ for 28h, naturally cooling the crystallization kettle, taking out the crystallization kettle, washing the crystallization kettle for 3 times respectively by using deionized water and absolute ethyl alcohol, drying the crystallization kettle, heating the crystallization kettle to 200 ℃ at a heating speed of 1 ℃/m1n, and calcining the gasification actinomycete mycelium for 1.8h to obtain the coal gangue-based porous material.
The grain of the porous material is in a spherical structure, the granularity is 3-3.8 mu m, and the aperture diameter is 900 nm. Specific surface area 292.37m 2 ·g -1 Total pore volume 0.163cm 3 ·g -1 . At room temperature, the adsorption rate of 28mg of the porous material to 20mg/L rhodamine B solution is shown in figure 4, namely the removal rate of 78m1n reaches 88.3%, which is improved by nearly 60% compared with the removal rate of raw coal gangue.
Claims (10)
1. A preparation method of a coal gangue-based porous material taking actinomycetes as a template is characterized by comprising the following specific steps:
s1, preparing actinomycete liquid with the mass concentration of 1 g/L-1.2 g/L;
s2, pretreating coal gangue to obtain a silicon-aluminum source precursor solution, and adding a silicon source and/or an aluminum source to adjust the silicon-aluminum ratio in the silicon-aluminum source precursor solution to obtain n (silicon source): n (aluminum source): n (deionized water) ═ 2-20: 1:3000 of synthetic mother liquor;
s3, mixing the actinomycete liquid with the synthetic mother liquid to obtain a mixed liquid, adjusting the pH value of the mixed liquid, and crystallizing, washing, drying and calcining the mixed liquid to obtain the porous material.
2. The method for preparing the gangue-based porous material taking the actinomycetes as the template according to claim 1, wherein in the step S2, the pretreatment specifically comprises the following steps:
s2.1, calcining the coal gangue powder with the particle size of 240-300 meshes at 800-850 ℃ for 3-5 h to obtain a first precursor;
s2.2, mixing the first precursor with 1.5-2 mol/L HCl solution, stirring for 2-3 h at 70-80 ℃, washing, filtering and drying to obtain a second precursor,
s2.3 reacting the second precursor with Na 2 CO 3 Mixing and calcining for 1-1.5 h at 750-880 ℃, dissolving the calcined product in deionized water according to the solid-to-liquid ratio of 1:4, stirring for 1-1.5 h, and filtering out coal gangue powder to obtain the silicon-aluminum source precursor solution.
3. The method for preparing the coal gangue-based porous material taking the actinomycetes as the template in the claim 1 is characterized in that in the step S3, the volume ratio of the actinomycetes bacterial liquid to the synthetic mother liquid is 1 (4-6).
4. The method for preparing the coal gangue-based porous material taking the actinomycetes as the template in the claim 1, wherein in the step S3, the pH value is adjusted to be 3-6 mol/L HCl solution to adjust the pH value of the mixed solution to 9.5-10.5, and the mixed solution is stirred for 1 hour.
5. The method for preparing the coal gangue-based porous material using actinomycetes as the template as claimed in claim 1, wherein in step S3, the mixed solution is placed in a hydrothermal crystallization kettle with a polytetrafluoroethylene lining, and the hydrothermal crystallization kettle is placed in an oven for crystallization.
6. The method for preparing the coal gangue-based porous material taking the actinomycetes as the template as claimed in claim 5, wherein in the step S3, the crystallization temperature is 160-180 ℃, and the crystallization time is 18-28 h.
7. The method for preparing the gangue-based porous material using actinomycetes as the template as claimed in claim 1, wherein in step S3, the calcination is carried out by heating to 180-200 ℃ at a heating rate of 1 ℃/min for 1-1.5 h.
8. The method for preparing the gangue-based porous material using actinomycetes as the template as claimed in claim 1, wherein in step S2, the silicon source is tetraethoxysilane or silica sol, and the aluminum source is sodium metaaluminate or sodium aluminate.
9. A gangue-based porous material using actinomycetes as a template, which is produced by the production method according to any one of claims 1 to 7.
10. The gangue-based porous material as claimed in claim 9, wherein the gangue-based porous material has a particle size of 2.5 μm to 3.5 μm and a pore size of 0.7 μm to 0.9 μm.
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