CN114797770A - Preparation process of activated carbon for efficiently adsorbing inorganic gas - Google Patents

Preparation process of activated carbon for efficiently adsorbing inorganic gas Download PDF

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CN114797770A
CN114797770A CN202210358457.4A CN202210358457A CN114797770A CN 114797770 A CN114797770 A CN 114797770A CN 202210358457 A CN202210358457 A CN 202210358457A CN 114797770 A CN114797770 A CN 114797770A
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activated carbon
solution
carbon fiber
scandium
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杨金杯
裴亮
陈文龙
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Shaanxi Pushida Environmental Protection Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0207Compounds of Sc, Y or Lanthanides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0277Carbonates of compounds other than those provided for in B01J20/043
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    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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Abstract

The invention discloses a preparation process of activated carbon for efficiently adsorbing inorganic gas, which comprises the following steps: step 1, weighing activated carbon fibers, dispersing the activated carbon fibers in deionized water, adding a silane coupling agent, and heating to obtain a pretreated substance of the activated carbon fibers; step 2, weighing a soft template, mixing the soft template with an ethanol solution, and sequentially dropwise adding sodium hydroxide, sodium carbonate, water glass and scandium chloride to obtain a pre-reaction solution; step 3, adding scandium diboride into the pre-reaction liquid, adding an activated carbon fiber pretreatment substance, and pouring into a reaction kettle for reaction to obtain an activated carbon fiber composite material pre-product; and 4, placing the activated carbon fiber composite material in a muffle furnace, and heating and roasting the activated carbon fiber composite material in an air atmosphere to obtain the activated carbon fiber composite material. The invention prepares the active ingredientsThe carbon material has greatly increased inorganic gas adsorbing capacity and can adsorb NOx and SO 2 、HCl、NH 3 And the like, to adsorb.

Description

Preparation process of activated carbon for efficiently adsorbing inorganic gas
Technical Field
The invention relates to the field of activated carbon, in particular to a preparation process of activated carbon for efficiently adsorbing inorganic gas.
Background
A large amount of pollutants discharged from industrial production such as mining, smelting, mechanical manufacturing, building materials, chemical industry and the like are inorganic pollutants, wherein oxides of sulfur, nitrogen and carbon and metal dust are main inorganic pollutants in the atmosphere, and are easy to cause various hazards, such as: harm human health, influence plant growth, destroy building materials, cause climate deterioration, etc.
The active carbon is a substance with developed pores and stable chemical properties, has a certain adsorption effect, can generally only adsorb substances matched with the pore diameter of the carbon, can only adsorb a certain or a certain specific gas, has a limited adsorption amount, and cannot simultaneously meet the requirements of NOx and SO 2 、HCl、NH 3 And the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation process of activated carbon for efficiently adsorbing inorganic gas.
The purpose of the invention is realized by adopting the following technical scheme:
a preparation process of activated carbon for efficiently adsorbing inorganic gas comprises the following steps:
step 1, activated carbon pretreatment:
weighing activated carbon fibers, dispersing the activated carbon fibers in deionized water, adding a silane coupling agent, heating to boil, carrying out heat preservation treatment, cooling, filtering, washing and drying to obtain an activated carbon fiber pretreatment (P-ACF);
step 2, preparing a pre-reaction solution:
weighing a soft template, mixing the soft template with an ethanol solution, dropwise adding a sodium hydroxide solution, stirring and mixing uniformly, then dropwise adding a sodium carbonate solution, dropwise adding a water glass solution, dropwise adding a scandium chloride solution, and continuously stirring uniformly after all the scandium chloride solution is dropwise added to obtain a pre-reaction solution (CM-Sc-RS);
step 3, preparing an activated carbon fiber composite material pre-product;
dropwise adding a scandium diboride mixed solution into a pre-reaction solution (CM-Sc-RS) while stirring, then adding an activated carbon fiber pretreatment substance, standing and aging at room temperature, then pouring into a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven for heat preservation, and after the reaction is finished, cooling, filtering, washing and drying to obtain an activated carbon fiber composite material pre-product;
and 4, roasting treatment:
and placing the activated carbon fiber composite material pre-product in a muffle furnace, and heating and roasting in an air atmosphere to obtain the activated carbon fiber composite material (CM-Sc/ACF-PM).
Preferably, in step 1, the activated carbon fiber includes one of polyvinyl alcohol-based activated carbon fiber, natural fiber-based activated carbon fiber, and lignin-based activated carbon fiber.
Preferably, in the step 1, the diameter of the activated carbon fiber is 10-20 μm, the specific surface area is 1500-2000 m/g, and the pore size is 2.0-5.0 nm.
Preferably, in the step 1, the silane coupling agent is at least one of gamma-aminopropyltriethoxysilane (KH-550), gamma-glycidoxypropyltrimethoxysilane (KH-560) and N- (. beta. -aminoethyl) -gamma-aminopropyltrimethoxysilane (KH-792).
Preferably, in the step 1, the mass ratio of the activated carbon fiber, the silane coupling agent and the deionized water is 1: 0.1-0.3: 10-15.
Preferably, in the step 2, the soft template is a polyethoxy-polyisopropoxy-polyethoxy triblock copolymer (EO) 106 PO 70 EO 106 ) And hexadecyl trimethyl ammonium bromide are mixed according to the mass ratio of 1: 6-8 to obtain the catalyst.
Preferably, in the step 2, the ethanol solution is an ethanol aqueous solution, and the mass fraction is 25-35%; the mass ratio of the soft template to the ethanol solution is 1: 35-50.
Preferably, in the step 2, the mass fraction of the sodium hydroxide solution is 5%, and the pH value of the sodium hydroxide solution added to the reaction system is 11.0-12.0.
Preferably, in the step 2, the mass fraction of the sodium carbonate solution is 15%, and the mass ratio of the sodium carbonate solution to the ethanol solution is 0.32-0.48: 1.
Preferably, in the step 2, the mass ratio of the scandium chloride to the deionized water in the scandium chloride solution is 1.51-2.27: 10, and the mass ratio of the scandium chloride solution to the ethanol solution is 0.85-0.94: 1.
Preferably, in the step 2, the mass fraction of the water glass solution is 40%, and the mass ratio of the water glass solution to the ethanol solution is 0.41-0.62: 1.
Preferably, in the step 2, after the sodium carbonate solution is dripped, stirring for 0.5-1 h, dripping the sodium silicate solution, and stirring again for 0.5-1 h; and after the scandium chloride solution is dropwise added, stirring for 2-4 h.
Preferably, in the step 3, the mass ratio of the activated carbon fiber pretreatment product, the scandium diboride mixed solution and the pre-reaction solution is 1: 1.3-1.8: 20-30.
Preferably, in the step 3, the particle size of scandium diboride in the scandium diboride mixed solution is 100-150 nm, and the scandium diboride mixed solution is obtained by mixing scandium diboride and deionized water according to a mass ratio of 1: 10.
Preferably, in the step 3, the standing and aging time is 3-6 h.
Preferably, in the step 3, the temperature of the oven is 120-150 ℃, and the time of heat preservation treatment is 48-60 hours.
Preferably, in the step 4, the temperature of the roasting treatment is 400-450 ℃, the temperature rise rate is 1-3 ℃/min, and the time of the roasting treatment is 4-6 h.
The beneficial effects of the invention are as follows:
1. the invention prepares an active carbon fiber composite material, which has very good inorganic gas adsorption capacity and can adsorb NOx and SO 2 、HCl、NH 3 And compared with the conventional activated carbon fiber, the activated carbon prepared by the invention has greatly improved adsorption capacity on inorganic gas.
2. The active carbon composite material prepared by the invention is prepared by loading scandium silicate/scandium carbonate/scandium diboride composite microspheres on the surface of active carbon, and the preparation process is mainly in-situ synthesis on the surface of the active carbon, so that not only is the active carbon and the composite microspheres combined more tightly, but also more composite microspheres can be loaded on the active carbon.
3. The preparation process of the scandium silicate/scandium carbonate/scandium diboride composite microsphere is improved in terms of the preparation method of MCM mesoporous microsphere, and the first method is to use a mixing mode of two soft templates, namely hexadecyl trimethyl ammonium bromide and polyethoxy-polyisopropoxy-polyethoxy triblock copolymer (EO) 106 PO 70 EO 106 ) And secondly, firstly, a sodium carbonate solution and a water glass solution are mixed and reacted with a scandium chloride solution together to generate scandium silicate and scandium carbonate, and then scandium diboride is added for embedding, so that scandium silicate, scandium carbonate and scandium diboride in the finally formed composite microsphere can be uniformly dispersed.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 is an SEM image of an activated carbon fiber composite (CM-Sc/ACF-PM) prepared in example 1 of the present invention.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but are not to be construed as limiting the implementable scope of the present invention.
The diameter of the activated carbon fiber used in the invention is 10-20 μm, the specific surface area is 1500-2000 m/g, and the pore size is 2.0-5.0 nm.
Activated Carbon Fiber (ACF) is a porous fibrous adsorption material, has the advantages of high specific surface area, high strength, less impurities, high temperature resistance and the like, and is widely applied to the aspects of air purification, sewage treatment, medical sanitation, bioengineering, chemistry, catalysts and the like. However, with the development of science and technology, the living standard of people is improved, and the requirements of people on the air environment are higher and higher, and the traditional activated carbon fiber has certain gas adsorption property but cannot meet the requirements, so that the adsorption modification of the activated carbon fiber becomes a popular research.
In the initial scheme of the invention, scandium silicate is loaded on the activated carbon fiber, although the inorganic gas adsorbability can be improved to a certain extent compared with that of the traditional silicate (magnesium silicate), the improvement is not ideal enough, SO that carbonate is added in the preparation process to prepare a double-mixed product of scandium carbonate and scandium silicate, the double-mixed product can better perform on the adsorption activity of NOx, SO2 and HCl gas, and the improvement is to further improve the adsorption activity of ammonia gas (NH 2) 3 ) The scandium diboride is a novel material and is mainly used in the field of semiconductors at present, a chemical bond is a mixed bond with covalent, ionic and metallic bond properties, and the chemical bond has better mechanical strength.
However, according to the detection of the present application, it is found that after scandium diboride is added in the process of the binding reaction, the finally formed ternary mixed product is resistant to NOx and SO 2 、HCl、NH 3 And various inorganic gases have better adsorbability.
The invention is further described below with reference to the following examples.
Example 1
A preparation process of activated carbon for efficiently adsorbing inorganic gas comprises the following steps:
step 1, activated carbon pretreatment:
weighing activated carbon fibers, dispersing the activated carbon fibers in deionized water, adding gamma-aminopropyltriethoxysilane (KH-550) into the deionized water, wherein the mass ratio of the activated carbon fibers to the KH-550 to the deionized water is 1:0.2:10, completely soaking, performing ultrasonic dispersion uniformly, heating to boil the deionized water, performing heat preservation treatment for 0.5h, cooling to room temperature, filtering, washing with pure water for at least three times, and performing vacuum drying to obtain an activated carbon fiber pretreatment (P-ACF);
step 2, preparing a pre-reaction solution:
weighing a soft template and an ethanol solution with the mass fraction of 30%, mixing the soft template and the ethanol solution according to the mass ratio of 1:50, dropwise adding a sodium hydroxide solution with the mass fraction of 5% until the pH value is 11.0-12.0, stirring and mixing uniformly, then dropwise adding a sodium carbonate solution with the mass fraction of 15% according to the mass ratio of 0.4:1 to the ethanol solution, stirring and mixing for 0.5h, then dropwise adding a water glass solution with the mass fraction of 40% according to the mass ratio of 0.53:1 to the ethanol solution, stirring again for 0.5h, then dropwise adding a scandium chloride solution according to the mass ratio of 1.92:10 to the scandium chloride solution and the deionized water to the scandium chloride solution and the ethanol solution according to the mass ratio of 0.88:1, and continuously stirring for 3h after all dropwise adding to obtain a pre-reaction solution (CM-Sc-RS);
step 3, preparing an activated carbon fiber composite material pre-product;
weighing scandium diboride with the particle size of 100-150 nm and deionized water, mixing the scandium diboride with the deionized water according to the mass ratio of 1:10 to obtain a scandium diboride mixed solution, dropwise adding the scandium diboride mixed solution into a pre-reaction solution (CM-Sc-RS), stirring and mixing for 0.5h, adding an activated carbon fiber pretreatment (P-ACF), wherein the mass ratio of the activated carbon fiber pretreatment, the scandium diboride mixed solution and the pre-reaction solution is 1:1.5:25, standing and aging at room temperature for 5h after complete infiltration, then pouring into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle into a 135 ℃ drying oven for heat preservation for 54h, taking out the reaction kettle after reaction is finished, naturally cooling at room temperature, filtering solid products in the reaction solution, washing for at least three times, and performing vacuum drying to obtain an activated carbon fiber composite material pre-product;
and 4, roasting treatment:
and (3) placing the activated carbon fiber composite material pre-product into a muffle furnace, heating to 400 ℃ at the speed of 2 ℃/min in the air atmosphere, roasting for 5h, cooling to room temperature along with the furnace, and obtaining the activated carbon fiber composite material (CM-Sc/ACF-PM).
In addition, a Scanning Electron Microscope (SEM) image of example 1 is shown in fig. 1.
Example 2
A preparation process of activated carbon for efficiently adsorbing inorganic gas comprises the following steps:
step 1, activated carbon pretreatment:
weighing polyvinyl alcohol-based active carbon fibers, dispersing the polyvinyl alcohol-based active carbon fibers in deionized water, adding gamma-glycidyl ether oxypropyltrimethoxysilane (KH-560) into the deionized water, wherein the mass ratio of the active carbon fibers to the KH-560 to the deionized water is 1:0.1:10, completely soaking, performing ultrasonic dispersion uniformly, heating to boil the deionized water, performing heat preservation treatment for 0.5h, cooling to room temperature, filtering, washing with pure water for at least three times, and performing vacuum drying to obtain an active carbon fiber pretreatment (P-ACF);
step 2, preparing a pre-reaction solution:
weighing a soft template and an ethanol solution with the mass fraction of 25%, mixing the soft template and the ethanol solution according to the mass ratio of 1:35, dropwise adding a sodium hydroxide solution with the mass fraction of 5% until the pH value is 11.0-12.0, stirring and mixing uniformly, then dropwise adding a sodium carbonate solution with the mass fraction of 15% according to the mass ratio of 0.32:1 to the ethanol solution, stirring and mixing for 0.5h, then dropwise adding a water glass solution with the mass fraction of 40% according to the mass ratio of 0.41:1 to the ethanol solution, stirring again for 0.5h, then dropwise adding a scandium chloride solution, wherein the mass ratio of scandium chloride to deionized water in the scandium chloride solution is 1.51:10, the mass ratio of the scandium chloride solution to the ethanol solution is 0.85:1, and stirring continuously for 2h after all dropwise adding to obtain a pre-reaction solution (CM-Sc-RS);
step 3, preparing an activated carbon fiber composite material pre-product;
weighing scandium diboride with the particle size of 100-150 nm and deionized water, mixing the scandium diboride with the deionized water according to the mass ratio of 1:10 to obtain a scandium diboride mixed solution, dropwise adding the scandium diboride mixed solution into a pre-reaction solution (CM-Sc-RS), stirring and mixing for 0.5h, adding an activated carbon fiber pretreatment (P-ACF), wherein the mass ratio of the activated carbon fiber pretreatment, the scandium diboride mixed solution and the pre-reaction solution is 1:1.3:20, standing and aging at room temperature for 3h after complete infiltration, then pouring into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle in a 120 ℃ drying oven for heat preservation for 60h, taking out the reaction kettle after the reaction is finished, placing the reaction kettle at room temperature for natural cooling, filtering solid products in the reaction solution, washing for at least three times by using pure water, and performing vacuum drying to obtain an activated carbon fiber composite material pre-product;
and 4, roasting treatment:
and (3) placing the activated carbon fiber composite material pre-product into a muffle furnace, heating to 400 ℃ at the speed of 1 ℃/min in the air atmosphere, roasting for 6h, cooling to room temperature along with the furnace, and obtaining the activated carbon fiber composite material (CM-Sc/ACF-PM).
Example 3
A preparation process of activated carbon for efficiently adsorbing inorganic gas comprises the following steps:
step 1, activated carbon pretreatment:
weighing activated carbon fibers, dispersing the activated carbon fibers in deionized water, adding N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane (KH-792), wherein the mass ratio of the activated carbon fibers to the KH-792 to the deionized water is 1:0.3:15, completely soaking, performing ultrasonic dispersion uniformly, heating to boil the deionized water, performing heat preservation treatment for 1h, cooling to room temperature, filtering, washing with pure water for at least three times, and performing vacuum drying to obtain an activated carbon fiber pretreatment (P-ACF);
step 2, preparing a pre-reaction solution:
weighing a soft template and an ethanol solution with the mass fraction of 35%, mixing the soft template and the ethanol solution according to the mass ratio of 1:50, dropwise adding a sodium hydroxide solution with the mass fraction of 5% until the pH value is 11.0-12.0, stirring and mixing uniformly, then dropwise adding a sodium carbonate solution with the mass fraction of 15% according to the mass ratio of 0.48:1, stirring and mixing for 1h, then dropwise adding a water glass solution with the mass fraction of 40%, stirring for 1h again according to the mass ratio of 0.62:1, then dropwise adding a scandium chloride solution according to the mass ratio of 2.27:10 of scandium chloride to deionized water in the scandium chloride solution, stirring for 4h after all the scandium chloride solutions are dropwise added to obtain a pre-reaction solution (CM-Sc-RS);
step 3, preparing an activated carbon fiber composite material pre-product;
weighing scandium diboride with the particle size of 100-150 nm and deionized water, mixing the scandium diboride with the deionized water according to the mass ratio of 1:10 to obtain a scandium diboride mixed solution, dropwise adding the scandium diboride mixed solution into a pre-reaction solution (CM-Sc-RS), stirring and mixing for 1h, then adding an activated carbon fiber pretreatment product (P-ACF), wherein the mass ratio of the activated carbon fiber pretreatment product, the scandium diboride mixed solution and the pre-reaction solution is 1:1.8:30, standing and aging at room temperature for 6h after complete infiltration, then pouring into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle in a 150 ℃ drying oven for heat preservation for 60h, taking out the reaction kettle after the reaction is finished, placing the reaction kettle at room temperature for natural cooling, filtering out solid products in the reaction solution, washing with pure water for at least three times, and performing vacuum drying to obtain an activated carbon fiber composite material pre-product;
and 4, roasting treatment:
and (3) placing the activated carbon fiber composite material pre-product into a muffle furnace, heating to 450 ℃ at the speed of 3 ℃/min in the air atmosphere, roasting for 6h, cooling to room temperature along with the furnace, and obtaining the activated carbon fiber composite material (CM-Sc/ACF-PM).
Comparative example 1
Compared with the example 1, the preparation process of the activated carbon for efficiently adsorbing the inorganic gas, which does not add scandium diboride, comprises the following steps:
step 1, activated carbon pretreatment: (same as example 1);
step 2, preparing a pre-reaction solution: (same as example 1);
step 3, preparing an activated carbon fiber composite material pre-product;
directly adding an activated carbon fiber pretreatment substance (P-ACF) into a pre-reaction liquid (CM-Sc-RS), wherein the mass ratio of the activated carbon fiber pretreatment substance to the pre-reaction liquid is 1:25, standing and aging at room temperature for 5 hours after complete infiltration, then pouring into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle in a 135 ℃ oven for heat preservation for 54 hours, taking out the reaction kettle after the reaction is finished, placing the reaction kettle at room temperature for natural cooling, filtering out a solid product in the reaction liquid, washing with pure water for at least three times, and performing vacuum drying to obtain an activated carbon fiber composite material pre-product;
step 4, firing treatment (same as example 1).
Comparative example 2
Compared with the example 1, the preparation process of the activated carbon for efficiently adsorbing the inorganic gas, which does not add scandium carbonate and scandium diboride, comprises the following steps:
step 1, activated carbon pretreatment: (same as example 1);
step 2, preparing a pre-reaction solution:
weighing a soft template, mixing the soft template with an ethanol solution with the mass fraction of 30%, dropwise adding a sodium hydroxide solution with the mass fraction of 5% until the pH value is 11.0-12.0, uniformly stirring, dropwise adding a water glass solution with the mass fraction of 40% at first, wherein the mass ratio of the water glass solution to the ethanol solution is 0.53:1, stirring for 0.5h, dropwise adding a scandium chloride solution, wherein the mass ratio of scandium chloride to deionized water in the scandium chloride solution is 1.92:10, the mass ratio of the scandium chloride solution to the ethanol solution is 0.88:1, and continuously stirring for 3h after all dropwise adding to obtain a pre-reaction solution;
step 3, preparing an activated carbon fiber composite material pre-product;
directly adding an activated carbon fiber pretreatment substance (P-ACF) into a pre-reaction liquid (CM-Sc-RS), wherein the mass ratio of the activated carbon fiber pretreatment substance to the pre-reaction liquid is 1:25, standing and aging at room temperature for 5 hours after complete infiltration, then pouring into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle in a 135 ℃ oven for heat preservation for 54 hours, taking out the reaction kettle after the reaction is finished, placing the reaction kettle at room temperature for natural cooling, filtering out a solid product in the reaction liquid, washing with pure water for at least three times, and performing vacuum drying to obtain an activated carbon fiber composite material pre-product;
step 4, firing treatment (same as example 1).
Comparative example 3
An activated carbon fiber having a diameter of 10 to 20 μm, a specific surface area of 1500 to 2000m/g, and a pore size of 2.0 to 5.0nm, is commercially available.
And (3) related experiment detection:
the activated carbon fibers obtained by the methods of the embodiment 1 and the comparative examples 1 to 3 of the present invention were subjected to gas adsorption detection, specifically as follows:
firstly, testing a gas to be tested:
NO/NO 2 /NH 3 /SO 2 HCl/gaseous mixture.
II, experimental materials:
the activated carbon fibers obtained by the methods of example 1 and comparative examples 1 to 3, four cylindrical glass containers (10L) with sealing plugs and an intelligent gas detector with the accuracy of 1ppm level.
Thirdly, experimental conditions:
room temperature (25 deg.C), dark, humidity 55%.
Fourthly, an experiment step:
1. taking four cylindrical glass containers with sealing plugs, cleaning the interiors of the glass containers, and then airing the interiors, wherein the four cylindrical glass containers are respectively marked as example 1, comparative example 2 and comparative example 3;
2. respectively weighing 10.00 +/-0.1 g of the activated carbon fibers obtained by the methods of the embodiment 1 and the comparative examples 1 to 3, and uniformly spreading the weighed activated carbon fibers on the bottom of a glass container;
3. respectively introducing inorganic mixed gas with the same concentration into four cylindrical glass containers according to calculation so as to ensure that the concentration of NO gas in the cylindrical glass containers is 1000ppm and the concentration of NO gas in the cylindrical glass containers is 1000ppm 2 Gas concentration of 1000ppm, SO 2 Gas concentration 1000ppm, NH 3 Gas concentration 500ppm and HCl gas concentration 200ppm, the remainder being air);
4. rapid detection of the actual concentration (C) of each gas in the cylindrical glass container after venting 0 ) Placing four cylindrical glass containers filled with activated carbon fiber in a dark room, adjusting the temperature to 25 deg.C and humidity to 55%, standing for 12 hr, and detecting the final concentration (C) of each gas in the cylindrical glass container 1 ) The absorption rate of the activated carbon fiber to gas was calculated by the following formula:
gas absorption (%) - (C) 0 -C 1 )/C 0 ×100%;
5. The results of the detection and calculation are shown in the following tables 1 to 5:
TABLE 1 absorption rate of NO gas by activated carbon fiber
Figure BDA0003583922750000081
TABLE 2 activated carbon fiber vs. NO 2 Absorption rate of gas
Figure BDA0003583922750000091
TABLE 3 activated carbon fiber vs. SO 2 Absorption rate of gas
Figure BDA0003583922750000092
TABLE 4 activated carbon fiber vs. NH 3 Absorption rate of gas
Figure BDA0003583922750000093
TABLE 5 absorption rate of activated carbon fiber for HCl gas
Figure BDA0003583922750000094
As can be seen from tables 1 to 5 above, the mixed gas (NO/NO) of example 1 of the present invention with respect to the inorganic gas 2 /NH 3 /SO 2 HCl), whereas comparative example 1, although the indices perform well, is inferior to example 1, in particular the absorption of ammonia is more different, whereas comparative example 2 and comparative example 3 perform more poorly. The data can show that the activated carbon prepared by the method has high-efficiency adsorption effect on inorganic gas.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. A preparation process of activated carbon for efficiently adsorbing inorganic gas is characterized by comprising the following steps:
step 1, activated carbon pretreatment:
weighing activated carbon fibers, dispersing the activated carbon fibers in deionized water, adding a silane coupling agent, heating to boil, carrying out heat preservation treatment, cooling, filtering, washing and drying to obtain an activated carbon fiber pretreatment (P-ACF);
step 2, preparing a pre-reaction solution:
weighing a soft template, mixing the soft template with an ethanol solution, dropwise adding a sodium hydroxide solution, stirring and mixing uniformly, then dropwise adding a sodium carbonate solution, dropwise adding a water glass solution, dropwise adding a scandium chloride solution, and continuously stirring uniformly after all the scandium chloride solution is dropwise added to obtain a pre-reaction solution (CM-Sc-RS);
step 3, preparing an activated carbon fiber composite material pre-product;
dropwise adding a scandium diboride mixed solution into a pre-reaction solution (CM-Sc-RS) while stirring, then adding an activated carbon fiber pretreatment substance, standing and aging at room temperature, then pouring into a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven for heat preservation, and after the reaction is finished, cooling, filtering, washing and drying to obtain an activated carbon fiber composite material pre-product;
and 4, roasting treatment:
and placing the activated carbon fiber composite material pre-product in a muffle furnace, and heating and roasting in an air atmosphere to obtain the activated carbon fiber composite material (CM-Sc/ACF-PM).
2. The process for preparing activated carbon for efficiently adsorbing inorganic gas as claimed in claim 1, wherein in the step 1, the activated carbon fiber comprises one of polyvinyl alcohol-based activated carbon fiber, natural fiber-based activated carbon fiber and lignin-based activated carbon fiber; the diameter of the activated carbon fiber is 10-20 μm, the specific surface area is 1500-2000 m/g, and the pore size is 2.0-5.0 nm.
3. The process for preparing activated carbon for highly efficient adsorption of inorganic gases as claimed in claim 1, wherein in step 1, the silane coupling agent is at least one of γ -aminopropyltriethoxysilane (KH-550), γ -glycidoxypropyltrimethoxysilane (KH-560), and N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane (KH-792).
4. The process for preparing activated carbon for highly adsorbing inorganic gases as claimed in claim 1, wherein in the step 2, the soft template is poly ethoxy-poly isopropoxy-poly ethoxy triblock copolymer (EO) 106 PO 70 EO 106 ) Mixing the ammonium bromide and hexadecyl trimethyl ammonium bromide according to the mass ratio of 1: 6-8 to obtain the ammonium bromide-hexadecyl trimethyl ammonium bromide mixture; the ethanol solution is 25 to 35 percent of ethanol water solution; the mass ratio of the soft template to the ethanol solution is 1: 35-50.
5. The process for preparing activated carbon capable of efficiently adsorbing inorganic gas according to claim 1, wherein in the step 2, the mass fraction of the sodium hydroxide solution is 5%, and the pH value of the sodium hydroxide solution added to the reaction system is 11.0-12.0.
6. The process for preparing the activated carbon capable of efficiently adsorbing the inorganic gas according to claim 1, wherein in the step 2, the mass fraction of the sodium carbonate solution is 15%, and the mass ratio of the sodium carbonate solution to the ethanol solution is 0.32-0.48: 1; the mass fraction of the water glass solution is 40%, and the mass ratio of the water glass solution to the ethanol solution is 0.41-0.62: 1.
7. The preparation process of the activated carbon for efficiently adsorbing the inorganic gas as claimed in claim 1, wherein in the step 2, the mass ratio of scandium chloride to deionized water in the scandium chloride solution is 1.51-2.27: 10, and the mass ratio of the scandium chloride solution to the ethanol solution is 0.85-0.94: 1.
8. The process for preparing the activated carbon capable of efficiently adsorbing the inorganic gas according to claim 1, wherein in the step 2, after the sodium carbonate solution is dropwise added, stirring is carried out for 0.5 to 1 hour, then the sodium silicate solution is dropwise added, and stirring is carried out again for 0.5 to 1 hour; and after the scandium chloride solution is dropwise added, stirring for 2-4 h.
9. The process for preparing the activated carbon for efficiently adsorbing the inorganic gas as claimed in claim 1, wherein in the step 3, the mass ratio of the activated carbon fiber pretreatment product, the scandium diboride mixed solution and the pre-reaction solution is 1: 1.3-1.8: 20-30; the particle size of scandium diboride in the scandium diboride mixed solution is 100-150 nm, and the scandium diboride mixed solution is obtained by mixing scandium diboride and deionized water according to the mass ratio of 1: 10; standing and aging for 3-6 h; the temperature of the oven is 120-150 ℃, and the time of heat preservation treatment is 48-60 h.
10. The process for preparing the activated carbon capable of efficiently adsorbing the inorganic gas according to claim 1, wherein in the step 4, the roasting treatment temperature is 400-450 ℃, the temperature rise rate is 1-3 ℃/min, and the roasting treatment time is 4-6 h.
CN202210358457.4A 2022-04-07 2022-04-07 Preparation process of activated carbon for efficiently adsorbing inorganic gas Pending CN114797770A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107551999A (en) * 2017-09-25 2018-01-09 江苏苏通碳纤维有限公司 The preparation method of activated carbon fiber-loaded ordered mesoporous silicon dioxide composite material
CN112520735A (en) * 2020-11-11 2021-03-19 陕西浦士达环保科技有限公司 Activated carbon for removing chloramine
CN112604665A (en) * 2020-11-11 2021-04-06 江苏浦士达环保科技股份有限公司 Preparation method of porous activated carbon heavy metal adsorption material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107551999A (en) * 2017-09-25 2018-01-09 江苏苏通碳纤维有限公司 The preparation method of activated carbon fiber-loaded ordered mesoporous silicon dioxide composite material
CN112520735A (en) * 2020-11-11 2021-03-19 陕西浦士达环保科技有限公司 Activated carbon for removing chloramine
CN112604665A (en) * 2020-11-11 2021-04-06 江苏浦士达环保科技股份有限公司 Preparation method of porous activated carbon heavy metal adsorption material

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