CN113426410A - Porous carbon material and preparation method thereof - Google Patents

Porous carbon material and preparation method thereof Download PDF

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Publication number
CN113426410A
CN113426410A CN202110666020.2A CN202110666020A CN113426410A CN 113426410 A CN113426410 A CN 113426410A CN 202110666020 A CN202110666020 A CN 202110666020A CN 113426410 A CN113426410 A CN 113426410A
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porous carbon
carbon material
salt
stirring
solvent
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伍晨迪
毛建平
封宗瑜
王堃
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Gree Electric Appliances Inc of Zhuhai
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Gree Electric Appliances Inc of Zhuhai
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    • 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
    • B01J20/20—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
    • B01D—SEPARATION
    • B01D53/00—Separation 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
    • B01D53/02—Separation 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
    • 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
    • B01J20/0203—Solid 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
    • B01J20/0259—Compounds of N, P, As, Sb, Bi
    • 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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid 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 surface properties or porosity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Abstract

The invention discloses a preparation method of a porous carbon material, which is characterized by comprising the following steps: dispersing ammonium salt, zinc oxide precursor salt and porous carbon in a solvent to obtain a precursor mixed solution; and adjusting the pH value of the precursor mixed solution to 8-11, and performing high-temperature compounding on solid components in the precursor mixed solution. The invention also discloses a porous carbon material.

Description

Porous carbon material and preparation method thereof
Technical Field
The invention relates to the technical field of environmental protection, and particularly relates to a porous carbon material and a preparation method thereof.
Background
CO2Excessive emissions are the main inducers of global environmental changes such as global warming, extreme weather and desertification. According to the current CO2The global air temperature is estimated to be increased by about 3 ℃ in 2050, the sea level is increased at that time, a large amount of land is submerged, and the world can be involved in disasters. In some chemical processes (such as natural gas purification, sterile ward, fermentation plant, etc.), CO in raw gas2The concentration control of (a) is very strict. CO in certain industries2The gas is very useful, has high economic value and is commonly used in the food industry and the crude oil exploitation industry. Thus, CO2Removal andpure CO2The separation technology development is very important, and the method has important social and practical significance. With CO2Is also a product of human metabolism, and can be used for exhaling CO every hour when adults are quiet2About 15L, and the discharge amount is larger when the device is in motion, and when the CO is in motion2After the concentration is accumulated to a certain degree, people can feel dizzy, nausea and vomiting. At 5% concentration, the breath is maintained for only 30 minutes, and above 10%, it is unconscious and even dead. Therefore, CO must be continuously removed2Controlling the CO in the cabin2And (4) concentration.
At present, indoor low concentration CO2The removal method of (2) is mainly a physical adsorption method, a membrane separation method, a metal compound absorption method, an alcohol amine absorption method, or the like. These methods have their own advantages, but most of them have the disadvantages of short life and low efficiency. Especially in the case of narrow closed/semi-closed space and complicated air composition, CO2The removal efficiency of (a) is very low.
Disclosure of Invention
Based on this, it is necessary to solve the problem of the conventional method that CO is generated in the condition of narrow closed/semi-closed space and complicated air composition2The problem of low removal efficiency, and provides a porous carbon material and a preparation method thereof.
A method for producing a porous carbon material, comprising the steps of:
dispersing ammonium salt, zinc oxide precursor salt and porous carbon in a solvent to obtain a precursor mixed solution;
and adjusting the pH value of the precursor mixed solution to 8-11, and performing high-temperature compounding on solid components in the precursor mixed solution.
In some embodiments, the solid component is obtained by solvent evaporation treatment, and the high-temperature compounding is performed at a temperature of 100-200 ℃ for 2-8 h.
In some embodiments, the pH of the precursor mixed solution is adjusted to 8-9, the temperature of the high-temperature compounding is 190-200 ℃, and the time is 2-3 h.
In some embodiments, the ammonium salt is selected from one or more of ammonium carbonate, ammonium nitrate, and ammonium chloride.
In some embodiments, the zinc oxide precursor salt is selected from one or more of zinc sulfate, zinc nitrate, and zinc chloride.
In some embodiments, the ammonium salt is ammonium carbonate and the zinc oxide precursor salt is zinc nitrate.
In some embodiments, the porous carbon is selected from activated carbon prepared from one or more of coconut shell, coal, and wood.
In some embodiments, the mass ratio of the ammonium salt to the zinc oxide precursor salt is 1 to 10.
In some embodiments, the mass ratio of the porous carbon to the zinc oxide precursor salt is 5 to 10.
Another object of the present invention is to provide a porous carbon material prepared by the method for preparing a porous carbon material according to any one of the above embodiments.
The invention provides a catalyst for CO2The adsorption-separated ZnO modified amino modified porous carbon material takes low-cost commercialized porous activated carbon as a carrier, adopts ZnO modification and amino modification, has uniformly distributed active components, and can enhance CO2Surface activation effect to make the porous carbon material and CO2Stronger acting force between them, CO2Is not easy to be separated. The modification by ZnO can enhance CO2Surface activation effect of (2) can activate CO2The carbon-oxygen bond effectively solves the problems of the porous carbon material and CO2The weak adsorption force causes CO2The problem of escape. Moreover, ZnO modification and amino modification are adopted, and CO can be adsorbed by chemical action with high selectivity2The air conditioner is basically not interfered by other gases, and can be suitable for narrow closed/semi-closed spaces with complicated air components. The method adopts commercial porous carbon with low cost and wide preparation raw materials as a carrier, and increases CO by utilizing developed pore structure and high specific surface area of the porous carbon2The contact area with the adsorbing material can effectively remove CO2Adsorbed onto porous carbon. The porous carbon material has the advantages of simple preparation process, low production cost, easy implementation and good economic benefit and social value.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Other than as shown in the operating examples, or where otherwise indicated, all numbers expressing quantities of ingredients, physical and chemical properties, and so forth used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the foregoing specification and attached claims are approximations that can be suitably varied by those skilled in the art in seeking to obtain the desired properties utilizing the teachings disclosed herein. The use of numerical ranges by endpoints includes all numbers within that range and any range within that range, for example, 1 to 5 includes 1, 1.1, 1.3, 1.5, 2, 2.75, 3, 3.80, 4, and 5, and the like.
The embodiment of the invention provides a preparation method of a porous carbon material, which comprises the following steps:
dispersing ammonium salt, zinc oxide precursor salt and porous carbon in a solvent to obtain a precursor mixed solution;
and adjusting the pH value of the precursor mixed solution to 8-11, and performing high-temperature compounding on solid components in the precursor mixed solution.
In some embodiments, the porous carbon is selected from activated carbon. The type of the activated carbon used as the porous carbon material is not particularly limited, and various known activated carbon species can be used. Examples of activated carbon species include activated carbons made from raw materials such as coconut shells, coal, and wood. These activated carbon species can be produced by any known method. Can be generally produced by steam activation of the raw material.
Activated carbon is a versatile and relatively inexpensive adsorbent produced from a wide variety of abundant carbonaceous materials such as coal, wood, coconut shell, and the like. The unique properties of activated carbon are associated with its carbon-based skeleton, which is highly porous, with pore sizes that can vary over a wide range, from visible cracks and fissures to molecular-scale cracks and fissures. The intermolecular attraction between these smallest pores creates an adsorption force that causes the adsorbed gas to condense into the pores at these molecular levels or causes the adsorbed liquid to settle out of solution into the pores at these molecular levels.
The porous carbon may have various forms such as thin films, monoliths, particles, powders, flakes, rods, nanopores and the like.
The porous carbon may have an average pore size of about 10nm to about 100nm and a specific surface area of about 5m2A/g to about 1,500m2In g and a pore volume of about 0.2cm3G to about 2cm3(ii) in terms of/g. For example, the porous carbon may have an average pore size of from about 60nm to about 120nm, from about 10nm to about 80nm, or from about 80nm to about 100nm, and a specific surface area of about 200m2A/g to about 1,000m2G, about 200m2G to about 800m2In g, or about 400m2G to about 900m2In g and a pore volume of about 0.3cm3G to about 1.8cm3G, about 0.2cm3G to about 2cm3In g, or about 0.25cm3G to about 1.5cm3(ii) in terms of/g. In another example, the porous carbon may have a pore size of at least 10nm, at least 30nm, at least 50nm, or at least 60nm to about 80nm, about 100nm, about 125nm, or about 150nm, and a specific surface area of at least 150m2A/g of at least 200m2A/g of at least 300m2A/g of at least 350m2Per g, or at least 400m2A/g to about 750m2G, about 800m2G, about 900m2A/g of about 1,000m2G, about 1,100m2In g, or about 1,250m2In terms of grams, and a pore volume of at least 0.4cm3At least 0.5 cm/g3/g，At least 0.6cm3In g, or at least 0.7cm3G to about 1cm3G, about 1.2cm3G, about 1.5cm3G, about 1.8cm3In g, or about 2cm3/g。
The specific surface area of the porous carbon refers to the total specific surface area of the porous carbon as measured according to Brunauer-Emmett-Teller or "BET" techniques (as described in s.brunauer, p.h.emmett, and e.teller, j.amer.chem.soc.,60,309 (1938)). BET techniques use an inert gas, such as nitrogen, to measure the amount of gas adsorbed on a material and are commonly used in the art to determine the accessible surface area of a material.
In some embodiments, the ammonium salt is selected from one or more of ammonium carbonate, ammonium nitrate, and ammonium chloride.
Zinc oxide precursor salt means a salt that forms zinc oxide on the porous carbon surface under suitable reaction conditions. In some embodiments, the zinc oxide precursor salt is selected from one or more of zinc sulfate, zinc nitrate, and zinc chloride.
In some embodiments, the ammonium salt is ammonium carbonate and the zinc oxide precursor salt is zinc nitrate.
In some embodiments, the mass ratio of the ammonium salt to the zinc oxide precursor salt is 1 to 10. Specifically, the mass ratio of the ammonium salt to the zinc oxide precursor salt is 1,2, 3, 4, 5, 6, 7, 8, 9, 10.
In some embodiments, the mass ratio of the porous carbon to the zinc oxide precursor salt is 5 to 10. Specifically, the mass ratio of the porous carbon to the zinc oxide precursor salt is 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, and 10.
"solvent" refers to the following: it will dissolve or disperse the reactants and provide a medium in which the reaction can take place. In some embodiments, the solvent may be selected from alcohols. Illustrative alcohols can include, but are not limited to, methanol, ethanol, propanol, tert-butanol, or any mixture thereof. Preferably from ethanol.
In one or more embodiments, the ammonium salt and the zinc oxide precursor salt are first dissolved in a solvent to obtain a salt solution, and then a quantity of the porous carbon material is added to the resulting salt solution. The ammonium salt and zinc oxide precursor salt may be stirred while dissolved in the solvent.
In order to carry out the reaction under alkaline conditions, the pH of the precursor mixture is adjusted to 8-11 by using an alkaline pH adjusting agent. Specifically, the pH of the precursor mixture solution after the pH adjustment is 8, 8.5, 9, 9.5, 10, 10.5, and 11.
The alkaline pH regulator is comprehensively considered from the aspects of regulating the alkalinity degree and the price, regulating the alkalinity, simultaneously introducing amino and not introducing other impurities to the reaction, and can be selected from ammonia water.
The amount of the alkaline pH adjuster used is an amount necessary to maintain the desired alkalinity of the precursor mixture.
In some embodiments, the solid component for high temperature compounding is obtained by evaporative solvent treatment. The temperature of high-temperature compounding is 100-200 ℃. The high-temperature compounding time can be 2-8 h.
In one or more embodiments, the salt solution, the precursor mixture, or the pH-adjusted precursor mixture may be stirred. For example, the salt solution, the precursor mixture, or the pH adjusted precursor mixture may be agitated to improve and/or maintain a uniform or substantially uniform distribution of the reactants within the solvent or a uniform or substantially uniform distribution of the solvent, solutes in the salt solution, the precursor mixture, or the pH adjusted precursor mixture. In one or more embodiments, the salt solution, the precursor mixture, or the pH adjusted precursor mixture is not agitated. The salt solution, precursor mixture, or pH adjusted precursor mixture may be mixed in one or more mixers. The mixer can be or include any device, system or combination of devices and/or systems capable of batch, and/or continuous mixing, blending, contacting, or otherwise combining two or more components. Illustrative mixers can include, but are not limited to, mechanical mixer agitation, ejectors, static mixers, mechanical/dynamic mixers, shear mixers, ultrasonic mixers, vibratory mixers, movement of the mixer itself, or any combination thereof. The mixer may include one or more heating jackets, heating coils, internal heating elements, cooling jackets, cooling coils, internal cooling elements, or the like to regulate the temperature therein. The mixer may be an open vessel or a closed vessel.
In some embodiments, the time period for stirring the pH-adjusted precursor mixture before evaporating the solvent may be 1 to 5 hours. Specifically, the precursor mixed solution after the pH adjustment may be stirred for 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, and 5 hours.
The evaporation solvent treatment of the precursor mixed solution after the pH adjustment may be performed such that the liquid in the precursor mixed solution is evaporated by 90% or more, for example, 95% or more, 98% or more, or 100% or more.
The precursor mixture after evaporation of the solvent may be heated in any desired atmosphere. For example, the precursor mixture after evaporation of the solvent may be heated in an inert gas atmosphere, for example, an atmosphere containing one or more inert gases. Illustrative inert gases may include, but are not limited to, nitrogen, argon, helium, neon, or any mixture thereof. In another example, the precursor mixed liquor after evaporation of the solvent may be heated in air, oxygen-enriched air (greater than 21 vol% oxygen), or oxygen-depleted air (less than or equal to 21 vol% oxygen). Other suitable gases may include, but are not limited to, carbon dioxide, methane, or mixtures thereof.
The high temperature compounding temperature can be 100 deg.C, 110 deg.C, 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 160 deg.C, 170 deg.C, 180 deg.C, 190 deg.C, 200 deg.C. The high-temperature compounding time can be 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h and 8 h. In some embodiments, the high-temperature compounding temperature is 150 ℃ to 200 ℃, and the high-temperature compounding time is 6h to 8 h.
In some embodiments, the precursor mixture after pH adjustment has a pH of 8-9, a high temperature compounding temperature of 190-200 ℃, and a high temperature compounding time of 2-3 h.
The embodiment of the invention also provides a porous carbon material prepared by the preparation method of the porous carbon material in any one of the embodiments.
The invention provides a catalyst for CO2Adsorption-separated ZnO-modified amino-modified porous carbon material, and adsorption-separated ZnO-modified amino-modified porous carbon materialThe low-cost and commercialized porous activated carbon is used as a carrier, ZnO modification and amino modification are adopted, active components are uniformly distributed, and CO can be enhanced2Surface activation effect to make the porous carbon material and CO2Stronger acting force between them, CO2Is not easy to be separated. The modification by ZnO can enhance CO2Surface activation effect of (2) can activate CO2The carbon-oxygen bond effectively solves the problems of the porous carbon material and CO2The weak adsorption force causes CO2The problem of escape. Moreover, ZnO modification and amino modification are adopted, and CO can be adsorbed by chemical action with high selectivity2The air conditioner is basically not interfered by other gases, and can be suitable for narrow closed/semi-closed spaces with complicated air components. The method adopts commercial porous carbon with low cost and wide preparation raw materials as a carrier, and increases CO by utilizing developed pore structure and high specific surface area of the porous carbon2The contact area with the adsorbing material can effectively remove CO2Adsorbed onto porous carbon. The porous carbon material has the advantages of simple preparation process, low production cost, easy implementation and good economic benefit and social value.
The following are specific examples.
Example 1: dissolving 1.39g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Example 2: dissolving 2.35g of ammonium nitrate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Example 3: dissolving 1.33g of ammonium chloride and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and drying for 2h at 100 ℃ to obtain the final composite material.
Example 4: dissolving 1.39g of ammonium carbonate and 1g of zinc chloride in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Example 5: dissolving 1.39g of ammonium carbonate and 1g of zinc nitrate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Example 6: dissolving 1.39g of ammonium carbonate and 1g of zinc nitrate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 5h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Example 7: dissolving 1.39g of ammonium carbonate and 1g of zinc nitrate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 5h, evaporating the solvent, and treating at 200 ℃ for 2h to obtain the final composite material.
Example 8: dissolving 1.39g of ammonium carbonate and 1g of zinc nitrate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 11, stirring for 5h, evaporating the solvent, and treating at 200 ℃ for 2h to obtain the final composite material.
Example 9: dissolving 1.39g of ammonium carbonate and 1g of zinc nitrate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 5h, evaporating the solvent, and treating at 200 ℃ for 6h to obtain the final composite material.
Example 10: dissolving 5g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Example 11: dissolving 0.2g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and drying for 2h at 100 ℃ to obtain the final composite material.
Example 12: dissolving 20g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Example 13: dissolving 1.39g of ammonium carbonate and 0.1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and drying for 2h at 100 ℃ to obtain the final composite material.
Example 14: dissolving 1.39g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coal-based activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Example 15: dissolving 1.39g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 8g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 9, stirring for 5h, evaporating the solvent, and treating at 200 ℃ for 2h to obtain the final composite material.
Example 16: dissolving 1.39g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 10g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 5h, evaporating the solvent, and treating at 190 ℃ for 2h to obtain the final composite material.
Example 17: dissolving 1.39g of ammonium carbonate and 1g of zinc sulfate in 100mL of ethanol, stirring to fully dissolve, then adding 9g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 190 ℃ for 3h to obtain the final composite material.
Example 18: dissolving 1.39g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at the high temperature of 300 ℃ for 2h to obtain the final composite material.
Example 19: dissolving 1.39g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating for 2h at 50 ℃ to obtain the final composite material.
Example 20: dissolving 1.39g of ammonium carbonate and 1g of zinc sulfate in 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and performing high-temperature treatment at 100 ℃ for 24h to obtain the final composite material.
Example 21: dissolving 1.39g of ammonium carbonate into 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 5h, evaporating the solvent, and treating at 200 ℃ for 2h to obtain the final composite material.
Example 22: dissolving 1g of zinc sulfate into 50mL of ethanol, stirring to fully dissolve, then adding 5g of coconut shell activated carbon, dropwise adding ammonia water, adjusting the pH value to 8, stirring for 1h, evaporating the solvent, and treating at 100 ℃ for 2h to obtain the final composite material.
Table 1 shows the CO of each example2And (5) the adsorption performance characterization result.
TABLE 1
Figure BDA0003116851470000091
Comparison of example 21 and example 7 shows that the addition of ZnO improves the CO control2The adsorption performance of the adsorbent shows that the ZnO and the amino group have a coordination function, so that the adsorbent and the CO have the same activity2The acting force between the two parts is stronger and is not easy to separate. Example 22 and example 1 compare and show that amino modification improves the CO of porous carbon2The adsorption performance of the adsorbent shows that the ZnO and the amino group have a coordination function, so that the adsorbent and the CO have the same activity2The acting force between the two parts is stronger and is not easy to separate. Comparison of example 18 and example 1 shows that the temperature for heat drying is set to CO of the obtained porous carbon2Has an important influence on the adsorption performance, and the activity of the porous carbon or the zinc oxide or the amino group loaded on the porous carbon can be reduced due to the overhigh drying temperature. Comparison of example 19 and example 1 shows that the temperature for heat drying is higher than the CO content of the obtained porous carbon2The adsorption performance of (A) has an important influence, and too low a drying temperature may not make the activated carbon sufficiently or firmly fixedSolid supported zinc oxide or amino groups. Comparison of example 20 with example 1 shows that the drying time for the CO of the porous carbon obtained2Has a significant effect that an excessively long drying time may reduce the activity of the porous carbon or the zinc oxide or amino group supported thereon. Comparison of example 11 with example 1 shows that excessive addition of ammonium carbonate affects the CO2 adsorption performance of the final porous carbon. Comparison of example 12 with example 1 shows that too small an amount of ammonium carbonate, outside the proper range, will affect the CO content of the final porous carbon2The adsorption performance of (3). Comparison of example 13 with example 1 shows that addition of the zinc oxide precursor salt in an amount too small to be within a suitable range will affect the CO of the finally obtained porous carbon2The adsorption performance of (3). The above embodiment shows that different precursor salts all affect the adsorption performance, wherein ammonium carbonate is used as the ammonium salt, zinc nitrate is used as the zinc salt, and the adsorption performance is optimal; the comparative examples show that the pH, the stirring time, the drying temperature and the drying time all affect the adsorption performance of the material. When the pH value is 8, the mixture is stirred for 5h and dried for 2h at 200 ℃, the composite material is provided with the most suitable synthesis condition and has the most suitable adsorption performance.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, so as to understand the technical solutions of the present invention specifically and in detail, but not to be understood as the limitation of the patent protection scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the patent of the invention is subject to the appended claims, and the description can be used for explaining the contents of the claims.

Claims (10)

1. A method for producing a porous carbon material, characterized by comprising the steps of:
dispersing ammonium salt, zinc oxide precursor salt and porous carbon in a solvent to obtain a precursor mixed solution;
and adjusting the pH value of the precursor mixed solution to 8-11, and performing high-temperature compounding on solid components in the precursor mixed solution.
2. The method for producing a porous carbon material according to claim 1, wherein the solid component is obtained by evaporating a solvent, and the temperature of the high-temperature compounding is 100 to 200 ℃ for 2 to 8 hours.
3. The preparation method of the porous carbon material according to claim 2, wherein the pH of the precursor mixed solution is adjusted to 8-9, the temperature of the high-temperature compounding is 190-200 ℃, and the time is 2-3 h.
4. The method for producing a porous carbon material according to claim 1, wherein the ammonium salt is one or more selected from ammonium carbonate, ammonium nitrate, and ammonium chloride.
5. The method for producing a porous carbon material according to claim 1, wherein the zinc oxide precursor salt is one or more selected from zinc sulfate, zinc nitrate, and zinc chloride.
6. The method for producing a porous carbon material according to claim 1, wherein the ammonium salt is ammonium carbonate and the zinc oxide precursor salt is zinc nitrate.
7. The method for producing a porous carbon material according to claim 1, wherein the porous carbon is selected from activated carbon produced from one or more of coconut shell, coal, and wood.
8. The method for producing a porous carbon material according to any one of claims 1 to 7, wherein the mass ratio of the ammonium salt to the zinc oxide precursor salt is 1 to 10.
9. The method for producing a porous carbon material according to claim 8, wherein the mass ratio of the porous carbon to the zinc oxide precursor salt is 5 to 10.
10. The porous carbon material produced by the method for producing a porous carbon material according to any one of claims 1 to 9.
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