CN108786733B - Nano-pore carbon sphere CO with micron scale2Method for preparing adsorbent - Google Patents

Nano-pore carbon sphere CO with micron scale2Method for preparing adsorbent Download PDF

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CN108786733B
CN108786733B CN201810636914.5A CN201810636914A CN108786733B CN 108786733 B CN108786733 B CN 108786733B CN 201810636914 A CN201810636914 A CN 201810636914A CN 108786733 B CN108786733 B CN 108786733B
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adsorbent
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carbon sphere
salt
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CN108786733A (en
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蔡进军
吴星星
任猛
王跃林
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Xiangtan University
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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
    • B01J20/28—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
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
    • 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
    • B01J20/28078—Pore diameter
    • B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
    • 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 nano-pore carbon sphere CO with micron scale2A preparation method of the adsorbent. Firstly, milk and salt with certain concentration are subjected to high-pressure thermal polycondensation in a reaction kettle to obtain a precursor; then, pre-carbonizing the hydrothermal precursor, mixing and grinding the pre-carbonized hydrothermal precursor with KOH, and carrying out high-temperature activation reaction; and (3) carrying out acid treatment, water washing and drying to obtain the nano-pore carbon sphere adsorbent with the high specific surface area and the micron-scale structure. The invention provides a nanoporous carbon sphere CO2The specific surface area of the adsorbent reaches 2091m2In terms of a/g, all pore sizes are in the microporous region, the particle size is about 5 microns, and the CO content is relatively high at zero degrees Celsius and atmospheric pressure2Adsorption amount, CO2/N2Adsorption selectivity and cyclic regeneration performance. The preparation method of the adsorbent is simple to operate, can realize resource recycling by taking the milk which is extremely easy to acidify and decay as a carbon source, successfully solves the problem of milk deterioration waste, and effectively reduces CO in the atmosphere2Concentration, and alleviating greenhouse effect.

Description

Nano-pore carbon sphere CO with micron scale2Method for preparing adsorbent
Technical Field
The invention relates to activated carbon, in particular to a micron-scale nano-pore carbon sphere CO2A preparation method of the adsorbent.
Background
Air pollution has always been a serious problem facing human society, and the excessive use of fossil fuels makes the air pollution problem more serious, such as global warming caused by greenhouse effect. Among the numerous greenhouse gases, CO2The characteristics of high content, long service life and the like are considered to be the most main causes of greenhouse effect. In the long run, the development of new clean energy is CO reduction2The optimal solution of the emission is achieved, but the new energy is still difficult to replace fossil energy due to the restriction of objective factors such as high cost, immature technology and the like. Fossil fuels remain the dominant energy resource available at present, and research has shown that thermal power plants contribute approximately 50% of CO by the year 20302Incremental emissions, and thus attempts to reduce CO by reducing fossil fuel use2The purpose of emission is not in line with the requirement of the times, and CO is effectively captured2Is the most promising method for solving the greenhouse effect at the present stage. Tradition ofCO recovery by organic amine solution chemical absorption2High efficiency, but has the defects of high cost, large energy consumption, strong corrosivity and the like. CO capture by solid adsorbent using pressure swing adsorption technology2Has the characteristics of low energy consumption, no corrosion, long service life and the like, has great prospect in the aspect of replacing organic amine chemical absorption, and develops high-efficiency CO2Porous adsorbents with adsorption properties are at hand.
Various solid adsorbents such as molecular sieves, metal organic frameworks, polymers, porous silicon, porous carbon materials and the like have been developed for CO2And (4) adsorbing. In terms of adsorption capacity, the metal organic framework and the porous carbon material are two adsorbents with the largest adsorption capacity at present, and particularly, the literature reports the existing CO of the metal organic framework at normal temperature and normal pressure2The adsorption amount is up to 8.5mmol/g (J.Am. chem. Soc., 2009, 131: 18198-18199). However, the metal organic framework has a complex preparation process, expensive raw material cost and high requirement on the environmental humidity of the adsorbent, so that the metal organic framework is limited in specific practical application. Compared with a metal organic framework, the porous carbon material has the advantages of large specific surface area, adjustable pore structure, good stability and the like, particularly simple preparation process and low cost, and the characteristics ensure that the porous carbon material is applied to CO2The adsorption field has huge practical application potential. Is currently used for CO2The adsorbed porous carbon materials are mainly active carbon with high specific surface area obtained by adopting a chemical activation/physical activation method, and the active carbon has no specific regular morphology. More recently, Jaronie et al reported a CO2The physical activation method is used for preparing the phenolic resin-based carbon microspheres, the particle size of the carbon microspheres is about 0.5 micron, and the specific surface area is as high as 2900m2In g, morphology of these microspheres vs. CO2The adsorption may have certain enhancement effect, namely CO at normal temperature and normal pressure2The adsorption amount reaches 4.55mmol/g (ACS appl. Mater Interface, 2013, 5: 1849-1855). Investigation and discovery aim at CO2The carbon microsphere adsorbent which is trapped efficiently is not abundant, and the carbon microsphere adsorbent with the micron scale larger than 2 microns is not available. Therefore, a low-cost nano-pore carbon sphere with micron scale is developed and applied to CO2High efficiency adsorption is necessary。
The milk is a natural animal metabolite rich in protein, is rich in other essential minerals for human bodies, and is a common drinking nutrient in daily life. However, milk itself is extremely easy to acidify and decay, and if deteriorated milk is directly poured into a waste water tank or used for irrigating farmlands, serious waste is caused, so that how to effectively utilize the milk is very important. Therefore, the deteriorated milk is converted into the high-added-value nano-pore carbon material, so that the resource utilization of waste can be effectively realized, and good economic value is created. Wang et al prepared specific surface area 1749m by using soybean milk powder as raw material and by silica sol template method2(iii) a hierarchical porous carbon material, which as electrode material retains 96% specific capacitance after 5000 cycles in 6M KOH (electrochimica acta, 2018, 261: 49-57). Ogale et al uses yoghourt as a carbon source, carries out hydrothermal carbonization, mixes the carbonized yoghourt with KOH in one step, grinds and activates to prepare a nitrogen-rich carbon material, and uses the nitrogen-rich carbon material as an electrode material at 1M H2SO4The specific capacitance at medium 2A/g can reach 225F/g, and the specific capacitance at 20A/g can still reach 200F/g (Journal of Materials Chemistry A, 2014, 3: 1208-. It is worth noting that none of the nanoporous carbon materials obtained by using the milk product as the carbon source in the above reports contain the micron spherical morphology. After the literature retrieval, the application of the porous carbon prepared by taking milk as the raw material in CO is found2Adsorption also belongs to the blank field. The invention takes milk as a carbon source to prepare the nano-pore carbon microsphere CO with the particle size of 5 microns2The adsorbent has simple preparation process and good CO2The adsorption selectivity and the regeneration performance provide a new way for the high-value recycling of the acidified putrid milk.
Disclosure of Invention
The invention aims to provide a micron-scale nano-pore carbon sphere CO2The preparation method of the adsorbent comprises the steps of mixing fresh milk solution serving as a carbon source with salt with a certain concentration, and then carrying out hydrothermal carbonization reaction; then pre-carbonizing to obtain pre-carbide; grinding the carbon nano-particles with an activating agent and then carrying out high-temperature activation treatment to obtain the nano-porous carbon micro-particles CO with good micron scale2An adsorbent; the method specifically comprises the following steps:
(1) dissolving salt in a milk solution, placing the milk solution in a polytetrafluoroethylene hydrothermal reaction kettle, and reacting for 12-72 hours at 130-240 ℃ to obtain a hydrothermal carbon precursor, wherein the hydrothermal carbon precursor can show different appearance colors such as brown yellow, brown, black and the like due to different reaction conditions;
(2) washing the hydrothermal carbon precursor with deionized water to obtain salt, drying, and performing a pre-carbonization reaction in a nitrogen atmosphere to completely convert the salt into black pre-carbide;
(3) mixing and grinding black pre-carbide and an activating agent KOH, and then carrying out activation treatment;
(4) acid washing, water washing and drying the activated carbide to obtain the nano-pore carbon spheres CO with micron scale2An adsorbent.
Further, in the step (1), the salt is preferably chloride, more preferably NaCl, KCl, LiCl, ZnCl2、CaCl2One or more than two of the above; the amount of the salt is 30-200 g/L, namely 3-20 g of the salt is added into every 100mL of milk solution.
Further, in the step (2), the salt washing process is carried out at the temperature of 60-90 ℃; the drying temperature is 100-140 ℃.
Further, in the step (2), the temperature of the pre-carbonization is 400-600 ℃, the time is 1-4 hours, and the temperature rise rate is 2-10 ℃/min.
Further, in the step (3), the mass ratio of the black pre-carbide to the activator KOH is 1: 1.5 to 3.
Further, in the step (3), the temperature of the activation treatment is 600-900 ℃, the time is 1-4 hours, and the temperature rise rate is 1-4 ℃/min.
Further, in the step (4), 2mol/L hydrochloric acid solution is adopted for acid washing, the acid washing temperature is 60 ℃, and the acid washing time is 2 hours.
The invention has the beneficial effects that:
according to the invention, the growth of the size of spherical particles can be promoted by adding salt in the hydrothermal carbonization process, the spherical shape is not damaged by activating with a specific activating agent KOH, all the pore diameters of the obtained material are located in the microporous region, and the particle size is about5 microns, the adsorbent has developed micropore pores and specific surface area as high as 2091m2A/g, higher CO at zero degrees Celsius and atmospheric pressure2Adsorption amount, CO2/N2Adsorption selectivity and cyclic regeneration performance. The preparation method of the adsorbent is simple to operate, can realize resource recycling by taking the milk which is extremely easy to acidify and decay as a carbon source, successfully solves the problem of milk deterioration waste, and effectively reduces CO in the atmosphere2Concentration, and alleviating greenhouse effect.
Drawings
Fig. 1 is a scanning electron microscope topography of the microspheroidal carbon adsorbent obtained in example 1.
Fig. 2 is an adsorption isotherm diagram of the microspheroidal carbon adsorbent obtained in example 1 at a nitrogen gas liquid nitrogen temperature.
FIG. 3 is a graph showing the pore size distribution of the microspheroidal carbon adsorbent obtained in example 1.
FIG. 4 shows the adsorption of microspheroidal carbon obtained in example 1 on CO2And N2Adsorption isotherm plot at 0 ℃.
Fig. 5 is a graph of the adsorptive regeneration performance of the microspheroidal carbon adsorbent obtained in example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
60mL of fresh milk solution is poured into a 100mL of hydrothermal reaction kettle with a polytetrafluoroethylene lining, and 6g of ZnCl is accurately weighed at the same time2Performing hydrothermal carbonization reaction on the @ KCl mixed salt (the molar ratio is 1: 1) at the constant temperature of 180 ℃ for 24 hours, washing the precipitate with a large amount of deionized water, and drying at 120 ℃ to obtain black powder; placing black powder in a nitrogen atmosphere tube furnace, heating to 500 ℃ at the speed of 2 ℃/min, and carrying out pre-carbonization treatment for 2h at constant temperature; and grinding the obtained pre-carbide and 2 times of KOH by mass, and heating to 800 ℃ at the speed of 2 ℃/min in a nitrogen atmosphere tube furnace for activation treatment for 1 h. And (3) taking out the sample after cooling, washing by using 2mol/L HCl solution, washing by using deionized water, and drying to obtain the nano-pore carbon spheres with the micron scale. The adsorbent specific surface area obtained from the nitrogen adsorption isotherm was 2091m2In terms of the number of microspheres in the microsphere, the number of pores is in the micropore region of less than 2 nm, as shown in FIGS. 2-3, and the size of the microspheres is about 5 μm, as shown in FIG. 1.
The adsorption test comprises the following specific steps: vacuum high-temperature degassing activation treatment (200 deg.C, 10h) is carried out on a volume method physical adsorption apparatus (Quantachrome Nova 4200e), and then CO is carried out2And N2Gas adsorption test at zero degrees and atmospheric pressure. The results show that CO2The adsorption capacity at 0 ℃ was 6.7mmol/g, at 1bar with N2The adsorption selectivity of (A) is as high as 37 times, as shown in FIG. 4. By the reaction of CO2The adsorption was subjected to a continuous cycle test, and it was found that the decrease in the adsorption amount was not large after 10 cycles, confirming that the cycle performance was excellent, as shown in fig. 5.
Example 2
60mL of fresh milk solution is poured into a 100mL of hydrothermal reaction kettle with a polytetrafluoroethylene lining, and 6g of ZnCl is accurately weighed at the same time2Performing hydrothermal carbonization reaction on the @ KCl mixed salt (the molar ratio is 1: 1) at the constant temperature of 180 ℃ for 24 hours, washing the precipitate with a large amount of deionized water, and drying at 120 ℃ to obtain black powder; placing black powder in a nitrogen atmosphere tube furnace, heating to 500 ℃ at the speed of 2 ℃/min, and carrying out pre-carbonization treatment for 2h at constant temperature; and grinding the obtained pre-carbide and 2 times of KOH by mass, and heating to 600 ℃ at the speed of 2 ℃/min in a nitrogen atmosphere tube furnace for activation treatment for 1 h. And (3) taking out the sample after cooling, washing by using 2mol/L HCl solution, washing by using deionized water, and drying to obtain the nano-pore carbon spheres with the micron scale. The adsorbent specific surface area obtained from the nitrogen adsorption isotherm was 1041m2/g。
Example 3
Pouring 60mL of fresh milk solution into a 100mL of hydrothermal reaction kettle with a polytetrafluoroethylene lining, simultaneously accurately weighing 6g of LiCl @ KCl mixed salt (the molar ratio is 1: 1), carrying out hydrothermal carbonization reaction at the constant temperature of 180 ℃ for 24h, washing precipitates with a large amount of deionized water, and drying at 120 ℃ to obtain black powder; placing black powder in a nitrogen atmosphere tube furnace, heating to 500 ℃ at the speed of 2 ℃/min, and carrying out pre-carbonization treatment for 2h at constant temperature; grinding the obtained pre-carbide with 2 times of KOH by mass in a nitrogen atmosphere tube furnace at the speed of 2 ℃/mAnd (3) increasing the in rate to 800 ℃ for activation treatment for 1 h. And (3) taking out the sample after cooling, washing by using 2mol/L HCl solution, washing by using deionized water, and drying to obtain the nano-pore carbon spheres with the micron scale. The specific surface area of the adsorbent obtained from the nitrogen adsorption isotherm was 1961m2/g。
Example 4
Pouring 60mL of fresh milk solution into a 100mL of hydrothermal reaction kettle with a polytetrafluoroethylene lining, simultaneously accurately weighing 6g of LiCl @ KCl mixed salt (the molar ratio is 1: 1), carrying out hydrothermal carbonization reaction at the constant temperature of 130 ℃ for 24h, washing the precipitate with a large amount of deionized water, and drying at 120 ℃ to obtain brown yellow powder; placing the brown yellow powder in a nitrogen atmosphere tube furnace, heating to 500 ℃ at the speed of 2 ℃/min, and carrying out pre-carbonization treatment for 2h at constant temperature; and grinding the obtained black pre-carbide and 2 times of KOH by mass, and heating to 800 ℃ at the speed of 2 ℃/min in a nitrogen atmosphere tubular furnace for activation treatment for 1 h. And (3) taking out the sample after cooling, washing by using 2mol/L HCl solution, washing by using deionized water, and drying to obtain the nano-pore carbon spheres with the micron scale. The adsorbent obtained from the nitrogen adsorption isotherm had a specific surface area of 1600 m2/g。

Claims (7)

1. Nano-pore carbon sphere CO with micron scale2The preparation method of the adsorbent is characterized by comprising the following steps:
(1) dissolving salt in a milk solution, placing the milk solution in a polytetrafluoroethylene hydrothermal reaction kettle, and reacting for 12-72 hours at 130-240 ℃ to obtain a hydrothermal carbon precursor;
(2) washing the hydrothermal carbon precursor with heated deionized water to remove salt, drying, and performing a pre-carbonization reaction in a nitrogen atmosphere to completely convert the hydrothermal carbon precursor into black pre-carbide;
(3) mixing and grinding black pre-carbide and an activating agent KOH, and then carrying out activation treatment;
(4) acid washing, water washing and drying the activated carbide to obtain the nano-pore carbon spheres CO with micron scale2An adsorbent;
in the step (1), the salt is NaCl, KCl, LiCl or ZnCl2、CaCl2One or more than two of。
2. The micro-nano-porous carbon sphere CO of claim 12The preparation method of the adsorbent is characterized in that in the step (1), the amount of the salt is 30-200 g/L, namely 3-20 g of salt is added into 100mL of milk solution.
3. The micro-nano-porous carbon sphere CO of claim 12The preparation method of the adsorbent is characterized in that in the step (2), the salt washing process is carried out at the temperature of 60-90 ℃; the drying temperature is 100-140 ℃.
4. The micro-nano-porous carbon sphere CO of claim 12The preparation method of the adsorbent is characterized in that in the step (2), the pre-carbonization temperature is 400-600 ℃, the time is 1-4 hours, and the heating rate is 2-10 ℃/min.
5. The micro-nano-porous carbon sphere CO of claim 12The preparation method of the adsorbent is characterized in that in the step (3), the mass ratio of the black pre-carbide to the activating agent KOH is 1: 1.5 to 3.
6. The micro-nano-porous carbon sphere CO of claim 12The preparation method of the adsorbent is characterized in that in the step (3), the temperature of the activation treatment is 600-900 ℃, the time is 1-4 hours, and the temperature rise rate is 1-4 ℃/min.
7. The micro-nano-porous carbon sphere CO of claim 12The preparation method of the adsorbent is characterized in that in the step (4), 2mol/L hydrochloric acid solution is adopted for acid washing, the acid washing temperature is 60 ℃, and the time is 2 hours.
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