CN110975814A - Preparation method of nickel oxide loaded modified activated carbon fiber adsorbent - Google Patents
Preparation method of nickel oxide loaded modified activated carbon fiber adsorbent Download PDFInfo
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- CN110975814A CN110975814A CN201911327845.0A CN201911327845A CN110975814A CN 110975814 A CN110975814 A CN 110975814A CN 201911327845 A CN201911327845 A CN 201911327845A CN 110975814 A CN110975814 A CN 110975814A
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- 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
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- 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
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- 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
- B01J20/28014—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 form
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0084—Solid storage mediums characterised by their shape, e.g. pellets, sintered shaped bodies, sheets, porous compacts, spongy metals, hollow particles, solids with cavities, layered solids
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Abstract
The invention belongs to the technical field of carbon material adsorption, and provides a preparation method of a nickel oxide loaded modified activated carbon fiber adsorbent. The method comprises the following steps: (1) pretreating the activated carbon fiber; (2) dipping the activated carbon fiber; (3) and (3) preparing the loaded nickel oxide activated carbon fiber. The preparation method is simple, when the activated carbon fiber is impregnated, the mixture is subjected to ultrasonic oscillation, so that the metal salt is fully loaded on the surface of the activated carbon fiber, and after modification, the hydrogen storage performance of the activated carbon fiber is improved by 28.4%, thereby providing a more effective treatment method and a research direction for adsorption, separation and storage of hydrogen.
Description
Technical Field
The invention belongs to the technical field of carbon material adsorption, and particularly relates to a preparation method of a nickel oxide loaded modified activated carbon fiber adsorbent, which is applied to hydrogen storage.
Background
With the development of human society, the demand of people for energy is increasing day by day, the traditional fossil energy not only has the gradual reduction of reserves, but also causes huge pollution to the environment, and therefore, the search for green renewable energy becomes an important task of human beings at present. The hydrogen energy is a novel renewable energy source, and has the advantages of wide source, high heat value, no pollution of products and the like. However, the development of hydrogen storage materials is a major bottleneck restricting the utilization of hydrogen energy, and the hydrogen storage capacity of the current hydrogen storage materials is far from the requirement of the U.S. department of energy. There are many methods for separation and storage of hydrogen, such as metal hydride storage, organic storage, adsorption storage, and the like. Among many hydrogen storage materials, the carbon-based material has the advantages of high specific surface area, uniform pore size distribution, mostly micropores, high adsorption and desorption speeds, stable chemical properties, good regeneration performance and the like. In recent years, carbon-based materials such as carbon nanotubes, mesoporous carbon, and novel activated carbon have come into the visual field of people.
The activated carbon fiber hydrogen storage is mainly affected by the specific surface area, micropore volume and surface chemical properties. However, in order to obtain an activated carbon fiber with a larger hydrogen storage capacity, the activated carbon fiber needs to be modified mainly from the pore structure and surface properties. The method for modifying the carbon material by impregnating the carbon material with metal salt so that the surface of the carbon material is loaded with the metal salt or the metal oxide is a common means for modifying the activated carbon. Takagi et al supported platinum and palladium on activated carbon fibers and showed a significant increase in hydrogen storage at 30 ℃ and 1bar to 0.61 wt.%, indicating that chemisorption of hydrogen onto metals occurred. Moradi et al prepared high specific surface and high pore volume activated carbon by microwave heating and modified with ferric nitrate to load ferric oxide with hydrogen storage of 1.45 wt.% under 303K, 20 bar. Cristia i.contesecu et al prepared and performed relevant characterization on activated carbon fibers containing palladium salt, and the results showed that the hydrogen storage amount reached 2.5 wt.% under 77K, 2MPa conditions. The increase of hydrogen storage amount caused by the overflow effect of hydrogen molecules on the transition metal and oxide nano particles is very obvious, and the surface modification of the activated carbon fiber has good application prospect. In conclusion, the hydrogen storage capacity of the activated carbon fiber prepared by the prior art does not reach the ideal hydrogen adsorption capacity, so that the hydrogen storage capacity is improved by the surface modification research of the activated carbon fiber, and the method is easy to operate and saves the cost.
Disclosure of Invention
The invention aims to solve the problems and provide a preparation method for preparing a modified activated carbon fiber adsorbent with a nickel oxide loaded on the surface.
The technical scheme of the invention is as follows:
a preparation method of a nickel oxide loaded modified activated carbon fiber adsorbent comprises the following steps:
(1) pretreatment of the activated carbon fiber: cutting the activated carbon fiber into squares, carrying out ultrasonic treatment in deionized water, and drying;
(2) impregnation of activated carbon fiber: soaking the cleaned activated carbon fiber in a nickel nitrate solution, ultrasonically vibrating, stirring in a water bath kettle, washing to be neutral, and drying for later use;
(3) preparing the nickel oxide loaded activated carbon fiber: and (3) placing the impregnated and dried activated carbon fiber in a tubular furnace, heating to 600-900 ℃ according to a program of 1-10 ℃/min under the protection of inert gas, and roasting or treating with microwave power of 2-5 kW for 15-60 min to obtain the nickel oxide loaded activated carbon fiber.
The nickel oxide is replaced by copper oxide or samarium oxide.
The specific surface area of the activated carbon fiber is 1019.2m2G, pore volume 0.5cm3/g。
In the step (2), the mixture is subjected to ultrasonic oscillation for 0.25 to 2 hours.
The nickel oxide, copper oxide or samarium oxide loaded modified activated carbon fiber adsorbent is applied to hydrogen storage, and the hydrogen storage performance of the modified activated carbon fiber is improved by 28.4%.
Compared with the prior art, the invention has the beneficial effects that:
(1) the activated carbon fiber adsorbent with the surface loaded with nickel oxide, which is prepared by adopting nickel nitrate to dip and modify activated carbon fiber and roasting, has a good microporous structure.
(2) The mixture of the activated carbon fiber and the salt solution is subjected to ultrasonic vibration, so that the metal salt can be uniformly dispersed on the surface of the activated carbon fiber and in the pore channel, and the load is more uniform.
(3) The metal oxide selected for loading is the oxide of the nickel of the eighth group and the samarium of the third sub-group.
(4) After dipping, roasting can decompose the metal salt into oxide, the oxide is combined with the wall of the activated carbon fiber hole more tightly, and the microporous structure is richer after roasting, which is beneficial to storing hydrogen.
(5) After the nickel oxide is loaded on the surface of the activated carbon fiber, the roughness of the inner surface and the roughness of the outer surface of the activated carbon fiber are increased, and the acting force field is enhanced, so that the stress is increased when hydrogen molecules contact the activated carbon fiber, and the adsorption capacity of hydrogen is improved by 28.4% compared with the original activated carbon fiber.
(6) The nickel oxide-loaded activated carbon fiber adsorbent has good hydrogen adsorption capacity under the conditions of 77K and 1bar, and has the advantages of safe and easily obtained adsorption conditions and simple and convenient operation.
Drawings
FIG. 1 shows N of the raw activated carbon fibers of example 1, comparative example and2adsorption-removal of attached figure.
FIG. 2 is a graph showing the pore size distribution of the raw activated carbon fibers of example 1 and comparative example.
Fig. 3 is an SEM image of the raw activated carbon fiber.
FIG. 4 is an SEM photograph of sample No. 11 of example 1.
FIG. 5 is an SEM photograph of sample No. 16 in example 1.
FIG. 6 is an SEM photograph of sample No. 21 in example 1.
FIG. 7 is an XPS spectrum of example 1.
FIG. 8 is a hydrogen sorption isotherm of example 1, comparative example, and activated carbon fiber stock.
Fig. 9 is a graph showing the main effect of hydrogen storage amount of the activated carbon fiber loaded with nickel oxide in example 1 and other different conditions.
FIG. 10 is a flow chart of a manufacturing process of the present invention.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
1. Example 1 (Experimental data, group 11)
Weighing 0.6g of cleaned activated carbon fiber, soaking in 80ml of nickel nitrate solution with the mass fraction of 0.5 wt.%, ultrasonically shaking for 30min, placing in a water bath kettle, stirring for 6h, washing to be neutral, placing in an oven at 80 ℃ for overnight, and taking out for later use. The impregnated and dried activated carbon fiber is put in a tube furnace to be heated to 600 ℃ at the heating rate of 6 ℃/min under the condition of nitrogen, and after the temperature is maintained for 60min, the activated carbon fiber is recovered to the room temperature at the same rate, and the activated carbon fiber loaded with the nickel oxide is prepared, wherein the nitrogen adsorption and desorption, the pore size distribution, the SEM, the XPS and the hydrogen storage performance of the adsorbent are shown in figures 1, 2, 4, 7 and 8.
2. Example 2
Weighing 0.6g of cleaned activated carbon fiber, soaking in 80ml of samarium nitrate solution with the mass fraction of 0.5 wt.%, ultrasonically shaking for 30min, placing in a water bath, stirring for 6h, washing to neutrality, placing in an oven at 80 ℃ for overnight, and taking out for later use. And (3) putting the impregnated and dried activated carbon fiber into a tubular furnace, heating to 600 ℃ at the heating rate of 6 ℃/min under the condition of nitrogen, keeping for 60min, and then recovering to room temperature at the same rate to obtain the samarium oxide-loaded activated carbon fiber.
3. Example 3
Weighing 0.6g of cleaned activated carbon fiber, soaking in 80ml of 0.5 wt.% copper nitrate solution, ultrasonically shaking for 30min, stirring in a water bath for 6h, washing to neutrality, placing in an oven at 80 ℃ overnight, and taking out for later use. And (3) putting the impregnated and dried activated carbon fiber into a tubular furnace, heating to 600 ℃ at the heating rate of 6 ℃/min under the condition of nitrogen, keeping for 60min, and then recovering to room temperature at the same rate to obtain the samarium oxide-loaded activated carbon fiber.
4. Example 4
Weighing 0.6g of cleaned activated carbon fiber, soaking in 80ml of nickel nitrate solution with the mass fraction of 0.5 wt.%, ultrasonically shaking for 30min, placing in a water bath kettle, stirring for 6h, washing to be neutral, placing in an oven at 80 ℃ for overnight, and taking out for later use. And (3) treating the impregnated and dried activated carbon fiber for 60min at the microwave power of 3kW to prepare the nickel oxide loaded activated carbon fiber.
5. Comparative example
Weighing 0.6g of cleaned activated carbon fiber, placing the fiber in a tubular furnace, heating to 600 ℃ at the heating rate of 6 ℃/min under the condition of nitrogen, keeping the temperature for 60min, and then recovering to room temperature at the same rate to obtain the activated carbon fiber which is only subjected to thermal activation treatment.
6. Test analysis shows that, compared with the comparative example and the original sample, in the example 1, the roughness of the inner surface and the roughness of the outer surface of the activated carbon fiber are increased due to the nickel oxide loading, and the acting force field is enhanced, so that the stress is increased when hydrogen molecules contact the activated carbon fiber, the adsorption quantity of hydrogen is increased, the hydrogen storage capacity of the material is greatly improved, and the hydrogen adsorption capacity is improved by 28.4%.
7. Design of L by orthogonal analysis25(65) And 25 groups of orthogonal experiments are used for inspecting the influence of the impregnation concentration A, the impregnation time B, the impregnation temperature C, the temperature rise rate D, the activation temperature E and the constant temperature time F on the hydrogen storage amount and the optimal modification conditions when the nickel salt is used for modifying the activated carbon fiber.
Samples No. 1-25, all of which are activated carbon fiber adsorbents with nickel oxide loaded on the surfaces, have certain hydrogen adsorption capacity and show a certain rule, and the rule is shown in FIG. 9.
Evaluation of hydrogen adsorption capacity of the adsorbent Using a Cahn-2000 high vacuum electronic balance system apparatus, the experimental method employed was mass analysis. The experimental process comprises four steps of adsorption weighing, adsorbent vacuum thermal desorption, system hydrogen purging and adsorption testing. Firstly, placing the adsorbent on a balance tray for weighing; and (4) covering a glass cover, pumping the system to vacuum by using a vacuum pump for heat desorption, recovering to room temperature after balancing, and purging the system by using hydrogen. During adsorption, balance adsorption balance amounts at 77K and hydrogen pressures of 5, 10, 15, 20, 25, 30, 50, 70 and 100kPa were recorded. The hydrogen adsorption performance of example 1 and the comparative example are shown in table 1.
The test result shows that in the embodiment 1, the roughness of the inner surface and the roughness of the outer surface of the activated carbon fiber are increased due to the nickel oxide loading, and the acting force field is enhanced, so that the stress is increased when hydrogen molecules contact the activated carbon fiber, and the adsorption quantity of hydrogen is increased; the mean value of the micropores is reduced, and the pore structure is more favorable for storing hydrogen, so that the hydrogen storage capacity of the material is greatly improved, and the hydrogen adsorption capacity is improved by 28.4%.
A series of activated carbon fiber adsorbents loaded with nickel oxide are prepared according to the method, the influence of A impregnation concentration, B impregnation time, C impregnation temperature, D heating rate, E activation temperature and F constant temperature time on hydrogen storage amount and the optimal conditions are marked as No. 1-25 when the activated carbon fiber is modified by an orthogonal analysis method, and tests show that the hydrogen storage amount is improved more or less after nickel oxide is loaded. The results of the hydrogen storage properties are shown in Table 2.
TABLE 1 hydrogen storage Properties of examples 1 and 2, comparative example, and raw activated carbon fiber
TABLE 2 Hydrogen sorption performance index of nickel oxide loaded modified activated carbon fiber
Claims (8)
1. A preparation method of a nickel oxide loaded modified activated carbon fiber adsorbent is characterized by comprising the following steps:
(1) pretreatment of the activated carbon fiber: cutting the activated carbon fiber into squares, carrying out ultrasonic treatment in deionized water, and drying;
(2) impregnation of activated carbon fiber: soaking the cleaned activated carbon fiber in a nickel nitrate solution, ultrasonically vibrating, stirring in a water bath kettle, washing to be neutral, and drying for later use;
(3) preparing the nickel oxide loaded activated carbon fiber: and (3) placing the impregnated and dried activated carbon fiber in a tubular furnace, heating to 600-900 ℃ according to a program of 1-10 ℃/min under the protection of inert gas, and roasting or treating with microwave power of 2-5 kW for 15-60 min to obtain the nickel oxide loaded activated carbon fiber.
2. The method according to claim 1, wherein the nickel oxide is replaced with copper oxide or samarium oxide.
3. The method according to claim 1 or 2, wherein in the step (2), the mixture is subjected to ultrasonic vibration for 0.25 to 2 hours.
4. The preparation method according to claim 1 or 2, wherein the modified activated carbon fiber adsorbent loaded with nickel oxide, copper oxide or samarium oxide is applied to hydrogen storage, and the hydrogen storage performance of the modified activated carbon fiber is improved by 28.4%.
5. The preparation method of claim 3, wherein the modified activated carbon fiber adsorbent loaded with nickel oxide, copper oxide or samarium oxide is applied to hydrogen storage, and the hydrogen storage performance of the modified activated carbon fiber is improved by 28.4%.
6. The method according to claim 1, 2 or 5, wherein the activated carbon fiber has a specific surface area of 1019.2m2G, pore volume 0.5cm3/g。
7. The method according to claim 3, wherein the activated carbon fiber has a specific surface area of 1019.2m2G, pore volume 0.5cm3/g。
8. The method according to claim 4, wherein the activated carbon fiber has a specific surface area of 1019.2m2G, pore volume 0.5cm3/g。
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| CN201911327845.0A CN110975814A (en) | 2019-12-20 | 2019-12-20 | Preparation method of nickel oxide loaded modified activated carbon fiber adsorbent |
| PCT/CN2020/089941 WO2021120507A1 (en) | 2019-12-20 | 2020-05-13 | Preparation method of nickel oxide-loaded modified activated carbon fiber adsorbent |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111996651A (en) * | 2020-08-31 | 2020-11-27 | 长沙柔织新材料科技有限公司 | Antistatic functional fabric and preparation method thereof |
| CN112030320A (en) * | 2020-09-07 | 2020-12-04 | 长沙柔织新材料科技有限公司 | Anti-static fiber blended fabric and preparation method thereof |
| WO2021120507A1 (en) * | 2019-12-20 | 2021-06-24 | 大连理工大学 | Preparation method of nickel oxide-loaded modified activated carbon fiber adsorbent |
| CN113607708A (en) * | 2021-08-06 | 2021-11-05 | 常州罗盘星检测科技有限公司 | Method for preparing oxygen sensitive membrane of dissolved oxygen sensor by loading fluorescent indicator and application |
| CN113690058A (en) * | 2021-09-09 | 2021-11-23 | 郑州大学 | Self-supporting NiO/ACNF composite electrode material and preparation method and application thereof |
| CN114146685A (en) * | 2021-12-09 | 2022-03-08 | 大连圣迈化学有限公司 | Nickel-based purifying agent and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021120507A1 (en) * | 2019-12-20 | 2021-06-24 | 大连理工大学 | Preparation method of nickel oxide-loaded modified activated carbon fiber adsorbent |
| CN111996651A (en) * | 2020-08-31 | 2020-11-27 | 长沙柔织新材料科技有限公司 | Antistatic functional fabric and preparation method thereof |
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| CN112030320A (en) * | 2020-09-07 | 2020-12-04 | 长沙柔织新材料科技有限公司 | Anti-static fiber blended fabric and preparation method thereof |
| CN112030320B (en) * | 2020-09-07 | 2021-08-13 | 浙江亿朋服饰有限公司 | Anti-static fiber blended fabric and preparation method thereof |
| CN113607708A (en) * | 2021-08-06 | 2021-11-05 | 常州罗盘星检测科技有限公司 | Method for preparing oxygen sensitive membrane of dissolved oxygen sensor by loading fluorescent indicator and application |
| CN113690058A (en) * | 2021-09-09 | 2021-11-23 | 郑州大学 | Self-supporting NiO/ACNF composite electrode material and preparation method and application thereof |
| CN114146685A (en) * | 2021-12-09 | 2022-03-08 | 大连圣迈化学有限公司 | Nickel-based purifying agent and preparation method and application thereof |
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| WO2021120507A1 (en) | 2021-06-24 |
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