NL2023943B1 - A New Method for Preparing Activated Carbon Catalyzing Oxygen Reduction Reaction (ORR) from Fast—growing Paper Mulberry - Google Patents

A New Method for Preparing Activated Carbon Catalyzing Oxygen Reduction Reaction (ORR) from Fast—growing Paper Mulberry Download PDF

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NL2023943B1
NL2023943B1 NL2023943A NL2023943A NL2023943B1 NL 2023943 B1 NL2023943 B1 NL 2023943B1 NL 2023943 A NL2023943 A NL 2023943A NL 2023943 A NL2023943 A NL 2023943A NL 2023943 B1 NL2023943 B1 NL 2023943B1
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dried
paper mulberry
orr
washed
activated carbon
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Liu Yanyan
Jiang Jianchun
Wang Kui
Sun Kang
Zhou Wenshu
Wei Linshan
Wu Dichao
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Inst Chemical Ind Forest Products Caf
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • 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
    • Y02E60/50—Fuel cells

Abstract

The invention discloses a new method for preparing catalytic oxygen reduction reaction (ORR) activated carbon from fast-growing paper mulberry. In the invention, catalytic 5 activated carbon (NAC) is prepared through low-temperature hydrothermal reaction and steam activation reaction with paper mulberry branches as the raw materials. The detailed steps are as follows: the paper mulberry branches are peeled, dried, crushed, dosed into a stainless steel reactor with PTFE lining, added with water and acid solution, stirred uniformly, sealed, and put in an oven for reaction. The reaction 10 products are naturally cooled down to the room temperature, filtered, washed with hot water and dried; the dried sample is roasted at high temperature in nitrogen atmosphere, activated with steam, washed and ground to obtain NAC. The synthetic method of the invention is simple, environment-friendly and easy to realize, and the catalyst prepared can be used to catalyze ORR.

Description

Technical Field
The invention relates to a new method for preparing activated carbon catalyzing oxygen reduction reaction (ORR) from paper mulberry branches.
Background Technology
Paper mulberry is a kind of perennial broad-leaved arbor which is an indigenous tree species unique in China widely distributed in South China, North China and east area of North-west China. Paper mulberry has advantages of fast growth, drought and barrenness resistance, high disease resistance, easy breeding and strong anti-pollution capacity. Paper mulberry is a wild economic tree species with high comprehensive benefits, is broadly applied in paper making, feed, pharmaceuticals and other industries, and plays an important role in environment protection and ecological remediation. Paper mulberry has high economical value and social value and attracts more and more attention. Therefore, paper mulberry shall be vigorously developed and utilized.
The energy and environment problem is a major challenge of sustainable development in the world. Carbon and particle emissions generated during use of fossil fuel tend to aggravate the greenhouse effect and result in air pollution. In order to realize sustainable development, new green energy must be developed to improve the energy utilization efficiency. Metal-air batteries and fuel batteries are important devices converting electrochemical energy and play a significant role in the new energy system. ORR is the positive reaction of metal-air batteries and various types of fuel batteries, and decides the performance of the above mentioned batteries like the discharge voltage and the output power. The preparation cost of ORR catalyst is the key factor affecting the application thereof. Commercial ORR catalyst (Pt/C) has low reserves, high cost and poor catalytic stability, which affect the industrial application thereof. Hetero-atom or metal-modified nanocarbon materials show the potential of being used as ORR catalyst. However, the preparation processes of carton materials like graphene and carbon nanotubes depend on fossil fuel to realize carbon-hydrogen bond activation,
AO 19.10.1072 NL dehydrogenation and carbonization, with harsh synthesis conditions, high energy consumption, low density, high preparation cost and certain harm from the process to the environment, thus restricting the application of the nanocarbon materials as cathode catalyst of fuel batteries. Therefore, researches in the field focus on developing nonnoble metal catalyst with high reserves, low cost, high efficiency and high stability. Activated carbon materials are expected to be the substitute catalyst to noble metal.
Wooden activated carbon has advantages of readily available raw materials, controllable preparation process, environment friendliness, sustainable production, and good ORR performance after surface modification, thus being expected to be used as cathode catalyst in metal-air batteries and fuel batteries. Paper mulberry is an important tree species in China for poverty alleviation. Domestic and foreign researches focus on paper mulberry increasingly, but the application of preparing bio-based carbon catalyst with paper mulberry as the raw materials has not been reported yet.
Content of the Invention
In view of the above mentioned status quo, the invention aims to provide a new method for preparing activated carbon catalyzing oxygen reduction reaction (ORR) from paper mulberry branches.
In order to realize the above mentioned purpose, the invention adopts the following technical scheme: the activated carbon is porous activated carbon containing nitrogen (NAC); catalytic activated carbon is prepared through low-temperature hydrothermal reaction and steam activation reaction with paper mulberry branches as the raw materials.
A new method for preparing activated carbon catalyzing oxygen reduction reaction (ORR) from paper mulberry branches, comprising the following steps:
(1) . The paper mulberry branches are peeled, dried, crushed, dosed into mixed liquid of water and acid for hydrothermal reaction, suction-filtered, washed with hot water and dried;
(2) . The dried sample obtained from (1) is activated with steam and roasted at high temperature in nitrogen and steam atmosphere;
AO 19.10.1072 NL (3). The sample obtained in (2) is washed with dilute hydrochloric acid, hot water and ethyl alcohol and dried to obtain NAC;
hr step (1), according to the volume ratio, acid: H2O = 1: 8.5-12.5; the hydrothermal temperature is 110-190 °C, and the hydrothermal duration is 5-30 h.
In step (2), according to the mass ratio, the sample after the hydrothermal reaction: steam = 1: 3.5-4.5; the roasting conditions are as follows: the sample is first heated to 800-850 °C in nitrogen atmosphere with a heating rate of 10.5-11.5 °C-min-l, and then roasted in steam atmosphere for 0.4-1.5 h.
In step (3), dilute hydrochloric acid has a concentration of 5.5-10.5 %, and boiling and washing with hot water is performed for 2-3 times.
Beneficial effects:
1. In the invention, ORR catalyst is prepared by using paper mulberry branches, with readily available raw materials, simple and controllable preparation process, environment friendliness and sustainable production;
2. In the invention, hemicellulose is removed through low-temperature hydrothermal reaction, and then activated carbon is prepared, being favorable for obtaining carbon materials with stable structure and abundant micropores, small pores and medium-sized pores, adsorbing the reaction products and solvent molecules during ORR catalysis, and letting the catalytic reaction be proceed;
3. In the invention, activated carbon is prepared through steam activation, which has advantages that the cost is low, no pollution occurs, and the reaction exhaust gas can be burnt to supply heat;
4. The catalyst has porous structure which is beneficial to oxygen molecule adsorption and ion transfer;
AO 19.10.1072 NL
5. The paper mulberry leaves have a crude protein content of up to 18 %-24 %, and the paper mulberry branches have a nitrogen element content of about 3 %. Nitrogen atoms are important active sites in ORR. Nitrogen atoms have high electronegativity which can induce nearby carbon atoms to generate local positive charge, thus being favorable for oxygen molecule adsorption and accelerating ORR; during high temperature reaction, part of the nitrogen elements escape, allowing carbon to form multi-directional edges or structure defects and have more active sites exposed, and improving the ORR activity. In the invention, the inherent nitrogen elements in the paper mulberry branches are utilized, the subsequent doping modification step is eliminated, and activated carbon is prepared through steam activation to be used as ORR catalyst which is of great practical significance;
6. The catalyst has high methanol poisoning resistance, good ORR catalysis stability and great industrial application potential;
7. Paper mulberry is an important tree species in China for poverty alleviation. The paper mulberry branches are used as the raw materials in the invention, improving the economic value added of paper mulberry and responding to the call of national policies of China.
Brief Description of the Drawings
Fig. 1: transmission electron micrograph of HTC (a), BC (b) and NAC (c). Fig. 2: x-ray powder diffraction diagram of HTC (a), BC (b) and NAC (c). Fig. 3: Raman spectrogram of HTC (a), BC(b) and NAC(c).
Fig. 4: performance charts of ORR catalysis of different catalyst. Linear sweep voltammogram (LSV) of HTC, BC and NAC (a), chronoamperometry diagram after addition of methanol during ORR catalysis with NAC (b) and long time chronoamperometry diagram of NAC (c).
Specific Embodiment Method
The invention is further described in details below in order for the invention to be more clear and clarified. It is understood that the specific embodiments described herein are only intended to explain the invention, rather than limiting the invention.
AO 19.10.1072 NL
A new method for preparing activated carbon catalyzing oxygen reduction reaction (ORR) from paper mulberry branches, comprising the following steps:
(1) . The paper mulberry branches are peeled, dried, crushed, dosed into mixed liquid of water and acid for hydrothermal reaction, suction-filtered, washed with hot water and dried;
(2) . The dried sample obtained from (1) is activated with steam and roasted at high temperature in nitrogen and steam atmosphere;
(3) . The sample obtained in (2) is washed with dilute hydrochloric acid, hot water and ethyl alcohol and dried to obtain NAC;
In step (1), according to the volume ratio, acid: H2O = 1:8.5-12.5; the hydrothermal temperature is 110-190 °C, and the hydrothermal duration is 5-30 h.
In step (2), the sample after the hydrothermal reaction: steam = 1:3.5-4.5; the roasting conditions are as follows: the sample is first heated to 800-850 °C in nitrogen atmosphere with a heating rate of 10.5-11.5 °C-min-1, and then roasted in steam atmosphere for 0.4-1.5 h.
In step (3), dilute hydrochloric acid has a concentration of 5.5-10.5 %, and boiling and washing with hot water is performed for 2-3 times.
Embodiment 1:
A method for preparing catalyst NAC, comprising the following steps:
(1) . The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and H3PO4 (85 %) (225 mL water and 25 mL H3PO4), added into a 500 mL reactor for 30h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 850 °C, heating is kept for 1 h after nitrogen is replaced with steam, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
AO 19.10.1072 NL
Embodiment 2:
A method for preparing catalyst BC, comprising the following steps:
(1) . The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and H3PO4 (85 %) (225 mL water and 25 mL H3PO4), added into a 500 mL reactor for 30h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 500 °C, heating is kept for 1 h, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
Embodiment 3:
A method for preparing catalyst HTC, comprising the following steps:
The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and H3PO4 (85 %) (225 mL water and 25 mL H3PO4), added into a 500 mL reactor for 30h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried.
Embodiment 4:
(1) . The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and H3PO4 (85 %) (225 mL water and 25 mL H3PO4), added into a 500 mL reactor for 5h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 850 °C, heating is kept for 1 h after nitrogen is replaced with steam, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
Embodiment 5:
(1). The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and H3PO4 (85 %) (225 mL water and 25 mL H3PO4), added into a 500
AO 19.10.1072 NL mL reactor for 15h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 850 °C, heating is kept for 1 h after nitrogen is replaced with steam, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
Embodiment 6:
(1) . The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and HC1 (36 %-38 %) (225 mL water and 25 mL HC1), added into a 500 mL reactor for 30h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 850 °C, heating is kept for 1 h after nitrogen is replaced with steam, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
Embodiment 7:
(1) . The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and H2SO4 (98 %) (225 mL water and 25 mL H2SO4), added into a 500 mL reactor for 30h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 850 °C, heating is kept for 1 h after nitrogen is replaced with steam, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
Embodiment 8:
(1). The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and HN03 (68 %) (225 mL water and 25 mL HNO3), added into a 500
AO 19.10.1072 NL mL reactor for 30h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 850 °C, heating is kept for 1 h after nitrogen is replaced with steam, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
Embodiment 9:
(1) . The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and HCOOH (85 %) (225 mL water and 25 mL HCOOH), added into a 500 mL reactor for 30h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 850 °C, heating is kept for 1 h after nitrogen is replaced with steam, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
Embodiment 10:
(1) . The paper mulberry branches are peeled, dried, crushed (30.2 g), dosed into mixed liquid of water and CH3COOH (99 %) (225 mL water and 25 mL CH3COOH), added into a 500 mL reactor for 30h of hydrothermal reaction at 180 °C, suction-filtered, washed with hot water and dried;
(2) . The dried sample (4.6 g) dried in step (1) is heated in nitrogen atmosphere at a rate of 10 °C-min-1 until reaching 850 °C, heating is kept for 1 h after nitrogen is replaced with steam, and the sample is naturally cooled down in nitrogen atmosphere;
(3) . The sample obtained in step (2) is washed with hydrochloric acid (8 %) and hot water, then washed with ethyl alcohol, and dried.
Structural Characterization of Catalyst
Fig. 1 shows the transmission electron micrograph of the catalyst HTC (a), BC (b) and NAC (c) which are prepared in embodiments 1-3. It can be seen from Fig. (a) that the
AO 19.10.1072 NL carbon plates are accumulated disorderly and the pore structure cannot be seen; it can be seen from Figs, (b) and (c) that the carbon plates are stacked and distributed in order, and the carbon plates in Fig. (c) are thinner and have clearer pore structure. Different morphological features of the three types of catalyst indicate that through further treatment after the hydrothermal reaction, the material morphology can be more regular, and porous carbon plates can be formed through steam activation.
Fig. 2 shows the x-ray powder diffraction diagram of the catalyst HTC, BC and NAC which are prepared in embodiments 1-3. It can be seen from Fig. 2 that the three types of catalyst all show characteristic diffraction peaks of carbon; due to difference of the carbonization degree, the peak of HTC at about 20 degrees is on the left; the peak of the catalyst at about 44 degrees corresponds to the crystal face of carbon (101).
Fig. 3 shows the Raman spectrogram of the catalyst HTC, BC and NAC which are prepared in embodiments 1-3. The peak D of HTC is right-most due to the large quantity of oxygen-containing functional groups in the sample after the hydrothermal reaction. The ID/IG value of the catalyst is respectively as follows: HTC: 0.66; BC: 0.69; NAC: 0.88.
Catalyst Performance Test
The catalyst HTC, BC and NAC which are prepared in embodiments 1 -3 are respectively subject to the ORR catalysis performance tests.
The linear sweep voltammetry (LSV) curve test, the methanol poisoning resistance test of NAC and the stability test are performed through a three-electrode system by using a rotating disk device and a CHI760E electrochemical workstation. The three-electrode system comprises a working electrode, a reference electrode and a counter electrode. Among the electrodes, the reference electrode is an Ag/AgCl electrode, and the counter electrode is a Pt-wire electrode; the working electrode is prepared as follows: the catalyst (4 mg) prepared in embodiments 1-3 is respectively weighed, put in a centrifugal tube, added with 720 pL absolute ethyl alcohol and 8()pL Nafion (5 wt %) solution in sequence, and ultrasonically dispersed for 60 minutes to obtain homogeneous solution, which is then taken at an amount of 10 pL with a pipette and dropped on a glassy carbon electrode for natural drying.
AO 19.10.1072 NL
The above mentioned tests are all performed in oxygen-saturated 0.1 M KOH, and the electrolyte used in the methanol poisoning resistance test is 0.1 M KOH+1 M methanol. The test conditions are as follows: the linear sweep speed is 5 mV s-1, the voltage in the methanol poisoning resistance test is 0.5 V (vs. RHE), and the rotating speed is 1600 rpm. The voltage in the chronoamperometry test is 0.5 V (vs. RHE).
Fig. 4 shows the performance charts of ORR catalysis of different catalyst, which are respectively the linear sweep voltammogram (LSV) of HTC, BC and NAC (rotating speed: 1600 rpm) (a), the chronoamperometry diagram after addition of methanol during ORR catalysis with NAC (b) and the chronoamperometry diagram of NAC (c). It can be seen from Fig. 4 (a) that NAC has the highest catalytic activity in the same conditions. It can be seen from Fig. 4 (b) that the NAC current drops very slightly after IM methanol is added, indicating that NAC has very high methanol poisoning resistance. It can be seen from Fig. 4 (c) that NAC has good stability, and the current holding rate after 14000 S is higher than 80 %.
AO 19.10.1072 NL

Claims (5)

ConclusiesConclusions (1) de papieren moerbeiboomtakken worden geschild, gedroogd, geplet, gedoseerd in gemengde vloeistof van water en zuur voor een hydro thermische reactie, afgezogen, gewassen met heet water en gedroogd;(1) the paper mulberry branches are peeled, dried, crushed, dosed in mixed liquid of water and acid for a hydro thermal reaction, filtered off, washed with hot water and dried; 1. Een nieuwe werkwijze voor het bereiden van actieve kool die een zuurstof reducerende reactie (ORR) katalyseert uit snelgroeiende papieren moerbei, met het kenmerk dat papieren moerbeiboomtakken als grondstoffen worden onderworpen aan een hydro thermische reactie met het bestaan van zuur, geroosterd bij hoge temperatuur in stikstofatmosfeer, geactiveerd met stoom, gewassen en gemalen om de actieve koolstof te verkrijgen waarbij de koolstofkatalysator poreuze actieve koolstof is die stikstof bevat (NAC).A new method for preparing activated carbon that catalyzes an oxygen-reducing reaction (ORR) from fast-growing paper mulberry, characterized in that paper mulberry branches as raw materials are subjected to a hydro-thermal reaction with the existence of acid roasted at high temperature in a nitrogen atmosphere, activated with steam, washed and ground to obtain the active carbon, the carbon catalyst being porous active carbon containing nitrogen (NAC). (2) het gedroogde monster verkregen uit (1) wordt geactiveerd met stoom en geroosterd bij hoge temperatuur in stikstof en stoomatmosfeer;(2) the dried sample obtained from (1) is activated with steam and roasted at high temperature in nitrogen and steam atmosphere; 2. Nieuwe werkwijze voor het bereiden van geactiveerde koolstof die ORR katalyseert uit papieren moerbeiboomtakken volgens conclusie 1, waarbij de werkwijze de volgende stappen omvat:A new method for preparing activated carbon catalysing ORR from paper mulberry branches according to claim 1, wherein the method comprises the following steps: 3. Nieuwe werkwijze voor het bereiden van geactiveerde koolstof die ORR katalyseert uit papieren moerbeiboomtakken volgens conclusie 2, waarbij in stap (1) de volumeverhouding zuur : ILO 1: 8,5-12,5 is; de hydro thermische temperatuur 110-190 °C en de hydro thermische duur 5-30 uur is. 4 A new method for preparing activated carbon catalysing ORR from paper mulberry branches according to claim 2, wherein in step (1) the volume ratio is acid: ILO 1: 8.5-12.5; the hydro thermal temperature is 110-190 ° C and the hydro thermal duration is 5-30 hours. 4 (3) het in (2) verkregen monster wordt gewassen met verdund zoutzuur, heet water en ethylalcohol en gedroogd om NAC te verkrijgen.(3) the sample obtained in (2) is washed with dilute hydrochloric acid, hot water and ethyl alcohol and dried to obtain NAC. 4. Werkwijze voor het bereiden van ORR-katalysator volgens conclusie 2, waarbij in stap (2) de massaverhouding van het monster na de hydro thermische reactie: stoom 1: 3,5-4,5 is; de roosteromstandigheden als volgt zijn: het monster wordt eerst verwarmd tot 800-850 °C in stikstofatmosfeer met een verwarmingssnelheid van 10,511,5 °C min'1, en vervolgens 0,4-1,5 uur in stoomatmosfeer geroosterd.The method for preparing ORR catalyst according to claim 2, wherein in step (2) the mass ratio of the sample after the hydro thermal reaction: steam is 1: 3.5-4.5; the grating conditions are as follows: the sample is first heated to 800-850 ° C in a nitrogen atmosphere with a heating rate of 10.511.5 ° C min -1 , and then roasted for 0.4-1.5 hours in steam atmosphere. AO 19.10.1072 NLAO 19.10.1072 NL 5. Werkwijze voor het bereiden van ORR-katalysator volgens conclusie 2, waarbij in stap (3) verdund zoutzuur een concentratie van 5,5-10,5% heeft en koken en wassen met heet water 2-3 keer wordt uitgevoerd.The process for preparing ORR catalyst according to claim 2, wherein in step (3) dilute hydrochloric acid has a concentration of 5.5-10.5% and boiling and washing with hot water is carried out 2-3 times. 5 6. Nieuwe werkwijze voor het bereiden van geactiveerde koolstof die ORR katalyseert uit papieren moerbeiboomtakken volgens conclusie 2, waarbij in stap (1) het gebruikte zuur elk van H3PO4, HC1, H2SO4, HNO3, HCOOH en CH3COOH kan zijn.6. A new method for preparing activated carbon catalyzing ORR from paper mulberry branches according to claim 2, wherein in step (1) the acid used each comprises H 3 PO 4 , HCl, H 2 SO 4 , HNO 3 , HCOOH and CH 3 can be COOH. AO 19.10.1072 NLAO 19.10.1072 NL Intensity (a.u.) Intensity (a.u.)Intensity (a.u.) Intensity (a.u.)
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CN109888311A (en) * 2019-03-04 2019-06-14 上海交通大学 Carbon composite oxygen reduction catalyst based on biomass derived and preparation method thereof

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