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A controllable preparation method of non-precious metal single-atom catalyst

A non-precious metal and catalyst technology, applied in the field of controllable preparation of non-precious metal single-atom catalysts, can solve problems such as lack of solutions, and achieve the effects of improving atom utilization, high catalytic activity, and strong stability

Inactive Publication Date: 2019-11-12
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, there is still a lack of effective solutions for the preparation of non-noble metal single-atom catalysts in the prior art

Method used

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  • A controllable preparation method of non-precious metal single-atom catalyst
  • A controllable preparation method of non-precious metal single-atom catalyst
  • A controllable preparation method of non-precious metal single-atom catalyst

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Embodiment 1

[0035] like figure 1 As shown, potassium permanganate is used to oxidize graphene to prepare graphene oxide: commercial graphite powder is treated in a mixture of sulfuric acid and potassium permanganate by Hummers method to obtain graphene oxide. The obtained brown product is a graphite flake with derivatized carboxylic acid groups on the edge and mainly phenolic hydroxyl groups and epoxy groups on the plane, which is exfoliated into graphene oxide by ultrasonic or high-shear vigorous stirring. Oxygen-containing functional groups such as hydroxyl, carboxyl and epoxy groups were prepared on graphene.

[0036] Weigh 0.0255g of graphene oxide and pour it into a beaker, add 10ml of ethanol, and sonicate for 2 hours. Weigh 0.0257g of graphene oxide and pour it into a beaker, add 10ml of methanol, and sonicate for 2 hours. Weigh 2.7304g Fe(C 5 h 7 o 2 ) 3 ·7H 2 O was put into a round-bottomed flask, and 25ml of deionized water was added to adjust the pH to 6.0. Start the ele...

Embodiment 2

[0038] Weigh 0.8772g CuSO 4 ·5H 2O and 1.8599 g FeCl 3 ·7H 2 O was put into a round-bottomed flask, added 25ml of deionized water, adjusted to pH 4.0, started the electric mixer, and stirred at 20°C for 30 minutes. Then the graphene oxide dispersion was mixed with the metal salt solution and sonicated at 60 °C for 2 h. Weigh 0.2099gNaBH 4 Dissolve in 10ml deionized water, NaBH 4 The solution was dropped dropwise into the mixed solution of the graphene oxide dispersion and the metal salt, reacted for 0.5 hour, and the obtained product was centrifuged and washed three times with deionized water. Finally put it into a freeze dryer to freeze dry. The metal atom loading capacity of the obtained single-atom catalyst is 1%, and the utilization efficiency of copper and iron metal atoms can reach 99.5%.

Embodiment 3

[0040] Weigh 0.0257g of graphene oxide and pour it into a beaker, add 10ml of methanol, and sonicate for 2 hours. Weigh 2.5304gFeCl 3 ·7H 2 O was put into a round-bottomed flask, and 25ml of deionized water was added to adjust the pH to 6.0. Start the electric mixer and stir for 30 minutes at 20°C. Then the graphene oxide dispersion was mixed with the metal salt solution and sonicated at 60 °C for 2 h. Weigh 0.2099g KBH 4 Dissolve KBH in 10ml deionized water 4 The solution was dropped dropwise into the mixed solution of the graphene oxide dispersion and the metal salt, reacted for 0.5 hour, and the obtained product was centrifuged and washed three times with deionized water. Finally put it into a freeze dryer to freeze dry. The metal atom loading capacity of the obtained single-atom catalyst is 5%, and the iron metal atom utilization efficiency can reach 100%.

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Abstract

The invention discloses a controllable preparation method of a non-noble metal single atom catalyst, which solves the problem that there is no preparation method of a non-noble metal single atom catalyst in the prior art, reduces the cost of the catalyst, improves the atom utilization rate, and prepares Single-atom catalysts have the advantages of high catalytic activity and strong stability. The technical solution is: including the following steps: 1) using a mixed acid oxidation method to prepare oxygen-containing functional groups on porous carrier materials; 2) mixing the oxidized porous carrier dispersion with an aqueous solution of non-noble metal salts, non-noble metal cations and The oxygen-containing functional groups on the porous carrier undergo a site-specific reaction and are loaded onto the porous material; 3) A reducing agent is used to reduce the non-noble metal cations loaded onto the porous material in situ to prepare a non-noble metal single atom catalyst.

Description

technical field [0001] The invention belongs to the technical field of high-efficiency industrial catalyst preparation, and specifically relates to a controllable preparation method of a non-noble metal single-atom catalyst, which uses a functionalized carrier to react with non-noble metal salts such as copper and iron at a fixed point, and then uses a strong reducing agent for in-situ reduction. The metal cations loaded on the carrier are converted into metal single atoms, realizing the controllable preparation of non-noble metal single atom catalysts. Background technique [0002] Single-atom catalysts are an emerging research hotspot in the field of heterogeneous catalysis, which means that the active components in the catalyst exist completely in the form of isolated single atoms, and are stabilized by interacting with supports or forming alloys with second metals. Compared with nano / subnanometer catalysts, single-atom catalysts have many advantages: (1) the active compo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745B01J37/00B01J37/16B01J35/10
CPCB01J23/745B01J37/00B01J37/16B01J35/60
Inventor 张其坤王帅花马晓晔张慧超
Owner SHANDONG NORMAL UNIV
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