A kind of two-dimensional ceramic material catalyst rich in unsaturated coordination and its preparation method and application

A technology for ceramic materials and catalysts, which is applied to two-dimensional ceramic material catalysts rich in unsaturated coordination and the fields of preparation and application thereof, can solve the problems of harsh operating conditions, strong corrosiveness, high toxicity of hydrofluoric acid, etc. Short cycle times and mild conditions

Active Publication Date: 2022-04-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, hydrofluoric acid is used to etch away atomic sheets of A to obtain MXene, but the operating conditions are harsh, and high-concentration hydrofluoric acid is highly toxic and highly corrosive, which makes the preparation method dangerous.
And if the etching time is too long, the temperature is too high and the concentration of hydrofluoric acid is too high, MXene will be dissolved to a certain extent, which will adversely affect the application of MXene

Method used

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  • A kind of two-dimensional ceramic material catalyst rich in unsaturated coordination and its preparation method and application
  • A kind of two-dimensional ceramic material catalyst rich in unsaturated coordination and its preparation method and application
  • A kind of two-dimensional ceramic material catalyst rich in unsaturated coordination and its preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] At room temperature, 3.04g Ti 3 AlC 2 Put it into 30mL hydrofluoric acid solution, the concentration of hydrofluoric acid solution is 30wt%, after magnetic stirring for 12h, centrifuge, the obtained solid is washed 5 times with deionized water, and dried to obtain nano-scale Ti which is rich in unsaturated coordination. 3 al x C 2 (x=0~1) catalyst, gained Ti 3 al x C 2 (x=0~1) The SEM picture of the catalyst is as follows Figure 1a and Figure 1b shown, from Figure 1a and Figure 1b It can be seen that the catalyst presents a two-dimensional layered stacking structure, and there are a large number of nanoscale gaps between the layers, which makes it easier to adsorb F, thereby breaking the C-F bond, and catalyzing the reaction of fluorine-containing alkanes to HF to prepare fluorine-containing olefins.

[0025] The nanoscale Ti rich in unsaturated coordination prepared above 3 al x C 2 (x=0~1) The catalyst is used to catalyze the cracking of 1,1-difluoroetha...

Embodiment 2

[0029] At room temperature, dilute concentrated hydrochloric acid with water to a concentration of 9 mol / L to form solution A. Measure 50mL solution A, add 5gLiF, stir magnetically for 10min, add 5g Ti 3 AlC 2 , reacted at 55°C for 12 hours, centrifuged, and the obtained solid was washed 5 times with deionized water and dried to obtain nano-scale Ti rich in unsaturated coordination. 3 al x C 2 (x=0~1) Catalyst. Obtained Ti 3 al x C 2 (x=0~1) The SEM picture of the catalyst is as follows figure 2 shown, from figure 2 It can be seen that the catalyst presents a two-dimensional layered stacking structure, and there are a large number of nanoscale gaps between the layers, which makes it easier to adsorb F, thereby breaking the C-F bond, and catalyzing the reaction of fluorine-containing alkanes to HF to prepare fluorine-containing olefins. Obtained Ti 3 al x C 2 (x=0~1) The XRD pattern of the catalyst is as follows image 3 shown, according to image 3 It can be se...

Embodiment 3

[0034] oxalic acid and Ti 3 AlC 2 (Ti 3 AlC 2 Quality is 3.01g) is mixed according to the molar ratio of 2:1 and placed in the ball mill jar, ball milled 2h with the rotating speed of 300r / min, the mixture after ball milling is put into tube furnace and carries out high-temperature roasting (high-temperature roasting process is: under nitrogen Under atmosphere, the temperature was raised from room temperature to 350 °C at 3 °C / min, followed by 3 hours of heat preservation, and then naturally cooled to room temperature), that is, nano-scale Ti rich in unsaturated coordination was obtained. 3 al x C 2 (x=0~1) Catalyst.

[0035] The nanoscale Ti rich in unsaturated coordination prepared above 3 al x C 2 (x=0~1) The catalyst is used to catalyze the cracking of 1,1-difluoroethane (HFC-152a) to prepare vinyl fluoride, and the reaction formula is as follows:

[0036]

[0037] The reaction conditions are: the catalyst is loaded into the fixed bed reactor, the catalyst load...

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Abstract

The invention discloses a two-dimensional ceramic material catalyst rich in unsaturated coordination and its preparation method and application. The preparation method of the two-dimensional ceramic material catalyst comprises the following steps: under the action of an etchant, the etchant The intercalation substance in the MAX phase material is intercalated and exfoliated to obtain a two-dimensional MXene material, that is, the two-dimensional ceramic material catalyst is obtained, and the MAX phase material is Ti 3 AlC 2 、Cr 2 AlC, V 2 AlC, Nb 2 At least one of AlC; the etchant is a mixture of hydrochloric acid and LiF, or oxalic acid. The catalyst prepared by the invention is a two-dimensional nano layered catalyst with unsaturated coordination. The catalyst synthesized by the method of the invention has good catalytic activity and stability in the reaction of preparing fluorine-containing olefins by removing HF from fluorine-containing alkanes.

Description

technical field [0001] The invention relates to a two-dimensional ceramic material catalyst rich in unsaturated coordination and its preparation method and application. Background technique [0002] Two-dimensional crystals refer to two-dimensional materials with a thickness of only one or several atoms. This material has unique properties and functions because of its absolute two-dimensional structure. Graphene is the most typical two-dimensional crystal with excellent properties, but graphene is not the end of two-dimensional atomic crystal materials, some two-dimensional crystals with special properties and other elements have become the focus of current research. MXene is a new type of two-dimensional crystal with a similar structure to graphene. Its chemical formula is M n+1 x n , n=1, 2, 3, M is an early transition metal element, X is carbon or / and nitrogen. As a new class of two-dimensional materials (a general term for metal carbonitrides), MXene, due to its intr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/22B01J35/02B01J37/08B01J37/00C07C17/25C07C21/18
CPCB01J27/22B01J35/0013B01J35/026B01J37/0018C07C17/25C07C21/18
Inventor 韩文锋杨虹刘兵刘永南俞威陆佳勤李西良唐浩东李瑛
Owner ZHEJIANG UNIV OF TECH
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