a coral-like pd 4 The preparation method of se compound

A compound, coral-like technology, applied in the field of nanomaterial synthesis and preparation, can solve the problems of cumbersome steps, high preparation cost, high process toxicity, etc., and achieve the effects of simple synthesis preparation process, mild reaction conditions, and improved catalytic activity.

Active Publication Date: 2022-05-03
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Claims
  • Application Information

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Problems solved by technology

The synthesis steps of organic selenides involved in this method are cumbersome, the preparation cycle is long and the required drugs are highly toxic, which is not conducive to green production; and the subsequent synthesis of tetrapalladium selenide needs to be carried out in a tube furnace under nitrogen protection. The cost is higher; Ajai K.Singh et al. (Dalton Trans, 2012,41,1142) have reported a kind of preparation method of four palladium selenide nanoparticles, with pre-prepared palladium selenium coexistence organic compound [PdCl2(PhSe-CH2C H2CH2-NH2)] is the common precursor of palladium selenide, which is mixed with tri-n-octylphosphine (TOC) and pyrolyzed at 280-300°C to obtain most of the tetrapalladium selenide block and a small part Nanoparticles about 38-43nm in diameter
This method has simple pyrolysis steps, but the pre-preparation of organic precursors also involves problems such as cumbersome steps and high toxicity, which is not conducive to rapid production in general
[0005] In summary, the current Pd 4 The preparation of Se compounds all has cumbersome preparation process steps, long preparation period, high process toxicity and high preparation cost, which is not conducive to batch preparation; in addition, the tetrapalladium monoselenide compounds prepared by the prior art are mostly Composed of bulk materials with uncontrollable structure, there is no clear method for the preparation of tetrapalladium selenide nanomaterials

Method used

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  • a coral-like pd <sub>4</sub> The preparation method of se compound
  • a coral-like pd <sub>4</sub> The preparation method of se compound
  • a coral-like pd <sub>4</sub> The preparation method of se compound

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Embodiment 1

[0034] A coral-like Pd 4 The preparation method of Se compound, comprises the following steps:

[0035] Step 1: Disperse 10 mg of graphene oxide (GO) in 7.5 ml of deionized water and stir evenly;

[0036] Step 2: Add 0.1mmol sodium tetrachloropalladate, 0.1mmol sodium citrate, 0.2mmol sodium hydroxide and 0.1mmol sodium borohydride in turn to the solution obtained in step 1, and then mix and stir for 20 minutes;

[0037] Step 3: Prepare another 7.5ml of deionized water, add 0.1mmol of selenous acid into the deionized water, and stir evenly;

[0038] Step 4: Mix the solutions obtained in Step 2 and Step 3, and stir evenly;

[0039] Step 5: Transfer the mixed solution obtained in Step 4 to a reaction kettle, and conduct a hydrothermal reaction at a temperature of 200° C. for 5 hours;

[0040] Step 6: After the reaction, cool down to room temperature naturally, then filter the solution to obtain the black precipitate, wash with deionized water, ethanol, and deionized water rep...

Embodiment 2

[0045] A coral-like Pd 4 The preparation method of Se compound, comprises the following steps:

[0046] Step 1: disperse 5 mg of graphene oxide (GO) in 15 ml of deionized water, and stir evenly;

[0047] Step 2: Add 0.1mmol sodium tetrachloropalladate, 0.1mmol sodium citrate, 0.2mmol sodium hydroxide and 0.1mmol sodium borohydride in turn to the solution obtained in step 1, and then mix and stir for 20 minutes;

[0048] Step 3: Prepare another 15ml of deionized water, add 0.025mmol of selenous acid into the deionized water, and stir evenly;

[0049] Step 4: Mix the solutions obtained in Step 2 and Step 3, and stir evenly;

[0050] Step 5: Transfer the mixed solution obtained in Step 4 to a reaction kettle, and conduct a hydrothermal reaction at a temperature of 250° C. for 10 hours;

[0051] Step 6: After the reaction, cool down to room temperature naturally, then filter the solution to obtain the black precipitate, wash with deionized water, ethanol, and deionized water re...

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Abstract

The invention provides a coral-like Pd 4 The preparation method of Se compound belongs to the technical field of synthesis and preparation of nanometer materials. The method uses selenous acid and sodium tetrachloropalladate as reaction substances, deionized water as reaction solvent, and synthesizes coral-like Pd in ​​one step by hydrothermal method. 4 Se compound nanomaterials, the synthesis process is simple, the toxicity is low, the reaction conditions are mild, the cost is low, and the synthesized Pd 4 Se has high purity and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of synthesis and preparation of nanomaterials, in particular to a coral-like tetrapalladium selenide (Pd 4 Se) The preparation method of compound. Background technique [0002] As an important class of noble metal catalysts, palladium metal and its compounds have excellent catalytic performance and wide applications in fields including organic cross-coupling reactions, hydrogen evolution reactions, oxygen reduction reactions, and magnesium-air batteries. However, the content of palladium on the earth is rare, as low as 0.0006PPM, and when it is used as a catalyst, it also has the problem of easy deactivation similar to other noble metal catalysts. Therefore, improving the catalytic efficiency of palladium catalysts through the preparation of corresponding compounds and nanostructure design has become the top priority for the sustainable development of related industries. [0003] Tetrapalladium selenide (P...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/04C25B11/077B82Y40/00
CPCC01B19/007B82Y40/00C01P2004/30
Inventor 熊杰郭倚天杜新川黄建文雷天宇陈伟晏超贻邬春阳王显福
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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