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Preparation method of coralline-like Pd4Se compound

A compound and coral-like technology, applied in the field of synthesis and preparation of nanomaterials, can solve the problems of cumbersome steps, high process toxicity, and high production cost, and achieve simple synthesis and preparation process, which is beneficial to intrinsic conductivity and avoids the interference of impurity phases Effect

Active Publication Date: 2021-03-30
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • 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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  • Preparation method of coralline-like Pd4Se compound
  • Preparation method of coralline-like Pd4Se compound
  • Preparation method of coralline-like Pd4Se compound

Examples

Experimental program
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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 well;

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

[0037] Step 3: Prepare 7.5ml of deionized water, add 0.1mmol of selenite into the deionized water, and stir well;

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

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

[0040] Step 6: After the reaction is completed, naturally cool to room temperature, and then filter the solution to obtain a black precipitate, which is repeatedly washed with deionized water, ethanol, an...

Embodiment 2

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

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

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

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

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

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

[0051] Step 6: After the reaction is completed, naturally cool to room temperature, and then filter the solution to obtain a black precipitate, which is repeatedly washed with deionized water, eth...

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Abstract

The invention provides a preparation method of a coralline-like Pd4Se compound, and belongs to the technical field of nano material synthesis and preparation. According to the method, seleninic acid and sodium tetrachloropalladate are used as reaction substances, deionized water is used as a reaction solvent, the coralline-like Pd4Se compound nano material is synthesized in one step through a hydrothermal method. The synthesis process is simple, is low in toxicity and is gentle in reaction conditions and low in cost; the synthesized Pd4Se is high in purity, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial synthesis and preparation, and in particular relates to a kind of coral-like tetrapalladium-selenide (Pd 4 Methods for the preparation of Se) compounds. Background technique [0002] As an important class of noble metal catalysts, palladium metal and its compounds have excellent catalytic performance and wide application in the fields including organic cross-coupling reaction, hydrogen evolution reaction, oxygen reduction reaction, magnesium-air battery and so on. However, the content of palladium on earth is scarce, as low as 0.0006PPM, and when used as a catalyst, it also has the same problem of easy deactivation as other precious metal catalysts. Therefore, improving the catalytic efficiency of palladium catalysts through the preparation of corresponding compounds and the design of nanostructures has become the top priority of the sustainable development of related industries. [0003] T...

Claims

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Application Information

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Patent Type & Authority Applications(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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