Synthesis of dicyandiamide modified palladium nano-catalyst and application of dicyandiamide modified palladium nano-catalyst in catalyzing semi-hydrogenation of phenylacetylene

A dicyandiamide and palladium nanotechnology, which is applied in the synthesis field of palladium nanocatalyst, can solve the problems of unclear active center site, complicated reaction, poor selectivity, etc., and achieve the effects of improving selectivity, simple synthesis and low cost.

Pending Publication Date: 2021-02-26
QUANZHOU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Lindella catalysts are commonly used in industry to catalyze alkynes to olefins, but their selectivity is poor and their activity is low, resulting in unclear active center sites and complex reactions.

Method used

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  • Synthesis of dicyandiamide modified palladium nano-catalyst and application of dicyandiamide modified palladium nano-catalyst in catalyzing semi-hydrogenation of phenylacetylene
  • Synthesis of dicyandiamide modified palladium nano-catalyst and application of dicyandiamide modified palladium nano-catalyst in catalyzing semi-hydrogenation of phenylacetylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of synthetic method and application of the palladium nano-catalyst modified by dicyandiamide

[0024] 1) Prepare 0.2 mol / L sodium tetrachloropalladate solution: Dissolve 1 g palladium chloride and 0.6592 g sodium chloride in 32 ml ultrapure water on an electronic balance with weighing paper to obtain 0.2 mol / L tetrachloropalladate solution Sodium chloropalladate solution, stored in the refrigerator for later use.

[0025] 2) Reduction of Pd particles: Use a manual pipette to take 30 mg sodium tetrachloropalladate solution, use a pipette to take 20 ml N,N dimethylformamide, use an electronic balance to weigh 100 mg polyvinylpyrrolidone and 200 mg sodium formate , Add the above raw materials into a thick-walled pressure-resistant bottle, ultrasonically mix for 10-20 minutes to aid in dispersion, then place it in an oil bath, set the temperature of the oil bath at room temperature to 160°C, keep it warm for 80 minutes, and then cool to room temperature. Then add et...

Embodiment 2

[0030] A kind of synthetic method of the palladium nano-catalyst modified by dicyandiamide

[0031] 1) Prepare 0.2 mol / L sodium tetrachloropalladate solution: same as Example 1.

[0032] 2) Reduction of Pd particles: Take 30 mg of sodium tetrachloropalladate solution, 20 ml of N,N dimethylformamide, 100 mg of polyvinylpyrrolidone, and 250 mg of sodium formate, add the above materials into a thick-walled pressure-resistant bottle, and ultrasonically mix for 10 minutes to help Disperse, then place in an oil bath, set the temperature of the oil bath at room temperature to 100°C, keep it warm for 240min, and then cool to room temperature. Then add ethanol and acetone and go through 3 times of centrifugation and purification to separate the Pd nanoparticles, and then dissolve them with 9mL N,N dimethylformamide to obtain a Pd nanoparticle solution;

[0033] 3) Preparation of dicyandiamide-modified Pd nanocatalyst: Take 3mL of Pd nanoparticle solution, add 720mg of dicyandiamide an...

Embodiment 3

[0035] A kind of synthetic method of the palladium nano-catalyst modified by dicyandiamide

[0036] 1) Prepare 0.2 mol / L sodium tetrachloropalladate solution: same as Example 1.

[0037]2) Reduction of Pd particles: Take 30 mg of sodium tetrachloropalladate solution, 20 ml of N,N dimethylformamide, 100 mg of polyvinylpyrrolidone, and 200 mg of sodium formate, add the above materials into a thick-walled pressure-resistant bottle, and ultrasonically mix for 20 minutes to help Disperse, then place in an oil bath, set the temperature of the oil bath at room temperature to 160°C, keep it warm for 80 minutes, and then cool to room temperature. Then add ethanol and acetone to undergo 4 times of centrifugation and purification to separate the Pd nanoparticles, and then dissolve them with 9mL N,N dimethylformamide to obtain a Pd nanoparticle solution;

[0038] 3) Preparation of dicyandiamide-modified Pd nanocatalyst: Take 3mL of Pd nanoparticle solution, add 700mg of dicyandiamide and...

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Abstract

The invention provides synthesis of a dicyandiamide modified palladium nano-catalyst and application of the dicyandiamide modified palladium nano-catalyst in catalyzing semi-hydrogenation of phenylacetylene. The synthesis comprises the following steps: firstly, dissolving polyvinylpyrrolidone, sodium formate and a sodium tetrachloropalladate solution into a thick-wall pressure-resistant bottle containing N, N-dimethylformamide or formamide together, then putting the thick-wall pressure-resistant bottle into an oil bath pan, reducing palladium through high temperature, then centrifugally separating out palladium nanoparticles, and dissolving to form a palladium nanoparticle solution; mixing the palladium nanoparticle solution with dicyandiamide and N, N-dimethylformamide, putting the mixture into the oil bath pan, keeping the temperature for a certain time at a high temperature to obtain a dicyandiamide-modified palladium nanoparticle solution, centrifugally separating out dicyandiamide-modified palladium nanoparticles, and dissolving the dicyandiamide-modified palladium nanoparticles into ethanol to obtain the dicyandiamide-modified palladium nano-catalyst. The dicyandiamide modified palladium nano-catalyst shows good performance in the application of catalyzing alkyne hydrogenation to prepare olefin, realizes high activity and high selectivity, and is low in price and environment-friendly.

Description

technical field [0001] The invention belongs to the field of selective hydrogenation, and in particular relates to the synthesis of a dicyandiamide-modified palladium nanometer catalyst and its application in catalyzing the semihydrogenation of phenylacetylene. Background technique [0002] The selective hydrogenation of triple-bonded alkynes to double-bonded alkenes is a very important and challenging reaction in chemical production. The phenylacetylene contained in styrene will affect the quality of olefins and affect the product performance of olefin synthesis. Improving the selectivity of olefins is the focus of research. Most of the catalytic reactions take place on the surface of the catalyst. The surface structure determines the catalytic properties. The change of the surface structure directly affects the ability of the catalyst. Surface modification of the catalyst is a good strategy. Highly active metals are generally selectively protected by organic or inorganic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C15/46C07C5/09
CPCB01J31/06C07C5/09B01J2231/645C07C15/46
Inventor 赵小静常延东潘晓阳
Owner QUANZHOU NORMAL UNIV
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