Polystyrene-loaded multiphase Cu/TEMPO catalyst nano-particles as well as preparation method and application thereof
A polystyrene and nanoparticle technology, applied in the field of catalysis, can solve problems such as the difficulty in accurately regulating the content of Cu/TEMPO catalyst components, the inability to control the ratio of ligands and TEMPO, and the inability to meet the requirements of different catalytic performances, etc., to achieve large-scale Effects of large-scale industrial production, improved catalytic performance, and ease of large-scale industrial production
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[0043] The specific preparation method of the styrene-p-chloromethylstyrene copolymer can be as follows: dissolving p-chloromethylstyrene and styrene in 1,4-dioxane under nitrogen protection, and then adding azobisiso Nitrile butadiene was heated to 60°C and stirred for 24 hours; after cooling to room temperature, the reaction was added dropwise to the stirred methanol solution to obtain white flocs, which were collected by filtration and dried to obtain styrene-p-chloromethylstyrene Copolymer, the yield is generally 40% to 80%. In the above preparation method, the mass of azobisisobutyronitrile is 0.1wt% to 2.0wt% of the total mass of the monomer; the mass of 1,4-dioxane is 10 to 30 times of the mass of the monomer; The molar ratio of styrene:styrene is 1:(0.4-20).
[0044] ②
[0045] The preparation method of the azide-containing copolymer can specifically be as follows: adding sodium azide and styrene-p-chloromethylstyrene copolymer to N,N-dimethylformamide under stirri...
Example Embodiment
[0057] Example 1
[0058] The present embodiment provides a polystyrene-supported heterogeneous Cu / TEMPO catalyst nanoparticle, which is prepared according to the following preparation method:
[0059] (1) Prepare raw materials:
[0060] 4-Methylaminopyridine-containing monomer: 100 ml N,N-dimethylformamide and 2.10 g 4-(N-methyl-N-(2-hydroxyethyl)amino) under nitrogen protection at 0°C Pyridine was added to the flask, followed by 906 mg of sodium hydride (60 wt% dispersed in mineral oil), stirred at room temperature for 1 hour; 2.71 g of p-chloromethylstyrene was added, stirred at room temperature for 24 hours; by column chromatography 2.14 g of 4-methylaminopyridine-containing monomer were isolated.
[0061] 4-methylaminopyridine-containing styrene polymer: 1.34 g of the above-mentioned 4-methylaminopyridine-containing monomer and 0.52 g of styrene were dissolved in 36 ml of 1,4-dioxane and added to the reaction flask; Under nitrogen protection, 19 mg of azobisisobutyroni...
Example Embodiment
[0074] Example 2
[0075] The present embodiment provides a polystyrene-supported heterogeneous Cu / TEMPO catalyst nanoparticle, which is prepared according to the following preparation method:
[0076] (1) Each raw material was prepared according to the method similar to Example 1, and the description is not repeated here.
[0077] (2) 140 mg of styrene polymer containing 4-methylaminopyridine (x=5%; weight average molecular weight is 10,000), 30 mg of TEMPO-containing styrene polymer (y=75%; weight average molecular weight is 10,000) ), 30 mg of ligand-containing styrene polymer (z=10%; weight average molecular weight 10000) were dissolved in 2 mL of tetrahydrofuran to obtain solution A.
[0078] (3) 9 mg of copper nitrate trihydrate and 200 mg of OP-10 emulsifier were dissolved in 10 ml of deionized water to obtain aqueous solution B.
[0079] (4) Under the condition of stirring at 15°C (400 rpm), the solution A was rapidly added to the aqueous solution B in less than 3s t...
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