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Method for preparing core-shell porous silica/iron oxide nanometer catalyst

A porous silica and iron oxide nanotechnology, applied in the fields of chemistry and nanomaterials, can solve the problems of sintering and growing of iron oxide grains, uncontrollable shape and size, etc., and achieve the effects of short production cycle and low cost

Active Publication Date: 2018-11-09
XIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing a core-shell porous silica / iron oxide nanocatalyst, which solves the problem that the iron oxide crystal grains are sintered and grown and the shape and size are uncontrollable in the heat treatment process

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  • Method for preparing core-shell porous silica/iron oxide nanometer catalyst
  • Method for preparing core-shell porous silica/iron oxide nanometer catalyst
  • Method for preparing core-shell porous silica/iron oxide nanometer catalyst

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Embodiment 1

[0044] A preparation method of a core-shell type porous silica / iron oxide nanocatalyst, specifically implemented according to the following steps:

[0045] Step 1, the synthesis of allyl malonate:

[0046] Add allylmalonic acid and benzyl alcohol to the anhydrous toluene solvent in sequence, add concentrated sulfuric acid with a concentration of 98wt% dropwise during the stirring process to carry out the catalytic shrinkage reaction, reflux at 120°C for 8 hours, and then use Dean- The Stark device removes the generated water, and the collected product is sequentially washed with saturated sodium bicarbonate, saturated saline and distilled water, and finally the product is purified by column chromatography;

[0047] Wherein, the mass ratio of allyl malonic acid and anhydrous toluene solvent is 0.166:1; The mass ratio of benzyl alcohol and anhydrous toluene solvent is 0.26:1; The mass ratio of allyl malonic acid and the concentrated sulfuric acid of 98wt% The ratio is 120:1; th...

Embodiment 2

[0058] A preparation method of a core-shell type porous silica / iron oxide nanocatalyst, specifically implemented according to the following steps:

[0059] Step 1, the synthesis of allyl malonate:

[0060] Add allylmalonic acid and benzyl alcohol to the anhydrous toluene solvent in sequence, add concentrated sulfuric acid with a concentration of 98wt% dropwise during the stirring process to carry out the catalytic shrinkage reaction, reflux reaction at 122°C for 7h, and then use Dean- The Stark device removes the generated water, and the collected product is sequentially washed with saturated sodium bicarbonate, saturated saline and distilled water, and finally the product is purified by column chromatography;

[0061] Wherein, the mass ratio of allyl malonic acid and anhydrous toluene solvent is 0.168:1; The mass ratio of benzyl alcohol and anhydrous toluene solvent is 0.323:1; The mass ratio of allyl malonic acid and the concentrated sulfuric acid of 98wt% The ratio is 118:...

Embodiment 3

[0073] A preparation method of a core-shell type porous silica / iron oxide nanocatalyst, specifically implemented according to the following steps:

[0074] Step 1, the synthesis of allyl malonate:

[0075] Add allylmalonic acid and benzyl alcohol to the anhydrous toluene solvent in sequence, add concentrated sulfuric acid with a concentration of 98wt% dropwise during the stirring process to carry out the catalytic shrinkage reaction, reflux reaction at 130°C for 9h, and then use Dean- The Stark device removes the generated water, and the collected product is sequentially washed with saturated sodium bicarbonate, saturated saline and distilled water, and finally the product is purified by column chromatography;

[0076] Wherein, the mass ratio of allyl malonic acid and anhydrous toluene solvent is 0.16:1; The mass ratio of benzyl alcohol and anhydrous toluene solvent is 0.35:1; The mass ratio of allyl malonic acid and the concentrated sulfuric acid of 98wt% The ratio is 119:1;...

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Abstract

The invention discloses a method for preparing a core-shell porous silica/iron oxide nanometer catalyst. The preparation method comprises the following concrete steps: step 1, synthesis of allyl malonate; step 2, a hydrosilylation reaction; step 3, a hydrogenation reduction reaction; and step 4, synthesis of the silica/iron oxide nanometer catalyst. Compared with conventional synthetic routes, thepreparation method of the invention has the advantages of practicality, easiness, short production cycle, low cost, and capacity of simultaneously controlling the morphology of iron oxide and the pore size of a silica carrier. The preparation method is implemented through a coordination reaction of a carbonyl precursor containing a POSS-carboxyl group and iron. By controlling the molar ratio of different groups in the reaction, calcination temperature, calcination time and the like, the influence of relevant synthesis parameters on the morphology and structure of the prepared silica/iron oxide nanometer catalyst can be determined.

Description

technical field [0001] The invention belongs to the technical field of chemistry and nanometer materials, and in particular relates to a preparation method of a core-shell porous silica / iron oxide nanocatalyst. Background technique [0002] Iron oxide is a very important inorganic non-metallic material, it is non-toxic, non-polluting, and can be used as magnetic material, polishing agent and pigment. Nanoscale iron oxide usually has significant surface effect, volume effect and small size effect, and it has good absorption and shielding effects on ultraviolet rays, and can be widely used in plastics, leather, coatings, inks, electronics, absorbing materials and Catalytic applications and other fields. At present, there are many preparation methods for the synthesis of nanostructured iron oxides with different morphologies, the main methods are template method, hydrothermal method, solid-phase chemical method and chemical vapor deposition method. Among them, the hydrotherma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745B01J35/00B01J37/08
CPCB01J23/745B01J35/0013B01J35/006B01J35/008B01J37/086
Inventor 王珍姚顺侯先亮方长青潘少菲
Owner XIAN UNIV OF TECH