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A kind of preparation method of magnetic carbonaceous solid acid catalyst

A solid acid catalyst and magnetic technology, applied in the field of carbon materials, can solve the problems of poor catalytic activity, underdeveloped pore structure, time-consuming and cumbersome preparation process, etc., and achieve the effect of simple preparation method, good repeatability and high water resistance

Inactive Publication Date: 2016-11-09
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the carbon-based solid acid obtained by this method still has some shortcomings, such as underdeveloped pore structure, low acidity, poor catalytic activity, and time-consuming and cumbersome preparation process.

Method used

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  • A kind of preparation method of magnetic carbonaceous solid acid catalyst
  • A kind of preparation method of magnetic carbonaceous solid acid catalyst
  • A kind of preparation method of magnetic carbonaceous solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Preparation of iron-based complexes

[0040] Soak 1.2 kg of cleaned banana peel fragments in 1.8 L of 1.0 mol / L ferric chloride aqueous solution and heat to dry at 80° C. to obtain a gray-black iron-based composite.

[0041] 2. Preparation of magnetic porous carbon materials

[0042] The obtained iron-based composite was calcined at 650° C. for 3 hours under the protection of an inert gas, washed with distilled water and absolute ethanol in sequence, and dried at 80° C. for 12 hours to obtain a magnetic porous carbon material.

[0043] 3. Preparation of magnetic carbonaceous solid acid catalyst

[0044] The obtained magnetic porous carbon material was mixed with fuming sulfuric acid at a mass ratio of 1:15, ultrasonically treated for 30 minutes, followed by sulfonation treatment at 120°C for 12 hours under airtight conditions, then cooled to room temperature, and slowly added to 500mL of distilled water, Filter, wash with distilled water until no sulfate ions exist...

Embodiment 2

[0047] In the preparation step 1 of the iron-based composite of the present embodiment, the concentration of the ferric chloride aqueous solution used is 0.8mol / L, and other steps are the same as in Example 1, and a magnetic carbonaceous solid acid catalyst is prepared, which presents a porous structure ( See Figure 4 ). Depend on Figure 5 It can be seen that both the obtained magnetic porous carbon material and the magnetic carbonaceous solid acid catalyst are composed of carbon-Fe 3 o 4 species composition. Infrared spectroscopy showed (see Figure 6 ), the surface of the resulting magnetic carbonaceous solid acid catalyst contains sulfonic acid groups.

Embodiment 3

[0049] In the step 1 of preparing the iron-based composite in this embodiment, the concentration of the ferric chloride aqueous solution used is 0.6 mol / L, and the other steps are the same as in the embodiment 1 to prepare a magnetic carbonaceous solid acid catalyst. Depend on Figure 7 It can be seen that the obtained magnetic carbonaceous solid acid catalyst presents a nanosheet-like mesoscopic structure, and Fe with different particle sizes 3 o 4 The nano crystallites are evenly distributed in the carbon skeleton. Energy spectrum analysis also shows that the magnetic carbonaceous solid acid catalyst is mainly composed of C, O and Fe elements ( Figure 8 ). Figure 9-10 It shows that the prepared magnetic carbonaceous solid acid catalyst not only retains the Fe2p species well, but also the sulfonic acid group is successfully modified. Fe2p photoelectron spectroscopy ( Figure 11 ) further reveals that the magnetic substance is Fe 3 o 4 instead of Fe 2 o 3 .

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Abstract

The invention discloses a preparation method of a magnetic carbonaceous solid acid catalyst. The method uses waste banana peels as raw materials. First, the banana peel fragments are soaked in a certain concentration of ferric chloride aqueous solution, and after the coordination modification of metal iron ions The iron-based composites that can form porous channels, and then use this composite as a carrier to construct magnetic porous carbon materials, and use the hydrothermal sulfonation method to functionalize the surface of magnetic porous carbon, and finally prepare magnetic carbonaceous solid acid catalyst. The method of the invention is simple and the conditions are mild, and the specific surface area of ​​the obtained magnetic carbonaceous solid acid catalyst is 160-1100m 2 / g, the pore volume is 0.17~0.74cm 3 / g, the average mesopore size is 6.1-11.4nm, and the highest acidity is 2.68mmol H + / g, and has high water resistance, stability, repeatability, and good external magnetic field separation ability, and exhibits extraordinary catalytic activity in the reaction of esterified oleic acid and methanol, and is expected to be used as a high-efficiency catalyst for Preparation of biodiesel by esterification.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and in particular relates to a method for preparing a magnetic carbonaceous solid acid catalyst using banana peel as a raw material. Background technique [0002] Carbonaceous solid acid catalysts are a new family of solid acids. Compared with non-carbon-based solid acids, they have unique properties such as high specific surface area, large pore capacity, high thermal stability and mechanical properties, and corrosion resistance. An environment-friendly catalyst has attracted more and more attention and has great application prospects in the field of catalysis. In order to improve the specific surface area, pore capacity, acidity and catalytic activity of carbonaceous solid acids, some methods have been reported successively, such as sulfonating various activated carbons, porous carbons, graphene, adjusting carbonization temperature of carbon supports and changing sulfonation conditions...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745B01J35/10C07C67/08C07C69/58
Inventor 张志琪刘瑞林安蕾高翔宇
Owner SHAANXI NORMAL UNIV
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