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Magnetic solid super strong acid catalyst and its preparing method

A solid superacid and catalyst technology, which is applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as difficult separation of reactants and catalysts, difficulty in separation of catalysts and products, and large waste of raw materials , to achieve the effect of saving raw materials, easy separation, and reducing environmental pollution

Inactive Publication Date: 2003-12-31
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the solid superacids used in reactions such as hydrocarbon alkylation, isomerization, and esterification at home and abroad mainly include SO 4 2- Promoted oxide superacids such as Ni, Zr, Sn, etc. In order to improve the catalytic activity of solid superacid catalysts, researchers should increase their acid strength as much as possible. The MCM-41 load SO published by the author Lei Ting et al. 4 2- / ZrO 2 In the article on the properties of super acid, the author used the impregnation process to prepare MCM-41 loaded SO 4 2- / ZrO 2 type solid superacid, but its disadvantages in the application of the solid superacid catalyst prepared above are that the separation of the catalyst and the product is difficult, the reaction interface is small and the mass transfer resistance is large
Among the existing methods for preparing solid superacid catalysts, the most commonly used methods are two-step synthesis and one-step synthesis. Both methods use impregnation in the preparation process, and the disadvantage is that raw materials are wasted in the preparation process. Large, high cost, and it is quite difficult to separate the reactant from the catalyst when catalyzing the liquid phase reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh Fe 3 o 4 with ZrO 2 Molar ratio is that 1: 80 magnetic solid superacid 1g joins in the three-necked flask that is equipped with thermometer, oil-water separator, condensing pipe, adds the glacial acetic acid of 8ml, the n-butanol of 51ml simultaneously, under magnetic stirring, reflux, The material was reacted in boiling state for 6h. Utilize the magnetic separation device to recover the catalyst, continue to do the esterification reaction, and analyze the content of the reaction product with a gas chromatograph, and calculate the yield of the ester to be 96.4%.

Embodiment 2

[0019] Take 75mL magnetic fluid (0.01molFe 3 o 4 / L), add 300mL distilled water and ultrasonically disperse for 30min (ultrasonic vibration frequency is 20-50kHz), transfer to a three-necked bottle, heat up to 65°C in an oil bath, and mechanically stir for 30min (stirring speed 600-800rpm); accurately weigh 19.335g of ZrOCl 2 , add 50mL of distilled water to dissolve and pour it into a separatory funnel, put ammonia water into another separatory funnel, raise the temperature to 75°C, and drop zirconium oxychloride and ammonia water (dropping speed: 2 drops / second) to ZrOCl 2 All the drops are finished; when the pH of the solution is adjusted to 13, stop adding ammonia water; stir and age at a constant temperature for 2 hours; transfer the solution into a 1000mL beaker, and use magnetic separation technology to make it settle; pour off the supernatant, add distilled water, and wash repeatedly to solution neutral and Cl-free - until the product is filtered by suction and dried...

Embodiment 3

[0021] Change Fe 3 o 4 with ZrO 2 Molar ratio, iron-based magnetic fluid (0.01mol Fe 3 o 4 / L) take 25mL, ZrOCl 2 Take by weighing 8.056g, other experimental conditions are with embodiment 2, can make Fe 3 o 4 with ZrO 2 A magnetic solid superacid catalyst with a molar ratio of 1:100, denoted as Fe 3 o 4 / ZrO 2 .

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Abstract

The magnetic solid super strong acid is prepared by using magnetic matter Fe3O4, Ni-Fe3O4, Co-Fe3O4, or Mn-Fe3O4 and super strong solid acid through improved chemical codeposition and homogenization. The technological process consists of preparation of magnetic fluid, supersonic dispersion, furmation of sol-gel solution, magnetic separation and washing, stoving and baking. The magnetism makes the separation and recovering of the catalyst and reaction product easy and possess high acidity and porosity. The catalyst is friendly to environment and high in efficiency and has wide application in alkylation, isolmerization, esterification, etc. of hydrocarbon.

Description

technical field [0001] The invention relates to a new solid acid-magnetic solid superacid catalyst. The invention also relates to a preparation method of the catalyst. Background technique [0002] At present, the solid superacids used in reactions such as hydrocarbon alkylation, isomerization, and esterification at home and abroad mainly include SO 4 2- Promoted oxide superacids such as Ni, Zr, Sn, etc. In order to improve the catalytic activity of solid superacid catalysts, researchers should increase their acid strength as much as possible. The MCM-41 load SO published by the author Lei Ting et al. 4 2- / ZrO 2 In the article on the properties of super acid, the author used the impregnation process to prepare MCM-41 loaded SO 4 2- / ZrO 2 Type solid superacid, but its shortcoming in the application of solid superacid catalyst of above-mentioned preparation is, the separation difficulty of catalyst and product, reaction interface is little and mass transfer resistanc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053B01J37/03
Inventor 张密林王君景晓燕段雪
Owner HARBIN ENG UNIV