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Preparation method of solid super-strong acid

A solid superacid and acidic technology, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of short life, inability of oxides to provide binding sites, and low specific surface area

Inactive Publication Date: 2009-08-26
ZHAOQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current research results show that the main reason for limiting the density of such solid superacid acid centers is that its specific surface area is low, which limits the number of acid centers formed. on the carrier, but the dispersion effect is not obvious, so the effect of increasing the acid content is not obvious
Another reason is that this type of solid superacid is formed by the combination of sulfate anion and oxide. The existing preparation conditions cannot provide enough binding sites only by the oxide itself, which also limits the number of acid centers of this type of solid superacid.
[0003] After years of research at home and abroad, a variety of SO 4 2- / MxOy type solid superacid catalyst, but most of them are still in the laboratory research stage, the price is high and the life is short. 4 2- / MxOy type solid superacid catalyst currently has two major problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: SO 4 2- / ZrO 2 -SiO 2 Preparation of solid superacid

[0022] Prepare 300 kg of 0.1-5mol / L ZrOCl in a 1000 liter container 2 solution, add 0.1-1mol / L sodium silicate solution to the solution until the pH is 4-9, age at room temperature for 1-24 hours, take the precipitate and wash until the pH is 6-8, and use 1%-15% Immerse in sulfate ion solution for 1-12 hours, then filter, take the precipitate and roast it at 300-800°C for 1-24 hours to prepare solid super acid SO 4 2- / ZrO 2 -SiO 2 .

[0023] ZrOCl in this embodiment 2 The solution can also be Zr(SO 4 ) 2 solution or other acidic zirconium salt solutions.

Embodiment 2

[0024] Example 2: SO 4 2- / TiO 2 -SiO 2 Preparation of solid superacid

[0025] Prepare 300 kg of 0.1-5mol / L TiCl in a 1000 liter container 4 solution, add 0.1-1mol / L sodium silicate solution to the solution until the pH is 4-9, age at room temperature for 1-24 hours, take the precipitate and wash until the pH is 6-8, and use 1%-15% Immerse in sulfate ion solution for 1-12 hours, then filter, take the precipitate and roast it at 300-800°C for 1-24 hours to prepare solid super acid SO 4 2- / TiO 2 -SiO 2 .

[0026] TiCl in this example 4 The solution can also use TiCl 2 solution or Ti(Et) 4 solution or other acidic titanium salt solutions.

Embodiment 3

[0027] Example three: SO 4 2- / SnO 2 -SiO 2 Preparation of solid superacid

[0028] Prepare 300 kg of 0.1-5mol / L SnCl in a 1000 liter container 4 solution, add 0.1-1mol / L sodium silicate solution to the solution until the pH is 4-9, age at room temperature for 1-24 hours, take the precipitate and wash until the pH is 6-8, and use 1%-15% Immerse in sulfate ion solution for 1-12 hours, then filter, take the precipitate and roast it at 300-800°C for 1-24 hours to prepare solid super acid SO 4 2- / SnO 2 -SiO 2 .

[0029] SnCl in this example 4 The solution can also use SnCl 2 solution or Sn(Et) 4 solution or other acidic tin salt solutions.

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Abstract

The invention relates to the making of a solid super strong acid using dual hydrolysis compounded acidic oxide as the center. In this way, it can realize high degree diffusion, significantly improved acid, activeness and option with reduced cost.

Description

technical field [0001] The present invention relates to a kind of preparation method of solid superacid, relate to a kind of SO 4 2- / MxOy (MxOy represents metal oxide) the preparation method of composite solid superacid. Background technique [0002] Since the late 1970s, it has been found that the SO 4 2- Supported on some metal oxides, after calcination under certain conditions, a kind of SO can be obtained. 4 2- / MxOy type solid acid, as determined by Hammett indicator, its acid strength can reach up to 10,000 times that of 100% sulfuric acid. Therefore, SO 4 2- / MxOy type solid acid is called solid superacid. Solid superacids can activate saturated hydrocarbons that are almost inactive under normal reaction conditions, enabling reactions such as isomerization, decomposition, alkylation, halogenation, nitration, oxidation, and polymerization of paraffins to proceed under mild conditions. Although the acid strength of solid super acid is generally weaker than tha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053C07C67/08
Inventor 郭海福王赵志
Owner ZHAOQING UNIV