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Technology for preparing solid acid catalyst by reversed-phase microemulsion method

A technology of solid acid catalyst and inverse microemulsion, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, chemical instrument and method, etc., and can solve the problems of dispersion of easily agglomerated particles, easy loss of sulfate radical, short service life, etc. problems, to achieve the effects of controllable particle size, simple steps, and improved catalytic efficiency

Active Publication Date: 2014-09-10
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The design of this nanoparticle synthesis method is expected to overcome the disadvantages of easy agglomeration, poor particle dispersion, and uneven size of solid superacids synthesized by traditional processes.
Single-component solid superacid catalyst plays an important role. Sulfate radicals are easy to lose during the reaction and are easily deactivated under high temperature conditions. Therefore, the single-component solid catalyst has good catalytic activity at the beginning, but its service life is short.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Add 0.8g of Ti(SO 4 ) 2 9H 2 O﹑0.8gAl(NO 3 ) 3 9H 2 O was added to 5mL deionized water, stirred, and set aside;

[0020] (2) Take 11mL Span-80, 11mL n-butanol, 25mL cyclohexane and 5mL of the solution in step (1) and mix evenly, stir for 30min to obtain a clear and transparent inverse microemulsion, set aside;

[0021] (3) Add 1.5 g of ammonium carbonate to 5 mL of deionized water, stir to obtain an ammonium carbonate solution;

[0022] (4) Mix 11mL of Span-80, 11mL of n-butanol, 25mL of cyclohexane with 5mL of the solution in the above step (3), and stir for 30-40min to obtain a clear and transparent inverse microemulsion for later use;

[0023] (5) Mix the solutions prepared in the above step (2) and step (4), stir the reaction for 1.5h, let it settle for 20h, filter, wash repeatedly with deionized water and ethanol, and use AgNO 3 Solution detection, until the filtrate does not contain Cl-, the filter cake is dried and set aside;

[0024] (6) Use 0.25mol·...

Embodiment 2

[0027] (1) Add 0.8g of Ti(SO 4 ) 2 9H 2 O﹑0.8gAl(NO 3 ) 3 9H 2 O was added to 6mL deionized water, stirred, and set aside;

[0028] (2) Mix 11ml of Span-80, 6mL of n-butanol, 25mL of cyclohexane with 6mL of the solution in the above step (1), and stir for 30-40min to obtain a clear and transparent inverse microemulsion for later use;

[0029] (3) Add 1.5 g of ammonium carbonate to 6 mL of deionized water, stir, and set aside;

[0030] (4) Mix 11ml of Span-80, 6mL of n-butanol, 25mL of cyclohexane with 6mL of the solution in the above step 3, stir for 30-40min to obtain a clear and transparent inverse microemulsion, and set aside;

[0031] (5) Mix the solutions prepared in the above step (2) and step (4), stir the reaction for 1.5h, let it settle for 20h, filter, wash repeatedly with deionized water and ethanol, and use AgNO 3 Solution testing until the filtrate is Cl-free - until the filter cake is dried and set aside;

[0032] (6) Use 0.25mol·L -1 (NH 4 ) 2 SO 4 ...

Embodiment 3

[0035] (1) Add 0.8g of Ti(SO 4 ) 2 9H 2 O﹑0.8gAl(NO 3 ) 3 9H 2 O was added to 5mL deionized water, stirred, and set aside;

[0036] (2) Mix 11ml of Span-80, 6mL of n-butanol, 25mL of cyclohexane with 5mL of the solution in the above step (1), stir for 30-40min to obtain a clear and transparent inverse microemulsion, and set aside;

[0037] (3) Add 1.5 g of ammonium carbonate to 5 mL of deionized water, stir, and set aside;

[0038] (4) Mix 11ml of Span-80, 6mL of n-butanol, 25mL of cyclohexane with 5mL of the solution in the above step (3), stir for 30-40min to obtain a clear and transparent inverse microemulsion, and set aside;

[0039] (5) Mix the solutions prepared in the above step (2) and step (4), stir the reaction for 1.5h, let it settle for 20h, filter, wash repeatedly with deionized water and ethanol, and use AgNO 3 Solution detection, until the filtrate does not contain Cl-, the filter cake is dried and set aside;

[0040] (6) Use 0.25mol·L -1 (NH 4 ) 2 SO...

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Abstract

The invention relates to a technology for preparing a solid acid catalyst by a reversed-phase microemulsion method. the technology comprises the following steps: mixing Ti(SO4)2.9H2O, Al(NO3)3.9H2O and deionized water to prepare an inorganic salt solution, adding a surfactant, a cosurfactant and an oil phase into the stirred inorganic salt solution and mixing to obtain a microemulsion A, mixing the surfactant, the cosurfactant, the oil phase and a stirred ammonium carbonate aqueous solution to obtain a microemulsion B, mixing A and B, filtering, dipping by the use of a (NH4)2SO4 solution, and calcining to obtain solid superacid. The catalyst provided by the invention has advantages of good dispersity of synthesized particles, small and controllable particle size and large specific surface area. In comparison with catalysts prepared by existing methods, the catalyst provided by the invention has better catalytic activity and its catalytic efficiency is raised by 5%-10%.

Description

technical field [0001] The invention relates to the preparation of a solid acid catalyst, in particular to TiO 2 -Al 2 o 3 / SO 4 2- The invention relates to a preparation process of solid superacid nano powder, which belongs to the technical field of catalyst preparation. Background technique [0002] Solid superacid catalysts can be widely used in cracking, alkylation, acylation, esterification, isomerization, polymerization, oligomerization and oxidation reactions in organic synthesis, and because of their low corrosion to equipment and low environmental pollution And other advantages, in green chemistry, environment-friendly catalysis, has a very broad application prospects. Traditional TiO 2 -Al 2 o 3 / SO 4 2- The preparation methods of solid superacid mainly include precipitation-impregnation method, hydrothermal method, co-precipitation method, sol-gel method, self-assembly method, etc., but these methods are cumbersome to operate, and the solid acid catalyst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053B01J37/00
Inventor 张志德王重斌陈玉琴满城娜
Owner SHANDONG NORMAL UNIV
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