Preparation method of mullite sol with low crystal transformation temperature, small particle size and adjustable NO3 <-> content

A small particle size, adjustable technology, applied in the direction of sol preparation, chemical instruments and methods, colloid chemistry, etc., can solve the problems of poor repeatability, long preparation cycle, complex process, etc. The effect of simple process

Pending Publication Date: 2022-05-27
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the prior art, in the preparation process of mullite sol, either the energy consumption is high, the preparation cycle is long, or the process parameters, temperature, and environmental humidity are strictly required, and an additional chelating agent needs to be added. The process is complicated and the repeatability is poor. ideal

Method used

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  • Preparation method of mullite sol with low crystal transformation temperature, small particle size and adjustable NO3 &lt;-&gt; content
  • Preparation method of mullite sol with low crystal transformation temperature, small particle size and adjustable NO3 &lt;-&gt; content
  • Preparation method of mullite sol with low crystal transformation temperature, small particle size and adjustable NO3 &lt;-&gt; content

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Effect test

Embodiment 1

[0039] A kind of low crystallizing temperature, small particle size, NO 3 - The preparation method of the mullite sol with adjustable content, comprises the steps:

[0040] (1) fully mixing ethyl orthosilicate with isopropanol and ethylene glycol to obtain a silanol mixed solution, then dispersing aluminum isopropoxide in the silanol mixed solution with high-speed stirring to obtain a silicoalumino alcohol with a concentration of 50wt% In the salt suspension, the molar ratio of Si element and Al element in the silicoaluminoalkoxide suspension is 1:2.6;

[0041] (2) refluxing the silicoaluminoalkoxide suspension at 60°C for 2h;

[0042] (3) get the molar concentration to be 0.8mol / L aluminum nitrate aqueous solution, mix with the silico-aluminum alkoxide suspension after step (2) backflow, wherein the mol ratio of aluminum nitrate aqueous solution and aluminum alkoxide is 1:6, and in 25 ℃ refluxed for 13h for the first hydrolysis to obtain aluminum-silicon precursor A, the s...

Embodiment 2

[0045] A kind of low crystallizing temperature, small particle size, NO 3 - The preparation method of the mullite sol with adjustable content, comprises the steps:

[0046] (1) fully mixing methyl silicate with n-butanol and ethanol to obtain a silanol mixed solution, then mechanically stirring and dispersing aluminum sec-butoxide in the silanol mixed solution to obtain a 15wt% silicoaluminoalkoxide suspension , the molar ratio of Si element to Al element in the silicoaluminoalkoxide suspension is 1:2.4;

[0047] (2) refluxing the silicoaluminoalkoxide suspension at 55°C for 3h;

[0048] (3) getting molar concentration is 0.15mol / L aluminum nitrate aqueous solution, mixes with the silicoaluminoalkoxide suspension after step (2) backflow, wherein the mol ratio of aluminum nitrate aqueous solution and silicoaluminoalkoxide suspension is 1:4, And reflux for 15h at 20 °C for the first hydrolysis to obtain aluminum-silicon precursor A, the second hydrolysis is to heat the alumin...

Embodiment 3

[0051] A kind of low crystallizing temperature, small particle size, NO 3 - The preparation method of the mullite sol with adjustable content, comprises the steps:

[0052] (1) fully mixing propyl orthosilicate with isopropanol and n-butanol to obtain a silanol mixed solution, then ultrasonically dispersing aluminum isopropoxide and aluminum sec-butoxide in the silanol mixed solution to obtain a concentration of 70wt% The silicoaluminoalkoxide suspension, the molar ratio of Si element and Al element in the silicoaluminoalkoxide suspension is 1:2.7;

[0053] (2) reflux the silicoaluminoalkoxide suspension at 65°C for 2.5h;

[0054] (3) get the molar concentration to be 1.1mol / L aluminum nitrate aqueous solution, mix with the silicoaluminum alkoxide suspension after step (2) backflow, wherein the mol ratio of the aluminum nitrate aqueous solution and the silicoaluminum alkoxide suspension is 1:10, And refluxed at 35 °C for 10 h for the first hydrolysis to obtain the aluminum-...

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Abstract

The invention discloses a preparation method of mullite sol with low crystal transformation temperature, small particle size and adjustable NO3 <-> content, and belongs to the field of preparation of mullite sol. The method comprises the following steps: (1) fully mixing a silicon source with an alcohol solvent to obtain a silanol mixed solution, and then uniformly dispersing aluminum alkoxide in the silanol mixed solution to obtain a silicon-aluminum alkoxide suspension; (2) carrying out reflux reaction on the silicon-aluminum alkoxide suspension at a proper temperature; and (3) taking a proper amount of an aluminum nitrate aqueous solution, mixing the aluminum nitrate aqueous solution with the silicon-aluminum alkoxide suspension subjected to reflux in the step (2), and carrying out step-by-step heating reflux to obtain the mullite sol with low crystal transformation temperature, small particle size and adjustable NO3 <-> content. The method has the advantages of no need of additional addition of a chelating agent, simple process, low requirements on synthesis equipment, good repeatability, no pollution and high safety, and is suitable for large-scale industrial production.

Description

technical field [0001] The present application relates to a kind of low crystallization temperature, small particle size, NO 3 - The invention discloses a preparation method of mullite sol with adjustable content, belonging to the field of preparation of mullite sol. Background technique [0002] Mullite has the advantages of high temperature resistance, high strength, and low thermal conductivity. It is usually used in high temperature refractory materials. The traditional preparation of mullite requires high sintering temperature and high energy consumption. The water-controlled aluminum-silicon hydrolysis process is carried out slowly and gradually or by controlling the system environment to achieve slow hydrolysis to reduce the sintering temperature. In recent years, various preparation methods for preparing mullite at low temperature have been reported in literature and patents published at home and abroad. [0003] Chen et al. (Design and preparation of high permeabi...

Claims

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Application Information

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IPC IPC(8): C01B33/26B01J13/00
CPCC01B33/26B01J13/0026C01P2002/72C01P2002/82C01P2002/88C01P2004/04C01P2004/51C01P2004/62Y02E60/10
Inventor 陈代荣朱健明焦秀玲王文贞刘洋张立贾玉娜
Owner SHANDONG UNIV
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