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Method for preparing self-assembled hollow alumina microspheres by using double precipitants

A hollow alumina, double precipitant technology, applied in the field of materials, can solve the problems of popularization and promotion, difficult to control the size of alumina, and achieve the effect of simplifying the process operation steps, reducing the loss of the target product, and improving the yield.

Pending Publication Date: 2021-06-18
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to prepare alumina powder raw materials with better growth orientation and small particle size, scientific researchers have launched research on production and preparation technology development and equipment research and development. In recent years, they have successfully explored microemulsion method, detonation method, precipitation method, There are various preparation methods such as sol-gel method, but the above methods involve highly polluting reagent template raw materials, and it is difficult to control the size of alumina prepared by production. At present, most of them are limited to the laboratory stage and have not been used in actual production. to further popularize and promote

Method used

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  • Method for preparing self-assembled hollow alumina microspheres by using double precipitants
  • Method for preparing self-assembled hollow alumina microspheres by using double precipitants
  • Method for preparing self-assembled hollow alumina microspheres by using double precipitants

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Experimental program
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Effect test

Embodiment 1

[0030] Step 1: Take 4.8g of polyaluminum chloride sol and 7.0g of malonylurea and add it to 50ml of dilute hydrochloric acid solution with a concentration of 1.0mol / L at the same time, stir at 100°C at a stirring rate of 400r / min for 15min until white The colloidal substance is completely dissolved to obtain solution A;

[0031] Step 2: Gradually add 50ml of methylpyrrolidone mixed solution in the volume ratio of methylpyrrolidone: dodecylalanine: deionized water = 2:1.5:1 to solution A, and stir until the solution is added dropwise Mix evenly, then add dropwise the xanthan gum mixed solution configured according to the mass ratio of xanthan gum: ammonia water: deionized water 7:1:16 to the solution until the pH value is 7.5, and finally at 100°C with 600r / min Stir at a stirring rate for 10 min to obtain solution B;

[0032] Step 3: Move the solution B to a microwave ultrasonic hydrothermal synthesizer, set the reaction temperature to 180°C, the ultrasonic frequency to 50KHz,...

Embodiment 2

[0037] Step 1: Add 6.5g of polyaluminum chloride sol and 6.8g of malonylurea to 40ml of dilute hydrochloric acid solution with a concentration of 1.2mol / L at the same time, stir at 120°C at a stirring rate of 500r / min for 20min until white The colloidal substance is completely dissolved to obtain solution A;

[0038] Step 2: Gradually add 40ml of methylpyrrolidone mixed solution in the volume ratio of methylpyrrolidone: dodecylalanine: deionized water = 1:1:1 to the solution A, and stir until the solution is added dropwise Mix evenly, then add dropwise the xanthan gum mixed solution prepared according to the mass ratio of xanthan gum: ammonia water: deionized water = 9:2:20 to the solution until the pH value is 7.2, and finally at 80°C at 500r / min The stirring rate was stirred for 5min to obtain solution B;

[0039] Step 3: Move the solution B to a microwave ultrasonic hydrothermal synthesizer, set the reaction temperature to 160°C, the ultrasonic frequency to 40KHz, and the ...

Embodiment 3

[0042] Step 1: Take 6.0g of polyaluminum chloride sol and 7.5g of malonylurea and add it to 60ml of dilute hydrochloric acid solution with a concentration of 0.5mol / L at the same time, stir at 80°C at a stirring rate of 300r / min for 10min until white The colloidal substance is completely dissolved to obtain solution A;

[0043] Step 2: Gradually add 60ml of methylpyrrolidone mixed solution in the volume ratio of methylpyrrolidone: dodecylalanine: deionized water = 3:1:1.5 to solution A, and stir until the solution is added dropwise Mix evenly, then add dropwise to the solution the xanthan gum mixed solution prepared according to the mass ratio of xanthan gum: ammonia water: deionized water = 8:3:18 until the pH value is 8.0, and finally at 120°C at 800r / min The stirring rate was stirred for 7min to obtain solution B;

[0044] Step 3: Move the solution B to a microwave ultrasonic hydrothermal synthesizer, set the reaction temperature to 200°C, the ultrasonic frequency to 60KHz...

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Abstract

The invention discloses a method for preparing self-assembled hollow alumina microspheres by using double precipitants. The method comprises the following steps: 1, taking polyaluminum chloride sol and malonyl urea, simultaneously adding polyaluminum chloride sol and malonyl urea into a diluted hydrochloric acid solution, heating and stirring the mixture until white gelatinoids are completely dissolved to obtain a solution A; 2, dropwise adding a mixed solution of methyl pyrrolidone, dodecyl aminopropionic acid and deionized water into the solution A, and adjusting the pH value to 7.2-8.0 to obtain a solution B; 3, transferring the solution B into a microwave ultrasonic hydrothermal synthesizer to react to obtain a white agglomerated solid C; and 4, uniformly mixing the solid C and aluminum fluoride in a vacuum tube furnace, and calcining to obtain self-assembled hollow aluminum oxide microspheres. The alumina obtained by taking a micro-nano spherical space structure naturally formed by xanthan gum as the growth template of the alumina seed crystal has the advantages of good grain orientation, uniform grain, high product purity, lower production and manufacturing cost and simple production process, and the preparation efficiency of the product is effectively improved.

Description

technical field [0001] The invention belongs to the field of materials, and in particular relates to a method for preparing self-assembled hollow alumina microspheres by using double precipitants. Background technique [0002] Alumina is mainly divided into α-Al according to the different crystal forms 2 o 3 , β-Al 2 o 3 and γ-Al 2 o 3 , where α-Al 2 o 3 As a stable phase, it is widely used in structural ceramics, refractory materials, aerospace and other fields because of its high hardness, high strength, good wear resistance and heat resistance, and β-Al 2 o 3 and γ-Al 2 o 3 Because of its special structure and physical and chemical properties, it occupies a place in the catalyst and its carrier, composite materials and other industries. With the development of science and technology, alumina has been widely used in bioceramics, electronic devices, environmental protection, new energy, etc. In order to meet the increasing application requirements, people's growt...

Claims

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Application Information

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IPC IPC(8): C01F7/30B01J13/02
CPCC01F7/306B01J13/02C01P2002/72C01P2004/03C01P2004/34
Inventor 曹丽云钟辛子黄剑锋欧阳海波杨子煊吴辰宇张颢淼蒋永
Owner SHAANXI UNIV OF SCI & TECH