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Method for preparing self-assembled hollow alumina microspheres by taking sesbania gum as template

A hollow alumina and self-assembly technology, applied in the field of materials, can solve the problems of difficulty in realizing alumina preparation, difficulty in large-scale promotion, limitation of alumina growth specificity, etc., so as to reduce the loss of target products, increase the precipitation width, and increase production. rate effect

Pending Publication Date: 2021-06-15
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 micro-nano-scale alumina with controllable morphology, scientific researchers have gradually explored production methods such as microemulsion method and sol-gel method for decades. However, the above production methods mostly use toxic organic reagents as templates. The growth specificity of the alumina produced is limited, it is difficult to realize the preparation of alumina with a specific structure, and it is difficult to achieve further large-scale promotion in actual production and life.

Method used

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  • Method for preparing self-assembled hollow alumina microspheres by taking sesbania gum as template
  • Method for preparing self-assembled hollow alumina microspheres by taking sesbania gum as template
  • Method for preparing self-assembled hollow alumina microspheres by taking sesbania gum as template

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Experimental program
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Effect test

Embodiment 1

[0032] Step 1: Add 5.5g of aluminum sulfate octadecahydrate, 6.0g of dicyandiamide and 7.5g of methylpyrrolidone into 70ml of deionized water in sequence, and ultrasonically disperse at 80°C for 25min to obtain a clear solution A;

[0033] Step 2: Gradually add 40ml of safflower gum solution with a concentration of 1.2mol / L dropwise to solution A, then add dropwise an ammonia solution with a concentration of 1.0mol / L until the pH value is 8.5, and finally at a temperature of 160°C with 500r / L The stirring rate of min was heated and magnetically stirred for 25 min to obtain solution B;

[0034] Step 3: Move solution B to a rotary micro-polymerization reactor, and set the following system to react in two stages for 8 hours: the pressure of the first stage is 40Pa, the temperature is 100°C, the rotation speed is 40r / min, and the micro-polymerization reaction time is 2h; the pressure of the second stage is 30Pa, the temperature is 180°C, the rotation speed is 100r / min, the micropo...

Embodiment 2

[0038] Step 1: Add 7.5g of aluminum sulfate octadecahydrate, 5.0g of dicyandiamide and 7.0g of methylpyrrolidone into 60ml of deionized water in sequence, and ultrasonically disperse at 70°C for 15 minutes to obtain a clear solution A;

[0039] Step 2: Gradually add 20ml of 2.4mol / L squash gum solution dropwise to solution A, then dropwise add ammonia solution with a concentration of 1.5mol / L until the pH value is 8.2, and finally at 170°C at 400r / L The stirring rate of min was heated and magnetically stirred for 15 min to obtain solution B;

[0040] Step 3: Move solution B to a rotary micro-polymerization reactor, and set the following system to react for 5 hours in two stages: the pressure of the first stage is 30Pa, the temperature is 80°C, the rotation speed is 100r / min, and the micro-polymerization reaction time is 1h; the pressure of the second stage is 40Pa, the temperature is 200°C, the rotation speed is 80r / min, and the micro-polymerization reaction time is 5h. After ...

Embodiment 3

[0046] Step 1: Add 6.5g of aluminum sulfate octadecahydrate, 7.0g of dicyandiamide and 6.2g of methylpyrrolidone into 80ml of deionized water in sequence, and ultrasonically disperse at 60°C for 22min to obtain a clear solution A;

[0047] Step 2: Gradually add 30ml of 2.0mol / L squash gum solution dropwise to solution A, then dropwise add ammonia solution with a concentration of 0.6mol / L until the pH value is 9.2, and finally at 180°C at 450r / L The stirring rate of min was heated and magnetically stirred for 20 min to obtain solution B;

[0048] Step 3: Move solution B to a rotary micro-polymerization reactor, and set the following system to react for 7 hours in two stages: the pressure of the first stage is 20Pa, the temperature is 60°C, the rotation rate is 70r / min, and the micro-polymerization reaction time is 1.5h; the pressure of the second stage is 50Pa, the temperature is 160°C, the rotation speed is 120r / min, the micro-polymerization reaction time is 4h, and the produc...

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Abstract

The invention discloses a method for preparing self-assembled hollow alumina microspheres by taking sesbania gum as a template. The method comprises the following steps: 1, adding aluminum sulfate octadecahydrate, dicyandiamide and methyl pyrrolidone into deionized water, and carrying out ultrasonic dispersion to obtain a clear solution A; 2, gradually dropwise adding a sesbania gum solution into the solution A, adjusting the pH value to 8.2-9.2, and performing magnetic stirring to obtain a solution B; 3, transferring the solution B into a rotary micro-polymerization reactor for micro-polymerization reaction, and collecting a product to obtain a solid C; 4, washing the solid C for multiple times, performing vacuum freeze drying, and performing collecting to obtain a white powdery solid D; 5, mixing the solid D with potassium aluminum fluoride, transferring the mixture into a muffle furnace, preserving heat, and performing cooling, washing and drying to obtain the self-assembled hollow aluminum oxide microspheres. A micro-nano spherical space structure naturally formed in the sesbania gum is used as a growth template of alumina seed crystals, the obtained alumina crystal grains are good in orientation and uniform, the production and manufacturing cost is lower, and the production process is simple.

Description

technical field [0001] The invention belongs to the field of materials, and in particular relates to a method for preparing self-assembled hollow aluminum oxide microspheres by using squash gum as a template. Background technique [0002] Since the 1930s, alumina raw materials have gradually shined in the field of construction and construction machinery components due to their low price and good mechanical properties, and have become an important experimental raw material. Alumina is mainly divided into three types according to different crystal forms: α-Al 2 o 3 , β-Al 2 o 3 and γ-Al 2 o 3 , where α-Al 2 o 3 The properties are stable, the strength of the particles is high, and it is usually used in the structural parts of aircraft, while β-Al 2 o 3 and γ-Al 2 o 3 Due to the particularity of the morphology, it is widely used in the fields of catalyst carrier and photoelectrocatalysis. Su Qiaoqiao, Chen Xiaojun, Zhou Long. Preparation of nanometer α-Al by chemical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/32
CPCC01F7/32C01P2004/03C01P2002/72C01P2004/34
Inventor 曹丽云钟辛子黄剑锋欧阳海波杨子煊吴辰宇蒋永张颢淼
Owner SHAANXI UNIV OF SCI & TECH
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