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Method for preparing ceramic hollow microspheres by using peristaltic pump assisted coaxial micro-fluidic system

A technology of a microfluidic system and a peristaltic pump is applied in the field of preparing ceramic hollow microspheres assisted by a peristaltic pump-assisted coaxial microfluidic system, which can solve the problems of high cost, low strength, weakening the advantages of hollow microspheres, and the like, and achieve a simple process flow. , low energy consumption, controllable sphere size and hollow rate

Inactive Publication Date: 2015-03-04
SHANGHAI JIAO TONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no patent report of ceramic hollow microspheres that can realize low-cost commercialization in my country. The commercialized glass hollow microspheres of 3M and PQ companies have low strength. Under pressure conditions, glass hollow microspheres are easy to break, resulting in actual During use, the performance of coatings and coatings decreases greatly, and the water absorption rate is high
In order to solve the problem of low strength of glass hollow microspheres, 3M company has developed high-strength ceramic hollow microspheres, whose chemical components are mainly alumina and zirconia series. ), which greatly weakens the advantages of hollow microspheres as fillers, and the cost is three times that of glass hollow microspheres
The porous ceramic microspheres obtained in this patent are spheres with open pores on the surface, which have high hygroscopicity, poor fluidity, low strength and low heat insulation effect
And obtaining the precursor of ceramic microspheres at low temperature requires a lot of energy refrigeration

Method used

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  • Method for preparing ceramic hollow microspheres by using peristaltic pump assisted coaxial micro-fluidic system
  • Method for preparing ceramic hollow microspheres by using peristaltic pump assisted coaxial micro-fluidic system
  • Method for preparing ceramic hollow microspheres by using peristaltic pump assisted coaxial micro-fluidic system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step 1: Add 8g of polyethersulfone to 90g of NMP, stir to dissolve, then add a mixture of 1.95g of stabilized zirconia ceramic powder and 0.05g of iron oxide powder, continue to stir and mix evenly, and age and degas to obtain a slurry.

[0035] Step 2: Use deionized water as the non-solvent. The inner tube 6 of the coaxial nozzle has a diameter of 0.15 mm and the outer tube 7 of the coaxial nozzle has a diameter of 0.5 mm. The distance between the coaxial nozzle 5 and the non-solvent tank 8 is set to 10 mm. First open the compressed nitrogen drive pressure system: compressed nitrogen cylinder 2, pressure reducing valve 10, precision pressure gauge 11, screw valve 12, rotameter 13 to deliver the driving pressure within 0.1MP, by adjusting the non-solvent pipeline The rotary valve and the peristaltic pump speed (0.5 rev / min) make the non-solvent in the non-solvent tank 3 smoothly drop out in droplet shape. Then pour the slurry prepared in step 1 into the slurry tank 1, ...

Embodiment 2

[0039] Step 1: Add 28g of polyethersulfone to 60g of NMP, stir to dissolve, then add a mixture of 11.5g of stabilized zirconia ceramic powder and 0.5g of iron oxide powder, continue to stir and mix evenly, age and degas to obtain a slurry.

[0040] Step 2: Use deionized water as a non-solvent. Choose a coaxial nozzle with a diameter of 0.5 mm in the inner tube 6 of the coaxial nozzle and a diameter of 1.2 mm in the outer tube 7 of the coaxial nozzle. Set the coaxial nozzle 5 and the non-solvent tank 8. The distance between them is 50mm. First open the compressed nitrogen drive pressure system: compressed nitrogen cylinder 2, pressure reducing valve 10, precision pressure gauge 11, screw valve 12, rotameter 13 to deliver the driving pressure within 0.1MP, by adjusting the non-solvent pipeline The rotary valve and the peristaltic pump speed (0.5 rev / min) make the non-solvent in the non-solvent tank 3 smoothly drop out in droplet shape. Then pour the slurry prepared in step 1 in...

Embodiment 3

[0044] Step 1: Add 30g of polyethersulfone to 60g of NMP, stir to dissolve, then add a mixture of 9.8g of stabilized zirconia ceramic powder and 0.2g of iron oxide powder, continue to stir and mix evenly, age and degas to obtain a slurry.

[0045] Step 2: Use deionized water as the non-solvent. The inner tube 6 of the coaxial nozzle has a diameter of 0.8 mm and the outer tube 7 of the coaxial nozzle has a diameter of 3.0 mm. The distance between the coaxial nozzle 5 and the non-solvent tank 8 is set to 50 mm. First open the compressed nitrogen driving pressure system: compressed nitrogen cylinder 2, pressure reducing valve 10, precision pressure gauge 11, screw valve 12, rotameter 13, the driving pressure of which the delivery pressure is within 0.2MP, by adjusting the non-solvent pipeline The rotary valve and the peristaltic pump speed (2.0 rev / min) make the non-solvent in the non-solvent tank 3 flow out smoothly in the form of droplets. Then pour the slurry prepared in step...

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Abstract

The invention relates to a method for preparing ceramic hollow microspheres by using a peristaltic pump assisted coaxial micro-fluidic system. The method comprises the following three steps: preparing precursor slurry, preparing a precursor and sintering. The dropping ceramic hollow microspheres precursor liquid drops are collected by utilizing a non-solvent induced phase separation principle, so that the outer surfaces of the dropping liquid drops are separated and cured, deformation and refusion of the liquid drops are effectively avoided, and the ceramic hollow microsphere precursor is obtained. The precursor is subjected to room-temperature drying and Muffle furnace sintering, and finally the ceramic hollow microspheres are obtained. Compared with the prior art, the ceramic hollow microspheres prepared by the invention are good in sphericity degree and controllable in sphere size and porosity, lots of energy and acid-base reagents do not need to be consumed, the process is simple and easy, and large-scale industrial production is easily realized.

Description

technical field [0001] The invention relates to a method for preparing ceramic hollow microspheres, in particular to a method for preparing ceramic hollow microspheres assisted by a coaxial microfluidic control system with a peristaltic pump. Background technique [0002] In recent years, ceramic / glass hollow microspheres have been widely used as filler materials, including lightweight fillers in polymers for various purposes; fillers in paint and coating materials; preparation of heat insulation and sound insulation dielectric materials; marine Develop and research buoyancy materials for deep water technology; composite materials of high-strength, non-deformable lightweight alloys and glass hollow microspheres, as well as filling materials for various insulation and heat insulation materials, etc. Hollow microspheres refer to a type of spherical shell material with a size ranging from a few nanometers to several millimeters and a hollow structure inside. The hollow part can...

Claims

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Application Information

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IPC IPC(8): C04B35/48C04B35/10C04B35/622
Inventor 郭芳威赵晓峰何勇
Owner SHANGHAI JIAO TONG UNIV
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