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Method for preparing big-diameter granules from micro and nano powder by means of interfacial polymerization

An interfacial polymerization, micro-nano technology, used in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of difficult to control the internal porosity of particles, poor sphericity and surface finish, and uneven particle size, and achieve true sphericity. High, wide particle size range, uniform particle size distribution effect

Inactive Publication Date: 2011-06-08
ZHENGZHOU UNIV
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  • Claims
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AI Technical Summary

Problems solved by technology

The spray drying method is only suitable for producing micron-sized particles; the particles produced by the boiling granulation method are loose, with poor sphericity and surface finish; the particles produced by the stirring granulation method are uneven in size; It is difficult to control the internal porosity of particles produced by molding method

Method used

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  • Method for preparing big-diameter granules from micro and nano powder by means of interfacial polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of 1.90mm large particles by nano-silica:

[0029] 1. Disperse 15g of nano-silica and 25g of triethylenetetramine in 100mL of water, and stir for 10 minutes at a speed of 5000r / min with a high-shear dispersing emulsifier;

[0030] 2. Add 42g of glycerol glycidyl ether and 15g of acid absorbing agent sodium carbonate into 100mL water, fully dissolve;

[0031] 3. Configure 2000mL terephthaloyl chloride n-hexane supersaturated solution, the liquid level height is 500mm, and the temperature is kept at 50°C;

[0032] 4. After quickly mixing the solutions prepared in steps 1 and 2, add the terephthaloyl chloride n-hexane supersaturated solution prepared in step 3 dropwise through a sieve plate with an aperture of 0.84 mm, and granulate while the droplets fall to the bottom .

[0033] After separation, the average particle size of the prepared spherical particles is 1.90mm, and the porosity is 40%.

Embodiment 2

[0035] Preparation of 3.04 mm Large Particles of Halloysite Nanotubes

[0036] 1. Disperse 15g of halloysite nanotubes and 15g of polyethyleneimine in 100mL of water, and stir at a speed of 5000r / min for 10 min with a high-shear dispersing emulsifier;

[0037] 2. Add 20g of glycerol glycidyl ether and 15g of sodium carbonate into 100mL of water, fully dissolve;

[0038] 3. Configure 2000mL hexamethylene diisocyanate toluene supersaturated solution, the liquid level height is 500mm, and the temperature is kept at 80°C;

[0039] 4. After quickly mixing the solutions prepared in steps 1 and 2, add the hexamethylene diisocyanate toluene supersaturated solution prepared in step 3 dropwise through a sieve plate with an aperture of 1.36 mm, and granulate while the droplets fall to the bottom.

[0040] After separation, the average particle size of the prepared spherical particles is 3.04mm, and the porosity is 48%.

Embodiment 3

[0042] Preparation of 3.04 mm Large Particles of Modified Halloysite Nanotubes

[0043] 1. Take 20g of halloysite nanotubes calcined at 400°C for 5h, reflux in the toluene solution of silane coupling agent Z6020 for 48h, and vacuum-dry after centrifugation;

[0044] 2. Disperse 15 g of the modified halloysite nanotubes and 15 g of polyethyleneimine prepared in step 1 in 100 mL of water, and stir for 10 min at a speed of 5000 r / min with a high-shear dispersing emulsifier;

[0045] 3. Add 20g of glycerol glycidyl ether and 15g of sodium carbonate into 100mL of water, fully dissolve;

[0046] 4. Configure 2000mL hexamethylene diisocyanate toluene supersaturated solution, the liquid level height is 500mm, and the temperature is kept at 80°C;

[0047] 5. After quickly mixing the solutions prepared in steps 2 and 3, add the hexamethylene diisocyanate toluene supersaturated solution prepared in step 4 dropwise through a sieve plate with an aperture of 1.36 mm, and granulate while th...

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Abstract

The invention belongs to the technical field of preparation of big-diameter granules, and particularly relates to a method for preparing big-diameter granules from micro and nano powder by means of interfacial polymerization. The method comprises the following steps of: dispersing the micro and nano powder into aqueous solution of polyamine to obtain solution A, preparing aqueous solution B of water-soluble epoxy compound or polyaldehyde, mixing the solution A and B, and adding the mixed solution into solution C drop by drop through a sieve plate with aperture of 0.01 to 12 millimeters to obtain the big-diameter granules, wherein the solution C is supersaturated organic solution of oil-soluble compound containing multiple acyl chloride or isocyanate functional groups, and the diameter of the granules is 0.1 to 10 millimeters. The method is wide in micro and nano powder application range; the prepared granules have wide diameter range, high real spherical degree, uniform diameter distribution, adjustable internal porosity and high mechanical strength (crushing strength, 150N); and the method is quick in granulation, requires simple equipment, and is particularly suitable for small-size operation.

Description

technical field [0001] The invention belongs to the technical field of preparation of large-diameter particles, and in particular relates to a method for preparing large-diameter particles by interfacial polymerization of micro-nano powder. Background technique [0002] Micro-nano powders are widely used in materials, catalysis, medicine, environment and other fields. However, due to the small particle size of the powder, it is difficult to separate in the medium, and the flow resistance is large when the fixed-bed reactor is filled. Therefore, it is key to manufacture large-sized particles while retaining their large specific surface area. The current granulation methods mainly include spray drying method, hot melt molding method, pressure molding granulation method, stirring granulation method and boiling granulation method. However, the above methods have significant limitations. The spray drying method is only suitable for producing micron-sized particles; the particl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/16
Inventor 张延武姜俊青闫利伟郑延辉张亚涛
Owner ZHENGZHOU UNIV
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