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Homogeneous crosslinking beta-cyclodextrin/wolfram carbine composite microsphere and method of producing the same

A composite microsphere and cyclodextrin technology, which is applied in the direction of microsphere preparation, chemical instruments and methods, microcapsule preparation, etc., can solve the problems that cannot meet the expansion requirements and have not yet been applied, and achieve low cost, good chemical stability, The effect of simple preparation process

Inactive Publication Date: 2009-04-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the density of these cyclodextrin polymer microspheres is close to that of water, which cannot meet the expansion requirements at high flow rates, so they have not been used in the expanded bed operation mode.

Method used

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  • Homogeneous crosslinking beta-cyclodextrin/wolfram carbine composite microsphere and method of producing the same
  • Homogeneous crosslinking beta-cyclodextrin/wolfram carbine composite microsphere and method of producing the same
  • Homogeneous crosslinking beta-cyclodextrin/wolfram carbine composite microsphere and method of producing the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At 60°C, mix 8g of β-cyclodextrin and 40g of 20% sodium hydroxide aqueous solution to prepare a solution. Under mechanical stirring, add 8g of epichlorohydrin dropwise to the solution for 30 minutes, and then continue stirring for 30 minutes to obtain viscous Glue: add 14g of tungsten carbide powder to the viscose, mix and stir evenly, at 50°C, under the condition of mechanical stirring speed of 300rpm, add 42g of high-speed vacuum pump oil and 126g of liquid paraffin oil dispersion phase, and add 0.84g of polyoxyethylene sorbitan monooleate was used as a dispersant, after stirring for 15min, 2.5g of epichlorohydrin was added, and stirred for 120min at 50°C with a mechanical stirring speed of 300rpm to obtain a black homogeneous Quality-type composite microspheres; cooled to 20°C, then mixed evenly with 0.5 times the volume of n-hexane, filtered under reduced pressure, filtered out the composite microspheres from the oil dispersed phase, and then divided into 2 parts wit...

Embodiment 2

[0031]At 90°C, mix 24g of β-cyclodextrin and 40g of 40% aqueous sodium hydroxide solution to prepare a solution. Under mechanical stirring, add 16g of epichlorohydrin dropwise to the solution for 45min, and then continue stirring for 120min to obtain viscous Glue: Add 120g of tungsten carbide powder to the viscose and mix it evenly. At 70°C and the mechanical stirring speed is 450rpm, add 266g of high-speed vacuum pump oil and 133g of liquid paraffin. 6.0g polyoxyethylene sorbitan monooleate as a dispersant, after stirring for 30min, add 30g of epichlorohydrin, and stir for 180min at 70°C with a mechanical stirring speed of 450rpm to obtain a black homogeneous type composite microspheres; cooled to 30°C, then mixed evenly with 1 times the volume of n-hexane, filtered under reduced pressure, filtered out the composite microspheres from the oil dispersed phase, and then divided into 3 times with 4 times the volume of n-hexane After washing, the composite microspheres were added ...

Embodiment 3

[0033] At 80°C, mix 20g of β-cyclodextrin and 40g of 25% aqueous sodium hydroxide solution to prepare a solution. Under mechanical stirring, add 10g of epichlorohydrin dropwise to the solution for 30min, and then continue stirring for 60min to obtain viscous Glue: add 30g of tungsten carbide powder to the viscose, mix and stir evenly, at 60°C, under the condition of mechanical stirring speed of 400rpm, add 90g of high-speed vacuum pump oil and 200g of liquid paraffin oil dispersion phase, and add 2.5g of polyoxyethylene sorbitan monooleate as a dispersant, after stirring for 30min, add 10g of epichlorohydrin, and stir for 150min at 60°C with a mechanical stirring speed of 400rpm to obtain a black homogeneous Type composite microspheres; suction filtration, washing, neutralization, sieving and flotation according to the method in Example 2, to obtain 72 mL of composite microspheres with a particle size of 75-180 μm and a density of 1.4 g cm -3 .

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Abstract

The invention discloses an isotropic crosslinking beta-cyclodextrin / tungsten carbide composite microsphere and a preparation method thereof. The preparation method comprises the following steps: firstly, beta-cyclodextrin is dissolved into a sodium hydroxide aqueous solution, and the mixture is dripped with epichlorohydrin and undergoes stirring reaction under heating condition, so as to generate viscose; secondly, the viscose is added with tungsten carbide powder, oil dispersed phase and a dispersant under the condition of mechanical stirring to form a reversed phase suspension dispersion system; thirdly, the epichlorohydrin is added into the reversed phase suspension dispersion system, and the composite microsphere is obtained after mechanical stirring reaction; and fourthly, after the reversed phase suspension dispersion system is cooled, the composite microsphere is filtered, cleaned and neutralized, and subjected to wet sieving and expanded bed floatation. The composite microsphere developed by the method has the advantages of good hydrophilicity and sphericity, stable properties, low cost, high density, easy adjustment and so on, and can be used as a substrate during the process of expanded bed absorption as shown by an expanding performance test experiment.

Description

technical field [0001] The invention relates to the synthesis of functional materials, in particular to a homogeneous crosslinked β-cyclodextrin / tungsten carbide composite microsphere and a preparation method thereof. Background technique [0002] Expanded bed adsorption (EBA) technology is a new type of biochemical separation technology, which integrates solid-liquid separation, concentration and initial purification, and can directly capture the target product from the feed liquid containing solid particles. Expanded bed is a special case of fluidized bed, which uses the physical properties of the adsorbent itself, combined with a special fluid distribution device, to obtain a stable fluidized bed with a small degree of back mixing, thus overcoming the inability of traditional fixed beds to deal with At the same time, because the adsorbent particles are stably graded in the expanded bed, the feed liquid passes through the bed in a form close to the plug flow, and the degre...

Claims

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Application Information

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IPC IPC(8): B01J13/02C08B37/16B01J20/26B01J20/28
Inventor 姚善泾赵珺林东强
Owner ZHEJIANG UNIV
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