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

A technology of composite microspheres and cyclodextrins, which is applied in the preparation of microspheres, chemical instruments and methods, microcapsule preparations, etc. Simple preparation process

Inactive Publication Date: 2010-07-14
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% aqueous sodium hydroxide solution to prepare a solution, add 8g of epichlorohydrin dropwise to the solution for 30min under mechanical stirring, and then continue stirring for 30min to obtain Viscose liquid; add 14g tungsten carbide powder to this viscose liquid and mix and stir evenly. Under the condition of 50°C and mechanical stirring speed of 300rpm, add 42g high-speed vacuum pump oil and 126g liquid paraffin oil dispersion phase, and Add 0.84g of polyoxyethylene sorbitan monooleate as a dispersant, stir for 15min, then add 2.5g of epichlorohydrin, and stir for 120min at 50°C with a mechanical stirring speed of 300rpm to obtain a black Homogeneous 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 separated with 2 times the volume of n-hexane After washing twice,...

Embodiment 2

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

Embodiment 3

[0033] At 80°C, mix 20g of β-cyclodextrin and 40g of 25% aqueous sodium hydroxide solution to prepare a solution, add 10g of epichlorohydrin dropwise to the solution under mechanical stirring for 30min, and then continue stirring for 60min to obtain Viscose liquid; add 30g of tungsten carbide powder to the viscose liquid and mix and stir evenly. Under the condition of 60°C and 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, stir for 30min, then add 10g of epichlorohydrin, and stir for 150min at 60°C with a mechanical stirring speed of 400rpm to obtain a black homogeneous Qualitative 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 between 75 and 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 generateviscose; 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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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02C08B37/16B01J20/26B01J20/28
Inventor 姚善泾赵珺林东强
Owner ZHEJIANG UNIV
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