A preparation method of carboxymethyl-β-cyclodextrin functionalized magnetic mesoporous silicon microspheres

A cyclodextrin and carboxymethyl technology, which is applied in the field of new material manufacturing for water treatment, can solve the problems of reduced adsorption performance, reduced specific surface area, and no protection, and achieves good adsorption performance, wide application prospects, and increased specific surface area. Effect

Active Publication Date: 2019-11-26
WUHAN UNIV OF TECH
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Problems solved by technology

Patent No. CN201310222225.7 (authorized public number is CN103310935 A) Chinese invention patent "Silicon dioxide nano-magnetic microspheres and its preparation method" discloses a preparation method of double-layer silica-coated magnetic nanoparticles. Nano-magnetic microspheres with a double-layer silica structure can increase the specific surface area through the outer porous silica layer to improve the adsorption efficiency of heavy metals, but only rely on the effect of the silica layer to remove heavy metal ions Poor, need to find ways to further improve its adsorption efficiency
In the Chinese invention patent "Preparation of β-cyclodextrin-modified magnetic nanoparticles" with patent number 201410714076.0 (authorized public number is CN104353431A), a preparation method of β-cyclodextrin-modified magnetic nanoparticles is provided , the prepared magnetic nanoparticles modified by β-cyclodextrin have a good ability to recognize guest molecules, but due to the dense SiO on the surface of the magnetic core 2 The presence of the layer reduces its specific surface area, resulting in a decrease in adsorption performance
In the Chinese invention patent "Preparation method of cyclodextrin-modified magnetic nano-adsorbent and its application in hemodialysis adsorption system" with the patent number CN201410208552.1, a cyclodextrin-modified magnetic nano-adsorbent Fe 3 o 4 -The preparation method of β-CD, and in this method Fe 3 o 4 Without protection, it is easy to be oxidized, and the preparation cycle is long, which limits its application. Therefore, it is necessary to improve the preparation method of this type of magnetic particles and expand its application range

Method used

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  • A preparation method of carboxymethyl-β-cyclodextrin functionalized magnetic mesoporous silicon microspheres
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  • A preparation method of carboxymethyl-β-cyclodextrin functionalized magnetic mesoporous silicon microspheres

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Embodiment 1

[0044] Example 1, see Figure 1-4 :

[0045] The invention provides a method for preparing carboxymethyl-β-cyclodextrin functionalized magnetic mesoporous silicon microspheres, comprising the following steps (see figure 1 ):

[0046] 1) Co-precipitation method to prepare Fe 3 o 4 :

[0047] Measure 500mL of 1.5mol / L NaOH solution into a three-necked flask, pass high-purity nitrogen gas (30mL / min), and heat in a water bath to 80°C; weigh 0.04mol FeCl in a molar ratio of 2:1 3 ·6H 2 O and 0.02mol FeCl 2 Dissolve 4H2O in 50ml of 0.5mol / L HCl, then slowly add it into NaOH solution, adjust the pH to 9.0, and react to form black particles, stop stirring after 0.5h of reaction, cool naturally, separate the solid product, and use it alternately Wash the solid product with ionized water and ethanol for 3 to 5 times, dry in a vacuum oven, and grind to obtain black crystal Fe 3 o 4 Granules, sealed bag preservation;

[0048] 2) Preparation of magnetic silicon:

[0049] Weigh 0...

Embodiment 2

[0064] This example is the same as the basic example 1, except that the amount of TEOS in step 2) is increased to 1 mL. Through characterization, it is found that the Fe obtained from this implementation case 3 o 4 @SiO 2 @SiO 2 - The thickness of the silica coating layer in the CM-β-CD particles was increased to 50 nm.

Embodiment 3

[0066] This embodiment is according to the basic embodiment 1, the difference is that the amount of TEOS in step 2) is reduced to 0.2 mL. Through characterization, it is found that the Fe obtained from this implementation case 3 o 4 @SiO 2 @SiO 2 - The thickness of the silica coating layer in the CM-β-CD particles was reduced to 10 nm.

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Abstract

The invention provides a preparation method of carboxymethyl-beta-cyclodextrin functionalized magnetic mesoporous silicon microspheres. The method includes the steps of: 1) preparing Fe3O4 via a coprecipitation method; 2) preparing SiO2-coated Fe3O4 particles (Fe3O4@SiO2), namely, magnetic silicon; 3) preparing mesoporous SiO2-coated Fe3O4@SiO2 particles (Fe3O4@SiO2@SiO2), namely, magnetic mesoporous silicon; 4) preparing carboxymethyl-beta-cyclodextrin (CM-beta-CD) via a wet process or a dry process; 5) preparing carboxymethyl-beta-cyclodextrin functionalized magnetic mesoporous silicon microspheres (Fe3O4@SiO2@SiO2-CM-beta-CD). In the invention, with Fe3O4 as an object, the functionalized magnetic mesoporous silicon microspheres are prepared through the coprecipitation method and Stobermethod, so that the method has simple processes and high-effective treatment, is low in cost, and supplies a new idea to preparation and application of magnetic adsorption microspheres. The product can improve effect of removing heavy metals in water by Fe3O4.

Description

technical field [0001] The invention relates to the technical field of manufacturing new materials for water treatment, in particular to a preparation method of carboxymethyl-β-cyclodextrin functionalized magnetic mesoporous silicon microspheres. Background technique [0002] Fe 3 o 4 Magnetic nanoparticles have the excellent properties of nanomaterials (such as small particle size, large surface area, etc.), and also have their own characteristics. When the particle size is less than 20nm, they exhibit superparamagnetism at room temperature; Modification, can have specific affinity adsorption with the target, and can quickly separate the target from the multi-component environment under the directional control of the external magnetic field; it has the advantages of simple preparation process, low price, low toxicity, structure and function The advantages of strong predictability and controllability make it have high application value in adsorption separation, catalysis a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30B01J13/02
CPCB01J13/02B01J20/103B01J20/22B01J20/28009B01J20/28019
Inventor 李柏林杨琴邹楠李晔高雪洁卢忆灵
Owner WUHAN UNIV OF TECH
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