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Magnetic hollow silica microspheres and its preparation process

A technology of hollow silica and silica, which is applied in the preparation of microspheres, microcapsule preparations, alkali metal oxides/hydroxides, etc., can solve the problem of difficult control of template particle size uniformity, and achieve magnetic nanoparticles The effect of controllable quantity, high product purity and simple operation

Active Publication Date: 2017-08-25
是大高分子材料山西有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the above artificial templates need to go through a series of surface modification and activation steps during the synthesis process, and the particle size uniformity of the synthesized templates is not easy to control, so the development of a new monodisperse, particle size controllable, core-encapsulated Fe 3 o 4 Magnetic hollow silica microspheres with controllable amount of nanoparticles need further research

Method used

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  • Magnetic hollow silica microspheres and its preparation process
  • Magnetic hollow silica microspheres and its preparation process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Dehydration of freshly collected cyanobacteria with different concentrations of ethanol

[0026] 2) Preparation of magnetic hollow silica microspheres using treated cyanobacteria as templates

[0027] Add 0.046mol Fe 3+ and 0.023mol Fe 2+ , to obtain solution I; mix absolute ethanol, double distilled water, and ammonia water in a volume ratio of 3:3:1 to obtain solution II. The preparation process is carried out in three steps:

[0028] Step 1: Add the treated cyanobacteria into solution I, stir at a low speed, and infiltrate at 20°C for 24 hours. After infiltration, wash the cyanobacteria three times with double distilled water to remove the solvent on the surface of the cyanobacteria;

[0029] The second step: Put the cyanobacteria treated in the first step into 23mL solution II, stir at a low speed, infiltrate at 20°C for 30h, wash with double distilled water three times, and centrifuge to obtain the magnetic Fe 3 o 4 particles of cyanobacteria;

[0030] Th...

Embodiment 2

[0033] The difference between this embodiment and the specific example 1 is: the process of preparing magnetic hollow silica microspheres using the treated cyanobacteria as a template, and other steps are the same as in the first example;

[0034] Add 0.046mol Fe 3+ and 0.023mol Fe 2+ , to obtain solution I; mix absolute ethanol, double distilled water, and ammonia water in a volume ratio of 3:3:1 to obtain solution II. The preparation process is carried out in three steps:

[0035] Step 1: Add the treated cyanobacteria into solution I, stir at low speed, and infiltrate at 30°C for 30 hours. After infiltration, wash the cyanobacteria three times with double distilled water to remove the solvent on the surface of the cyanobacteria;

[0036] The second step: Put the cyanobacteria treated in the first step into 23mL solution II, stir at a low speed, infiltrate at 25°C for 40h, and obtain the magnetic Fe contained inside. 3 o 4 particles of cyanobacteria;

[0037] The third ...

Embodiment 3

[0040] The difference between this embodiment and the specific example 1 is: the process of preparing magnetic hollow silica composite microspheres using the treated cyanobacteria as a template, and other steps are the same as in the first example;

[0041] Add 0.046mol Fe to 100mL of double distilled water that has passed nitrogen 3+and 0.023mol Fe 2+ , to obtain solution I; mix absolute ethanol, double distilled water, and ammonia water in a volume ratio of 5:5:2 to obtain solution II. The preparation process is carried out in three steps:

[0042] Step 1: Add the treated cyanobacteria into solution I, stir at a low speed, and infiltrate at 40°C for 48 hours. After infiltration, wash the cyanobacteria three times with double distilled water to remove the solvent on the surface of the cyanobacteria;

[0043] The second step: Put the cyanobacteria treated in the first step into 24mL solution II, stir at a low speed, infiltrate at 25°C for 48h, and obtain the magnetic Fe con...

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Abstract

The invention relates to a method for preparing magnetic hollow silicon dioxide microspheres by using cyanobacteria as a template. The process is to infiltrate the treated cyanobacteria in stages, coat the surface with silicon dioxide, and then undergo high-temperature treatment to obtain the target product. In the first step, the treated cyanobacteria are added to the mixed solution of Fe2+ or Co2+ or Mn2+ and Fe3+ or Co3+ salt for infiltration, and then washed with double distilled water three times; in the second step, the infiltrated cyanobacteria after centrifugation are added to the alkaline alcohol aqueous solution for infiltration , to obtain cyanobacteria containing magnetic particles inside, wash three times with double distilled water, and centrifuge; the infiltrated cyanobacteria after centrifugation in the third step are coated with silica, and centrifuged; the centrifuged products are dried and calcined at high temperature to remove the cyanobacteria template , to obtain magnetic hollow silica microspheres. The invention has the advantages of simple operation, easy process control, environmental protection and low cost; the obtained product has high purity, uniform particle size, fast magnetic response speed, regular shape, no hard agglomeration, and is suitable for large-scale production. It has a wide range of applications in enzymes, protein separation, etc.

Description

technical field [0001] The invention belongs to the technical field of magnetic materials, in particular to a preparation method of magnetic hollow silicon dioxide composite microspheres. Background technique [0002] Cyanobacteria mainly grow in fresh water and are important phytoplankton in fresh water. They often multiply in large numbers in warm seasons to form "algae blooms", causing serious environmental pollution. Therefore, the comprehensive utilization of cyanobacteria has achieved major economic and social benefits. [0003] Magnetic hollow silica particles are a kind of adsorbent and adsorbent carrier with excellent properties. They have the characteristics of light weight, high specific surface area and strong adsorption force. Hydrogen and other high-tech fields. The template method is commonly used to prepare magnetic hollow microspheres. F. Caruso et al. using polymer electrolytes, Fe 3 o 4 and silica self-assembled layer by layer on the polystyrene micros...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02B01J20/10B01J20/30C02F1/28B01J20/28
Inventor 任天瑞张博张雷于广金杨姗庞文文关策王全喜
Owner 是大高分子材料山西有限公司
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