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Method for preparing layer dihydroxy composite metal oxide flower-like microsphere through hydrothermal synthesis

A layered double hydroxyl and composite metal technology, applied in the direction of oxide/hydroxide preparation, microsphere preparation, chemical instruments and methods, etc., can solve the problems of a large number of organic solvents, large energy consumption, and low stripping efficiency, and achieve The method is simple and easy, the preparation method is simple, and the effect of uniform particle size

Inactive Publication Date: 2009-09-30
BEIJING UNIV OF CHEM TECH
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  • Abstract
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Problems solved by technology

However, the specific surface area of ​​the LDHs shell prepared by the above method is small, the binding force with the PSS or PS core, or the organic solvent stripping method requires a large amount of organic solvent, and the stripping efficiency is extremely low; or the energy consumption is relatively large; these The limitations will greatly limit the energy-saving industrial production and further application of LDHs microspheres

Method used

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  • Method for preparing layer dihydroxy composite metal oxide flower-like microsphere through hydrothermal synthesis
  • Method for preparing layer dihydroxy composite metal oxide flower-like microsphere through hydrothermal synthesis
  • Method for preparing layer dihydroxy composite metal oxide flower-like microsphere through hydrothermal synthesis

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Experimental program
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Effect test

Embodiment 1

[0026] A: Weigh 1.19g Zn(NO 3 ) 2 ·6H 2 O and 0.75g Al(NO 3 ) 3 9H 2 O was dissolved in deionized water to make 100mL mixed salt solution, put the solution into a four-necked flask, blow nitrogen and stir to dissolve the salt; then weigh 0.424g Na 2 CO 3 Dissolve 0.384g NaOH in deionized water to make 100mL mixed alkali solution; weigh 3.0g sulfonated polystyrene and dissolve in deionized water to make 50mL suspension;

[0027] B: Pour the sulfonated polystyrene suspension prepared in step A into the salt solution, and stir for 4 hours to make it evenly mixed;

[0028] C: Quickly titrate the alkali solution prepared in step A to the mixed solution in step B, centrifuge and wash the resulting solution, remove the supernatant, and redisperse the obtained slurry in the N 2 in deionized water and made into solution. Put the obtained solution into a high-temperature and high-pressure reactor for hydrothermal crystallization at 80°C for 18 hours;

[0029] D: Put the colloid...

Embodiment 2

[0031] A: Weigh 1.19g Zn(NO 3 ) 2 ·6H 2 O and 0.75g Al(NO 3 ) 3 9H 2 O was dissolved in deionized water to make 100mL mixed salt solution, put the solution into a four-necked flask, blow nitrogen and stir to dissolve the salt; then weigh 0.424g Na 2 CO 3 Dissolve 0.384g NaOH in deionized water to make 100mL mixed alkali solution; weigh 3.0g sulfonated polystyrene and dissolve in deionized water to make 50mL suspension;

[0032] B: Pour the sulfonated polystyrene suspension prepared in step A into the salt solution, and stir for 4 hours to make it evenly mixed;

[0033] C: Quickly titrate the alkali solution prepared in step A to the mixed solution in step B, centrifuge and wash the resulting solution, remove the supernatant, and redisperse the obtained slurry in the N 2 in deionized water and made into solution. Put the obtained solution into a high-temperature and high-pressure reactor for hydrothermal crystallization at 60°C for 18 hours;

[0034] D: Put the colloid...

Embodiment 3

[0036] A: Weigh 11.9g Zn(NO 3 ) 2 ·6H 2 O and 7.5gAl(NO 3 ) 3 9H 2 O was dissolved in deionized water to make 100mL mixed salt solution, put the solution into a four-necked flask, blow nitrogen and stir to dissolve the salt; then weigh 4.24gNa 2 CO 3 Dissolve 3.84g NaOH in deionized water to make 100mL mixed alkali solution; weigh 4.0g sulfonated polystyrene and dissolve in deionized water to make 50mL suspension;

[0037] B: Pour the sulfonated polystyrene suspension prepared in step A into the salt solution, and stir for 4 hours to make it evenly mixed;

[0038] C: Quickly titrate the alkali solution prepared in step A to the mixed solution in step B, centrifuge and wash the resulting solution, remove the supernatant, and redisperse the obtained slurry in the N 2 in deionized water and made into solution. Put the obtained solution into a high-temperature and high-pressure reactor for hydrothermal crystallization at 80°C for 18 hours;

[0039] D: Put the colloidal sl...

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Abstract

The invention relates to a method for preparing a layer dihydroxy composite metal oxide flower-like microsphere through hydrothermal synthesis, which belongs to the technical field of anion type layer structure functional materials. The microsphere has the following general formula: [M<2+>1-xM<3+>x(OH)2]<x+>.(A<n->x / n.mH2O. The method comprises the following steps: firstly, adsorbing metal salt ions with heterogeneous charges on the surface of a sulfonated polystyrene microsphere; and secondly, growing hydrotalcite on the surface of the sulfonated polystyrene microsphere by a method of high-temperature and high-pressure hydrothermal synthesis. The method has the advantages that the hydrotalcite with uniform grain size and uniform phase composition can be obtained; and simultaneously, the method has low cost, is simple and convenient to implement and has industrial production prospect. The sulfonated polystyrene / hydrotalcite nucleocapsid structural microsphere has good hydrophilicity and has application prospect of adsorbing and separating macromolecular proteins in water.

Description

technical field [0001] The invention belongs to the technical field of anionic layered structure functional materials, in particular to a hydrothermal preparation method of layered dihydroxy composite metal oxide flower-like microspheres, which grow double hydroxyl composite metal oxides on the surface of sulfonated polystyrene Flower-like shell. Background technique [0002] Layered double hydroxyl compound metal oxides (also known as hydrotalcite-like, LDHs for short) are a kind of anionic layered structure functional materials, which are composed of parallel and positively charged laminates, and the layers are composed of balanced anions and water molecules. . Its chemical composition general formula is: [M 2+ 1-x m 3+ x (OH) 2 ] x+ (A n- x / n )·mH 2 O, where M 2+ , M 3+ are the divalent and trivalent metal ions on the laminate, A n- Represents interlayer anions. Due to its unique crystal structure and physical and chemical properties, this kind of material s...

Claims

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Application Information

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IPC IPC(8): C01B13/00C01B13/14B01J13/02
Inventor 徐赛龙徐婷杨迎生张法智段雪
Owner BEIJING UNIV OF CHEM TECH
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