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Minute particle with needlelike surface and its manufacturing method

A manufacturing method and particle technology, which is applied in thin material processing, transportation and packaging, etc., can solve problems such as complex processes, and achieve the effect of expanding the surface area

Inactive Publication Date: 2008-06-18
KAWAMURA INST OF CHEM RES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In addition, in the production method, the complex is obtained through the process of introducing amino groups, imino groups, etc. into the silica skeleton through chemical bonds and coordinating them with metal ions, and the process is complicated.

Method used

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  • Minute particle with needlelike surface and its manufacturing method
  • Minute particle with needlelike surface and its manufacturing method
  • Minute particle with needlelike surface and its manufacturing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0124] Hereinafter, although an Example and a reference example demonstrate this invention more concretely, this invention is not limited to these. Unless otherwise specified, "%" means "mass %".

[0125] [Shape Analysis Using Scanning Electron Microscope]

[0126] The separated and dried sample was placed on a glass slide, and observed using a surface observation device VE-7800 produced by KEYENCE CORPORATION.

[0127] [Determination of metal content in silica by ICP]

[0128] Accurately weigh the separated and dried sample, and decompose it with a microwave sample decomposition device. Add ultra-pure water to the decomposition liquid, measure the amount of metal in the liquid with Optima 3300DV produced by Perkin Elmer, and calculate the metal content.

Synthetic example 1

[0130]

[0131] 3 g of commercially available linear polyethyloxazoline (number-average molecular weight 50,000, average degree of polymerization 5,000, manufactured by Aldrich) was dissolved in 15 mL of 5M aqueous hydrochloric acid. The solution was heated to 90° C. using an oil bath, and stirred at this temperature for 10 hours. Add 50ml of acetone to the reaction solution to completely precipitate the polymer, filter the precipitate, and wash with methanol three times to obtain white polyethyleneimine powder. use 1 H-NMR (heavy water) identifies the gained powder, confirms that the peak 1.2ppm (CH 3 ) and 2.3ppm (CH 2 )Completely disappear. That is, it was shown that polyethyloxazoline was completely hydrolyzed and converted into polyethyleneimine.

[0132] This powder was dissolved in 5 mL of distilled water, and 50 mL of 15% ammonia water was added dropwise to the solution while stirring. After the mixed solution was allowed to stand overnight, the precipitated pol...

Embodiment 1～5

[0134]

[0135] A certain amount of L-PEI powder obtained above was weighed and dispersed in distilled water to prepare a 1% L-PEI dispersion. The dispersion liquid was heated to 90° C. using an oil bath to obtain a completely transparent L-PEI aqueous solution. In the obtained L-PEI aqueous solution, add the metal ion species shown in Table 1 (embodiment 1: Cu(II) Nitrate; Example 2: Mn(II) nitrate; Example 3: Al(III) nitrate; Example 4: Eu(III) hydrochloride; Example 5: Zr(IV) nitrate) salt compound, and then, the solution was left at room temperature for 24 hours to obtain a L-PEI metal complex solution.

[0136] Add 1 mL of tetramethoxysilane (TMOS) and ethanol mixed solution (volume ratio 1 / 1) in the obtained PEI metal complex solution (1 mL), react at room temperature for 1 hour (TMOS is relative to the The usage ratio of ethylimine unit is 40 times equivalent). The generated solids were separated with a centrifugal separator, and the ethanol centrifugal separation pr...

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Abstract

The present invention provides organic-inorganic composite particles containing metal complexes, which have multiple needle-like structures on the surface and contain metal complexes; and a simple manufacturing method of the particles. This can be achieved by inducing a metal complex composed of a polymer having a linear polyethyleneimine skeleton and a metal ion to induce composite particles with a fine needle-like surface containing the metal complex inside the silica. Needle-shaped surface particles with multiple nanoscale needle-like structures on the surface of the particles. The needle-like structure of the resulting needle-shaped surface particles and the spatial structure of the particles can be controlled by changing the metal ion species and the metal complex support medium.

Description

technical field [0001] The present invention relates to acicular surface fine particles containing a metal complex composed of a polymer having a linear polyethyleneimine chain and a metal ion, and a method for producing the acicular surface fine particles. Silica particles, and its surface has a fine needle-like structure. Background technique [0002] The composite material with metal complexes immobilized on silica can be effectively used in chemical reaction catalysts, electrochemical sensors, solid polymer electrolytes and other applications. In particular, a complex in which a metal complex is introduced into mesoporous silica is expected to have many advantages such as the large surface area of ​​the silica surface, and the presence of complexing active sites in the nanovoids inside the silica. Large-scale distribution, rapid diffusion of substrates, high heat resistance of catalyst supports, high acid resistance, etc., therefore, the metal complex immobilization tec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/14C08K3/36C08L79/02
CPCC08J2379/02C08J3/212C08K3/36C08K5/0091C08L79/02Y10T428/2995C08J3/14
Inventor 金仁华诸培新
Owner KAWAMURA INST OF CHEM RES
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