Method for preparing high-efficiency ultraviolet-resistant titanium-dioxide nano granules

A titanium dioxide and nanoparticle technology is applied in the field of preparing high-efficiency anti-ultraviolet titanium dioxide nanoparticles, which can solve the problems of inability to improve sun protection factor and high sun protection factor, and achieve the effects of good anti-ultraviolet performance and simple preparation method.

Inactive Publication Date: 2012-08-22
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Titanium dioxide single active ingredient can be made into high sun protection factor products, while zinc oxide cannot improve sun protection factor

Method used

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  • Method for preparing high-efficiency ultraviolet-resistant titanium-dioxide nano granules
  • Method for preparing high-efficiency ultraviolet-resistant titanium-dioxide nano granules
  • Method for preparing high-efficiency ultraviolet-resistant titanium-dioxide nano granules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Amphiphilic triblock polymer PEO- b -PDMA- b -Synthesis of PS

[0035] Using 0.500g of brominated polyoxyethylene (PEO-Br) as a macroinitiator, 0.036g of catalyst cuprous bromide (CuBr), 0.044g of ligand PMDETA, and 1.580g of monomer dimethacrylate Add methylaminoethyl ester (DMA) and 4mL solvent into a 50mL round bottom flask for atom transfer radical polymerization (ATRP) at 30 o C. After 6 hours of reaction, 3.800g of styrene was diluted and added to the reaction flask to continue the reaction for 24 hours. The obtained polymer was rotary evaporated, passed through a silica gel column, concentrated, precipitated, pumped, and finally placed in a vacuum oven for 24 hours to obtain the block polymer PEO 43 - b -PDMA 40 - b -PS 140 .

[0036] 2) Polymers self-assemble to form micelles

[0037] The polymer was dissolved in tetrahydrofuran (THF), and a 20mg / mL solution was prepared, and methanol 60 times the volume of THF was added dropwise to the THF solution ...

Embodiment 2

[0044] 1) Amphiphilic triblock polymer PEO- b -PDMA- b -Synthesis of PS

[0045] 0.500g of macroinitiator PEO 43 -Br, 0.036g of catalyst cuprous bromide (CuBr), 0.044g of ligand PMDETA, 1.180g of monomer dimethylaminoethyl methacrylate (DMA) and 3mL of methanol solvent were added to a 50mL round bottom flask In, conduct atom transfer radical polymerization (ATRP), temperature 30 o C. After 6 hours of reaction, 2.800 g of styrene was dissolved in 3 mL of p-xylene, and the reaction was continued for 24 hours. The obtained polymer was rotary evaporated, passed through a silica gel column, concentrated, precipitated, pumped, and finally placed in a vacuum oven for 24 hours to obtain the block polymer PEO 43 - b -PDMA 30 - b -PS 100 .

[0046] 2) Polymers self-assemble to form micelles

[0047] Dissolve the polymer in dichloromethane, prepare a 30mg / mL solution, add dropwise ethanol 80 times the volume of dichloromethane to the above solution at a rate of 10d / min under st...

Embodiment 3

[0052] 1) Amphiphilic triblock polymer PEO- b -PDMA- b -Synthesis of PS

[0053] With 1.000g of brominated polyoxyethylene (PEO-Br) as macromolecular initiator, 0.072g of catalytic

[0054] The agent cuprous bromide (CuBr), 0.088g of the ligand PMDETA, 3.160g of the monomer dimethylaminoethyl methacrylate (DMA) and 5mL of methanol solvent were added to a 50mL round bottom flask for free atom transfer radical polymerization (ATRP), temperature 30 o C. After 6 hours of reaction, dissolve 3.300g of styrene in 6mL of p-xylene, add it into the reaction flask and continue to react for 24 hours. After post-treatment, the block polymer PEO is obtained 43 - b -PDMA 40 - b -PS 120 .

[0055] 2) Polymers self-assemble to form micelles

[0056] Dissolve the polymer in dichloromethane, prepare a 20 mg / mL solution, add ethanol 80 times the volume of dichloromethane dropwise to the THF solution at a rate of 10 d / min under stirring, and obtain a milky white solution after stirring f...

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Abstract

The invention belongs to the technical field of materials and particularly relates to a method for preparing titanium-dioxide nano granules with the performance of high-efficiency ultraviolet resistance. An amphiphilic three-block polymer PEO-b-PDMA-b-PS is synthesized by an atom transfer radical polymerization (ATRP) reaction, and polymeric micelles with uniform particle-size distribution are also formed by macromolecular self-assembly. Then, the sol-gel reaction of deposited titanate occurs on the micelles in situ, organic / inorganic hybrid titanium-dioxide nano granules are obtained after drying, and then inorganic titanium-dioxide nano granules can also be obtained after further calcining. According to the method for preparing the titanium-dioxide nano granules with the performance of the high-efficiency ultraviolet resistance, the titanium-dioxide nano granules with the performance of the high-efficiency ultraviolet resistance can be prepared; and moreover, the magnitude of the particle size of the nano granules can be controlled by controlling the pH value of an environment and the polymerization degree of each chain segment of the polymer. The method has a simple preparing process and low cost and is convenient to operate, and the prepared product is safe and nontoxic, has favorable dispersing performance in water and can be applied to the fields of sun-screen cosmetics, catalytic degradation and the like.

Description

technical field [0001] The invention relates to a method for preparing high-efficiency anti-ultraviolet titanium dioxide nanoparticles. Background technique [0002] With the increase of toxic gases discharged in modern industry, the ozone layer in the atmosphere is constantly being destroyed, so that more and more ultraviolet rays are irradiated to the surface of human skin. The photochemical reaction caused by excessive ultraviolet radiation causes a series of changes in human body functions, and may cause damage to the skin, eyes and immune system in particular. In order to reduce the damage of ultraviolet rays in the sun to the human body, sunscreen has become a very useful product. It contains active ingredients that absorb or block UV radiation, protecting the skin from sun damage. Current sunscreens include organic and inorganic sunscreens. Organic ingredients are often difficult to degrade and may cause damage to human skin, while inorganic sunscreens are more hydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K8/90A61K8/29A61Q17/04
Inventor 杜建忠肖杰
Owner TONGJI UNIV
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