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Preparation method of metal oxide/hollow microsphere composite filler

A technology of hollow microspheres and composite fillers, applied in chemical instruments and methods, fibrous fillers, reflection/signal coatings, etc., can solve the problems of high cost, low efficiency of reflection and heat insulation, and weak joint effect of titanium dioxide and hollow microspheres, etc. problems, to achieve the effect of easy peptization, uniform and compact coating

Active Publication Date: 2020-11-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the dispersibility of metal raw materials in water seriously affects the coating and film formation of titanium dioxide in this method. If the dispersibility is not good, a uniformly coated titanium dioxide / hollow microsphere composite cannot be formed, which will affect the reflection and heat insulation performance of the filler.
In the disclosed method of CN201210477077.9, the electroless plating method is used to plate a layer of nano-silver film on the surface of the hollow microspheres, and then a layer of titanium dioxide film is added by the hydrothermal method, but this method uses precious metals, and the cost is relatively high
[0004] In addition, many patents disclose that coatings with reflective heat insulation function mostly use hollow microspheres and titanium dioxide as coating components, and form coating products with reflective heat insulation function through mechanical mixing. For example, CN201710899781.6 discloses an acrylate emulsion as The substrate contains titanium dioxide, hollow microspheres, and a fluorine-containing silicon coating, but the titanium dioxide and hollow microspheres are mechanically mixed, the combined effect of titanium dioxide and hollow microspheres is not strong, and the reflection and heat insulation efficiency is low

Method used

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  • Preparation method of metal oxide/hollow microsphere composite filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1000g of tetrabutyl titanate and 1000g of 1-butyl-3-methylimidazole hydroxide were respectively placed in a container, and stirred evenly at room temperature to obtain a titanium dioxide precursor. Take 25g of titanium dioxide precursor and place it in a reaction tank, put 25g of glass hollow microspheres into it, stir evenly, then add 18g of isopropanol, continue to stir evenly, then add 14.4g of tetraethoxysilane, continue to stir evenly, then add A small amount of 2% sodium hydroxide solution was used to adjust the pH of the slurry to 8.5. Put it in a closed autoclave, react at 120°C for 24 hours, take it out and filter until the water content of the filter cake is 39%, add 62.5g of titanium dioxide precursor and stir evenly, then slowly add 180g of 60% ethanol aqueous solution and 3.4 g methyl acrylate, adjust the pH value to 8.5 with ethylenediamine, seal and continue to stir at 200°C and 2MPa at a low speed for 4h, dry at 100°C for 3h, and bake at 500°C for 4h to ...

Embodiment 2

[0038] 1000g of zinc nitrate and 1000g of 1-butyl-3-methylimidazolium acetate were respectively placed in containers, and stirred evenly at room temperature to obtain a zinc oxide precursor. Put 10g of ceramic microbeads into 50g of zinc oxide precursor, stir evenly, then add 22g of ethylene glycol, continue to stir evenly, then add 11g of dimethylvinylethoxysilane, continue to stir evenly, then add 10% The pH of the slurry was adjusted to 9.0 with sodium bicarbonate. Put it in a closed autoclave, react at 100°C and 1MPa for 20 hours, take it out and filter until the water content of the filter cake is 52%, add 250g of zinc oxide precursor and stir evenly, then slowly add 542.5g of 80% ethanol aqueous solution and 15.5g of dimethyl acrylate, adjust the pH value to 9 with diethylamine, seal and continue to stir at 250°C and 1MPa at a low speed for 6h, dry at 100°C for 3h, and bake at 500°C for 4h to obtain the final composite filler T-2.

Embodiment 3

[0040] 2000g of tetrabutyl titanate and 1000g of 1-butyl-3-methylimidazole hydroxide were respectively placed in a container, and stirred evenly at room temperature to obtain a titanium dioxide precursor. Put 50g of glass hollow microspheres into 67.5g of metal titanium precursor, stir evenly, then add 18.2g of propanol, continue to stir evenly, then add 5.2g of dimethylethoxysilane, continue to stir evenly, then add 20 % ammonia solution to adjust the pH value of the slurry to 9.5. Put it in a closed autoclave, react at 60°C and 3MPa for 30 hours, take it out and filter until the water content of the filter cake is 46%, add 58.1g of titanium dioxide precursor and stir evenly, then slowly add 191.2g of 90% at 10r / min Ethanol aqueous solution and 10.5g methyl acrylate, adjust the pH value to 8 with propylamine, seal and continue stirring at 250°C and 1MPa at a low speed for 6h, dry at 100°C for 3h, and bake at 500°C for 4h to obtain the final composite filler T-3.

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Abstract

The invention discloses a preparation method of a composite filler. According to the method, a metal oxide precursor is formed at first, hollow microspheres are introduced in the growth process of metal oxide crystal nucleuses, a silane coupling agent is added, metal oxide crystals and the hollow microspheres are combined in order through hydrolysis of the silane coupling agent, and agglomerationof metal oxide on the surfaces of the hollow microspheres is avoided; and metal oxide crystals in an ordered array are formed and then are rapidly hydrolyzed and crosslinked together with a metal oxide precursor, so rapid accumulation and growth of a metal oxide layer are realized, a tightly combined metal oxide wrapping layer is obtained by means of calcination and the like, and a flat reflectinglayer on the surface of the formed filler is effectively controlled. According to the method, the density and reflectance ratio of a surface reflection layer can be improved, and the heat insulationeffect of the obtained composite filler is improved.

Description

technical field [0001] The invention relates to a preparation method of a metal oxide / hollow microsphere composite filler, in particular to a preparation method of a composite filler with solar light reflection and heat insulation function. Background technique [0002] Hollow glass microspheres are hollow and closed spheres, which contain a certain amount of gas and have low thermal conductivity. Therefore, hollow glass microspheres have the characteristics of sound insulation and heat insulation, and are excellent fillers for various thermal insulation materials and sound insulation products. At the same time, hollow microspheres are also widely used as a filler in thermal insulation coatings. [0003] At present, there are many methods for preparing hollow microspheres for reflective heat-insulating coatings, and the usual method is to use the sol-gel method to coat TiO on the surface of hollow microspheres. 2 coating. For example, CN1583908A, CN200610127227.8, etc., co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/30C09C1/40C09C3/12C09C3/06C09D5/33
CPCC09C1/309C09C1/407C09C3/006C09C3/066C09C3/12C09D5/004
Inventor 刘名瑞赵巍李世瀚王晓霖李遵照王佩弦
Owner CHINA PETROLEUM & CHEM CORP
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