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Preparation method of polymethyl methacrylate/zirconium dioxide composite material

A technology of polymethyl methacrylate and zirconium dioxide, which is applied in the field of composite materials, can solve problems such as complex preparation process, difficult control, and different systems, and achieve high refractive index, good transparency, and simple and easy-to-operate preparation method Effect

Active Publication Date: 2013-11-20
嘉兴高正新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned traditional method often has complex preparation process and many operation steps, and although the reaction mechanism of the solvothermal method involved in the present invention has similarities with the sol-gel method, the preparation process has considerable differences
In addition, the research group of the present invention studied the preparation of polymethyl methacrylate / titanium dioxide nanocomposites by solvothermal method in the early stage, but due to the difference of the system, the two are quite different in nature
Zirconium precursors are more active and difficult to control than titanate precursors

Method used

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  • Preparation method of polymethyl methacrylate/zirconium dioxide composite material
  • Preparation method of polymethyl methacrylate/zirconium dioxide composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1.645g of methyl methacrylate, 0.355g of vinyltrimethoxysilane, 35g of tetrahydrofuran and 0.05g of azobisisobutyronitrile were successively added into the autoclave. Concentrated hydrochloric acid was then added to pH=1. Then, 0.4 g of zirconium n-propoxide, 0.8 g of acetylacetone and 0.5 g of deionized water were sequentially added into the autoclave. Cover the lid, put it into a metal can, put it into an incubator with a temperature of 80° C., and react for 10 hours. After the reaction is completed, the metal tank is completely cooled, and then the reactor is taken out. The prepared product solution was spin-coated on a silicon wafer by using a homogenizer at a rotation speed of 3000 rpm and a spin-coating time of 40 seconds. Then put the coated silicon wafer into an oven at 80°C for 1 hour, at 100°C for 1 hour, and at 150°C for 2 hours for annealing. The obtained film is the polymethyl methacrylate / zirconia composite material.

[0028] The film that obtains is p...

Embodiment 2

[0030] 1.532g of methyl methacrylate, 0.428g of vinyltriacetoxysilane, 50g of toluene and 0.20g of dicumyl peroxide were successively added into the autoclave. Concentrated hydrochloric acid was then added to pH=1. Then, 2.0 g of zirconium isopropoxide, 4.0 g of benzoylacetone and 1.0 g of deionized water were successively added into the autoclave. Cover the lid, put it into a metal can, put it into a thermostat with a temperature of 100° C., and react for 8 hours. After the reaction is completed, the metal tank is completely cooled, and then the reactor is taken out. The prepared product solution was spin-coated on a silicon wafer by using a homogenizer at a rotation speed of 2500 rpm and a spin-coating time of 60 seconds. Then put the coated silicon wafer into an oven at 80°C for 2 hours, 100°C for 1 hour, and 150°C for 1 hour for annealing. The obtained film is the polymethyl methacrylate / zirconia composite material.

[0031] The film that obtains is polymethyl methacry...

Embodiment 3

[0033]Add 1.546g of methyl methacrylate, 0.521g of γ-glycidyl etheroxypropyl trimethoxysilane, 0.216g of maleic anhydride, 30g of N,N-dimethylformamide and 0.17g of dimethylmethoxysilane in the autoclave Benzoyl. Concentrated hydrochloric acid was then added to pH=1. Then, 1.6 g of zirconium acetate, 3.2 g of dibenzoylmethane and 0.6 g of deionized water were successively added into the autoclave. Cover the lid, put it into a metal can, put it into a thermostat with a temperature of 70° C., and react for 12 hours. After the reaction is completed, the metal tank is completely cooled, and then the reactor is taken out. The prepared product solution was spin-coated on a silicon wafer by using a homogenizer at a rotation speed of 3500 rpm and a spin-coating time of 50 seconds. Then put the coated silicon wafer into an oven at 80°C for 1 hour, 110°C for 2 hours, and 150°C for 2 hours for annealing. The obtained film is the polymethyl methacrylate / zirconia composite material.

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Abstract

The invention discloses a preparation method of a polymethyl methacrylate / zirconium dioxide composite material. The preparation method comprises the following steps of: adding methyl methacrylate, a silicane-containing comonomer, a synergistic comonomer, a solvent and an initiating agent in proportion to a high-pressure reactor so as to prepare a mixed solution A; adding concentrated hydrochloric acid for adjusting pH to 1; sequentially adding a zirconium precursor, a chelating agent and deionized water; controlling reaction temperature and time and reacting in an airtight system; and after completion of reaction, coating the obtained solution on a silicon wafer to form a film, and carrying out annealing treatment, thus obtaining the polymethyl methacrylate / zirconium dioxide composite thin film. According to the solvothermal preparation method, polymethyl methacrylate polymerization and zirconium dioxide generation can be completed at the same time through one-step synthesis; therefore, the preparation method has the advantages of few steps, simple operation and mild reaction conditions and is favorable for industrial production. The prepared polymethyl methacrylate / zirconium dioxide composite thin film has relatively high refractive index and good transparency and can be widely applied to the field of optics.

Description

technical field [0001] The invention relates to the technical field of composite materials, in particular to a method for preparing a polymethyl methacrylate / zirconia composite material. Background technique [0002] The abbreviated code name of polymethyl methacrylate is PMMA, commonly known as plexiglass, which is by far the most excellent and relatively affordable variety of synthetic transparent materials. Its transparency is excellent, and the light transmittance reaches 92%, which is higher than that of glass; it has outstanding aging resistance. Its specific gravity is less than half that of ordinary glass, but its resistance to fragmentation is several times higher; it has good insulation and mechanical strength; it has strong corrosion resistance to acids, alkalis, and salts, and is easy to process. However, as an organic material, polymethyl methacrylate has a low refractive index, only 1.49. Zirconium dioxide has high refractive properties (refractive index 2.1 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L33/12C08K3/22C08F220/14C08F230/08
Inventor 金婕妤戚嵘嵘朱健李海波
Owner 嘉兴高正新材料科技股份有限公司