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A kind of organic-inorganic hybrid molecular composite material with high refractive index and its preparation method

A technology of refractive index and composite materials, applied in the direction of 4/14 organic compounds without C-metal bonds, titanium organic compounds, organic chemistry, etc., can solve the effects of product thermal stability and hydrolytic stability, hydrolysis and condensation reactions Difficult to complete, time-consuming and other issues, to achieve the effect of good industrial application prospects, high stability, high weather resistance

Active Publication Date: 2019-07-05
武汉铌欧能源材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] 1. The uncontrollable problem of the hydrolysis reaction and the polycondensation reaction that occurs and proceeds almost simultaneously; these two reactions are almost simultaneously affected by the following multiple factors, including: the stoichiometric ratio of the reactants, the reaction medium, the type of catalyst, and the temperature of the reaction process Control, the chemical activity of the precursor reactant itself and other reaction conditions;
[0007] 2. Hydrolysis and condensation reactions are difficult to complete
In the final product, unhydrolyzed alkoxy groups and uncondensed hydroxyl groups will affect the thermal stability and hydrolytic stability of the product
[0008] 3. The use of traditional sol-gel technology for industrial production to prepare organic-inorganic hybrid polymer composites has the disadvantages of low yield, long time consumption and high energy consumption

Method used

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  • A kind of organic-inorganic hybrid molecular composite material with high refractive index and its preparation method
  • A kind of organic-inorganic hybrid molecular composite material with high refractive index and its preparation method
  • A kind of organic-inorganic hybrid molecular composite material with high refractive index and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0059] The preparation method of zirconium oxygen cluster complex, main steps are as follows:

[0060] 1) 6.0 grams of benzyl alcohol and 0.71 grams of benzylic acid are uniformly mixed to form solution A; 1.35 grams of deionized water and 6.0 grams of benzyl alcohol are uniformly mixed to form solution B;

[0061] 2) Slowly add 12.0 g of tetra-tert-butoxyzirconium butanol solution (commercially available, with a mass fraction of 80%) into solution A, and stir evenly for 10 minutes to form solution C;

[0062] 3) Pass solution B through a 50 ml constant pressure dropping funnel, and slowly add it dropwise into solution C under the condition of uniform stirring to form uniform solution D;

[0063]4) Transfer all the obtained solution D to a pre-cleaned and dried autoclave and seal it. Slowly heat the solution D in the autoclave to 230°C. The pressure in the autoclave depends on the solvent (butanol and some benzyl alcohol) It will rise at about 1.7 MPa (MPa), heat preservation...

Embodiment 2

[0068] Repeat the synthetic procedure of embodiment 1, but to the mole number ratio of zirconium atom (marked as H 2 O / Zr), the temperature of reaction, the time of reaction make adjustment, to compare and optimize, the parameter change of experiment is listed in table 1. Other experimental conditions were kept the same.

[0069] Table 1 The refractive index of the surface-modified zirconium-oxygen cluster complex solution synthesized under various conditions

[0070] serial number h 2 O / Zr

[0071] From Table 1 and figure 1 It can be seen that the molar ratio of the initial reactant water and zirconium is 3.0, the reaction temperature is 230 ° C, and the reaction time is the best synthetic condition for 4 hours, and the refractive index of the product solution is the highest: n 20 D = 1.639.

Embodiment 3

[0073] Repeat the synthesis procedure of Example 1, but in the use of surface modifiers, in addition to benzyl alcohol, cinnamic acid is used to replace the benzylic acid in Example 1, and the reagents and synthesis procedures of all other reactions are completely the same as in Example 1 Same, the final product is also a transparent homogeneous liquid, and the n of the product 20 D = 1.6310.

[0074] The surface modifier with benzilic acid as an auxiliary is better than cinnamic acid, and the refractive index of the product solution is higher: n 20 D = 1.639.

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Abstract

The invention discloses an organic-inorganic hybrid molecule composite material with a high refraction coefficient. The organic-inorganic hybrid molecule composite material mainly comprises, by mass, 2 to 52% of a metal-oxo cluster compound and a derivative thereof, 2 to 88% of an active monomer contain a phenoxyl group, 0 to 90% of a monomer or oligomer of a polymerizable active group, 0 to 10% of a curing aid and 0 to 10% of an additive. The particle size of the metal-oxo cluster compound synthesized in the invention is in a sub-nanometer range, so the metal-oxo cluster compound is a key component for improving the refraction coefficient of the composite material; and organic-inorganic hybrid molecule composite material prepared from the metal-oxo cluster compound has high optical transparency, high refraction coefficient, high stability, high weatherability and the like, presents good industrial application prospects and is extensively applicable to a plurality of high-tech fields like new energy, optical materials, photoelectronic devices and functional paint.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to an organic-inorganic hybrid molecular composite material with high refractive index and a preparation method thereof. Background technique [0002] In the past ten years, high-refractive-index optical materials have aroused more and more strong interest in both basic research and high-tech application circles. This is due to the broad application prospects and great potential of this type of material in numerous technological and industrial fields. These applications include advanced optoelectronic device manufacturing, optical lens manufacturing, holographic recording materials, anti-reflective films in optical and solar cells, optical adhesives and packaging materials in LED and OLED manufacturing, 193nm immersion lithography Photoresist materials used (photoresists for 193-nm immersion lithography), micro-lens materials in high-brightness electronic displays, etc....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/30C08F283/10C08F220/30C08F2/44C08K5/00C07F7/00C07F7/28
CPCC07F7/003C07F7/28C08F120/30C08F220/30C08F220/302C08F283/10C08K5/0091C08F220/301
Inventor 王执锴刘伟邓渝林王思哲郑焱
Owner 武汉铌欧能源材料有限公司
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