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Method for preparing polyhedral oligomeric silsesquioxanes containing titanium phenyl

A technology of silsesquioxane and polysilsesquioxane, applied in the direction of titanium organic compounds, can solve problems such as co-precipitation side reactions and achieve the effect of strong reactivity

Active Publication Date: 2011-02-16
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the problem that the existing method for preparing silsesquioxane-titanium dioxide hybrid polymers is prone to co-precipitation side reactions, and provides a method for preparing titanium-containing phenyl semi-cage silsesquioxane

Method used

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  • Method for preparing polyhedral oligomeric silsesquioxanes containing titanium phenyl
  • Method for preparing polyhedral oligomeric silsesquioxanes containing titanium phenyl
  • Method for preparing polyhedral oligomeric silsesquioxanes containing titanium phenyl

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specific Embodiment approach 1

[0016] Specific embodiment one: the preparation method of the titanium-containing phenyl semi-cage silsesquioxane of the present embodiment is carried out according to the following steps: one, the volume ratio of phenyltrimethoxysiloxane and dehydrated alcohol is 1 : 4.5~5.5, the volume ratio of phenyltrimethoxysiloxane to acetic acid is 1:0.025~0.035, and the volume ratio of phenyltrimethoxysiloxane to water is 1:3~4. 1-phenyltrimethoxysiloxane, absolute ethanol, acetic acid and water; 2. Add the 1-phenyltrimethoxysiloxane, absolute alcohol and acetic acid weighed in step 1 to the container with reflux stirring device , stir evenly to obtain a mixed liquid, and then drop the water weighed in step 1 into the mixed liquid at a rate of 30 drops / minute to 35 drops / minute under the condition of stirring; ℃ and kept under reflux for 60h-65h, then the obtained mixture was left to age at room temperature for 40h-50h, the mixture was layered, and the upper layer was separated to obta...

specific Embodiment approach 2

[0018] Specific embodiment two: the difference between this embodiment and specific embodiment one is that in step one, the volume ratio of one-phenyltrimethoxysiloxane to absolute ethanol is 1:4.6~5.3, one-phenyltrimethoxysiloxane The volume ratio of oxane to acetic acid is 1:0.027~0.033, and the volume ratio of phenyltrimethoxysiloxane to water is 1:3.2~3.8. Weigh phenyltrimethoxysiloxane, anhydrous Ethanol, acetic acid and water. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0019]Specific embodiment three: the difference between this embodiment and specific embodiment one is that in step one, the volume ratio of one phenyltrimethoxysiloxane to absolute ethanol is 1:5.0, one phenyltrimethoxysiloxane The volume ratio of acetic acid is 1:0.030, and the volume ratio of monophenyltrimethoxysiloxane to water is 1:3.5. Weigh monophenyltrimethoxysiloxane, absolute ethanol, acetic acid and water. Others are the same as in the first embodiment.

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Abstract

The invention provides a method for preparing polyhedral oligomeric silsesquioxanes containing titanium phenyl, which relates to a method for preparing phenyl polyhedral oligomeric silsesquioxanes containing titanium phenyl. The method solves the problem that coprecipitation side effects are easy to occur by the method of the prior art for preparing a silsesquioxane-titanium dioxide hybrid polymer. The method comprises the following steps: 1) dropwise adding water to a mixed liquid of A-phenyl-trimethoxy silane, absolute alcohol and acetic acid, and carrying out heating, backflow and ageing on the mixed liquid to obtain phenyl heptamertic cyclopentyl silsesquioxanes; 2) preparing titanium oxide sol by using tetrabutyl titanate; and 3) dripping the titanium oxide sol to the polyhedral oligomeric silsesquioxanes, making the mixed sol of the titanium oxide sol and the polyhedral oligomeric silsesquioxanes stand for 40-50 hours at 8-12 DEG C, and drying the obtained sol to obtain the polyhedral oligomeric silsesquioxanes containing titanium phenyl. The method has the advantages that the method does not have any side effects, the target products are pure, and the polymer is not mixed with precipitates of titanium dioxide and silsesquioxanes. The method can be used for producing reinforced and modified materials of resinous polymers.

Description

technical field [0001] The invention relates to a preparation method of phenyl semi-cage silsesquioxane. Background technique [0002] Phenyl semi-cage silsesquioxane is a ring-shaped nanoscale cage molecule connected by silicon and oxygen as the skeleton, and phenyl substituents are connected externally. At the same time, the physical size of phenyl semi-cage silsesquioxane and Most polymers are on the same order of magnitude. Their size is similar to that of the smallest silicon powder particles, and their role is equivalent to nanoscale reinforcing fibers, resulting in a strong resistance to thermal deformation. At the same time, compared with other silicon powders, organic silicon compounds and fillers, the cage The phenyl group outside the skeleton greatly improves the chemical compatibility with the polymer, and can be connected to the polymer chain through a chemical bond. When the phenyl semi-cage silsesquioxane is added to the resin in the form of monomer or copoly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28
Inventor 秦伟方亮吴晓宏
Owner HARBIN INST OF TECH
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