Preparation method of cage type octaphenylsilsesquioxane(OPS)

A technology of octaphenylsilane and sesquioxane, which is applied in the field of organic-inorganic hybrid materials, can solve the problems of complex process, long cycle, difficult separation, etc., and achieve good product stability, short reaction cycle, and good repeatability Effect

Active Publication Date: 2019-06-14
BEIJING INSTITUTE OF TECHNOLOGYGY
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Problems solved by technology

In 1958, Sprung and Guenther (Sprung M M, Guenther F O. The hydrolysis of n-Amyltriethoxysilane and phenyltriethoxysilane. J Polym Sci. 1958,28:17-34.) Alkaline hydrolysis of phenyltriethoxysilane to obtain polymers Rearrangement prepared cage-type octaphenylsilsesquioxane, but its yield is still very low, only 9%, and due to the problem of condition control, the product has a large number of isomers, which are difficult to separate
In 1964, Brown et al. (Brown J F, Vogt L H, Prescott P I.Preparation and characterization of the lower equilibratedphenylsilsesquioxanes.J Am Chem Sci.1964,86:1120-1125.) Caged octaphenylsilsesquioxanes in equilibrium The reaction of oxane has been further studied, and the process has been further improved. Using phenyltrichlorosilane as raw material, add acid hydrolysis in benzene, remove the acid layer, wash with water and then catalyze with alkali, reflux for 4 hours, and place After 4 days, reflux for another 24 hours, so that the yield reached 88%; the vast majority of the preparation of cage-type octaphenylsilsesquioxane that appeared in the literature in recent years is completed by this method, which is also reported in the literature The method with the highest yield, although the yield is improved, the preparation process requires multi-step reactions, the cycle is long, the process is complicated, and it is not suitable for industrial production
[0004] In 2012, Chinese patent CN102643304A disclosed a method for preparing cage-type octaphenylsilsesquioxane. The method uses phenyltriethoxysilane or phenyltrimethoxysilane as a monomer raw material, and the organic alcohol is Solvent, under the catalysis of hydrochloric acid, prepare cage octaphenylsilsesquioxane through one-step hydrolysis and polycondensation; although this method is relatively simple, the yield is still low, only about 70%
In 2015, Chinese patent CN105111233A also disclosed a preparation method of octaphenyl cage silsesquioxane, which uses phenylsilane as raw material, adopts low-temperature feeding and two-step hydrolysis process, and prepares octaphenyl cage Type silsesquioxane, but this method is only an improvement to the synthetic method proposed by Brown in 1964, and the steps are still relatively complicated, requiring low-temperature feeding and two-step hydrolysis processes, and the low yield is only about 80%
[0005] In the existing technology, the synthesis route of cage octaphenylsilsesquioxane generally has the problems of complex production process and low yield

Method used

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  • Preparation method of cage type octaphenylsilsesquioxane(OPS)

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preparation example Construction

[0025] The invention provides a preparation method of cage-type octaphenylsilsesquioxane, which comprises the following steps: mixing phenylsilane, an organic solvent, a basic catalyst and water, performing hydrolysis and polycondensation reaction, and obtaining cage-type octaphenylsilsesquioxane Silsesquioxane.

[0026] In the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.

[0027] In the present invention, the phenylsilane preferably includes phenyltrichlorosilane, phenyltrimethoxysilane or phenyltriethoxysilane.

[0028] In the present invention, the basic catalyst preferably includes potassium hydroxide, lithium hydroxide, sodium hydroxide, potassium carbonate, sodium carbonate, lithium carbonate, sodium methoxide, sodium ethoxide, tetramethylammonium hydroxide and tetraethylhydrogen One or more of ammonium oxides, more preferably potassium hydroxide, lithium hydroxide,...

Embodiment 1

[0039] Add 19.84g of phenyltrimethoxysilane and 200mL of isopropanol into a 500mL three-necked flask equipped with a reflux condenser, a constant pressure dropping funnel, a temperature control device and a magnetic stirrer, and mix evenly at 25°C and 100rpm. Raise the temperature to 85°C, then dissolve 0.3g KOH in 10mL distilled water to obtain a KOH solution, slowly add the KOH solution to the obtained system dropwise at a rate of 0.3mL / min, start timing after the dropwise addition, and react for 48 hours to obtain a white reaction solution ;

[0040] Suction-filter the obtained white reaction liquid, wash alternately with distilled water and absolute ethanol three times to obtain a filter cake, and dry the filter cake in a vacuum oven at 80° C. for 10 h to obtain cage-type octaphenylsilsesquioxane. The productive rate is 95.3% based on the amount of phenylsilane, and the purity is 99.8%. The structure diagram is as follows: figure 1 shown.

[0041] figure 2 It is the FT...

Embodiment 2

[0047] Add 21.16g of phenyltrichlorosilane and 100mL of dichloromethane into a 500mL three-neck flask equipped with a reflux condenser, a constant pressure dropping funnel, a temperature control device, and a magnetic stirrer, mix well at 25°C and 150rpm, and heat up to 45°C, then dissolve 0.5g of tetraethylammonium hydroxide in 10mL of distilled water to obtain a tetraethylammonium hydroxide solution, and slowly drop the tetraethylammonium hydroxide solution into the resulting system at a rate of 0.3mL / min , start timing after the dropwise addition, and react for 24 hours to obtain a white reaction solution;

[0048] Suction-filter the resulting white reaction solution, wash alternately with distilled water and absolute ethanol three times to obtain a filter cake, and dry the filter cake in a vacuum oven at 80°C for 10 hours to obtain cage-type octaphenylsilsesquioxane. The yield is 96.1%, the purity is 99.8%, and the molecular weight is 1033.3.

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Abstract

The invention relates to the technical field of organic-inorganic hybrid materials, in particular to a preparation method of cage type octaphenylsilsesquioxane(OPS). The preparation method comprises the following steps that phenylsilane, an organic dissolvent, a basic catalyst and water are mixed to be subjected to a hydrolytic polycondensation reaction, and the cage type OPS is obtained. According to the preparation method of the cage type OPS, phenylsilane is used as a raw material, the raw material is easy to obtain, a one-step hydrolytic polycondensation technology is adopted, material feeding is carried out at a time, the operation is convenient, the reaction cycle is short, and the repeatability is good; meanwhile, the yield coefficient is high, the purity is high, and the stabilityof a product is good; cage type OPS with single molecular weight and high yield coefficient can be prepared in a controllable mode, the preparation method is an environmental-friendly type OPS synthesizing method, and industrial production can be easily carried out.

Description

technical field [0001] The invention relates to the technical field of organic-inorganic hybrid materials, in particular to a preparation method of cage octaphenylsilsesquioxane. Background technique [0002] Cage octaphenylsilsesquioxane (OPS), its structural formula is (C 6 h 5 SiO 1.5 ) 8 , the structural formula is shown in formula I, which has good heat resistance, weather resistance, chemical resistance, thermal oxidation resistance, electrical insulation, optical transparency, water resistance and flame retardancy, etc., and can be applied to polymer modification properties, thermal insulation materials, low dielectric materials, coating coatings, gas separation membranes and other fields, which have aroused great research interest. [0003] Since the 1960s, Barry et al. (Barry A J, Daudt William H, Domicone J J, et al. Crystalline organosilsesquioxanes. J Am Chem Soc. 1955, 77:4248-4252.) prepared the cage octaphenylsilsesquioxanes for the first time oxane, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/06C08G77/08
Inventor 杨荣杰秦兆鲁张文超
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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