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Preparation method of octaphenyl silsesquioxane

A technology of silsesquioxane and octaphenyl cage, applied in the direction of silicon organic compounds and the like, can solve the problems of unsuitability for industrial production, low yield, complicated preparation method, etc., and achieves short preparation cycle, high yield, and high preparation simple craftsmanship

Inactive Publication Date: 2015-12-02
ORINKO NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Octaphenyl POSS was obtained by Brown et al. in 1960 by using phenyltrichlorosilane after hydrolysis of potassium hydroxide through a complex multi-step condensation reaction. Its preparation method is complicated and the yield is low, so it is not suitable for industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] (1) Place a 500mL three-neck flask equipped with a condenser and a stirrer in an ice-water bath, fill the inside with an inert gas for protection, then add 100mL of benzene and 150mL of deionized water, and then add 28g of phenyltriethoxy Silane; turn on the stirrer to carry out the hydrolysis reaction for 40min and let it stand; finally use a separating funnel to filter off the water layer at the bottom of the three-necked flask, wash the organic phase three times with deionized water and then dry it with anhydrous sodium sulfate to obtain the precursor Hydrolyzate;

[0027] (2) Prepare 100 mL of 0.5 mol / L potassium hydroxide ethanol solution, and put it into the three-necked flask in (1) for mixing together with the precursor hydrolyzate. Reflux reaction at 110°C for 72h, filter to obtain a white substance, wash with dichloromethane for more than 3 times, and then put it in a vacuum drying oven at 60°C for 24h to obtain a molecular weight of 1.5×10 5 , Octaphenyl cla...

example 2

[0029] (1) Put a 500ml three-necked flask equipped with a condenser tube and a stirrer in an ice-water bath, fill it with an inert gas for protection, then add a mixture of 100ml toluene and 200mL deionized water, and then add 28g of phenyltrimethoxy base silane; start stirring and carry out hydrolysis reaction for 20min and then let it stand; finally use a separatory funnel to filter off the water layer at the bottom of the three-necked flask, and wash the organic phase three times with saturated sodium chloride solution, and then use anhydrous sodium sulfate on it. Carry out drying to obtain precursor hydrolyzate;

[0030] (2) Prepare 150 mL of 2 mol / L sodium hydroxide acetone solution, put it into the three-necked flask in (1) together with the precursor hydrolyzate and mix it. Reflux at 250°C for 5 hours, filter to obtain a white substance, wash with ether three times, and dry in a vacuum oven at 70°C for 24 hours to obtain a molecular weight of 6.8×10 4 , The yield of oc...

example 3

[0032] (1) Place a 500ml three-necked flask equipped with a condenser tube and a stirrer in an ice-water bath, fill the inside with an inert gas for protection, then add 30ml tetrahydrofuran and 30mL deionized water, and slowly add 15g phenyltrichlorosilane Add it slowly. Turn on the stirrer and carry out the hydrolysis reaction for 60 minutes, then let it stand, and finally filter the water layer at the bottom of the three-necked flask with a separatory funnel, wash the organic phase with methanol three times, and then dry it with anhydrous sodium sulfate to obtain the precursor hydrolyzate;

[0033] (2) Prepare 30mL of solution according to the ratio of acetone / ethanol=4:1, then add tetraethyl sodium hydroxide to form a 1mol / L mixture; put it into the three-necked flask in (1) together with the precursor hydrolyzate mix in. Reflux at 20°C for 100 hours to obtain a white product. After the product was filtered out, washed with acetone, recrystallized and purified with dichl...

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Abstract

The invention discloses a preparation method of octaphenyl silsesquioxane. The preparation method comprises the steps of firstly, placing a reactor into an ice-water bath, adding a mixed solution of an organic solvent and deionized water into the reactor, and then, adding phenylsilane; then, starting to stir to carry out hydrolysis reaction for 20-60 minutes, then, standing, washing an organic phase, and drying to obtain a precursor hydrolysis product; adding the precursor hydrolysis product into an original reaction vessel, then, adding a mixture of a catalyst and a solvent into the original reaction vessel, and carrying out backflow reaction at the temperature of 20-250 DEG C for 5-100 hours to separate out a great number of white sediments; and then, purifying in a way of filtering, washing or dissolving and re-crystallizing the sediments, and drying to obtain octaphenyl silsesquioxane. According to the preparation method, octaphenyl-functionalized POSS with relatively high molecular weight and relatively high yield is controllably prepared by taking phenylsilane as a raw material through a low-temperature feeding and two-step hydrolysis process; in addition, the preparation process is simple, the yield is relatively high, and the preparation period is short.

Description

technical field [0001] The invention belongs to the field of organic polymer materials, and in particular relates to a preparation method of octaphenyl clathrate silsesquioxane. technical background [0002] Hybrid materials are composites of two different types of materials. In the past, people used large-scale hybridization to obtain some materials with better performance, which have the characteristics of easy processing of organic polymers and high strength of inorganic materials. However, only hybridization on a large scale cannot meet the high technical requirements for materials in the current information age. To this end, small-scale hybridization, that is, hybridization at the nanoscale and molecular level, has been proposed in order to obtain multifunctional, high-density integrated composite materials. [0003] The general molecular formula of cage polysilsesquioxane (POSS) is expressed as (RSiO 3 / 2 )n (n≥4), which is a nanoparticle composed of a skeleton form...

Claims

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Application Information

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IPC IPC(8): C07F7/21
Inventor 陶慷李玉玲李荣群任东方
Owner ORINKO NEW MATERIAL CO LTD
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