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Polycarboxylic cage type phenyl sesquialter siloxane and method for synthesizing same

A technology of phenyl silsesquioxane and silsesquioxane, which is applied in the field of nanomaterials, can solve the problems that the synthesis method of polycarboxy cage silsesquioxane has not been reported, and achieve controllability, cost reduction, and wide range of synthetic raw materials Effect

Inactive Publication Date: 2008-08-27
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Chinese invention patent (publication number: CN1844126A) has reported adopting water and hydrazine as reducing agent, and the preparation method of corresponding catalytic system (Fe / C) to prepare aminophenyl silsesquioxane containing aminophenyl silsesquioxane, is only to Laine synthetic route Improvement, there is no report about polycarboxy cage silsesquioxane and its synthetic method

Method used

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  • Polycarboxylic cage type phenyl sesquialter siloxane and method for synthesizing same
  • Polycarboxylic cage type phenyl sesquialter siloxane and method for synthesizing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Polybrominated cage octaphenylsilsesquioxane (SiO 1.5 ) 8 (C 6 h 5 ) 4 {C 6 h 4 Br} 4 Synthesis:

[0021] Add 30g of dry cage octaphenylsilsesquioxane, 2.85g of Fe and 300ml of CH to a 500ml three-necked flask 2 Cl 2 ; Add 12ml of Br dropwise under mechanical stirring 2 . React at room temperature for 6 hours, add 150ml of 10% NaHSO 3 Stop the reaction. The layers were separated, the organic phase was washed three times with water, and the solid crude product was obtained by rotary evaporation. Dry it, dissolve it in a small amount of ethyl acetate, and settle it with 800ml of methanol to obtain a large amount of white precipitate; repeat the precipitation two to three times. After drying, 38 g of white powder was obtained, which was polybromocage octaphenylsilsesquioxane, and the yield was 90%.

Embodiment 2

[0023] Polycarboxy cage octaphenylsilsesquioxane (SiO 1.5 ) 8 (C 6 h 5 ) 4 {C 6 h 4 COOH} 4 Synthesis:

[0024] In a dry 250ml three-necked flask, under nitrogen protection, add 12g (bromine 35.2mmol) (SiO 1.5 ) 8 (C 6 h 5 ) 4 (C 6 h 4 Br) 4 With 80ml of freshly distilled THF; stir mechanically until the temperature reaches -75°C and is stable; slowly add 75ml of Bu-Li (1.6M) dropwise, after the addition is complete and stir for 2.5 hours, slowly add 50ml of 1M HCl dropwise to terminate the reaction. NaOH was added to the water layer to obtain a transparent solution, and concentrated hydrochloric acid was added, a large amount of white solid precipitated, filtered and washed with water 3-5 times. 6.89 g of white solid powder was obtained as polycarboxy cage octaphenylsilsesquioxane (-COOH=4), with a yield of 64%.

Embodiment 3

[0026] Polycarboxy cage octaphenylsilsesquioxane (SiO 1.5 ) 8 (C 6 h 5 ) 4 {C 6 h 4 COOH} 4 Synthesis:

[0027] In a dry 250ml three-neck flask under the protection of nitrogen, carefully add 0.977g (-Br:Bu-Li=1:4.0) metal lithium flakes to 100ml of freshly distilled ether, and mechanically stir until the temperature reaches -10°C and is stable; Slowly add 12g (SiO 1.5 ) 8 (C 6 h 5 ) 4 (C 6 h 4 Br) 4 (bromo group 35.2mmol) and 20ml of freshly distilled ether solution, the time is 3 hours, after the dropwise addition is completed and stirred for 5 hours, dry CO2 Gas for 10 to 12 hours; slowly drop 50ml of ethanol to terminate the reaction. NaOH was added to the water layer to obtain a transparent solution, and concentrated hydrochloric acid was added, a large amount of white solid precipitated, filtered and washed with water 3-5 times. 5.60 g of white solid powder was obtained, which was polycarboxy cage octaphenylsilsesquioxane (-COOH=4), and the yield was 52%....

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Abstract

The invention provides a polycarboxylic cage type phenylsilsesquioxane-co and a relative synthesis method, which formula is (SiO<1.5>)<n>(C<6>H<5>)<x>{C<6>H(COOH)<q>}<y>, wherein when n is 8, 10 and 12, respectively corresponding to hexahedron, octahedron and decahedron cage type structures, x is integer from 0 to n-1, y is integer from 1 to n, x+y=n, p is integer from 2 to 4, and q is integer from 1 to 3. The preparation method comprises reacting cage type phenylsilsesquioxane-co and liquid bromine at normal temperature to obtain polybrominated cage type phenylsilsesquioxane-co, to be reacted with organic metallizing reagent, dry ice or carbon dioxide, to prepare the polycarboxylic cage type phenylsilsesquioxane-co. The invention has the advantages of wide material resource, simple synthesis and high yield, with wide application in polymer modification, organic and inorganic nanometer hybrid material, low-dielectric material or medical material.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials. It relates to a polycarboxy cage phenyl silsesquioxane and a synthesis method thereof. The polycarboxy cage phenyl silsesquioxane synthesized by the method can be widely used in polymer modification and organic-inorganic nano-hybrid materials , low dielectric materials, medical materials, architectural coatings, luminescent materials and other fields. Background technique [0002] The development of material science has made the performance requirements of materials higher and higher. Pure organic or inorganic materials can no longer meet some special performance requirements, while hybrid materials have comprehensive excellent properties of both organic and inorganic materials. Their thermal properties, Mechanical properties, optical properties, electrical properties, etc. have been greatly improved. Among them, cage silsesquioxane (POSS) has a typical organic / inorganic hybrid nano...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 王忠刚冷世伟张步峰
Owner DALIAN UNIV OF TECH
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