Preparation method of ring trapezoidal nitrophenyl silsesquioxane

A technology of silsesquioxane and nitrophenyl, applied in the direction of silicon organic compounds, etc., to achieve the effects of high yield, mild reaction conditions and simple operation

Active Publication Date: 2016-12-07
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The existing research on cyclic trapezoidal phenylsilsesquioxane has just started. With reference to the existing nitration process of cage-type oligomeric phenylsilsesquioxane, fuming nitric acid with a higher concentration is used to combine with phenylsilsesquioxane. The hemioxane is dispersed in a heterogeneous phase under vigorous stirring, and the cage-type oligomeric nitrophenylsilsesquioxane is synthesized by reacting for 20-24 hours. This process is applied to the nitration of the ring ladder-shaped phenylsilsesquioxane, which will lead to Fracture of ring trapezoidal structure

Method used

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  • Preparation method of ring trapezoidal nitrophenyl silsesquioxane
  • Preparation method of ring trapezoidal nitrophenyl silsesquioxane
  • Preparation method of ring trapezoidal nitrophenyl silsesquioxane

Examples

Experimental program
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Effect test

Embodiment 1

[0026] 1) Add 4g of cyclic trapezoidal phenylsilsesquioxane (PPSQ) and 20mL of dichloromethane into a 250mL three-necked flask with reflux condenser, constant pressure dropping funnel, temperature control device, nitrogen protection and magnetic stirring, and stir , the temperature of the ice-water bath was controlled at 0°C, and 20mL of 80% nitric acid, 40mL of acetic anhydride, and 10mL of acetic acid were slowly added dropwise in sequence for about 1 hour. After the addition, the temperature was raised to 30°C and reacted for 6 hours to obtain a reaction solution.

[0027] 2) The reaction solution obtained in step 1) is poured into 50 mL of ice water, the mixed solution is rotary evaporated to remove dichloromethane, and a yellow solid is precipitated, which is filtered by suction to obtain a filter cake, which is successively washed with saturated Na 2 CO 3 Wash the filter cake with solution until there are no air bubbles, wash with distilled water until the filtrate is ne...

Embodiment 2

[0032] 1) Add 8g of cyclic trapezoidal phenylsilsesquioxane (PPSQ) and 40mL of dichloromethane into a 500mL three-necked flask with reflux condenser, constant pressure dropping funnel, temperature control device, nitrogen protection and magnetic stirring, and stir , the temperature of the ice-water bath was controlled at 0°C, and 40mL of 80% nitric acid, 80mL of acetic anhydride, and 20mL of acetic acid were slowly added dropwise in sequence for about 1 hour. After the addition, the temperature was raised to 30°C and reacted for 7 hours to obtain a reaction solution.

[0033] 2) The reaction solution obtained in step 1) is poured into 100 mL of ice water, the mixed solution is rotary evaporated to remove dichloromethane, and a yellow solid is precipitated, which is filtered by suction to obtain a filter cake, which is successively washed with saturated Na 2 CO 3 Wash the filter cake with solution until there are no air bubbles, wash with distilled water until the filtrate is n...

Embodiment 3

[0035]1) Add 8g of cyclic trapezoidal phenylsilsesquioxane (PPSQ) and 60mL of dichloromethane into a 500mL three-necked flask with reflux condenser, constant pressure dropping funnel, temperature control device, nitrogen protection and magnetic stirring, and stir , the temperature of the ice-water bath was controlled at 0°C, and 40mL of 75% nitric acid, 80mL of acetic anhydride, and 20mL of acetic acid were slowly added dropwise in sequence for about 1 hour. After the addition, the temperature was raised to 35°C and reacted for 6 hours to obtain a reaction solution.

[0036] 2) The reaction solution obtained in step 1) is poured into 100 mL of ice water, the mixed solution is rotary evaporated to remove dichloromethane, and a yellow solid is precipitated, which is filtered by suction to obtain a filter cake, which is successively washed with saturated Na 2 CO 3 Wash the filter cake with solution until there are no air bubbles, wash with distilled water until the filtrate is ne...

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Abstract

The invention relates to a preparation method of ring trapezoidal nitrophenyl silsesquioxane and belongs to the technical field of organic-inorganic hybrid materials. The method comprises the steps that ring trapezoidal phenyl silsesquioxane and a solvent are added into a reactor and stirred, the temperature of the reactor is controlled to be 0-10 DEG C, nitric acid, acetic anhydride and acetic acid are dropwise added in sequence, then the temperature of the reactor is raised to 25-35 DEG C, reaction time is 4-8 hours, and reaction liquid is obtained; the reaction liquid is subjected to rotary steaming and suction filtration and washed with a saturated Na2CO3 solution, distilled water and ethyl alcohol in sequence, filter cakes are dried, the drying temperature is 40-100 DEG C, and lastly ring trapezoidal nitrophenyl silsesquioxane is obtained. The reaction conditions are mild, repeatability is good, and the method has the advantages of a high yield, a short cycle and easy operation and is suitable for expanded production; the obtained product can be further subjected to an ammoniation reaction, an alkynylation reaction and other reactions to synthesize new ring trapezoidal silsesquioxane derivatives.

Description

technical field [0001] The invention relates to a method for preparing ring-ladder nitrophenylsilsesquioxane (PNPSQ), which belongs to the field of organic-inorganic hybrid material science. Background technique [0002] Polyhedral oligomeric silsesquioxane (POSS) refers to the molecular formula (RSiO 1.5 ) n The POSS molecular structure not only contains the "skeleton" structure of inorganic siloxane, but also introduces organic groups through side groups. The dense inorganic silicon-containing inner core can restrain its chain movement and endow it with good heat resistance, and the corresponding organic side groups endow it with good toughness and processability. This typical inorganic-organic hybrid material simultaneously It has the basic characteristics of organic polymers and inorganic ceramics. In addition to the excellent performance of POSS, polyphenylsilsesquioxane (PPSQ) with a regular structure also has excellent film-forming properties and good solubility in...

Claims

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Application Information

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IPC IPC(8): C07F7/21
CPCC07F7/21
Inventor 杨荣杰吴义维张文超
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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