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Method of preparing star-type multi-arm silicon oil

A technology of silicone oil and star shape, which is applied in the field of preparation of star-shaped multi-arm silicone oil, can solve the problems of restricting the application of silicone oil, defects in mechanical properties, high degree of branching, etc., and achieve process control, low apparent viscosity, and controllable molecular weight Effect

Inactive Publication Date: 2007-08-15
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the molecular structure of traditional silicone oil is mostly linear silicone oil. When the molecular weight is greater than 200,000, the viscosity of the silicone oil becomes very large, and the molecular weight exceeds 500,000, it becomes silicone rubber, which restricts the wider application of silicone oil.
Moreover, materials such as silicone rubber have defects in their mechanical properties due to the molecular structure of linear silicone oil
Existing studies have shown that branched silicone oil has better rheological properties and the ability to enhance the mechanical strength of materials, but it is difficult to obtain silicone oil with large molecular weight and high degree of branching by traditional preparation methods. Star multi-arm silicone oil is branched silicone oil Among them, there is no report on the synthesis of star-shaped multi-arm silicone oil, but only branched silicone oil.

Method used

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  • Method of preparing star-type multi-arm silicon oil
  • Method of preparing star-type multi-arm silicon oil
  • Method of preparing star-type multi-arm silicon oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1.136g (0.48%) of anhydrous tetramethylammonium octaoxide POSS and 236.8g (99.52%) of octamethylcyclotetrasiloxane were placed in a 500mL three-necked bottle, 80°C, mechanically stirred at 300rpm, and reacted under nitrogen protection for 24 After the reaction, the temperature was raised to 145°C for half an hour to obtain a hydroxyl-terminated star-shaped eight-arm methyl silicone oil with a molecular weight of about 200,000 and a room temperature viscosity of less than 10 PaS.

Embodiment 2

[0026] 1.136g (0.17%) of anhydrous tetramethylammonium octaoxide POSS was dissolved in 10mL of ethanol (or 10mL of xylene), and then mixed with 236.8g (35.18%) of octamethylcyclotetrasiloxane and 435.2g (64.65%) Mix tetramethyltetraphenylcyclotetrasiloxane, put it in a 1000mL three-neck bottle, remove ethanol under reduced pressure, and react at 85°C, magnetic stirring at 1000rpm, under argon protection for 36 hours, and heat up to 150°C after the reaction After cooling for one hour, the hydroxyl-terminated star-shaped eight-arm methyl phenyl silicone oil is obtained, with a molecular weight of about 600,000 and a room temperature viscosity of less than 20 PaS.

Embodiment 3

[0028] 1.136g (1.25%) anhydrous tetramethylammonium octaoxide POSS with 88.8g (97.33%) hexamethylcyclotrisiloxane and 1.296g (1.42%) hexamethyldisiloxane (MM), placed in 250mL In a three-necked bottle, react for 48 hours at 75°C, magnetically stirred at 500rpm, and protected by high-purity nitrogen. After the reaction, the temperature is raised to 140°C for half an hour. After cooling down, methyl-terminated star-shaped eight-arm methyl silicone oil is obtained, with a molecular weight of 10. About 10,000, the room temperature viscosity is less than 10PaS.

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Abstract

The invention discloses a preparing method of star type multi-armed silicon oil, which comprises the following steps: allocating 0.01-50.90% oxygenate four methylamine group cage model eight poly double half siloxane,16.90-99.99% ring type siloxane low-molecular polymer and 0-65.50% terminated agent with mass percent; controlling temperature at 20-130 deg.c; stirring under protection of air and inert gas; reacting at 10 min-48 h; rising temperature to 135-200 deg.c; disintegrating and removing oxygenate four methylamine group; getting end product.

Description

technical field [0001] The invention relates to a preparation method of silicone oil, in particular to a preparation method of star multi-arm silicone oil. Background technique [0002] Cage silsesquioxane (Polydehral Oligomer Silsesquioxane, POSS) is a typical organic-inorganic nano-hybrid structural unit, and also a class of nano-modifiers for polymer materials with excellent properties. Tetramethylammonium octaoxide POSS is a class of cage silsesquioxanes (Ronald H.Baney, MakiItoh, Akihito Sakakibara, Toshio Suzukit, Chem.Rev.1995,95,1409-1430; Yuan Changyou, Hu Haruno organosilicon material, 2001, 15(2): 1), which has high yield and good chemical activity, which is beneficial to industrial production. [0003] At the same time, silicone oil has a wide range of applications due to its excellent performance. It is not only used as a special material in aviation, cutting-edge technology, and military technology departments, but also in various sectors of the national econ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38
Inventor 贾叙东袭锴何辉葛仁杰余学海
Owner NANJING UNIV
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