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A kind of high temperature resistant polysiloxane containing conjugated structure in main chain and preparation method thereof

A technology of conjugated structure and polysiloxane, which is applied in the field of high-temperature-resistant polysiloxane and its preparation, can solve the problems that cannot meet the heat-resistant requirements of silicone rubber, achieve wide application range, improve heat resistance and stability sexual effect

Active Publication Date: 2019-09-27
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using quaternary ammonium alkali silicon alkoxide or quaternary phosphorus alkali silicon alkoxide as catalyst, γ-trifluoropropylmethylcyclotrisiloxane, octamethylcyclotetrasiloxane, 1,3-diphenylboroxine tetra ring as raw material, tetramethyldivinyldisiloxane as end-capping agent, and ring-opening polymerization is carried out to synthesize α, ω-terminal vinyl silicone oil containing boron in the main chain of phenyl fluorocarbon group. The silicone rubber prepared by this method is resistant to The heat temperature reaches 465°C, which cannot meet the heat resistance requirements of silicone rubber under special conditions

Method used

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  • A kind of high temperature resistant polysiloxane containing conjugated structure in main chain and preparation method thereof
  • A kind of high temperature resistant polysiloxane containing conjugated structure in main chain and preparation method thereof
  • A kind of high temperature resistant polysiloxane containing conjugated structure in main chain and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add 1.1 mol of boric acid and 0.5 mol of solvent diethylene glycol dimethyl ether in a beaker, add in a 100 mL four-necked flask after dissolving, then add 1 mol of maleic anhydride dropwise, ventilate nitrogen, and heat up to 120°C, with mechanical stirring at a speed of 450r / min, stirring and reacting for 5h.

[0030] (2) Cool down the reactor to 60° C., add 0.2 mol of hydrochloric acid, then dropwise add 2 mol of dimethyldichlorosilane, and react for 2 hours. Add K2CO3 to adjust the pH value to 6.5, remove the inorganic substance KCl, then add 0.02 mol of hexamethyldisiloxane dropwise for capping, and react for 4 hours. Reduce the pressure until the gauge pressure of the vacuum pump is -0.05MPa, and exclude low boiling substances. A polyborosiloxane containing a conjugated structure is obtained. Its heat resistance reaches 480°C. Take 100 parts of the product and 5 parts of dicumyl peroxide and keep the temperature at 110°C for 3 hours, and the heat resistance...

Embodiment 2

[0032] (1) Add 1.1mol of boric acid in a beaker, 0.5mol of solvent diethylene glycol dimethyl ether, dissolve and add in a 100mL four-necked flask, then add 1mol of fumaryl chloride dropwise, nitrogen, and heat up to 120°C, with mechanical stirring at a speed of 450r / min, stirring and reacting for 5h.

[0033] (2) Cool down the reactor to 60° C., add 0.1 mol of sulfuric acid, then dropwise add 2 mol of dimethyldimethoxysilane, and react for 2 hours. Add K2CO3 to adjust the pH value to 6.5, remove the inorganic substance KCl, then add 0.02 mol of hexamethyldisiloxane dropwise for capping, and react for 4 hours. Reduce the pressure until the gauge pressure of the vacuum pump is -0.05MPa, and exclude low boiling substances. A polyborosiloxane containing a conjugated structure is obtained. Its heat resistance reaches 485°C. Take 100 parts of the product and 5 parts of dicumyl peroxide and keep the temperature at 110°C for 3 hours, and the heat resistance of the prepared silicon...

Embodiment 3

[0035] (1) Add 1.1 mol of phenylboronic acid ester and 0.5 mol of triglyme as a solvent in a beaker, dissolve it and add it to a 100 mL four-neck flask, then add 1 mol of phthalic anhydride dropwise, pass through nitrogen, and Under the atmosphere, the temperature was raised to 120° C., mechanically stirred at a speed of 450 r / min, and stirred for 5 hours.

[0036] (2) Cool down the reactor to 60° C., add 0.1 mol of sulfuric acid, dropwise add 2 mol of dimethyldimethoxysilane, and react for 2 hours. Add K2CO3 to adjust the pH value to 6.5, remove the inorganic substance KCl, then add 0.02 mol of hexamethyldisiloxane dropwise for capping, and react for 4 hours. Reduce the pressure until the gauge pressure of the vacuum pump is -0.05MPa, and exclude low boiling substances. A polyborosiloxane containing a conjugated structure is obtained. Its heat resistance reaches 500°C. Take 100 parts of the product and 5 parts of dicumyl peroxide and keep the temperature at 110°C for 3 hou...

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Abstract

The invention discloses high-temperature-resistant polysiloxane with the main chain containing conjugated structure and a preparation method thereof; the high-temperature-resistant polysiloxane has a structural formula shown in the description, wherein R1 is hydroxyl or aryl and R2 is vinylidene or phenyl, with (x+z):y=2-2.5:1 and x+y+z=500-1200; an unoccupied orbit on boron of the main chain and hydroxyl, vinylidene or phenyl form a hyperconjugated structure. The prepared polysiloxane with the main chain containing conjugated structure can tolerate a temperature of 480 DEG C and above, heat resistance and stability in rubber are greatly improved, and the polysiloxane is applicable to the industries such as building, automobile, aircraft material, and special material, and is more widely applicable.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a high-temperature-resistant polysiloxane whose main chain contains a conjugated structure and a preparation method thereof. Background technique [0002] With the rapid development of modern mechanical equipment, silicone rubber has been widely used in many occasions because of its good elasticity, electrical insulation, thermal conductivity and high and low temperature resistance. At present, in some special occasions, silicone rubber needs to have high temperature resistance, and the general applicable temperature of silicone rubber is between 200-300 ° C, so higher requirements are put forward for the heat resistance of silicone rubber. Polyborosiloxane has good physical and chemical properties. The heat resistance of silicone rubber prepared from polyborosiloxane is greatly improved due to the introduction of boron-oxygen bonds. On the basis of polybo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/42
Inventor 周正发沈宏坤夏洋洋徐卫兵马海红任凤梅
Owner HEFEI UNIV OF TECH