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Polyphenyl ether-polyorganosiloxane photo-crosslinking thin film based on graft copolymer and preparation method of polyphenyl ether-polyorganosiloxane photo-crosslinking thin film

A graft copolymer, polysiloxane optical technology, applied in the field of polyphenylene ether-polysiloxane photo-crosslinked film and its preparation, can solve the problems of high temperature resistance and high loss damping performance in wide temperature range , to achieve the effects of good capacity expansion, high loss performance and excellent damping performance

Active Publication Date: 2018-09-14
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most photo-crosslinked damping materials cannot have good high temperature resistance and wide temperature range, high loss damping performance at the same time.

Method used

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  • Polyphenyl ether-polyorganosiloxane photo-crosslinking thin film based on graft copolymer and preparation method of polyphenyl ether-polyorganosiloxane photo-crosslinking thin film
  • Polyphenyl ether-polyorganosiloxane photo-crosslinking thin film based on graft copolymer and preparation method of polyphenyl ether-polyorganosiloxane photo-crosslinking thin film
  • Polyphenyl ether-polyorganosiloxane photo-crosslinking thin film based on graft copolymer and preparation method of polyphenyl ether-polyorganosiloxane photo-crosslinking thin film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Preparation of allyl polyphenylene ether

[0062] Under the condition of nitrogen protection, dissolve 10g of polyphenylene ether in 100mL of chlorobenzene, then add 1g of benzoyl peroxide and 4g of N-bromosuccinimide in sequence, heat and reflux for 1.5h; precipitate the product with methanol, After washing, filtering and drying, brominated polyphenylene ether was obtained. Dissolve 10g of brominated polyphenylene ether in 500mL of tetrahydrofuran at a temperature of 40°C under nitrogen protection, and then add 20mL of allylmagnesium bromide tetrahydrofuran solution (1mol / L) dropwise to it. After the dropwise addition, React at 40°C for 3 hours; precipitate the product with methanol, wash, filter and dry to obtain allylated polyphenylene ether.

[0063] (2) Preparation of silicon-hydrogen bond-terminated polysiloxane

[0064] Dissolve 5.8mL of trifluoropropylmethylcyclotrisiloxane in 2mL of anhydrous tetrahydrofuran, then add 13.5mL of n-butyllithium solution (1....

Embodiment 2

[0073] The allyl polyphenylene ether prepared in 8.1g embodiment 1, the polyphenylene ether-polysiloxane graft copolymer prepared in 1g embodiment 1, 0.9g vinyl polytrifluoropropyl methylsiloxane , 1.07g of trimethylolpropane tris(3-mercaptopropionate) and 0.27g of (2,4,6-trimethylbenzoyl)diphenylphosphine oxide were dissolved in 500mL of tetrahydrofuran to obtain solution E.

[0074] Level the solution E on the polytetrafluoroethylene carrier, irradiate it under a UV lamp with a wavelength of 365nm for 5 minutes, take out the sample, and dry it fully to obtain a graft copolymer modified polyphenylene ether-polysiloxane photocrosslinker. Linked film. Its thermogravimetric analysis (TGA) curve, loss factor-temperature curve (obtained by dynamic mechanical analysis DMA test) and cold-field scanning electron microscope (SEM) photos of the brittle fracture section are shown in the attached Figure 4 , attached Figure 5 And attached Figure 6 .

Embodiment 3

[0076] The allyl polyphenylene ether prepared in 7.65g embodiment 1, the polyphenylene ether-polysiloxane graft copolymer prepared in 1.5g embodiment 1, 0.85g vinyl polytrifluoropropyl methylsiloxane Alkanes, 1.02 g of trimethylolpropane tris(3-mercaptopropionate) and 0.26 g of (2,4,6-trimethylbenzoyl)diphenylphosphine oxide were dissolved in 500 mL of tetrahydrofuran to obtain solution E.

[0077] Level the solution E on the polytetrafluoroethylene carrier, irradiate it under a UV lamp with a wavelength of 365nm for 5 minutes, take out the sample, and dry it fully to obtain a graft copolymer modified polyphenylene ether-polysiloxane photocrosslinker. Linked film. Its thermogravimetric analysis (TGA) curve, loss factor-temperature curve (obtained by dynamic mechanical analysis DMA test) and cold-field scanning electron microscope (SEM) photos of the brittle fracture section are shown in the attached Figure 4 , attached Figure 5 And attached Figure 6 .

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Abstract

The invention discloses a polyphenyl ether-polyorganosiloxane photo-crosslinking thin film based on a graft copolymer and a preparation method of the polyphenyl ether-polyorganosiloxane photo-crosslinking thin film. The preparation method comprises the following steps: (1) preparing allylated polyphenyl ether; (2) synthesizing silicon-hydrogen bond terminated polysiloxane by taking n-butyllithiumas an initiator and taking chlorodimethylsilane as an end capping agent; (3) carrying out copolymerization on the allylated polyphenyl ether and the silicon-hydrogen bond terminated polysiloxane to prepare a polyphenyl ether-polyorganosiloxane graft copolymer; and (4) blending the polyphenyl ether-polyorganosiloxane graft copolymer with polyphenyl ether and polyorganosiloxane, and carrying out photo-crosslinking to obtain a photo-crosslinking thin film. Compared with the prior art, the polyphenyl ether-polyorganosiloxane photo-crosslinking thin film based on the graft copolymer not only has awide effective damping temperature range, but also has good heat resistance and high loss factors, the damping property is shown in a temperature range from 152 DEG C to 223 DEG C, the effective damping temperature range is greater than 60 DEG C, and the loss factor (tan delta) is greater than or equal to 0.9. In addition, the photo-crosslinking preparation method is adopted, and has the advantages of rapidness, high efficiency and energy conservation.

Description

technical field [0001] The invention relates to a polyphenylene ether-polysiloxane photocrosslinked film based on a graft copolymer and a preparation method thereof, belonging to the field of polymer materials. technical background [0002] With the development of science and technology, the problems of noise and undesirable vibration are becoming more and more serious. Therefore, as a functional material for vibration and noise reduction, polymer damping materials have been widely used in the fields of aerospace, military, ships, automobiles and building materials. In some advanced equipment, such as high-speed trains and aircraft, severe vibrations will occur when the equipment is running at high speed, and the temperature of the fuselage has been in a relatively high and wide temperature range for a long time. However, common polymer materials have poor heat resistance and are difficult to adapt to high-temperature working environments; in addition, polymer materials onl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08J3/24C08L71/12C08L83/12C08L83/07C08G77/46
CPCC08G77/46C08J3/246C08J5/18C08J2371/12C08J2483/04C08J2483/12
Inventor 梁国正申达顾嫒娟袁莉
Owner SUZHOU UNIV
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