CN108641337A - A kind of polyphenylene ether-poly siloxanes photo-crosslinking damping material and preparation method thereof - Google Patents
A kind of polyphenylene ether-poly siloxanes photo-crosslinking damping material and preparation method thereof Download PDFInfo
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- CN108641337A CN108641337A CN201810476010.0A CN201810476010A CN108641337A CN 108641337 A CN108641337 A CN 108641337A CN 201810476010 A CN201810476010 A CN 201810476010A CN 108641337 A CN108641337 A CN 108641337A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/48—Polymers modified by chemical after-treatment
- C08G65/485—Polyphenylene oxides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J3/28—Treatment by wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2371/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
- C08J2371/12—Polyphenylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The present invention relates to a kind of polyphenylene oxide polysiloxanes photo-crosslinking damping materials and preparation method thereof.Include the following steps, under the action of radical initiator and N bromo-succinimides, bromo-reaction occurs for the methyl on polyphenylene oxide phenyl ring, obtains brominated polyphenylether.The brominated polyphenylether is reacted with allylic bromination magnesium, obtains the polyphenylene oxide of allylation.Suitable photoinitiator and multi-thiol is added into the allyl-polyphenylene ether vinyl polysiloxane solution prepared by a certain percentage, the crosslinking curing under ultra violet lamp, after drying, you can obtain polyphenylene oxide polysiloxanes photo-crosslinking damping material.Compared with prior art, polyphenylene oxide polysiloxanes damping material disclosed by the invention has the characteristics that high temperature resistant, wide temperature range, and the temperature range of displaying damping capacity is 143~223 DEG C, and effective damping temperature range is up to 75 DEG C.In addition, using the preparation method of photo-crosslinking, industrial rapid production and energy-efficient basic demand are met.
Description
Technical field
The present invention relates to a kind of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragms and preparation method thereof, belong to macromolecule material
Material field.
Technical background
With the getting worse of noise pollution and bad vibration problem, there is the higher losses factor（tanδ）Macromolecule resistance
Damping material is used widely in industries such as aerospace, automobile and buildings, more becomes the sophisticated industries such as bullet train, aircraft
Field there is an urgent need for critical material.But there is poor heat resistance in polymer damping material.In particular, when bullet train and
When aircraft high-speed cruising, violent vibration is will produce, and body temperature is in higher temperature range, therefore, urgently
Need one kind under the conditions of higher temperatures（>140℃）Show damping capacity, and effective damping temperature range（tanδ>=0.3 humidity province
Between）It is wide（≥60℃）Damping material.
Currently, polymer damping material is broadly divided into rubber, polyurethane and epoxy resin three categories.Wherein, ENREF9 rubbers
Glue and polyurethanes damping material are not met respectively often in 0 DEG C or less and 0~90 DEG C displaying high damping properties in higher temperatures condition
Under（>140℃）The requirement of lower display damping capacity.Most of epoxy resin show the temperature of damping capacity also below 140 DEG C, now
There is technology by the way that by ceramic filler to epoxy resin, it is expected to show damping capacity in high temperature range, but piezoelectricity is made pottery
The content of porcelain is up to 38wt% and 44wt% respectively, deteriorates the craftsmanship of resin, in addition, the solidification temperature of this epoxy resin is high
（150℃）, the time it is long（7h）, do not have commercial viability.Therefore, existing polymer damping material cannot have both good technique
Property, high temperature resistant and wide temperature range performance.
Photo-crosslinking has the advantages that energy-efficient, and Preliminary Applications is achieved in damping material.Currently, photo-crosslinking damps
Material is broadly divided into polyurethanes, esters of acrylic acid, mercaptan-alkene hydrocarbon system etc., but these photo-crosslinking damping materials cannot have both
High-fire resistance and wide temperature range characteristic.
In conclusion using fast energy-saving method, develop high temperature resistant, damping material with wide-temperature range be still one it is huge and have
The challenge of practical value.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of silicone cross-linked damping material of polyphenylene ether-poly and its preparations
Method.
The present invention adopts the following technical scheme that：
A kind of preparation method of polyphenylene ether-poly siloxanes photo-crosslinking material, includes the following steps：
（1）Under nitrogen, benzoyl peroxide, N- bromo-succinimides are added in the aromatic hydrocarbon solvent containing polyphenylene oxide, returned
Brominated polyphenylether is obtained by the reaction in stream；
（2）Under nitrogen, at 0~60 DEG C, allylic bromination magnesium is added dropwise in the tetrahydrofuran containing brominated polyphenylether, is reacted
Obtain allylation polyphenylene oxide；
（3）Allylation polyphenylene oxide, polysiloxanes, multi-thiol, photoinitiator are added in tetrahydrofuran, polyphenylene oxide-is obtained
Polysiloxanes photo-crosslinking system；Polyphenylene ether-poly siloxanes photo-crosslinking system is reacted by ultraviolet lighting, obtains polyphenylene ether-poly silicon
Oxygen alkane photo-crosslinking material.
A kind of preparation method of polyphenylene ether-poly siloxanes photo-crosslinking system, includes the following steps：
（1）Under nitrogen, benzoyl peroxide, N- bromo-succinimides are added in the aromatic hydrocarbon solvent containing polyphenylene oxide, returned
Brominated polyphenylether is obtained by the reaction in stream；
（2）Under nitrogen, at 0~60 DEG C, allylic bromination magnesium is added dropwise in the tetrahydrofuran containing brominated polyphenylether, is reacted
Obtain allylation polyphenylene oxide；
（3）Allylation polyphenylene oxide, polysiloxanes, multi-thiol, photoinitiator are added in tetrahydrofuran, polyphenylene oxide-is obtained
Polysiloxanes photo-crosslinking system.
A kind of preparation method of allylation polyphenylene oxide, includes the following steps：
（1）Under nitrogen, benzoyl peroxide, N- bromo-succinimides are added in the aromatic hydrocarbon solvent containing polyphenylene oxide, returned
Brominated polyphenylether is obtained by the reaction in stream；
（2）Under nitrogen, at 0~60 DEG C, allylic bromination magnesium is added dropwise in the tetrahydrofuran containing brominated polyphenylether, is reacted
Obtain allylation polyphenylene oxide.
In above-mentioned technical proposal, the aromatic hydrocarbon solvent is toluene, one kind in chlorobenzene or their arbitrary combination；
The multi-thiol is trimethylolpropane tris（3-thiopropionate）, pentaerythrite four（3- mercaptopropionic acids）Ester and containing plural number
One kind in the polymer of a thiol group or their arbitrary combination；The photoinitiator is（2,4,6- trimethylbenzene first
Acyl group）Diphenyl phosphine oxide, N, N- dimethyl -4- pyridines amine, one kind in benzoin dimethylether or their arbitrary group
It closes；The polysiloxane structure formula is as follows：
Wherein R1For one kind in vinyl, methyl and hydroxyl, R2For one kind in methyl, vinyl and trifluoro propyl methyl.
Preferably, the number-average molecular weight of the polysiloxanes is 5000~50000, and containing there are two and it is more than two
Unsaturated carbon carbon bond, wherein 65≤m+n≤650；It is described it is a plurality of be 3 and 3 or more.
In above-mentioned technical proposal, step（1）In, benzoyl peroxide, N- bromo-succinimides, polyphenylene oxide mass ratio
For（5~15）∶（25~80）: 100, the time of back flow reaction is 1~6h；
Step（2）In, allylic bromination magnesium, brominated polyphenylether mass ratio be（5~40）: 100, the time of reaction is 1~6h；
Step（3）In, allylation polyphenylene oxide, polysiloxanes, multi-thiol, photoinitiator mass ratio be 100:（5~70）∶
（10~20）∶（2~5）, the wavelength of ultraviolet lighting reaction is 365 nanometers, and the time is 2~8 minutes.
The invention also discloses polyphenylene ether-polies prepared by the preparation method of above-mentioned polyphenylene ether-poly siloxanes photo-crosslinking material
Siloxanes photo-crosslinking material；And polyphenylene ether-poly silica prepared by the preparation method of upper polyphenylene ether-poly siloxanes photo-crosslinking system
Alkane photo-crosslinking system；Or allylation polyphenylene oxide prepared by the preparation method of above-mentioned allylation polyphenylene oxide.It also discloses
Allylation polyphenylene oxide or polyphenylene ether-poly siloxanes photo-crosslinked structure, which tie up to, to be prepared in polyphenylene ether-poly siloxanes photo-crosslinking material
Application.
The preparation method of polyphenylene ether-poly siloxanes photo-crosslinking material disclosed by the invention can carry out according to the following steps：
By mass,
（1）Under the conditions of nitrogen protection, 100 parts of polyphenylene oxide are dissolved in 1000~2000 parts of aromatic hydrocarbon solvents, then successively
5~15 parts of benzoyl peroxides and 25~80 parts of N- bromo-succinimides are added；1~6h of heating reflux reaction；It is molten with alcohols
Product is precipitated in agent, and washing after filtering, drying, obtains brominated polyphenylether.
（2）In temperature for 0~60 DEG C and under the conditions of nitrogen protection, by 100 parts of steps（1）Obtained brominated polyphenylether is molten
Solution is in 5000 parts of tetrahydrofurans；Then, 5~40 parts of allylic bromination magnesium are added dropwise；It is anti-at 0~60 DEG C after dripping
Answer 1~6h；Product is precipitated with alcohols solvent, washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）By step（3）100 parts of allyl-polyphenylene ethers obtained, 5~70 parts of polysiloxanes, 10~20 parts of multi-thiols
It is dissolved in 5000 parts of tetrahydrofurans with 2~5 parts of photoinitiators, obtains solution A.
（4）By solution A, levelling takes out sample in the case where wavelength is the ultraviolet lamp of 365nm after 2~8min of irradiation on carrier,
It is film to get to polyphenylene ether-poly siloxanes photo-crosslinking material after fully dry.
The alcohols solvent is methanol, ethyl alcohol, normal propyl alcohol, isopropanol, one kind in n-butanol or theirs is arbitrary
Combination；The carrier should be unable to polyphenylene ether-poly siloxanes photo-crosslinking film blocking, such as Haloport F, glass
Carrier or aluminum alloy support.
The effective damping temperature Centralized of polyphenylene ether-poly siloxanes photo-crosslinking damping material prepared by the present invention is 143~223
DEG C, and 60 DEG C of the equal ＞ of its effective damping temperature range, it is a kind of damping material that can show wide temperature range characteristic at high temperature；Meanwhile
Polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm disclosed by the invention uses the preparation process of optical cross-linking method, has efficiently section
The characteristics of energy, solve technological problems when common high temperature resistant damping material consumption energy consumption.As can be seen that light prepared by the present invention is handed over
Connection damping material has both energy-efficient technique, wide temperature range damping property and excellent high temperature resistance.
Compared with prior art, the advantageous effect that the present invention obtains is：
1. polyphenylene ether-poly siloxanes photo-crosslinking damping material prepared by the present invention is in hot conditions（143~223 DEG C）Under have
Excellent damping capacity, effective damping temperature range are above 60 DEG C, up to 75 DEG C, to for its in aerospace, military affairs, height
It is applied in the fields such as fast train and provides reliable basis.These excellent performances mainly have benefited from polyphenylene ether-poly siloxanes light
Cross-linked material has suitable phase degree of scatter, unique photo-crosslinking network structure and the higher glass transition of polyphenylene oxide itself
Temperature.
2. polyphenylene ether-poly siloxanes photo-crosslinking damping material prepared by the present invention has high-damping efficiency, fissipation factor
0.8 or so.This, which is primarily due to poly- fluorosilicone, has larger polarity side group, can increase the in-fighting of material；In addition, Gao Rou
The addition of the poly- fluorosilicone strand of property can improve the molecular chain movement ability of photo-crosslinking film, make material by external force
When can convert more mechanical energy to interior energy and consume.
3. polyphenylene ether-poly siloxanes photo-crosslinking damping material prepared by the present invention has good heat resistance, vitrifying
Transition temperature concentrates on 190~200 DEG C, initial pyrolyzation temperature（The temperature of mass loss 5wt%）Up to 250 DEG C（Nitrogen gas
Atmosphere, heating rate are 10 DEG C/min）.This is mainly due to the cross-linked network structure of photo-crosslinking material and polyphenylene oxide and poly- silicon
The excellent heat resistance of oxygen alkane itself.
4. polyphenylene ether-poly siloxanes photo-crosslinking damping material prepared by the present invention uses the preparation process of photo-crosslinking, tool
Have the characteristics that energy-efficient, and reaction condition is mild, easily controllable and realize, is convenient for industrialized production.
Description of the drawings
Fig. 1 is the synthetic reaction formula of allyl-polyphenylene ether prepared by the embodiment of the present invention 1；
Fig. 2 is the nuclear magnetic resonance spectroscopy of allyl-polyphenylene ether prepared by the embodiment of the present invention 1（1H-NMR）；
Fig. 3 is that the Fourier of allyl-polyphenylene ether prepared by the embodiment of the present invention 1 is infrared（FTIR）Spectrogram；
Fig. 4 is polyphenyl prepared by polyphenylene ether-poly siloxanes photo-crosslinking film, comparative example 1 prepared by the embodiment of the present invention 1,2 and 3
Fissipation factor-temperature curve of polyphenylene ether-poly siloxanes photo-crosslinking film prepared by ether photo-crosslinking film and comparative example 2（Dynamically
Mechanical analysis DMA tests to obtain）；
Fig. 5 is polyphenyl prepared by polyphenylene ether-poly siloxanes photo-crosslinking film, comparative example 1 prepared by the embodiment of the present invention 1,2 and 3
The thermogravimetric analysis of polyphenylene ether-poly siloxanes photo-crosslinking film prepared by ether photo-crosslinking film and comparative example 2（TGA）Curve（Nitrogen
Atmosphere, heating rate are 10 DEG C/min）.
Specific implementation mode
Below in conjunction with the accompanying drawings, embodiment and comparative example, technical solution of the present invention will be further described.
Embodiment 1
（1）The preparation of brominated polyphenylether
Referring to attached drawing 1, it is the synthetic reaction formula of allyl-polyphenylene ether of the present invention.In the present embodiment, specific method is：In nitrogen
Under the conditions of gas shielded, 10g polyphenylene oxide is dissolved in 100mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides and 4g N- bromines
For succimide, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains brominated polyphenylene
Ether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.Its nuclear magnetic resonance spectroscopy（1H-NMR）In Fu
Leaf is infrared（FTIR）Collection of illustrative plates is shown in attached drawing 2 and attached drawing 3 respectively.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.95g allylations polyphenylene oxide, 0.05g vinyl trifluompropyl methyl polysiloxane, 0.12g trimethylolpropane tris
（3-thiopropionate）And 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans,
Obtain solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.Its fissipation factor-temperature curve（Dynamic mechanical
Analysis DMA tests to obtain）And thermogravimetric analysis（TGA）Curve is shown in attached drawing 4 and attached drawing 5 respectively.
Referring to attached drawing 2, it is the nuclear magnetic resonance spectroscopy of allyl-polyphenylene ether prepared by embodiment 1（1H-NMR）.It can by figure
Know, at c（δ=4.9ppm）At d（δ=5.7ppm）Peak be-CH2-CH=CH2The formant of middle double bond hydrogen atom, shows allyl
Base polyphenylene oxide successfully synthesizes.In addition, according to1In H-NMR on double bond and phenyl ring methyl the ratio between proton peak integral area, can obtain
To the grafting rate of allyl-polyphenylene ether.The allyl grafting rate that polyphenylene oxide is obtained after being computed is 10.6%, i.e. y: z = 197 :
58。
Referring to attached drawing 3, it be allyl-polyphenylene ether prepared by embodiment 1 Fourier it is infrared（FTIR）Collection of illustrative plates.It can by figure
Know, in 913cm-1Occur the out-of-plane bending vibration peak of allyl at wavelength, also indicates that polyphenylene oxide success allylation.
Embodiment 2
Allylation polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.12g tri- prepared by 0.9g embodiments 1
Hydroxymethyl-propane three（3-thiopropionate）And 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL
In tetrahydrofuran, solution A is obtained.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.Its fissipation factor-temperature curve（Dynamic mechanical
Analysis DMA tests to obtain）And thermogravimetric analysis（TGA）Curve is shown in attached drawing 4 and attached drawing 5 respectively.
Embodiment 3
Allylation polyphenylene oxide, 0.15g vinyl trifluompropyl methyl polysiloxane, 0.11g prepared by 0.85g embodiments 1
Trimethylolpropane tris（3-thiopropionate）And 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in
In 50mL tetrahydrofurans, solution A is obtained.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.Its fissipation factor-temperature curve（Dynamic mechanical
Analysis DMA tests to obtain）And thermogravimetric analysis（TGA）Curve is shown in attached drawing 4 and attached drawing 5 respectively.
The preparation of 1 polyphenylene oxide photo-crosslinking film of comparative example
Allyl-polyphenylene ether, 0.13g trimethylolpropane tris prepared by 1g embodiments 1（3-thiopropionate）And 0.03g（2,
4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 45mL tetrahydrofurans, obtains solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene oxide photo-crosslinking film.Its fissipation factor-temperature curve（Dynamic mechanical analysis DMA is surveyed
Examination obtains）And thermogravimetric analysis（TGA）Curve is shown in attached drawing 4 and attached drawing 5 respectively.
2 polyphenylene ether-poly siloxanes photo-crosslinking film of comparative example
Allylation polyphenylene oxide, 0.5g vinyl trifluompropyl methyl polysiloxane, 0.08g tri- prepared by 0.5g embodiments 1
Hydroxymethyl-propane three（3-thiopropionate）And 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL
In tetrahydrofuran, solution A is obtained.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.Its fissipation factor-temperature curve（Dynamic mechanical
Analysis DMA tests to obtain）And thermogravimetric analysis（TGA）Curve is shown in attached drawing 4 and attached drawing 5 respectively.
Referring to attached drawing 4, it is the polyphenylene ether-poly siloxanes photo-crosslinking film of the preparation of the embodiment of the present invention 1,2 and 3, compares
The fissipation factor-of polyphenylene ether-poly siloxanes photo-crosslinking film prepared by polyphenylene oxide photo-crosslinking film and comparative example 2 prepared by example 1
Temperature curve（Dynamic mechanical analysis DMA tests to obtain）.As seen from the figure, the polyphenylene oxide photo-crosslinking film and ratio that prepared by comparative example 1
Effective damping temperature range compared with the polyphenylene ether-poly siloxanes photo-crosslinking film of the preparation of example 2 is respectively 51 DEG C（166~218 DEG C）With 49
℃（156~205 DEG C）, the requirement of not up to wide temperature range（60 DEG C of ＞）.In contrast, polyphenyl prepared by embodiment 1,2 and 3
The effective damping temperature range of ether-polysiloxanes photo-crosslinking film is respectively 62 DEG C（153~213 DEG C）、75℃（142~217 DEG C）With
65℃（158~223 DEG C）, meet the requirement of wide temperature range.On the other hand, comparative example 1 prepare polyphenylene oxide photo-crosslinking film and
The fissipation factor of polyphenylene ether-poly siloxanes photo-crosslinking film prepared by comparative example 2 is respectively 0.60 and 0.54, and embodiment 1,2
The fissipation factor of the polyphenylene ether-poly siloxanes photo-crosslinking film prepared with 3 is respectively 0.80,0.78 and 0.77, illustrates limited amount
The presence of poly- fluorosilicone can be obviously improved the damping capacity of polyphenylene oxide photo-crosslinking film.In addition, prepared by embodiment 1,2 and 3
Polyphenylene ether-poly siloxanes photo-crosslinking film effective damping temperature Centralized in 143~223 DEG C of high temperature range.To sum up institute
It states, polyphenylene ether-poly siloxanes photo-crosslinking film prepared by embodiment 1,2 and 3 meets the requirement of high temperature resistant and wide temperature range simultaneously.
Referring to attached drawing 5, it is prepared by polyphenylene ether-poly siloxanes photo-crosslinking film, comparative example 1 prepared by embodiment 1,2 and 3
Polyphenylene oxide photo-crosslinking film and comparative example 2 prepare polyphenylene ether-poly siloxanes photo-crosslinking film thermal weight loss（TGA）Curve.
As can be seen that the initial pyrolyzation temperature of comparative example 1（The temperature of mass loss 5wt%）It is 213 DEG C；It is prepared by embodiment 1,2 and 3
Polyphenylene ether-poly siloxanes photo-crosslinking film and comparative example 2 prepare polyphenylene ether-poly siloxanes photo-crosslinking film it is initial heat point
It is respectively 232 DEG C, 236 DEG C, 249 DEG C and 253 DEG C to solve temperature, illustrates that the addition of poly- fluorosilicone can be obviously improved polyphenylene oxide light
The thermal stability of cured film.
Embodiment 4
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in the in the mixed solvent of 50mL chlorobenzenes and 50ml toluene, then successively
1g benzoyl peroxides and 4g N- bromo-succinimides, heating reflux reaction 1.5h is added；Product is precipitated with ethyl alcohol, washs,
After filtering, drying, brominated polyphenylether is obtained.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
3.4mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；With
Product is precipitated in ethyl alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.95g allylations polyphenylene oxide, 0.05g vinyl trifluompropyl methyl polysiloxane, 0.12g trimethylolpropane tris
（3-thiopropionate）And 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans,
Obtain solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film, 63 DEG C of effective damping temperature range is that one kind can be
The damping material of wide temperature range characteristic is shown under high temperature.
Embodiment 5
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with the ethanol solution containing 50% methanol, washs, warp
After filtering, drying, brominated polyphenylether is obtained.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
27.6mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；With
Product is precipitated in ethanol solution containing 50% methanol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.95g allylations polyphenylene oxide, 0.05g vinyl trifluompropyl methyl polysiloxane, 0.12g trimethylolpropane tris
（3-thiopropionate）And 0.04g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans,
Obtain solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 2min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film, 62 DEG C of effective damping temperature range is that one kind can be
The damping material of wide temperature range characteristic is shown under high temperature.
Embodiment 6
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 200mL chlorobenzenes, then sequentially adds 1.5g benzoyl peroxide first
Acyl and 2.5g N- bromo-succinimides, heating reflux reaction 6h；Product is precipitated with isopropanol, washs, after filtering, drying,
Obtain brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；With different
Product is precipitated in propyl alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.95g allylations polyphenylene oxide, 0.05g vinyl trifluompropyl methyl polysiloxane, 0.06g trimethylolpropane tris
（3-thiopropionate）, 0.06g pentaerythrites four（3- mercaptopropionic acids）Ester and 0.02g（2,4,6- trimethylbenzoyls）Hexichol
Base phosphine oxide is dissolved in 50mL tetrahydrofurans, obtains solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film, 68 DEG C of effective damping temperature range is that one kind can be
The damping material of wide temperature range characteristic is shown under high temperature.
Embodiment 7
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 100mL toluene, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 60 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 1h at 60 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.95g allylations polyphenylene oxide, 0.05g vinyl trifluompropyl methyl polysiloxane, 0.19g pentaerythrites four（3-
Mercaptopropionic acid）Ester and 0.03g N, N- dimethyl -4- pyridines amine solvents obtain solution A in 50mL tetrahydrofurans.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film, 65 DEG C of effective damping temperature range is that one kind can be
The damping material of wide temperature range characteristic is shown under high temperature.
Embodiment 8
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 100mL chlorobenzenes, then sequentially adds 0.5g benzoyl peroxide first
Acyl and 8g N- bromo-succinimides, heating reflux reaction 1h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.95g allylations polyphenylene oxide, poly- two methyl siloxane of 0.05g vinyl, 0.05g pentaerythrites four（3- sulfydryls
Propionic acid）Ester and 0.03g benzoin dimethylethers are dissolved in 50mL tetrahydrofurans, obtain solution A.
By solution A, levelling takes out sample in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 8min on aluminum alloy support,
Fully to get to polyphenylene ether-poly siloxanes photo-crosslinking film after drying, 64 DEG C of effective damping temperature range is that one kind can be in high temperature
The damping material of the lower wide temperature range characteristic of displaying.
Embodiment 9
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
Be 0 DEG C and under the conditions of nitrogen protection in temperature, 10g brominated polyphenylethers be dissolved in 500mL tetrahydrofurans, then to its
In 20mL allylic bromination magnesium tetrahydrofuran solutions are added dropwise（1mol/L）, after dripping, react 6h at 0 DEG C；Use methanol
Product is precipitated, washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.95g allylations polyphenylene oxide, 0.05g vinyldimethicones, 0.13g pentaerythrites four（3- sulfydryls third
Acid）Ester and 0.02g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide and 0.01g benzoin dimethylethers are dissolved in 50mL tetra-
In hydrogen furans, solution A is obtained.
By solution A, levelling takes out sample, fills in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 2min on glass carrier
To get to polyphenylene ether-poly siloxanes photo-crosslinking film after point dry.
Embodiment 10
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 100mL chlorobenzenes, then sequentially adds 0.5g benzoyl peroxide first
Acyl and 2.5g N- bromo-succinimides, heating reflux reaction 6h；Product is precipitated with ethyl alcohol, washing after filtering, drying, obtains
To brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 60 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
3.4mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 1h at 60 DEG C；With
Product is precipitated in ethyl alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm（Mercaptan）
By 0.9g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.09g trimethylolpropane tris
（3-thiopropionate）And 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans,
Obtain solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 11
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 200mL chlorobenzenes, then sequentially adds 1.5g benzoyl peroxide first
Acyl and 8g N- bromo-succinimides, heating reflux reaction 1h；Product is precipitated with isopropanol, washing after filtering, drying, obtains
To brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 60 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
27.6mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 1h at 60 DEG C；With
Product is precipitated in isopropanol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.18g trimethylolpropane tris
（3-thiopropionate）And 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans,
Obtain solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 12
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL toluene, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.13g pentaerythrites four（3- mercaptos
Base propionic acid）Ester and 0.04g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, is obtained molten
Liquid A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 13
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 0.5g benzoyl peroxide first
Acyl and 2.5g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with ethyl alcohol, washs, after filtering, drying,
Obtain brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 60 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
3.4mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 1h at 60 DEG C；With
Product is precipitated in ethyl alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.90g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.09g pentaerythrites four（3- mercaptos
Base propionic acid）Ester and 0.02g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, is obtained molten
Liquid A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 14
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1.5g benzoyl peroxide first
Acyl and 8g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with isopropanol, washs, after filtering, drying,
Obtain brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 60 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
27.6mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 1h at 60 DEG C；With
Product is precipitated in isopropanol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.18g pentaerythrites four（3- mercaptos
Base propionic acid）Ester and 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, is obtained molten
Liquid A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 15
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
Be 0 DEG C and under the conditions of nitrogen protection in temperature, 10g brominated polyphenylethers be dissolved in 500mL tetrahydrofurans, then to its
In 20mL allylic bromination magnesium tetrahydrofuran solutions are added dropwise（1mol/L）, after dripping, react 6h at 0 DEG C；Use methanol
Product is precipitated, washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.13g season pentaerythrites four（3-
Mercaptopropionic acid）Ester and 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, is obtained
Solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 8min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 16
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 6h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyldimethicones, 0.13g season pentaerythrites four（3- sulfydryls third
Acid）Ester and 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, obtains solution A.
By solution A, levelling takes out sample, fills in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 8min on glass carrier
To get to polyphenylene ether-poly siloxanes photo-crosslinking film after point dry.
Embodiment 17
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 6h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyldimethicones, 0.13g season pentaerythrites four（3- sulfydryls third
Acid）Ester and 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, obtains solution A.
By solution A, levelling takes out sample in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 8min on aluminum alloy support,
To get to polyphenylene ether-poly siloxanes photo-crosslinking film after fully dry.
Embodiment 18
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL toluene, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.13g pentaerythrites four（3- mercaptos
Base propionic acid）Ester and 0.03g N, N- dimethyl -4- pyridines amine solvents obtain solution A in 50mL tetrahydrofurans.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 19
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL toluene, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.13g pentaerythrites four（3- mercaptos
Base propionic acid）Ester and 0.03g benzoin dimethylethers are dissolved in 50mL tetrahydrofurans, obtain solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 20
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL toluene, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.9g allylations polyphenylene oxide, 0.1g vinyl trifluompropyl methyl polysiloxane, 0.13g pentaerythrites four（3- mercaptos
Base propionic acid）Ester, 0.02g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide and 0.01g benzoin dimethylethers are dissolved in
In 50mL tetrahydrofurans, solution A is obtained.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 21
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in the in the mixed solvent of 50mL chlorobenzenes and 50ml toluene, then successively
1g benzoyl peroxides and 4g N- bromo-succinimides, heating reflux reaction 1.5h is added；Product is precipitated with ethyl alcohol, washs,
After filtering, drying, brominated polyphenylether is obtained.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
3.4mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；With
Product is precipitated in ethyl alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.85g allylations polyphenylene oxide, 0.15g vinyl trifluompropyl methyl polysiloxane, 0.11g trimethylolpropane tris
（3-thiopropionate）And 0.03g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans,
Obtain solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film, 69 DEG C of effective damping temperature range is that one kind can be
The damping material of wide temperature range characteristic is shown under high temperature.
Embodiment 22
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with the ethanol solution containing 50% methanol, washs, warp
After filtering, drying, brominated polyphenylether is obtained.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
27.6mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；With
Product is precipitated in ethanol solution containing 50% methanol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.85g allylations polyphenylene oxide, 0.15g vinyldimethicones, 0.11g trimethylolpropane tris（3- mercaptos
Base propionic ester）And 0.04g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, is obtained molten
Liquid A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 2min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 23
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 200mL chlorobenzenes, then sequentially adds 1.5g benzoyl peroxide first
Acyl and 2.5g N- bromo-succinimides, heating reflux reaction 6h；Product is precipitated with isopropanol, washs, after filtering, drying,
Obtain brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；With different
Product is precipitated in propyl alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.85g allylations polyphenylene oxide, 0.15g vinyldimethicones, 0.06g trimethylolpropane tris（3- mercaptos
Base propionic ester）, 0.06g pentaerythrites four（3- mercaptopropionic acids）Ester and 0.02g（2,4,6- trimethylbenzoyls）Dipheny oxide
Change phosphine to be dissolved in 50mL tetrahydrofurans, obtains solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 24
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 100mL toluene, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 60 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 1h at 60 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.85g allylations polyphenylene oxide, 0.15g vinyl trifluompropyl methyl polysiloxane, 0.17g pentaerythrites four（3-
Mercaptopropionic acid）Ester and 0.03g N, N- dimethyl -4- pyridines amine solvents obtain solution A in 50mL tetrahydrofurans.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 25
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 100mL chlorobenzenes, then sequentially adds 0.5g benzoyl peroxide first
Acyl and 8g N- bromo-succinimides, heating reflux reaction 1h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.85g allylations polyphenylene oxide, 0.15g vinyl trifluompropyl methyl polysiloxane, 0.04g pentaerythrites four（3-
Mercaptopropionic acid）Ester and 0.03g benzoin dimethylethers are dissolved in 50mL tetrahydrofurans, obtain solution A.
By solution A, levelling takes out sample in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 8min on aluminum alloy support,
Fully to get to polyphenylene ether-poly siloxanes photo-crosslinking film after drying, 70 DEG C of effective damping temperature range is that one kind can be in high temperature
The damping material of the lower wide temperature range characteristic of displaying.
Embodiment 26
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
Be 0 DEG C and under the conditions of nitrogen protection in temperature, 10g brominated polyphenylethers be dissolved in 500mL tetrahydrofurans, then to its
In 20mL allylic bromination magnesium tetrahydrofuran solutions are added dropwise（1mol/L）, after dripping, react 6h at 0 DEG C；Use methanol
Product is precipitated, washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 0.85g allylations polyphenylene oxide, 0.15g vinyl trifluompropyl methyl polysiloxane, 0.12g pentaerythrites four（3-
Mercaptopropionic acid）Ester and 0.02g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide and 0.01g benzoin dimethylethers are dissolved in
In 50mL tetrahydrofurans, solution A is obtained.
By solution A, levelling takes out sample, fills in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 2min on glass carrier
To get to polyphenylene ether-poly siloxanes photo-crosslinking film after point dry.
Embodiment 27
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 1g allylations polyphenylene oxide, 0.7g vinyl trifluompropyl methyl polysiloxane, 0.15g pentaerythrites four（3- sulfydryls
Propionic acid）Ester and 0.02g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, obtains solution
A。
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 28
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 100mL toluene, then sequentially adds 0.5g benzoyl peroxide first
Acyl and 8g N- bromo-succinimides, heating reflux reaction 1h；Product is precipitated with ethyl alcohol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
Be 0 DEG C and under the conditions of nitrogen protection in temperature, 10g brominated polyphenylethers be dissolved in 500mL tetrahydrofurans, then to its
In 20mL allylic bromination magnesium tetrahydrofuran solutions are added dropwise（1mol/L）, after dripping, react 6h at 0 DEG C；Use ethyl alcohol
Product is precipitated, washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 1g allylations polyphenylene oxide, 0.7g vinyl trifluompropyl methyl polysiloxane, 0.15g trimethylolpropane tris（3-
Mercaptopropionic acid ester）And 0.05g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, is obtained
Solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 8min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 29
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 125mL chlorobenzenes, then sequentially adds 1g benzoyl peroxides
With 4g N- bromo-succinimides, heating reflux reaction 1.5h；Product is precipitated with methanol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
In temperature for 40 DEG C and under the conditions of nitrogen protection, 10g brominated polyphenylethers are dissolved in 500mL tetrahydrofurans, then to
20mL allylic bromination magnesium tetrahydrofuran solutions are wherein added dropwise（1mol/L）, after dripping, react 3h at 40 DEG C；Use first
Product is precipitated in alcohol, and washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 1g allylations polyphenylene oxide, 0.05g vinyl trifluompropyl methyl polysiloxane, 0.15g pentaerythrites four（3- sulfydryls
Propionic acid）Ester and 0.02g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, obtains solution
A。
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 5min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Embodiment 30
（1）The preparation of brominated polyphenylether
Under the conditions of nitrogen protection, 10g polyphenylene oxide is dissolved in 100mL toluene, then sequentially adds 0.5g benzoyl peroxide first
Acyl and 8g N- bromo-succinimides, heating reflux reaction 1h；Product is precipitated with ethyl alcohol, washing after filtering, drying, obtains
Brominated polyphenylether.
（2）The preparation of allyl-polyphenylene ether
Be 0 DEG C and under the conditions of nitrogen protection in temperature, 10g brominated polyphenylethers be dissolved in 500mL tetrahydrofurans, then to its
In 20mL allylic bromination magnesium tetrahydrofuran solutions are added dropwise（1mol/L）, after dripping, react 6h at 0 DEG C；Use ethyl alcohol
Product is precipitated, washing after filtering, drying, obtains allylation polyphenylene oxide.
（3）The preparation of polyphenylene ether-poly siloxanes photo-crosslinking damping diaphragm
By 1g allylations polyphenylene oxide, 0.05g vinyl trifluompropyl methyl polysiloxane, 0.15g trimethylolpropane tris（3-
Mercaptopropionic acid ester）And 0.05g（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide is dissolved in 50mL tetrahydrofurans, is obtained
Solution A.
By solution A, levelling takes out in the case where wavelength is the ultraviolet lamp of 365nm after irradiation 8min on Haloport F
Sample, it is fully dry after to get to polyphenylene ether-poly siloxanes photo-crosslinking film.
Claims (10)
1. a kind of preparation method of polyphenylene ether-poly siloxanes photo-crosslinking material, which is characterized in that include the following steps：
（1）Under nitrogen, benzoyl peroxide, N- bromo-succinimides are added in the aromatic hydrocarbon solvent containing polyphenylene oxide, returned
Brominated polyphenylether is obtained by the reaction in stream；
（2）Under nitrogen, at 0~60 DEG C, allylic bromination magnesium is added dropwise in the tetrahydrofuran containing brominated polyphenylether, is reacted
Obtain allylation polyphenylene oxide；
（3）Allylation polyphenylene oxide, polysiloxanes, multi-thiol, photoinitiator are added in tetrahydrofuran, polyphenylene oxide-is obtained
Polysiloxanes photo-crosslinking system；Polyphenylene ether-poly siloxanes photo-crosslinking system is reacted by ultraviolet lighting, obtains polyphenylene ether-poly silicon
Oxygen alkane photo-crosslinking material.
2. the preparation method of polyphenylene ether-poly siloxanes photo-crosslinking material according to claim 1, it is characterised in that：The virtue
Fragrant hydrocarbon solvent is toluene, one kind in chlorobenzene or their arbitrary combination；The multi-thiol is trimethylolpropane tris
（3-thiopropionate）, pentaerythrite four（3- mercaptopropionic acids）One kind in ester and polymer containing a plurality of thiol groups,
Or their arbitrary combination；The photoinitiator is（2,4,6- trimethylbenzoyls）Diphenyl phosphine oxide, N, N- diformazans
Base -4- pyridines amine, one kind in benzoin dimethylether or their arbitrary combination；The polysiloxane structure formula is as follows：
Wherein R1For one kind in vinyl, methyl and hydroxyl, R2For one kind in methyl, vinyl and trifluoro propyl methyl.
3. the preparation method of polyphenylene ether-poly siloxanes photo-crosslinking material according to claim 2, it is characterised in that：It is described poly-
The number-average molecular weight of siloxanes 5000~50000, and containing there are two and more than two unsaturated carbon carbon bonds, wherein 65≤
m+n≤650；It is described it is a plurality of be 3 and 3 or more.
4. the preparation method of polyphenylene ether-poly siloxanes photo-crosslinking material according to claim 1, it is characterised in that：
Step（1）In, benzoyl peroxide, N- bromo-succinimides, polyphenylene oxide mass ratio be（5~15）∶（25~80）∶
100, the time of back flow reaction is 1~6h；
Step（2）In, allylic bromination magnesium, brominated polyphenylether mass ratio be（5~40）: 100, the time of reaction is 1~6h；
Step（3）In, allylation polyphenylene oxide, polysiloxanes, multi-thiol, photoinitiator mass ratio be 100:（5~70）∶
（10~20）∶（2~5）, the wavelength of ultraviolet lighting reaction is 365 nanometers, and the time is 2~8 minutes.
5. the polyphenylene ether-poly silica that according to claim 1 prepared by the preparation method of polyphenylene ether-poly siloxanes photo-crosslinking material
Alkane photo-crosslinking material.
6. a kind of preparation method of polyphenylene ether-poly siloxanes photo-crosslinking system, which is characterized in that include the following steps：
（1）Under nitrogen, benzoyl peroxide, N- bromo-succinimides are added in the aromatic hydrocarbon solvent containing polyphenylene oxide, returned
Brominated polyphenylether is obtained by the reaction in stream；
（2）Under nitrogen, at 0~60 DEG C, allylic bromination magnesium is added dropwise in the tetrahydrofuran containing brominated polyphenylether, is reacted
Obtain allylation polyphenylene oxide；
（3）Allylation polyphenylene oxide, polysiloxanes, multi-thiol, photoinitiator are added in tetrahydrofuran, polyphenylene oxide-is obtained
Polysiloxanes photo-crosslinking system.
7. the preparation method of polyphenylene ether-poly siloxanes photo-crosslinking system according to claim 6, it is characterised in that：
Step（1）In, benzoyl peroxide, N- bromo-succinimides, polyphenylene oxide mass ratio be（5~15）∶（25~80）∶
100, the time of back flow reaction is 1~6h；
Step（2）In, allylic bromination magnesium, brominated polyphenylether mass ratio be（5~40）: 100, the time of reaction is 1~6h；
Step（3）In, allylation polyphenylene oxide, polysiloxanes, multi-thiol, photoinitiator mass ratio be 100:（5~70）∶
（10~20）∶（2~5）.
8. a kind of preparation method of allylation polyphenylene oxide, which is characterized in that include the following steps：
（1）Under nitrogen, benzoyl peroxide, N- bromo-succinimides are added in the aromatic hydrocarbon solvent containing polyphenylene oxide, returned
Brominated polyphenylether is obtained by the reaction in stream；
（2）Under nitrogen, at 0~60 DEG C, allylic bromination magnesium is added dropwise in the tetrahydrofuran containing brominated polyphenylether, is reacted
Obtain allylation polyphenylene oxide.
9. the polyphenylene ether-poly silica that according to claim 6 prepared by the preparation method of polyphenylene ether-poly siloxanes photo-crosslinking system
Alkane photo-crosslinking system；Or the allylation polyphenyl that according to claim 8 prepared by the preparation method of allylation polyphenylene oxide
Ether.
10. allylation polyphenylene oxide described in claim 9 or polyphenylene ether-poly siloxanes photo-crosslinked structure tie up to preparation claim
Application in the 5 polyphenylene ether-poly siloxanes photo-crosslinking materials.
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