CN109293924A - A kind of epoxy modified silicone alkane and its preparation can the cured epoxy modified silicone/epoxide resin material of UV-LED - Google Patents
A kind of epoxy modified silicone alkane and its preparation can the cured epoxy modified silicone/epoxide resin material of UV-LED Download PDFInfo
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- CN109293924A CN109293924A CN201810963046.1A CN201810963046A CN109293924A CN 109293924 A CN109293924 A CN 109293924A CN 201810963046 A CN201810963046 A CN 201810963046A CN 109293924 A CN109293924 A CN 109293924A
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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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/02—Polysilicates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
Abstract
The invention discloses a kind of epoxy modified silicone alkane and its preparation can the cured epoxy modified silicone/epoxide resin material of UV-LED.Epoxy modified silicone alkane resin the preparation method comprises the following steps: ethyl orthosilicate and ethyl alcohol are mixed, hydrochloric acid and water hydrolysis is added, the silane coupling agent for having cycloaliphatic epoxy groups is added, epoxidation modification is up to aliphatic epoxy modified organic silicone resin.The present invention forms silica solution by teos hydrolysis, it is carried out using silane coupling agent epoxy-modified, stable epoxy modified silicone resin system is formed, is solidified using UV-LED light source, the conversion ratio of the epoxy group for the epoxy resin composite material being prepared is 70% or more, surface drying time is only 20 ~ 30s, curing rate is fast, and curing performance is good, 10% of solidification process energy consumption less than traditional UV lamps solidification process energy consumption, economy and the feature of environmental protection are had both, while improving working efficiency.
Description
Technical field
The present invention relates to photo-curing material technical fields, more particularly, to a kind of epoxy modified silicone alkane and its system
Standby can the cured epoxy modified silicone/epoxide resin material of UV-LED.
Background technique
Photo-curing material refers under ultraviolet light, and the monomer in material is made using the ultraviolet light of different wave length and energy
Polymer is aggregated into, to make it dry the material of film forming.With the rapid development of modern industry, photo-curing material also complies with city
Field demand constantly updates formula, and material is made to have more excellent performance.It is constantly promoted with photo-curing material performance and to be matched,
For the light source that photo-curing material uses in the curing process there has also been further requirement, common UV- mercury lamp is a large amount of in addition to generating
Ultraviolet light other than can also generate infrared energy, it is very high so as to cause energy consumption in solidification process.On the other hand, photocuring mistake
A part of light intensity energy consumption in journey can be such that workpiece to be machined temperature increases, and by taking organosilicon/epoxy composite material as an example, solidify
Cheng Zhong, surface temperature are often raised to 60 DEG C or so, can have a great impact when processing some thermally sensitive materials.
To solve the problem above-mentioned, many researchers propose to use UV-LED for solidification work that light source is photo-curing material
Skill provide energy, UV-LED light source have energy conservation and environmental protection, small in size, long service life, low using voltage, switch time is short, puts
The advantages that heat is small can be widely applied to curing field as a kind of novel light source, at present towards higher efficiency of initiation,
The directions such as low pollution, light intensity be more stable are developed.As UV-LED technology is applied in curing field, UV-LED is expected to take
Become the principal light source in Light Curing for UV- mercury lamp.
It is solid to not adding the epoxy modified silicone of photosensitizer or tertiary amine/epoxy composite material to carry out light using UV-LED light source
It when change, tends not to reach relatively good epoxy conversion ratio, or even does not add the modification of the alicyclic epoxy of photosensitizer or tertiary amine organic
Silicone/epoxy composite material, the curing time for needing more to lengthen just are able to achieve solidifying requirements, so to alicyclic epoxy
The research that modified organic silicone resin/epoxy resin composite material is formulated has a very big significance.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the defect of existing organic siliconresin/epoxy resin composite material and not
Foot, reduce UV- mercury lamp to the ultraviolet radioactive of environment and human body, a kind of epoxy modified silicone alkane is provided, by organosilicon into
Row is epoxy-modified, while using UV-LED as light source, and the alicyclic epoxy modified organic silicone resin of preparation is simple and easy to get, uses
It is convenient, it is suitble to industrialized production to use.
The object of the present invention is to provide one kind can the cured epoxy modified silicone/epoxide resin material of UV-LED.
Another object of the present invention is to provide it is a kind of it is above-mentioned can the cured epoxy modified silicone/epoxy resin of UV-LED
The preparation method of material.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of aliphatic epoxy modified organic silicone resin, is prepared by following steps:
S1. ethyl orthosilicate and ethyl alcohol are mixed, are warming up to 50 ~ 60 DEG C, hydrochloric acid and water is added, react 1 ~ 2h, wherein hydrochloric acid with
6 ~ 7:1 of molar ratio of 0.2 ~ 0.3:1 of molar ratio of ethyl orthosilicate, water and ethyl orthosilicate, ethyl alcohol and ethyl orthosilicate mix
Conjunction molar ratio is 5.6 ~ 6.5:1；
S2. the silane coupling agent with epoxy group is added in the reaction product of above-mentioned S1,4 ~ 5h is reacted at 50 ~ 60 DEG C, is removed
Go ethyl alcohol and moisture up to aliphatic epoxy modified organic silicone resin, wherein the molar ratio of silane coupling agent and ethyl orthosilicate is
0.5~1.0:1。
Hydrochloric acid serves as the effect of catalyst in the reaction and water one works and promotes ethyl orthosilicate and silane coupling agent
It is hydrolyzed.
The changes of contents of hydrochloric acid has a certain impact to the stability of alicyclic epoxy modified organic silicone resin.
The variation of water content also has a certain impact to the synthesis of alicyclic epoxy modified organic silicone resin, when system water contains
When measuring less, water cannot be guaranteed that siloxanes hydrolyzes enough, and based on polymerization is polymerize with dealcoholysis, reaction is controlled by hydrolysis, due to steric hindrance
The effect of effect, hydrolytic process are generally easy to carry out in the end of silicon oxygen bond, form linear silicon oxygen by constantly hydrolyzing, polymerizeing
Chain.As water consumption continues growing, the hydrolysis rate of siloxanes increases, this will lead to is basically completed in polymerization initial stage hydrolysis,
Hydrolysate concentration is higher in system, and each siloxane molecule hydrolyzes to form Si-OH key and increases, and polymerize at this time then with de-
Based on water polymerization, reaction tends to multidimensional, forms three-dimensional short-chain structure.When the dosage of water is more than the upper limit, reaction can become more to aggravate
Strong, the micelle of generation is excessive, micelle easily gather into bulky grain even gel, be guarantee colloidal sol seal storage when stability and
The dosage of the performance of cured later film, water should have an Appropriate.
Ethyl alcohol serves as the effect of cosolvent in the reaction system, it has played good dissolution, while its energy to system
It is enclosed in around micelle and forms hydration shell, objectively playing repulsive interaction.With the increase of ethanol content, the stabilization of system
Property is improved to some extent, but the more high hydrolysis that can also inhibit ethyl orthosilicate and silane coupling agent of the content of ethyl alcohol, and
And finally use the ethyl alcohol that removing system is also evaporated under reduced pressure when alicyclic epoxy modified organic silicone resin.
The silica solution of synthesis is carried out in silane coupling agent addition system with epoxy group epoxy-modified.
Preferably, the molar ratio of hydrochloric acid and ethyl orthosilicate is 0.24:1 in S1, and the molar ratio of water and ethyl orthosilicate is
The mixing molar ratio of 6.5:1, ethyl alcohol and ethyl orthosilicate is 6.5:1.
Preferably, the silane coupling agent described in S2 with epoxy group is [2- (7- oxabicyclo [4.1.0] hept- 3- yl)
Ethyl] silane, the molar ratio of silane coupling agent and ethyl orthosilicate is 0.5:1.
[2- (7- oxabicyclo [4.1.0] hept- 3- yl) ethyl] silane A-186(epoxy coupling agents) pairing in addition system
At silica solution carry out it is epoxy-modified, as the stability of the increase system of A-186 is improved to some extent, containing longer
Strand, in methoxyl group and the corresponding alkoxy cohydrolysis in ethyl orthosilicate TEOS molecule of sol-gel process one end
And polycondensation, be bound up on A-186 on micelle in a manner of being chemically bonded, and the organic long-chain of the other end have with decentralized medium it is good
Intermiscibility can be fully extended in decentralized medium, to form stronger steric hindrance, hinder the further coalescence of micelle.Together
When A-186 surface absorbed layer formation can be obviously reduced interparticle Van der Waals force, the stability of system is improved, to extend
Gel time, when A-186 dosage is less, the stability of system is poor, this is because being not enough to when the dosage of coupling agent is very few
Micelle surface is completely covered, but micelle can be adsorbed on macromolecule chain section, so that colloidal sol enhances the sensibility of electrolyte
And become prone to assemble, so that the stability reduction of the system.
Preferably, S1 is incorporated as being added dropwise simultaneously in middle hydrochloric acid and water, and rate of addition is 0.8 ~ 1.0 mL/min.
Preferably, the rate of addition of [2- (7- oxabicyclo [4.1.0] hept- 3- yl) ethyl] silane described in S2 be 0.8 ~
1.5mL/min。
Rate of addition may make very much system reaction speed increase fastly, cause system gel, rate of addition can make very much slowly
System reaction not exclusively, is unable to get more stable product.
A kind of alicyclic epoxy modified organic silicon/epoxy resin composite material, the component including following mass fraction meter: rouge
Epoxy-modified 5 ~ 10 parts of organic siliconresin of ring race；70 ~ 90 parts of epoxy resin；2 ~ 8 parts of cation light initiator；Photosensitizer 1 ~
3 parts；0 ~ 3 part of tertiary amine.
Preferably, the component including following mass fraction meter: 5 ~ 10 parts of organic siliconresin of alicyclic epoxy modification；Epoxy
79 ~ 84 parts of resin；2 ~ 8 parts of cation light initiator；1 ~ 3 part of photosensitizer；2 ~ 3 parts of tertiary amine.
Preferably, 6 ~ 8 parts of cation light initiator.
Preferably, the epoxy resin is bisphenol A diglycidyl ether (BADGE), 3,4- epoxycyclohexyl -3,4 epoxy
The one or more of hexahydrobenzoid acid ester (CE), 1,6 hexanediol diglycidylether (HDDGE).
Preferably, the cation light initiator is Diaryl iodonium hexafluorophosphate, mixed type liquid triaryl hexafluoro
Stibate, 4- (thiophenyl) phenyl diphenyl sulphur hexafluorophosphate, bis- (4,4 '-thioether triphenyl sulphur) hexafluorophosphates, 4-
The one or more of isobutyl phenenyl -4'- aminomethyl phenyl iodine hexafluorophosphate.
Preferably, the photosensitizer is 2- chlorothiaxanthenone (CTX), 2,4- diethyl thioxanthone (DETX), isopropyl
One or more of thioxanthone (ITX), cumarin, camphorquinone.
Preferably, the tertiary amine is N, N dimethyl aniline, triethylamine, N, N, 3,5- tetramethyl aniline (TMA), N, N- bis-
The one or more of methylethanolamine, triethanolamine.
A kind of preparation method of above-mentioned alicyclic epoxy modified organic silicon/epoxy resin composite material, includes the following steps:
The modified organic siliconresin of alicyclic epoxy is added in epoxy resin, as basis material, cationic photopolymerization is then added and causes
Agent, photosensitizer, tertiary amine are protected from light 10 ~ 20min of ultrasound, are protected from light 10 ~ 12h of ageing, carry out photocuring under UV-LED light source.
It preferably must be held in light protected environment after above-mentioned nanocomposite constituents mixing, it is light-exposed to cause ultraviolet light curing reaction.
If not being protected from light, also there are a certain amount of ultraviolet light, meeting part initiation reaction, so that the epoxy conversion ratio measured is inclined in environment
It is low.
Preferably, the curing light source is UV-LED365 nm.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides a kind of epoxy modified silicone alkane, form silica solution by teos hydrolysis, utilize silane idol
Join agent carry out it is epoxy-modified, form stable epoxy modified silicone resin system, by the epoxy modified silicone resin with
Epoxy resin, cationic initiator component be prepared and can use the cured photo-curing material of UV-LED light source, be prepared into
For the conversion ratio of the epoxy group of the epoxy resin composite material arrived 70% or more, surface drying time is only 20 ~ 30s, curing rate
Fastly, curing performance is good, and solidification process energy consumption has both economy less than the 10% of traditional UV lamps solidification process energy consumption
And the feature of environmental protection, while UV-LED light source can accomplish that moment opens and closes, and without preheating and temperature fall time, improve work effect
Rate.
Specific embodiment
The present invention is further illustrated With reference to embodiment, but embodiment the present invention is not done it is any
The restriction of form.Unless otherwise indicated, source chemicals used in the embodiment of the present invention are the source chemicals routinely bought.
Embodiment 1
A kind of aliphatic epoxy modified organic silicone resin, is prepared by following steps:
S1. ethyl orthosilicate and dehydrated alcohol are added to equipped with agitating paddle, reflux condensing tube, thermometer and separatory funnel
In four-hole boiling flask, be fixed in thermostatical oil bath, then 50 DEG C at a temperature of be added dropwise while stirring mass fraction be 37% salt
Acid and deionized water drip off in 15min and continue to stir 1h, wherein the molar ratio 0.24:1 of hydrochloric acid and ethyl orthosilicate, water
With the molar ratio 6.5:1 of ethyl orthosilicate, the mixing molar ratio of ethyl alcohol and ethyl orthosilicate is 6.5:1；
S2. trimethoxy [2- (7- oxabicyclo [4.1.0] hept- 3- yl) ethyl] silicon is added in the reaction product of above-mentioned S1
Alkane reacts 5h at 50 DEG C, and then discharging is sealed, and obtains the epoxy-modified organic siliconresin colloidal sol of clear, makes
With being evaporated under reduced pressure before the colloidal sol, up to aliphatic epoxy modified organic silicone resin after removing ethyl alcohol and moisture, wherein [2-
(7- oxabicyclo [4.1.0] hept- 3- yl) ethyl] molar ratio of silane and ethyl orthosilicate is 0.5:1.
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the group including following mass fraction meter
Point: 5 parts of organic siliconresin of alicyclic epoxy modification；84 parts of bisphenol A diglycidyl ether (BADGE)；Three virtue of mixed type liquid
8 parts of base hexafluoro antimonate；ITX3 parts；0 part of tertiary amine.
Embodiment 2
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the component including following mass fraction meter: real
Apply 10 parts of organic siliconresin that 1 alicyclic epoxy of example is modified；79 parts of bisphenol A diglycidyl ether (BADGE)；Mixed type liquid
8 parts of triaryl hexafluoro antimonate；ITX3 parts；0 part of tertiary amine.
Embodiment 3
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the component including following mass fraction meter: real
Apply 5 parts of organic siliconresin that the alicyclic epoxy of example 1 is modified；- 3,4 epoxycyclohexyl formic acid esters (CE) 86 of 3,4- epoxycyclohexyl
Part；6 parts of hexafluorophosphate of bis- (4,4 '-thioether triphenyl sulphur)；1 part of camphorquinone；2 parts of triethylamine.
Embodiment 4
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the component including following mass fraction meter: real
Apply 10 parts of organic siliconresin that the alicyclic epoxy of example 1 is modified；- 3,4 epoxycyclohexyl formic acid esters (CE) of 3,4- epoxycyclohexyl
81 parts；6 parts of hexafluorophosphate of bis- (4,4 '-thioether triphenyl sulphur)；1 part of camphorquinone；2 parts of triethylamine.
Embodiment 5
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the component including following mass fraction meter: real
Apply 5 parts of organic siliconresin that the alicyclic epoxy of example 1 is modified；86 parts of 1,6 hexanediol diglycidylether (HDDGE)；Bis- (4,
4 '-thioether triphenyl sulphur) 6 parts of hexafluorophosphate；3 parts of camphorquinone；0 part of tertiary amine.
Embodiment 6
A kind of aliphatic epoxy modified organic silicone resin, is prepared by following steps:
S1. ethyl orthosilicate and dehydrated alcohol are added to equipped with agitating paddle, reflux condensing tube, thermometer and separatory funnel
In four-hole boiling flask, be fixed in thermostatical oil bath, then 50 DEG C at a temperature of be added dropwise while stirring mass fraction be 37% salt
Acid and deionized water drip off in 15min and continue to stir 1h, wherein the molar ratio 0.24:1 of hydrochloric acid and ethyl orthosilicate, water
With the molar ratio 6.5:1 of ethyl orthosilicate, the mixing molar ratio of ethyl alcohol and ethyl orthosilicate is 6.5:1；
S2. trimethoxy [2- (7- oxabicyclo [4.1.0] hept- 3- yl) ethyl] silicon is added in the reaction product of above-mentioned S1
Alkane reacts 5h at 50 DEG C, and then discharging is sealed, and obtains the epoxy-modified organic siliconresin colloidal sol of clear, makes
With being evaporated under reduced pressure before the colloidal sol, up to aliphatic epoxy modified organic silicone resin after removing ethyl alcohol and moisture, wherein [2-
(7- oxabicyclo [4.1.0] hept- 3- yl) ethyl] molar ratio of silane and ethyl orthosilicate is 1.0:1.
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the group including following mass fraction meter
Point: 10 parts of organic siliconresin of alicyclic epoxy modification；81 parts of 1,6 hexanediol diglycidylether (HDDGE)；Bis- (4,4 '-
Thioether triphenyl sulphur) 6 parts of hexafluorophosphate；3 parts of camphorquinone；0 part of tertiary amine
Comparative example 1
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the component including following mass fraction meter: rouge
Epoxy-modified 4 parts of organic siliconresin of ring race；- 3,4 89 parts of epoxycyclohexyl formic acid esters (CE) of 3,4- epoxycyclohexyl；Bis- (4,
4 '-thioether triphenyl sulphur) 6 parts of hexafluorophosphate；0 part of photosensitizer, 0 part of tertiary amine.
Comparative example 2
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the component including following mass fraction meter: rouge
Epoxy-modified 10 parts of organic siliconresin of ring race；- 3,4 84 parts of epoxycyclohexyl formic acid esters (CE) of 3,4- epoxycyclohexyl；It is double
6 parts of hexafluorophosphate of (4,4 '-thioether triphenyl sulphur)；0 part of photosensitizer, 0 part of tertiary amine.
Comparative example 3
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the component including following mass fraction meter: rouge
Epoxy-modified 15 parts of organic siliconresin of ring race；65 parts of bisphenol A diglycidyl ether (BADGE)；Mixed type liquid triaryl six
8 parts of fluorine antimonate；0 part of photosensitizer, 0 part of tertiary amine.
Comparative example 4
A kind of alicyclic epoxy modified organic silicone resin/epoxy resin composite material, the component including following mass fraction meter: rouge
Epoxy-modified 15 parts of organic siliconresin of ring race；82 parts of bisphenol A diglycidyl ether (BADGE)；Mixed type liquid triaryl six
8 parts of fluorine antimonate；0 part of photosensitizer, 0 part of tertiary amine.
As a result it detects
(1) conversion ratio of epoxy group
The conversion ratio of epoxy group turns for alicyclic epoxy modified organic silicone resin/epoxy resin composite material epoxide epoxy group group
Rate, detection method are as follows:
The Magna360 type Fourier Transform Infrared Spectrometer that test is manufactured using U.S. Nicolet company, pressing potassium bromide troche,
4000 ~ 400cm-1Wave-number range in sample is detected, light application time 5 minutes.
Testing result is shown in Table 1.
(2) surface drying time
Surface drying time reaction can the cured speed of response sample to a certain extent, detection method are as follows:
Test is tested using the photo solidification machine of UV-LED 365nm light source, and the sample prepared is smeared on the glass sheet, is applied
Layer passes sequentially through photo solidification machine, observing and recording sample from thick becomes the solid time with a thickness of 100um.
Testing result is shown in Table 1.
By the above experiment we it can be found that the higher solidification for sample of the conversion ratio of epoxy group is more advantageous,
The surface drying time of composite material is smaller.It is found, is added in the composite a certain amount of by the comparison of embodiment and comparative example
Photosensitizer or tertiary amine can be improved the conversion ratio of epoxy group, and can shorten the surface drying time of composite material.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (10)
1. a kind of aliphatic epoxy modified organic silicone resin, which is characterized in that be prepared by following steps:
S1. ethyl orthosilicate and ethyl alcohol are mixed, are warming up to 50 ~ 60 DEG C, hydrochloric acid and water is added, react 1 ~ 2h, wherein hydrochloric acid with
6 ~ 7:1 of molar ratio of 0.2 ~ 0.3:1 of molar ratio of ethyl orthosilicate, water and ethyl orthosilicate, ethyl alcohol and ethyl orthosilicate mix
Conjunction molar ratio is 5.6 ~ 6.5:1；
S2. the silane coupling agent with epoxy group is added in the reaction product of above-mentioned S1,4 ~ 5h is reacted at 50 ~ 60 DEG C, is removed
Go ethyl alcohol and moisture up to aliphatic epoxy modified organic silicone resin, wherein the molar ratio of silane coupling agent and ethyl orthosilicate is
0.5~1.0:1。
2. aliphatic epoxy modified organic silicone resin as described in claim 1, which is characterized in that hydrochloric acid and ethyl orthosilicate in S1
Molar ratio be 0.24:1, the molar ratio of water and ethyl orthosilicate is 6.5:1, and the mixing molar ratio of ethyl alcohol and ethyl orthosilicate is
6.5:1。
3. aliphatic epoxy modified organic silicone resin as described in claim 1, which is characterized in that with epoxy group described in S2
Silane coupling agent is [2- (7- oxabicyclo [4.1.0] hept- 3- yl) ethyl] silane, and silane coupling agent and ethyl orthosilicate rub
You are than being 0.5:1.
4. preferably, S1 is incorporated as being added dropwise simultaneously in middle hydrochloric acid and water, rate of addition is 0.8 ~ 1.0 mL/min.
5. one kind can the cured epoxy modified silicone/epoxide resin material of UV-LED, which is characterized in that including following mass parts
The component of number meter: 5 ~ 10 parts modified of organic siliconresin of alicyclic epoxy described in claim 1 ~ 4 any one, epoxy resin 70
~ 90 parts, 2 ~ 8 parts of cation light initiator, 1 ~ 3 part of photosensitizer, 0 ~ 3 part of tertiary amine.
6. a kind of modified organic silicon of alicyclic epoxy described in claim 5/epoxide resin material, which is characterized in that including as follows
The component of mass fraction meter: 5 ~ 10 parts modified of organic siliconresin of alicyclic epoxy, 79 ~ 84 parts of epoxy resin, cationic photopolymerization draw
Send out 2 ~ 8 parts of agent, 1 ~ 3 part of photosensitizer, 2 ~ 3 parts of tertiary amine.
7. a kind of excellent alicyclic epoxy modified organic silicon/epoxide resin material as claimed in claim 5, which is characterized in that described
Epoxy resin be bisphenol A diglycidyl ether (BADGE), -3,4 epoxycyclohexyl formic acid esters (CE) of 3,4- epoxycyclohexyl, 1,
The one or more of 6- hexanediol diglycidyl ether (HDDGE).
8. a kind of excellent alicyclic epoxy modified organic silicon/epoxide resin material as claimed in claim 5, which is characterized in that described
Cation light initiator is Diaryl iodonium hexafluorophosphate, mixed type liquid triaryl hexafluoro antimonate, 4- (thiophenyl) benzene
Base diphenyl sulphur hexafluorophosphate, bis- (4,4 '-thioether triphenyl sulphur) hexafluorophosphates, 4- isobutyl phenenyl -4'- methylbenzene
The one or more of base iodine hexafluorophosphate.
9. a kind of modified organic silicon of alicyclic epoxy described in claim 5/epoxide resin material preparation method, including walk as follows
It is rapid: the modified organic siliconresin of alicyclic epoxy being added in epoxy resin, as basis material, cationic photopolymerization is then added
Initiator, photosensitizer, tertiary amine are protected from light 10 ~ 20min of ultrasound, are protected from light 10 ~ 12h of ageing, carry out photocuring under UV-LED light source.
10. preparation method as claimed in claim 9, which is characterized in that the curing light source is UV-LED365 nm.
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| CN114149656A (en) * | 2021-12-07 | 2022-03-08 | 浙江省开化七一电力器材有限责任公司 | Curable thermosetting resin and application thereof in high-voltage insulator for switch cabinet |
| CN114687246A (en) * | 2022-02-17 | 2022-07-01 | 固德电材系统（苏州）股份有限公司 | Epoxy-based silicone resin sizing agent, mica plate and preparation method and application thereof |
| CN116904160A (en) * | 2023-07-18 | 2023-10-20 | 韦尔通科技股份有限公司 | Aging-resistant high-adhesion UV (ultraviolet) curing adhesive and preparation method and application method thereof |
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| CN113354924A (en) * | 2021-06-24 | 2021-09-07 | 哈尔滨工业大学无锡新材料研究院 | Glass fiber composite material with low surface tension and preparation method thereof |
| CN114149656A (en) * | 2021-12-07 | 2022-03-08 | 浙江省开化七一电力器材有限责任公司 | Curable thermosetting resin and application thereof in high-voltage insulator for switch cabinet |
| CN114149656B (en) * | 2021-12-07 | 2023-06-09 | 浙江省开化七一电力器材有限责任公司 | Curable thermosetting resin and application thereof in high-voltage insulator for switch cabinet |
| CN114687246A (en) * | 2022-02-17 | 2022-07-01 | 固德电材系统（苏州）股份有限公司 | Epoxy-based silicone resin sizing agent, mica plate and preparation method and application thereof |
| CN116904160A (en) * | 2023-07-18 | 2023-10-20 | 韦尔通科技股份有限公司 | Aging-resistant high-adhesion UV (ultraviolet) curing adhesive and preparation method and application method thereof |
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