CN110305487A - Visible-light curing organosilicon composite material and preparation method - Google Patents
Visible-light curing organosilicon composite material and preparation method Download PDFInfo
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- 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
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- 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
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- 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
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Abstract
Visible-light curing organosilicon composite material and preparation method is related to a kind of preparation of visible-light curing organic siliconresin and the preparation of organic silicon composite.Photo-curable silicone composite material of the present invention combines cation photocuring and radical UV curing, the advantages of playing the two hybrid UV-curing, generate good synergistic effect, it being capable of sufficiently cured epoxy base functional group and unsaturated double-bond functional group, not only increase solidification rate and reaction conversion ratio, the cure shrinkage for reducing organic siliconresin composite material simultaneously improves organic siliconresin overall performance after solidification, and preparation method is simple and easy to do.
Description
Technical field
The invention belongs to organosilicon field of compound material more particularly to a kind of organic silicon composite of visible-light curing and its
Preparation method.
Background technique
Photocuring technology is-item energy conservation and clean and environment-friendly technology, it is energy saving --- and energy consumption is only traditional mercury lamp
1/10th, and without solvent, have protective effect to ecological environment, poison gas and carbon dioxide will not be discharged to atmosphere, thus by
It is described as " green technology ".Photocuring technology is concluded have the characteristics that " 5E ": efficient (Efficient), wide adaptability
(Enabling), economical (Economical), energy saving (Energy Saving), environmentally friendly (Environmental Friendly).
Therefore, photocuring technology is got more and more applications in Material Field.
The basic structural unit of organosilicon product is made of silicon-oxygen chain link, and side chain then passes through silicon atom and other are each
Kind organic group is connected.Therefore, not only contain " organic group " in the structure of organosilicon product, but also contain " inorganic structure ", this
The function of characteristic and inorganic matter that kind special composition and molecular structure make it integrate organic matter.Organosilicon material has table
The fundamental propertys such as face tension is low, viscosity-temperature coefficient is small, compressibility is high, gas permeability is high, and have high-low temperature resistant, electric insulation,
The excellent characteristics such as resistance to oxidation stability, weatherability, fire retardant, hydrophobic, corrosion-resistant, non-toxic and tasteless and physiological inertia are widely applied
In the industries such as aerospace, electric, building, transport, chemical industry, weaving, food, light industry, medical treatment.Currently, world's organosilicon
The direction of material technology development is high-performance, multi-functional and Composite, by the new additive of the progress of compounding technique and addition,
And by changing the modification technologies such as crosslinking method, copolymerization, blending, realizes that organic polymer is compound with organosilicon material, be current
The important directions of organic silicon technology development.In numerous synthetic resin, silicone resin is in outstanding person wherein.It has tasteless
It is nontoxic, be not afraid of high temperature and the characteristics of resist severe cold, at 300 degrees Celsius and subzero 90 degrees Celsius " with great composure ", " face is not
Change colour ", do not lose original intensity and elasticity still.There are also good electrical insulating properties, oxytolerant ageing resistance, fast light anti-aging for silicone resin
Property and mildew resistance, chemical stability etc..Due to being provided with these excellent performances, so that silicone resin plays in modern medicine
Extensive important function.
If introducing on polysiloxane strand has photosensitive group, make photo curable organic
Silicon materials, then curing efficiency will greatly improve, not only energy saving, can also reduce pollution.Organosilicon material and photocuring technology
Combination, not only can promote the development of organosilicon material, but also add new varieties for photo-curing material.It can be under illumination condition
It polymerize, crosslinks reactive group and be generally divided into two classes: radical UV curing group and cation photocuring group.Mesh
Before, the Photocurable Silicone Material of synthesis mainly introduces acrylate photosensitive group in the siloxane molecule chain of organosilicon
Or epoxy photosensitive group.According to the difference of ultraviolet curing group, photo-curable silicone prepolymer is broadly divided into: vinylated poly- silicon oxygen
Alkane, acrylate functional polysiloxanes, epoxy polysiloxanes, styrenyl polysiloxanes etc..Photocuring of the present invention has
Machine silicon composite provides a kind of organic siliconresin and preparation method thereof with acrylate group and epoxy group, has
The advantages that solidification rate is fast, consumes energy low, and performance is good.
Summary of the invention
The present invention is intended to provide a kind of organic silicon composite, especially provides a kind of organic silicon composite of visible-light curing
And preparation method thereof.
The organic silicon composite of visible-light curing of the present invention is by organic siliconresin, cation light initiator, freedom
Base photoinitiator, photosensitizer, nanofiller, nano-photo catalytic particle, pigment composition；It is calculated according to mass fraction, relative to having
100 parts of machine silicone resin calculating, 0.8-12 parts of cation light initiator, 0.8-10 parts of free radical photo-initiation, photosensitizer 0.1-2
Part, 15-70 parts of nanofiller, 1-8 parts of nano-photo catalytic particle, 0-1 parts of pigment.
Siloxanes of the above-mentioned organic siliconresin by one or more containing alkyl and the siloxanes containing aromatic radical with contain ring
The siloxanes of oxygroup and siloxanes containing unsaturated double-bond react under the effect of the catalyst to be prepared.
Above-mentioned cation light initiator is xanthone base phenyl salt compounded of iodine, Fluorenone base phenyl salt compounded of iodine, isopropylbenzene cyclopentadienyl (II)
Hexafluorophosphate, dialkyl benzene formyl sulfosalt, triaryl (1- pyrene) bismuth salt, dialkyl benzene formyl sulfosalt, dialkyl benzene formyl
Sulfosalt, bis- (5- fluorine thiophene -2- base) iodine formates, S, S- dialkyl group-S- (diformazan oxyphenyl) sulfosalt and Phenylsulfanylphenyl
One of diphenyl sulfosalt or more than one.
Above-mentioned free radical photo-initiation is (2,4,6- trimethylbenzoyl) diphenyl phosphine oxide, 2- methyl-1-(4- first
Sulfenyl phenyl) -2- morpholinyl -1- acetone, 2- isopropyl thioxanthone, 4- dimethylaminobenzoic acid ethyl ester, 1- hydroxy-cyclohexyl
Phenyl ketone, 2- hydroxy-2-methyl -1- phenyl -1- acetone, benzoin dimethylether, methyl o-benzoylbenzoate, tetramethyl rice Chi
One of ketone, 2,4- diethyl thioxanthone and the chloro- 4- propoxyl group thioxanthone of 1- or more than one.
Above-mentioned photosensitizer include, but are not limited to camphorquinone, naphthalene, anthracene, pyrene, N- unsaturated double-bond carbazole, benzophenone,
One of dibenzoyl, 3,5- diphenyl dithieno [3,2-b:2,3-a] anthracene, cumarin and curcumin or more than one.
Above-mentioned nanofiller be one of gas-phase silica, talcum powder, mica powder or more than one, wherein gas phase hard charcoal
Black, talcum powder, the specific surface area of mica powder is 1000 mesh or more.
Above-mentioned nano-photo catalytic particle is gallium phosphide (GdP), GaAs (GdAs), titanium dioxide (TiO2), zinc oxide
(ZnO), tin oxide (SnO2), zirconium dioxide (ZrO2), cadmium sulfide (CdS), zinc sulphide (ZnS), tungsten oxide (WO3), titanium dioxide
One of silicon (SiO2) or more than one composition.
Above-mentioned pigment is conventional reagent, selects specific color according to product.
The preparation method for organic silicon resin is as follows:
1. by least one of the siloxanes containing alkyl and siloxanes containing aromatic radical and the siloxanes containing epoxy group and containing
The siloxanes of unsaturated double-bond is mixed with catalysts and solvents, in the case where temperature is 50~85 DEG C, the anti-5~9h of mechanical stirring, 120
The solvent for removing remnants is vacuumized at DEG C and low-boiling-point substance obtains organic siliconresin.
2. mole of the epoxy group in unsaturated double-bond and epoxy radical siloxane in the siloxanes of above-mentioned unsaturated double-bond
Than being 0.3 ~ 3；The quality of the above-mentioned siloxanes containing unsaturated double-bond accounts for the 10%~50% of all siloxanes gross masses；It is above-mentioned to contain
The quality of the siloxanes of epoxy group accounts for the 6-35% of all siloxanes gross masses.
The siloxanes containing alkyl is dimethyldimethoxysil,ne, methyldiethoxysilane, triethoxy (1- benzene
Base unsaturated double-bond) silane, methyltriethoxysilane, di ethoxy di methyl-monosilane, ethyl trimethoxy silane, methyl two
Methoxy silane, hexamethyldisiloxane, triethoxysilane, propyl-triethoxysilicane, 1,3- diethoxy -1,1,3,3-
One of tetramethyl disiloxane and double trimethylsiloxy group methyl-monosilanes or more than one.
The siloxanes containing epoxy group is γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane, 3- [(2,3)-epoxy
Third oxygen] hydroxypropyl methyl dimethoxysilane, 3- [the third oxygen of (2,3)-epoxy] propyl trimethoxy silicane, 3- [(2,3)-epoxy third
Oxygen] propyl-triethoxysilicane, 2- (7- oxabicyclo [4.1.0] hept- 3- yl) ethyl trimethoxy silicon, 5,6- epoxyhexyl three
Ethoxysilane, trimethoxy [2- (3,4- 7-oxa-bicyclo[4.1.0 base) methyldiethoxysilane 2- (3,4- epoxycyclohexyl) second
One of base trimethoxy silane and 2- (3,4- epoxycyclohexyl) ethyl triethoxysilane or more than one.
The siloxanes containing aromatic radical is octaphenylcyclotetrasiloxane, 1,1- diethoxy pentane, phenyl methyl diformazan
Oxysilane, dimethoxydiphenylsilane, phenyl t-butyl methyl dimethoxysilane, phenyltrimethoxysila,e, three second
Oxygroup (1- phenyl unsaturated double-bond) silane, tetramethyl tetraphenyl cyclotetrasiloxane, benzene unsaturated double-bond ethyl trimethoxy silicon
One of alkane, phenyl triethoxysilane, phenyl methyl diethoxy silane or more than one.
The siloxanes containing unsaturated double-bond is γ-methacryloxypropyl trimethoxy silane, 3- methyl-prop
Alkene acryloxypropylethoxysilane triethoxysilane, 3- methacryloxypropylmethyl dimethoxysilane, 3- methacryloxypropyl
Base hydroxypropyl methyl diethoxy silane, allyltriethoxysilane, 5- hexenyl trimethoxy silane, 10- alkenyl hendecane
Base trimethoxy silane, unsaturated double-bond trimethoxy silane, unsaturated double-bond triethoxysilane, methyl unsaturated double-bond two
One kind of two unsaturated double-bond siloxanes of Ethoxysilane, methyl unsaturated double-bond dimethoxysilane and tetramethyl or it is a kind of with
On.
The catalyst includes acidic catalyst or basic catalyst, and the acidic catalyst includes hydrochloric acid, sulfuric acid, phosphorus
Acid, nitric acid, phosphorous acid, hypophosphorous acid, acid iodide or peroxophosphoric acid；The basic catalyst includes sodium hydroxide, potassium hydroxide, hydroxide
Aluminium, sodium bicarbonate, ammonium hydrogen carbonate, sodium carbonate or tetramethyl oxyammonia.
Visible light organosilicon composite material and preparation method thereof of the present invention is as follows:
1) nanofiller, nano-photocatalyst material are weighed, is added in organic siliconresin, is stirred evenly；
2) free radical photo-initiation, cation light initiator, photosensitizer are weighed, is uniformly mixed, is added to above-mentioned organic siliconresin
In, it stirs evenly；
3) pigment is weighed, is added in above-mentioned organic siliconresin, stirs evenly, vacuum outgas is multiple up to visible-light curing organosilicon
Condensation material.
The preparation method of the organic silicon composite of visible-light curing of the present invention does not represent and can prepare or utilize
Only form of the invention.Unless otherwise stated, otherwise all technical and scientific terms used herein all has and the present invention
The normally understood meaning of technical field those of ordinary skill is identical.Visible-light curing organosilicon provided by the present invention is compound
Material preparation method is easy, introduces that free radical-cationic hybrid photocuring system gives full play to free radical and cationic photopolymerization is solid
The characteristics of change system, generates good synergistic effect, being capable of abundant cured epoxy base functional group and unsaturated double-bond function base
Group, not only increases solidification rate, while reducing the cure shrinkage of organic siliconresin composite material, has after improving solidification
Machine silicone resin performance.
Specific embodiment
With embodiment, the present invention will be further described below.
Embodiment 1
By 112g water, 36g ethyl alcohol and 4.3g hypophosphorous acid are added in flask, then by 67.4g 10-alkenyl undecyl trimethoxy
Silane, 5,6-epoxyhexyl of 59.5g triethoxysilane, 52.0g di ethoxy di methyl-monosilane and 28.6g octaphenyl ring four
Siloxanes is added in above-mentioned solution, and a polycondensation reaction 5h is hydrolyzed under the conditions of 85 DEG C, reaction system liquid separation is obtained organosilicon tree
The mixture of rouge and water is washed 4 times with 30% ethanol water, is finally vacuumized at 120 DEG C and is removed remaining solvent and low boiling
Object obtains organic siliconresin.
Organic siliconresin 100g above is taken, 35g gas-phase silica, 5g nano-titanium dioxide is taken to be added to organic siliconresin
In, it stirs evenly；Weigh 4g dialkyl benzene formyl sulfosalt, 5g dialkyl benzene formyl sulfosalt, 0.8g 2- isopropyl thioxanthone,
1g camphorquinone is uniformly mixed, and is then added in above-mentioned silicone resin mixture, is stirred evenly；Blue 0.5g is added,
Mix uniform to color, vacuum outgas is up to the organic silicon composite of visible-light curing.
Embodiment 2
By 150g water, 5.3g glacial acetic acid and 45g ethyl alcohol are added in flask, then 72.5g 2- (3,4 one epoxycyclohexyl) ethyl three
Methoxy silane, 5-hexenyl of 76.0g trimethoxy silane and 83.5g methyldiethoxysilane are added in above-mentioned solution,
A polycondensation reaction 9h is hydrolyzed under the conditions of 50 DEG C；Reaction system liquid separation is obtained into the mixture of organic siliconresin and water, with 30% second
Alcohol solution is washed 4 times, is finally vacuumized at 120 DEG C and is removed remaining solvent and low-boiling-point substance, organic siliconresin.
Organic siliconresin 100g above is taken, 30g talcum powder, 40g gas-phase silica, 1g nano-titanium dioxide is taken to be added to
In machine silicone resin, stir evenly；Weigh 5g triaryl (1- pyrene) bismuth salt, 2g dialkyl benzene formyl sulfosalt, 5g dialkyl benzene first
Acyl sulfosalt, 0.1g 4- dimethylaminobenzoic acid ethyl ester, 2g camphorquinone are uniformly mixed, and it is mixed to be then added to above-mentioned organic siliconresin
It closes in object, stirs evenly；White colours 0.2g is added, mixes uniform to color, vacuum outgas is up to visible-light curing organosilicon
Composite material.
Embodiment 3
By 140g water, 49.0g ethyl alcohol and 4.0g phosphoric acid are added in flask, then by 79.0g propyl-triethoxysilicane, 79.5g
γ-methacryloxypropyl trimethoxy silane, 65.5g methyldiethoxysilane and 31.0g phenyl t-butyl methyl
Dimethoxysilane is added in above-mentioned solution, and hydrolysis-polycondensation reaction 8h, reaction system liquid separation is had under the conditions of 70 DEG C
The mixture of machine silicone resin and water is washed 4 times with 30% ethanol water, finally vacuumized at 120 DEG C remove remaining solvent and
Low-boiling-point substance, organic siliconresin.
Organic siliconresin 100g above is taken, 25g talcum powder, 18g gas-phase silica, 8g nano-titanium dioxide is taken to be added to
In machine silicone resin, stir evenly；Weigh 4g Phenylsulfanylphenyl diphenyl sulfosalt, 3g 2- hydroxy-2-methyl -1- phenyl -1- third
Ketone, 0.2g 4- dimethylaminobenzoic acid ethyl ester, 0.1g camphorquinone are uniformly mixed, and are then added to above-mentioned organic siliconresin mixing
In object, stir evenly；Gray color 0.8g is added, mixes uniform to color, vacuum outgas is multiple up to visible-light curing organosilicon
Condensation material.
Embodiment 4
By 155g water, 3.5g hydrochloric acid and 55g ethyl alcohol are added in flask, then 75g dimethyldimethoxysil,ne, 73.8g 3-
[the third oxygen of (2,3)-epoxy] propyl-triethoxysilicane, 61.2g phenyltrimethoxysila,e, 65.0g 11- acetoxyl group 11
Alkyl triethoxysilane is added in above-mentioned solution, and a polycondensation reaction 7h is hydrolyzed under the conditions of 80 DEG C；Reaction system liquid separation is obtained
It to the mixture of organic siliconresin and water, is washed 4 times with 30% ethanol water, is finally vacuumized at 120 DEG C and remove the molten of remnants
Agent and low-boiling-point substance, organic siliconresin.
Organic siliconresin 100g above is taken, 15g gas-phase silica, 8g nano-titanium dioxide is taken to be added to organic siliconresin
In, it stirs evenly；Weigh 0.8g xanthone base phenyl salt compounded of iodine, 5g 2- isopropyl thioxanthone, 5g 4- Dimethylaminobenzene first
Acetoacetic ester, 1g camphorquinone, 0.5g cumarin are uniformly mixed, and are then added in above-mentioned silicone resin mixture, are stirred evenly；
White colours 1g is added, mixes uniform to color, vacuum outgas is up to the organic silicon composite of visible-light curing.
Embodiment 5
By 160g water, 56g ethyl alcohol and 4.5g hydrochloric acid are added in flask, then by 75g methyldiethoxysilane, 45.0g trimethoxy
Base [2- (3,4- 7-oxa-bicyclo[4.1.0 base) methyldiethoxysilane, 50.0g phenyl methyl dimethoxysilane, 31.0g 3- first
Base acryloxypropyl dimethoxysilane is added in above-mentioned solution, and a polycondensation reaction 6h is hydrolyzed under the conditions of 80 DEG C,
Reaction system liquid separation is obtained into the mixture of organic siliconresin and water, is washed 4 times with 30% ethanol water, is finally taken out at 120 DEG C
Remaining solvent and low-boiling-point substance is removed in vacuum, obtains organic siliconresin.
Organic siliconresin 100g above is taken, 25g gas-phase silica, 15g mica powder, 2g nano-titanium dioxide is taken to be added to
In machine silicone resin, stir evenly；Weigh 1g dialkyl benzene formyl sulfosalt, 2g triaryl (1- pyrene) bismuth salt, 2.0g 2- methyl-
1- (4- methyl mercapto phenyl) -2- morpholinyl -1- acetone, 0.5g camphorquinone, 0.3g cumarin are uniformly mixed, and are then added to above-mentioned
It in silicone resin mixture, stirs evenly, vacuum outgas is up to the organic silicon composite of visible-light curing.
Embodiment 6
By 150g water, 65g ethyl alcohol and 5.5g phosphoric acid are added in flask, then by 59g methyldiethoxysilane, three second of 26g propyl
Oxysilane, 15g dimethoxydiphenylsilane, 48.0g 3- [the third oxygen of (2,3)-epoxy] propyl trimethoxy silicane, 40.0g
Phenyl methyl dimethoxysilane, 43.0g γ-methacryloxypropyl trimethoxy silane are added in above-mentioned solution,
A polycondensation reaction 6h is hydrolyzed under the conditions of 85 DEG C, reaction system liquid separation is obtained into the mixture of organic siliconresin and water, with 30% ethyl alcohol
Aqueous solution is washed 4 times, is finally vacuumized at 120 DEG C and is removed remaining solvent and low-boiling-point substance, obtains organic siliconresin.
Organic siliconresin 100g above is taken, 20g gas-phase silica, 18g mica powder, 2g nano-titanium dioxide, 2g dioxy are taken
Change zirconium to be added in organic siliconresin, stir evenly；Weigh 1.5g dialkyl benzene formyl sulfosalt, 1.5g triaryl (1- pyrene) bismuth
Salt, 1.5g 4- dimethylaminobenzoic acid ethyl ester, 2.0g 2- methyl-1-(4- methyl mercapto phenyl)-2- morpholinyl-1- acetone,
0.5g camphorquinone, 0.3g cumarin, 0.8g blue pigment are uniformly mixed, and are then added in above-mentioned silicone resin mixture,
It stirs evenly, vacuum outgas is up to the organic silicon composite of visible-light curing.
Claims (10)
1. the organic silicon composite of visible light, it is characterised in that light-initiated by organic siliconresin, cation light initiator, free radical
Agent, photosensitizer, nanofiller, nano-photo catalytic particle, pigment composition；It is calculated according to mass fraction, relative to organic siliconresin
100 parts of calculating, 0.8-12 parts of cation light initiator, 0.8-10 parts of free radical photo-initiation, 0.1-2 parts of photosensitizer, nanometer is filled out
15-70 parts, 1-8 parts of nano-photo catalytic particle, 0-1 parts of pigment of material.
2. the organic silicon composite of visible light as described in claim 1, it is characterised in that cation light initiator is xanthone
Base phenyl salt compounded of iodine, Fluorenone base phenyl salt compounded of iodine, isopropylbenzene luxuriant (II) hexafluorophosphate, dialkyl benzene formyl sulfosalt, triaryl
(1- pyrene) bismuth salt, dialkyl benzene formyl sulfosalt, dialkyl benzene formyl sulfosalt, bis- (5- fluorine thiophene -2- base) iodine formates, S,
One of S- dialkyl group-S- (diformazan oxyphenyl) sulfosalt and Phenylsulfanylphenyl diphenyl sulfosalt or more than one.
3. the organic silicon composite of visible light as described in claim 1, it is characterised in that free radical photo-initiation is (2,4,6-
Trimethylbenzoyl) diphenyl phosphine oxide, 2- methyl-1-(4- methyl mercapto phenyl)-2- morpholinyl-1- acetone, 2- isopropyl
Thioxanthone, 4- dimethylaminobenzoic acid ethyl ester, 1- hydroxycyclohexylphenylketone, 2- hydroxy-2-methyl -1- phenyl -1- acetone,
Benzoin dimethylether, methyl o-benzoylbenzoate, tetramethyl Michler's keton, 2,4- diethyl thioxanthone and chloro- the third oxygen of 4- of 1-
One of base thioxanthone or more than one.
4. the organic silicon composite of visible light as described in claim 1, it is characterised in that photosensitizer includes, but are not limited to camphor
Quinone, naphthalene, anthracene, pyrene, N- unsaturated double-bond carbazole, benzophenone, dibenzoyl, 3,5- diphenyl dithieno [3,2-b:2,
3-a] one of anthracene, cumarin and curcumin or more than one.
5. the organic silicon composite of visible light as described in claim 1, it is characterised in that nanofiller is gas-phase silica, cunning
One of mountain flour, mica powder or more than one, wherein gas-phase silica, talcum powder, the specific surface area of mica powder is 1000 mesh
More than.
6. the organic silicon composite of visible light as described in claim 1, it is characterised in that nano-photo catalytic particle is gallium phosphide
(GdP), GaAs (GdAs), titanium dioxide (TiO2), zinc oxide (ZnO), tin oxide (SnO2), zirconium dioxide (ZrO2), sulphur
One of cadmium (CdS), zinc sulphide (ZnS), tungsten oxide (WO3), silica (SiO2) or more than one composition.
7. the organic silicon composite of visible light as described in claim 1, it is characterised in that above-mentioned organic siliconresin by a kind of or
More than one siloxanes containing alkyl and the siloxanes containing aromatic radical and the siloxanes containing epoxy group and the silicon containing unsaturated double-bond
Oxygen alkane reacts under the effect of the catalyst to be prepared.
8. organic siliconresin as claimed in claim 7, it is characterised in that the unsaturation in the siloxanes of above-mentioned unsaturated double-bond
The molar ratio of epoxy group in double bond and epoxy radical siloxane is 0.3 ~ 3；The quality of the above-mentioned siloxanes containing unsaturated double-bond accounts for
The 10%~50% of all siloxanes gross masses；The quality of the above-mentioned siloxanes containing epoxy group accounts for the 6- of all siloxanes gross masses
35%；
The siloxanes containing alkyl is dimethyldimethoxysil,ne, methyldiethoxysilane, (1- phenyl is or not triethoxy
It is saturated double bond) silane, methyltriethoxysilane, di ethoxy di methyl-monosilane, ethyl trimethoxy silane, methyl dimethoxy oxygen
Base silane, hexamethyldisiloxane, triethoxysilane, propyl-triethoxysilicane, 1,3- diethoxy -1,1,3,3- tetramethyl
One of base disiloxane and double trimethylsiloxy group methyl-monosilanes or more than one；
The siloxanes containing epoxy group is γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane, 3- [(2,3)-epoxy third
Oxygen] hydroxypropyl methyl dimethoxysilane, 3- [the third oxygen of (2,3)-epoxy] propyl trimethoxy silicane, 3- [the third oxygen of (2,3)-epoxy]
Propyl-triethoxysilicane, 2- (7- oxabicyclo [4.1.0] hept- 3- yl) ethyl trimethoxy silicon, three second of 5,6- epoxyhexyl
Oxysilane, trimethoxy [2- (3,4- 7-oxa-bicyclo[4.1.0 base) methyldiethoxysilane 2- (3,4- epoxycyclohexyl) ethyl
One of trimethoxy silane and 2- (3,4- epoxycyclohexyl) ethyl triethoxysilane or more than one；
The siloxanes containing aromatic radical is octaphenylcyclotetrasiloxane, 1,1- diethoxy pentane, phenyl methyl dimethoxy
Silane, dimethoxydiphenylsilane, phenyl t-butyl methyl dimethoxysilane, phenyltrimethoxysila,e, triethoxy
(1- phenyl unsaturated double-bond) silane, tetramethyl tetraphenyl cyclotetrasiloxane, benzene unsaturated double-bond ethyl trimethoxy silane, benzene
One of ethyl triethoxy silicane alkane, phenyl methyl diethoxy silane or more than one；
The siloxanes containing unsaturated double-bond is γ-methacryloxypropyl trimethoxy silane, 3- methacryl
Oxygroup propyl-triethoxysilicane, 3- methacryloxypropylmethyl dimethoxysilane, 3- methacryloxy third
Ylmethyl diethoxy silane, allyltriethoxysilane, 5- hexenyl trimethoxy silane, 10- alkenyl undecyl three
Methoxy silane, unsaturated double-bond trimethoxy silane, unsaturated double-bond triethoxysilane, methyl unsaturated double-bond diethoxy
The one or more of two unsaturated double-bond siloxanes of base silane, methyl unsaturated double-bond dimethoxysilane and tetramethyl；
The catalyst includes acidic catalyst or basic catalyst, and the acidic catalyst includes hydrochloric acid, sulfuric acid, phosphoric acid, nitre
Acid, phosphorous acid, hypophosphorous acid, acid iodide or peroxophosphoric acid；The basic catalyst includes sodium hydroxide, potassium hydroxide, aluminium hydroxide, carbon
Sour hydrogen sodium, ammonium hydrogen carbonate, sodium carbonate or tetramethyl oxyammonia.
9. organic siliconresin as claimed in claim 7, it is characterised in that the preparation method is as follows: by the siloxanes containing alkyl and containing
At least one of siloxanes of aromatic radical and the siloxanes containing epoxy group and siloxanes and catalyst containing unsaturated double-bond
Mixed with solvent, in the case where temperature is 50~85 DEG C, the anti-5~9h of mechanical stirring, vacuumized at 120 DEG C remove remaining solvent and
Low-boiling-point substance obtains organic siliconresin.
10. the organic silicon composite of visible light as described in claim 1, it is characterised in that the preparation method is as follows:
1) nanofiller, nano-photocatalyst material are weighed, is added in organic siliconresin, is stirred evenly；
2) free radical photo-initiation, cation light initiator, photosensitizer are weighed, is uniformly mixed, is added to above-mentioned organic siliconresin
In, it stirs evenly；
3) pigment is weighed, is added in above-mentioned organic siliconresin, stirs evenly, vacuum outgas is multiple up to visible-light curing organosilicon
Condensation material.
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| CN113372816A (en) * | 2021-05-21 | 2021-09-10 | 无锡时生高分子科技有限公司 | Solvent-free UV (ultraviolet) curing type organic silicon three-proofing adhesive |
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