CN109111896A - A kind of preparation method of high-intensity weather-proof high casting glue - Google Patents
A kind of preparation method of high-intensity weather-proof high casting glue Download PDFInfo
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- CN109111896A CN109111896A CN201810727020.7A CN201810727020A CN109111896A CN 109111896 A CN109111896 A CN 109111896A CN 201810727020 A CN201810727020 A CN 201810727020A CN 109111896 A CN109111896 A CN 109111896A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The present invention relates to a kind of preparation methods of high-intensity weather-proof high casting glue, belong to technical field of chemical material preparation.Basalt fibre is introduced into casting glue by the present invention, basalt fibre has excellent mechanical property, resistance to ag(e)ing, in ultraviolet light, temperature change dramatically, good stability is able to maintain under the conditions of air pollution is serious, nano-titanium dioxide is introduced into casting glue by the present invention, nanometer titanic oxide material excellent in optical properties, there is the performance of radiation protection, organic silicone oil also plays shock resistance in casting glue system, improve the effect of intensity, organic silicone oil and containing hydrogen silicone oil are in casting glue preparation process, it can be with intermolecular formation Si -- H bond each in casting glue, Si-O key and Si-C key, the bond energy of these keys is very big, stable structure, combine each molecular layer and each molecular radical, strand, reinforce the microstructure space of casting glue, form fine and close molecular network, improve the impact resistance and mechanical property of casting glue, It has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of high-intensity weather-proof high casting glue, belong to technical field of chemical material preparation.
Background technique
Casting glue is also known as electronic pastes, is an extensive address.For the bonding of electronic component, sealing, encapsulating and painting
Cover protection.Casting glue belongs to liquid before uncured, has mobility, glue viscosity is according to the material, performance, production of product
The difference of technique and different from.Casting glue is just able to achieve its use value after being fully cured.
Encapsulating is exactly that liquid polyurethane compound is filled device of the people equipped with electronic component, route with mechanical or manual mode
It is interior, the thermosetting polymer insulating materials haveing excellent performance is solidified under room temperature or heating condition.Its effect is: strengthening electricity
The globality of sub- device improves the resistance to external shock, vibration；It improves and insulate between internal element, route, be conducive to device
Miniaturization, lightweight；It avoids element, route from directly exposing, improves waterproof, the humidity resistance of device.Epoxy pouring sealant application model
It encloses extensively, technical requirements are multifarious, various in style.Being divided to from condition of cure has normal temperature cure and two classes that are heating and curing.From dosage form
Above being divided to has two class of bi-component and one pack system.Multicomponent dosage form, it is rare as commodity due to inconvenient to use.Normal temperature cure ring
Oxygen casting glue is generally bi-component, it is difficult to realize automated production, generally be chiefly used in the encapsulating of Low-voltage Electronic device or should not heat
Cured occasion uses.Be heating and curing bi-component epoxy casting glue, is the kind that dosage is maximum, purposes is most wide.Silicon rubber encapsulating
Glue: room temperature vulcanized silicone rubber；Room temperature vulcanized silicone rubber or silicon gel are used for the encapsulating of electric element, improve usability
Energy and steadiness parameter, and it is liquid before vulcanization, it is easy to use convenient for perfusion.
Electron pouring sealant type is very more, divides from material type, at present using most most common predominantly 3 kinds, i.e.,
Epoxy resin embedding adhesive, organic siliconresin casting glue, polyurethane pouring sealant, and these three material casting glues can segment several hundred kinds
Different products.Wherein epoxy resin casting glue is cheap, low temperature flexibility is poor, weatherability is poor；Organic silicon casting glue valence
Lattice are high, electrical insulating property is poor；Polyurethanes casting glue combines the advantage of epoxy resin and organic silicon casting glue, and soft or hard
Degree, curing rate can be adjusted by formula, be widely used in encapsulating field.
Therefore, invent that a kind of intensity is high and the casting glue of good weatherability has actively meaning to technical field of chemical material preparation
Justice.
Summary of the invention
The technical problems to be solved by the invention: being directed to current casting glue shock resistance, poor toughness, weatherability weakness
Defect provides a kind of preparation method of high-intensity weather-proof high casting glue.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of high-intensity weather-proof high casting glue, it is characterised in that specific preparation step are as follows:
(1) by mass fraction be 20~25% phthalic anhydride and mass fraction be 30~35% propylene glycol solution by quality
Than in 1:3 investment beaker, with stirring, beaker being heated to, reaction gel is made after isothermal reaction, according to parts by weight, is claimed
Take 30~35 parts of reaction gels, 20~24 parts of methyl methacrylates, 1~3 part of methyl ethyl ketone peroxide and 2~4 parts of epoxyeicosatrienoic acid cobalts
Mixed impregnant liquor is stirred to get in investment blender；
(2) 300~600g basalt fibre is weighed, impregnates basalt fibre with above-mentioned mixed impregnant liquor, and be put into hot press,
Precompressed compacting, after compacting, elevated pressure increases progress hot pressing, and pressure and cooled to room temperature are kept after hot pressing,
Solidliquid mixture is obtained, it is spare；
(3) under the conditions of ice-water bath, titanium tetrachloride solution and deionized water 1:5 in mass ratio are stirred investment round-bottomed flask
In obtain dispersion liquid, into round-bottomed flask be added dispersion liquid quality 3~5% sodium dihydrogen phosphate, ebuillition of heated reflux, returned
Reflux product is put into centrifugal separator and is centrifugally separating to obtain separation solid by apoblema, is washed with distilled water 3~5 times, is put into
It is dry in baking oven, it grinds and 300 meshes excessively obtains sieving；
(4) according to parts by weight, 20~23 parts of vinyl silicone oils, 3~5 parts of containing hydrogen silicone oils and 3~5 parts of above-mentioned sievings are weighed to throw
Enter in high speed shear dispersion machine, shearing dispersion obtains coagulant liquid, according to parts by weight, weighs 50~54 parts of vinyl silicone oils, 0.5
~0.8 portion of platinized platinum, 0.1~0.3 part of alkynyl hexamethylene and 20~24 parts of spare solidliquid mixtures put into high shear homomixer
In, 15~20min of shearing dispersion obtains dispersion liquid under the revolving speed of 1000~1100r/min；
(5) by etc. quality coagulant liquid and dispersion liquid with blender stir to get mixed liquor, mixed liquor is put in quiet in vacuum tank
It sets to be put in again after 15~20min under room temperature and stands 24~26h to get high-intensity weather-proof high casting glue.
The mass fraction of phthalic anhydride as described in step (1) is 20~25%, and the mass fraction of propylene glycol solution is
30~35%, speed of agitator is 300~350r/min in beaker, and mixing time is 15~20min, beaker heating temperature to 190~
220 DEG C, the isothermal reaction time is 20~30min.
Precompressed pressure is 2.5~2.8MPa in hot press described in step (2), and the pressing time is 12~13h, hot pressing pressure
By force to 5.0~5.5MPa, for hot pressing temperature to 120~130 DEG C, hot pressing time is 3.0~3.5h.
The mass fraction of titanium tetrachloride solution described in step (3) is 50~70%, and ebuillition of heated return time is 5.0
~5.4h, the temperature in baking oven are 70~80 DEG C, and drying time is 14~16h.
In high-speed shearing machine described in step (4) revolving speed be 1200~1300r/min, shearing jitter time be 20~
25min。
The revolving speed of blender described in step (5) is 600~700r/min, and mixing time is 30~40min, vacuum tank
Middle vacuum degree is 800~900MPa.
The method have the benefit that:
(1) unsaturated polyester (UP) is made using phthalic anhydride, propylene glycol, methyl methacrylate as raw material first in the present invention, then
Unsaturated polyester (UP) is suppressed to basalt fibre under conditions of high temperature and pressure and obtains solidliquid mixture, then with titanium tetrachloride solution
Nano-titanium dioxide is made for raw material boiling reflux, finally by organic silicone oil, solidliquid mixture, unsaturated polyester (UP), nano-silica
Change titanium and other auxiliary agents and be put into high shear homomixer and disperse to be made high-intensity weather-proof high casting glue, the present invention is by basalt
Fiber is introduced into casting glue, basalt fibre have excellent mechanical property, resistance to ag(e)ing, ultraviolet light, temperature change dramatically,
Good stability is able to maintain under the conditions of air pollution is serious, under conditions of high temperature and pressure, basalt fibre and insatiable hunger
With polyester molecule crosslinking curing, intermolecular force is formed, while by the modified encapsulating glue material of organic silicone oil, reaction generates Si-H
The bonded casting glue internal structure closed other molecules and form branch densification, the bond energy that reaction generates Si-C key is very big, chemical property
Stablize, can be improved degree of stability of the casting glue in various environment, so that the weatherability of casting glue is further increased, the present invention
Nano-titanium dioxide is introduced into casting glue, nanometer titanic oxide material excellent in optical properties has the performance of radiation protection, changes simultaneously
It learns property to stablize, can still remain stable under rugged environment, will not decompose, to improve the weatherability of casting glue；
(2) basalt fibre of excellent in mechanical performance is introduced into casting glue by the present invention, and basalt fibre density is big, rigidity is strong,
There is good shock resistance effect, while the nano-titanium dioxide introduced also has good mechanical property, nano-titanium dioxide point
It is dispersed in casting glue system, forms covalent bond, intermolecular force and other chemical bonds between strand each in system
With joint efforts, the microstructure crosslinking degree of system is improved, improves the impact resistance of casting glue to a certain degree, organic silicone oil is filling
Also played in sealing system shock resistance, improve intensity effect, organic silicone oil and containing hydrogen silicone oil in casting glue preparation process,
Can be with intermolecular formation Si -- H bond each in casting glue, Si-O key and Si-C key, the bond energy of these keys is very big, stable structure, connection
Each molecular layer and each molecular radical, strand are closed, the microstructure space of casting glue is reinforced, fine and close molecular network is formed, mentions
The impact resistance and mechanical property of high casting glue, have broad application prospects.
Specific embodiment
By mass fraction be 20~25% phthalic anhydride and mass fraction be 30~35% propylene glycol solution by matter
It measures than 15~20min is mixed with the revolving speed of 300~350r/min in 1:3 investment beaker, beaker is heated to 190~
220 DEG C, reaction gel is made after 20~30min of isothermal reaction, according to parts by weight, weigh 30~35 parts of reaction gels, 20~
Mixing is stirred to get in 24 parts of methyl methacrylates, 1~3 part of methyl ethyl ketone peroxide and 2~4 parts of epoxyeicosatrienoic acid cobalt investment blenders
Maceration extract；300~600g basalt fibre is weighed, impregnates basalt fibre with above-mentioned mixed impregnant liquor, and be put into hot press,
It is 2.5~2.8MPa in pressure, suppresses 12~13h under conditions of room temperature, after compacting, elevated pressure to 5.0~5.5MPa,
Temperature is increased to 120~130 DEG C, continues 3.0~3.5h of hot pressing, pressure and cooled to room temperature are kept after hot pressing, is obtained
It is spare to solidliquid mixture；Titanium tetrachloride solution and deionized water under the conditions of ice-water bath, by mass fraction for 50~70%
1:5 in mass ratio is stirred in investment round-bottomed flask and obtains dispersion liquid, and dispersion liquid quality 3~5% is added into round-bottomed flask
Sodium dihydrogen phosphate, ebuillition of heated 5.0~5.4h of reflux, obtains reflux product, reflux product is put into centrifugal separator and is centrifuged
Isolated separation solid is washed with distilled water 3~5 times, is put into baking oven dry 14~16h under conditions of 70~80 DEG C,
It grinds and crosses 300 meshes and obtain sieving；According to parts by weight, weigh 20~23 parts of vinyl silicone oils, 3~5 parts it is hydrogeneous
In silicone oil and 3~5 parts of above-mentioned sieving investment high speed shear dispersion machines, dispersion is sheared under the revolving speed of 1200~1300r/min
20~25min obtains coagulant liquid, according to parts by weight, weigh 50~54 parts of vinyl silicone oils, 0.5~0.8 portion of platinized platinum, 0.1~
In 0.3 part of alkynyl hexamethylene and 20~24 parts of spare solidliquid mixture investment high shear homomixers, in 1000~1100r/
15~20min of shearing dispersion obtains dispersion liquid under the revolving speed of min；By etc. quality coagulant liquid and dispersion liquid blender with 600
The revolving speed of~700r/min stirs 30~40min and obtains mixed liquor, and mixed liquor is put in vacuum tank, vacuum degree be 800~
Under conditions of 900MPa, it is put in again after 15~20min of standing under room temperature and stands 24~26h to get high-intensity weather-proof high casting glue.
Example 1
By mass fraction be 20% phthalic anhydride and mass fraction be 30% propylene glycol solution 1:3 in mass ratio put into burn
15min is mixed with the revolving speed of 300r/min in cup, beaker is heated to 190 DEG C, is made anti-after isothermal reaction 20min
Gel is answered, according to parts by weight, weighs 30 parts of reaction gels, 20 parts of methyl methacrylates, 1 part of methyl ethyl ketone peroxide and 2 parts
Mixed impregnant liquor is stirred to get in epoxyeicosatrienoic acid cobalt investment blender；300g basalt fibre is weighed, is soaked with above-mentioned mixed impregnant liquor
Stain basalt fibre, and be put into hot press, it is 2.5MPa in pressure, suppresses 12h under conditions of room temperature, after compacting, rises
High Voltage increases temperature to 120 DEG C, continues hot pressing 3.0h, pressure is kept after hot pressing and naturally cools to room to 5.0MPa
Temperature obtains solidliquid mixture, spare；Titanium tetrachloride solution and deionized water under the conditions of ice-water bath, by mass fraction for 50%
1:5 in mass ratio is stirred in investment round-bottomed flask and obtains dispersion liquid, and the phosphorus of dispersion liquid quality 3% is added into round-bottomed flask
Acid dihydride sodium, ebuillition of heated reflux 5.0h, obtains reflux product, reflux product is put into centrifugal separator and is centrifugally separating to obtain
Solid is separated, is washed with distilled water 3 times, dry 14h under conditions of 70 DEG C is put into baking oven, grinds and cross 300 meshes
Obtain sieving；According to parts by weight, 20 parts of vinyl silicone oils, 3 parts of containing hydrogen silicone oils and 3 parts of above-mentioned sieving investment high speeds are weighed
It shears in dispersion machine, shearing dispersion 20min obtains coagulant liquid under the revolving speed of 1200r/min, according to parts by weight, weighs 50 parts
Vinyl silicone oil, 0.5 portion of platinized platinum, 0.1 part of alkynyl hexamethylene and 20 parts of spare solidliquid mixtures put into high shear homomixer
In, shearing dispersion 15min obtains dispersion liquid under the revolving speed of 1000r/min；By etc. quality coagulant liquid and dispersion liquid stirring
Device obtains mixed liquor with the revolving speed stirring 30min of 600r/min, and mixed liquor is put in vacuum tank, is 800MPa's in vacuum degree
Under the conditions of, it is put under room temperature and stands for 24 hours to get high-intensity weather-proof high casting glue again after standing 15min.
Example 2
By mass fraction be 22% phthalic anhydride and mass fraction be 32% propylene glycol solution 1:3 in mass ratio put into burn
17min is mixed with the revolving speed of 320r/min in cup, beaker is heated to 200 DEG C, is made anti-after isothermal reaction 25min
Gel is answered, according to parts by weight, weighs 32 parts of reaction gels, 22 parts of methyl methacrylates, 2 parts of methyl ethyl ketone peroxides and 3 parts
Mixed impregnant liquor is stirred to get in epoxyeicosatrienoic acid cobalt investment blender；450g basalt fibre is weighed, is soaked with above-mentioned mixed impregnant liquor
Stain basalt fibre, and be put into hot press, it is 2.7MPa in pressure, suppresses 12.5h under conditions of room temperature, after compacting,
Elevated pressure increases temperature to 125 DEG C, continues hot pressing 3.2h, pressure is kept after hot pressing and is naturally cooled to 5.2MPa
Room temperature obtains solidliquid mixture, spare；Under the conditions of ice-water bath, the titanium tetrachloride solution and deionization that are 60% by mass fraction
Water 1:5 in mass ratio is stirred in investment round-bottomed flask and obtains dispersion liquid, and dispersion liquid quality 4% is added into round-bottomed flask
Sodium dihydrogen phosphate, ebuillition of heated reflux 5.2h, obtains reflux product, reflux product is put into centrifugal separator and is centrifugated
It to separation solid, is washed with distilled water 4 times, is put into baking oven dry 15h under conditions of 75 DEG C, grinds and cross 300 mesh
Sieve obtains sieving；According to parts by weight, it is high that 22 parts of vinyl silicone oils, 4 parts of containing hydrogen silicone oils and 4 parts of above-mentioned sieving investments are weighed
In speed shearing dispersion machine, shearing dispersion 22min obtains coagulant liquid under the revolving speed of 1250r/min, according to parts by weight, weighs 52
Part vinyl silicone oil, 0.7 portion of platinized platinum, 0.2 part of alkynyl hexamethylene and 22 parts of spare solidliquid mixtures put into high shear agitations
In machine, shearing dispersion 17min obtains dispersion liquid under the revolving speed of 1050r/min；By etc. quality coagulant liquid and dispersion liquid with stirring
It mixes device and mixed liquor is obtained with the revolving speed stirring 35min of 650r/min, mixed liquor is put in vacuum tank, is 850MPa in vacuum degree
Under conditions of, it is put in again after standing 17min under room temperature and stands 25h to get high-intensity weather-proof high casting glue.
Example 3
By mass fraction be 25% phthalic anhydride and mass fraction be 35% propylene glycol solution 1:3 in mass ratio put into burn
20min is mixed with the revolving speed of 350r/min in cup, beaker is heated to 220 DEG C, is made anti-after isothermal reaction 30min
Gel is answered, according to parts by weight, weighs 35 parts of reaction gels, 24 parts of methyl methacrylates, 3 parts of methyl ethyl ketone peroxides and 4 parts
Mixed impregnant liquor is stirred to get in epoxyeicosatrienoic acid cobalt investment blender；600g basalt fibre is weighed, is soaked with above-mentioned mixed impregnant liquor
Stain basalt fibre, and be put into hot press, it is 2.8MPa in pressure, suppresses 13h under conditions of room temperature, after compacting, rises
High Voltage increases temperature to 130 DEG C, continues hot pressing 3.5h, pressure is kept after hot pressing and naturally cools to room to 5.5MPa
Temperature obtains solidliquid mixture, spare；Titanium tetrachloride solution and deionized water under the conditions of ice-water bath, by mass fraction for 70%
1:5 in mass ratio is stirred in investment round-bottomed flask and obtains dispersion liquid, and the phosphorus of dispersion liquid quality 5% is added into round-bottomed flask
Acid dihydride sodium, ebuillition of heated reflux 5.4h, obtains reflux product, reflux product is put into centrifugal separator and is centrifugally separating to obtain
Solid is separated, is washed with distilled water 5 times, dry 16h under conditions of 80 DEG C is put into baking oven, grinds and cross 300 meshes
Obtain sieving；According to parts by weight, 23 parts of vinyl silicone oils, 5 parts of containing hydrogen silicone oils and 5 parts of above-mentioned sieving investment high speeds are weighed
It shears in dispersion machine, shearing dispersion 25min obtains coagulant liquid under the revolving speed of 1300r/min, according to parts by weight, weighs 54 parts
Vinyl silicone oil, 0.8 portion of platinized platinum, 0.3 part of alkynyl hexamethylene and 24 parts of spare solidliquid mixtures put into high shear homomixer
In, shearing dispersion 20min obtains dispersion liquid under the revolving speed of 1100r/min；By etc. quality coagulant liquid and dispersion liquid stirring
Device obtains mixed liquor with the revolving speed stirring 40min of 700r/min, and mixed liquor is put in vacuum tank, is 900MPa's in vacuum degree
Under the conditions of, it is put in again after standing 20min under room temperature and stands 26h to get high-intensity weather-proof high casting glue.
Comparative example
With the high-intensity weather-proof high casting glue of Dongguan company production as a comparison case to high-intensity weather-proof high produced by the present invention
High-intensity weather-proof high casting glue in casting glue and comparative example carries out performance detection, and testing result is as shown in table 1:
Test method:
Shore hardness test is detected by GB2411 standard；
Tensile strength test is detected by 6329 standard of GB/T；
Elongation at break test is detected using elongation at break test machine；
Impact strength test impact strength tester is detected；
Heat distortion temperature test is detected by GB1634-79 standard；
Weatherability test process are as follows: each casting glue is received into ultraviolet light irradiation, irradiation used ultraviolet-uisible spectrophotometer after 6 hours
Test yellowness index；
Yellowness index test method is tested by the saying of xanthochromia series Δ Yi, is divided by yellowness index:
0 grade: without discoloration, Δ Yi≤1.5；
1 grade: very light discolouration, 1.6 < Δ Yi≤3.0；
2 grades: light discolouration, 3.1 < Δ Yi≤6.0；
3 grades: obvious discoloration, 6.1 < Δ Yi≤9.0；
4 grades: larger discoloration, 9.1 < Δ Yi≤12.0；
5 grades: serious discoloration, 12.0 < Δ Yi；
1 casting glue performance measurement result of table
High, tensile strength and extension at break according to the high-intensity weather-proof high casting glue hardness produced by the present invention of data among the above
Rate is high, excellent in cushion effect, good toughness, and heat distortion temperature is high, and weatherability test post yellowing index is low, good weatherability, has wide
Wealthy application prospect.
Claims (6)
1. a kind of preparation method of high-intensity weather-proof high casting glue, it is characterised in that specific preparation step are as follows:
(1) by mass fraction be 20~25% phthalic anhydride and mass fraction be 30~35% propylene glycol solution by quality
Than in 1:3 investment beaker, with stirring, beaker being heated to, reaction gel is made after isothermal reaction, according to parts by weight, is claimed
Take 30~35 parts of reaction gels, 20~24 parts of methyl methacrylates, 1~3 part of methyl ethyl ketone peroxide and 2~4 parts of epoxyeicosatrienoic acid cobalts
Mixed impregnant liquor is stirred to get in investment blender；
(2) 300~600g basalt fibre is weighed, impregnates basalt fibre with above-mentioned mixed impregnant liquor, and be put into hot press,
Precompressed compacting, after compacting, elevated pressure increases progress hot pressing, and pressure and cooled to room temperature are kept after hot pressing,
Solidliquid mixture is obtained, it is spare；
(3) under the conditions of ice-water bath, titanium tetrachloride solution and deionized water 1:5 in mass ratio are stirred investment round-bottomed flask
In obtain dispersion liquid, into round-bottomed flask be added dispersion liquid quality 3~5% sodium dihydrogen phosphate, ebuillition of heated reflux, returned
Reflux product is put into centrifugal separator and is centrifugally separating to obtain separation solid by apoblema, is washed with distilled water 3~5 times, is put into
It is dry in baking oven, it grinds and 300 meshes excessively obtains sieving；
(4) according to parts by weight, 20~23 parts of vinyl silicone oils, 3~5 parts of containing hydrogen silicone oils and 3~5 parts of above-mentioned sievings are weighed to throw
Enter in high speed shear dispersion machine, shearing dispersion obtains coagulant liquid, according to parts by weight, weighs 50~54 parts of vinyl silicone oils, 0.5
~0.8 portion of platinized platinum, 0.1~0.3 part of alkynyl hexamethylene and 20~24 parts of spare solidliquid mixtures put into high shear homomixer
In, 15~20min of shearing dispersion obtains dispersion liquid under the revolving speed of 1000~1100r/min；
(5) by etc. quality coagulant liquid and dispersion liquid with blender stir to get mixed liquor, mixed liquor is put in quiet in vacuum tank
It sets to be put in again after 15~20min under room temperature and stands 24~26h to get high-intensity weather-proof high casting glue.
2. a kind of preparation method of high-intensity weather-proof high casting glue according to claim 1, it is characterised in that: step (1)
Described in the mass fraction of phthalic anhydride be 20~25%, the mass fraction of propylene glycol solution is 30~35%, in beaker
Speed of agitator is 300~350r/min, and mixing time is 15~20min, and beaker heating temperature is to 190~220 DEG C, isothermal reaction
Time is 20~30min.
3. a kind of preparation method of high-intensity weather-proof high casting glue according to claim 1, it is characterised in that: step (2)
Described in hot press in precompressed pressure be 2.5~2.8MPa, the pressing time be 12~13h, hot pressing pressure to 5.0~
5.5MPa, for hot pressing temperature to 120~130 DEG C, hot pressing time is 3.0~3.5h.
4. a kind of preparation method of high-intensity weather-proof high casting glue according to claim 1, it is characterised in that: step (3)
Described in the mass fraction of titanium tetrachloride solution be 50~70%, ebuillition of heated return time is 5.0~5.4h, in baking oven
Temperature is 70~80 DEG C, and drying time is 14~16h.
5. a kind of preparation method of high-intensity weather-proof high casting glue according to claim 1, it is characterised in that: step (4)
Described in high-speed shearing machine in revolving speed be 1200~1300r/min, shearing jitter time be 20~25min.
6. a kind of preparation method of high-intensity weather-proof high casting glue according to claim 1, it is characterised in that: step (5)
Described in the revolving speed of blender be 600~700r/min, mixing time is 30~40min, in vacuum tank vacuum degree be 800~
900MPa。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810727020.7A CN109111896A (en) | 2018-07-05 | 2018-07-05 | A kind of preparation method of high-intensity weather-proof high casting glue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810727020.7A CN109111896A (en) | 2018-07-05 | 2018-07-05 | A kind of preparation method of high-intensity weather-proof high casting glue |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109111896A true CN109111896A (en) | 2019-01-01 |
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| JP2015038165A (en) * | 2013-07-17 | 2015-02-26 | イズミ物産株式会社 | Organosiloxane-based silicone resin adhesive and method for producing the same |
| CN105086919A (en) * | 2015-08-07 | 2015-11-25 | 东莞市新星有机硅科技有限公司 | Nanometer titanium oxide modified organic silicon bonding agent and preparation method thereof |
| CN105778513A (en) * | 2014-12-18 | 2016-07-20 | 北京科化新材料科技有限公司 | Liquid silicone rubber compound |
| CN106978133A (en) * | 2017-04-21 | 2017-07-25 | 广州惠利电子材料有限公司 | LED packaging silicon rubbers and its preparation method and application |
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| JP2015038165A (en) * | 2013-07-17 | 2015-02-26 | イズミ物産株式会社 | Organosiloxane-based silicone resin adhesive and method for producing the same |
| CN105778513A (en) * | 2014-12-18 | 2016-07-20 | 北京科化新材料科技有限公司 | Liquid silicone rubber compound |
| CN105086919A (en) * | 2015-08-07 | 2015-11-25 | 东莞市新星有机硅科技有限公司 | Nanometer titanium oxide modified organic silicon bonding agent and preparation method thereof |
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