CN105368203B - A kind of ageing-resistant reflecting coating - Google Patents
A kind of ageing-resistant reflecting coating Download PDFInfo
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- CN105368203B CN105368203B CN201510778493.6A CN201510778493A CN105368203B CN 105368203 B CN105368203 B CN 105368203B CN 201510778493 A CN201510778493 A CN 201510778493A CN 105368203 B CN105368203 B CN 105368203B
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Abstract
The invention discloses a kind of ageing-resistant reflecting coating, raw material includes by weight：63~66 parts of water-based acrylic resin, 25~28 parts of waterborne polyurethane resin, 12~15 parts of water-compatible amino resin, 10~15 parts of modified glass microspheres, 17~20 parts of nanomete talc powder, 7~10 parts of bentonite, 13~16 parts of gas-phase silica, 1.5~1.8 parts of silane coupling agent, 5~10 parts of microencapsulated powder oil, 15~18 parts of zinc borate, 22~25 parts of nano-aluminum hydroxide, 2.3~3.8 parts of ABS toughener, 1~2 part of antifoaming agent, 1.2~1.5 parts of mould inhibitor, 12~15 parts of pigment.Reflecting effect of the present invention is good, and wear-resisting, corrosion resistance and ageing-resistant performance are outstanding.
Description
Technical field
The present invention relates to reflecting coating technical field more particularly to a kind of ageing-resistant reflecting coatings.
Background technology
Reflectorized material institute includes resin, pigment, glass microballoon etc. using main raw material(s), and any the same raw material are to reflective
What the performance influence of product was crucial.Wherein, adhering resin must have good workability, splendid bonding energy
Power also requires adhering resin water proofing property, washability, surface layer resin to require to have good if surface does not have the product of protective layer
Transparency, ideal refractive index, excellent weatherability and stability, connecing for each layer resin must also have good compatibility,
The optical characteristics requirement of reflectorized material product, requirement and manufacturing process requirement could be met in this way；For pigment, then require
High transparency, form and aspect stability then require high refractive index, high transparency with the good compatibility of resin for glass microballoon
Property, low devitrification rate, good circularity, good granularity consistency and dispersibility.Often anticorrosion is ageing-resistant for existing reflecting coating
Performance is not ideal enough, and the compartment time is needed to become spraying of doing over again, time-consuming and laborious.
Invention content
Technical problems based on background technology, the present invention propose a kind of ageing-resistant reflecting coating, and reflecting effect is good,
Wear-resisting, corrosion resistance and ageing-resistant performance are outstanding.
A kind of ageing-resistant reflecting coating proposed by the present invention, raw material include by weight：Water-based acrylic resin 63~
66 parts, 25~28 parts of waterborne polyurethane resin, 12~15 parts of water-compatible amino resin, 10~15 parts of modified glass microspheres, nanometer cunning
17~20 parts of mountain flour, 7~10 parts of bentonite, 13~16 parts of gas-phase silica, 1.5~1.8 parts of silane coupling agent, microencapsulation is red
5~10 parts of phosphorus, 15~18 parts of zinc borate, 22~25 parts of nano-aluminum hydroxide, 2.3~3.8 parts of ABS toughener, antifoaming agent 1~2
Part, 1.2~1.5 parts of mould inhibitor, 12~15 parts of pigment.
Preferably, the preparation method of modified glass microspheres is：Glass microballoon is placed in absolute ethyl alcohol and is impregnated, is then carried out
It is cleaned by ultrasonic, after vacuum drying, is placed in the mixed solution containing ruthenium ion and impregnates, then heat up, keep the temperature, filter, wash, does
Dry, firing obtains modified glass microspheres.
Preferably, in the preparation method of modified glass microspheres, the mixed solution containing ruthenium ion includes：0.3~0.6mol/
L yttrium nitrates, 0.5~0.8mol/L triethanolamines, solvent are water.
Preferably, in the preparation method of modified glass microspheres, the temperature of ultrasonic cleaning is 38~41 DEG C, ultrasonic cleaning when
Between be 16~20min, the power of ultrasonic cleaning is 550~580w.
Preferably, in the preparation method of modified glass microspheres, glass microballoon is placed in 1~2h of immersion in absolute ethyl alcohol, so
After be cleaned by ultrasonic, after vacuum drying, be placed in the mixed solution containing ruthenium ion 1~2h of dipping, then heat up 77~80 DEG C,
3.5~3.8h is kept the temperature, is filtered, is washed, it is dry, it fires 18~22min for 500~530 DEG C and obtains modified glass microspheres.
Preferably, the glass microballoon preparation method in modified glass microspheres is as follows：
S1, after mixing aluminum nitrate, zirconium nitrate, cerous nitrate and calcium nitrate, it is added to the water dissolving and obtains mixed solution, then
Sodium hydroxide solution is added dropwise, filter cake cleaning is placed in water and carries out ultrasonic disperse, then heating water bath by filtering, heating water bath
Nitric acid is added dropwise in the process to pH=3~4, obtains colloidal sol a；
S2, ethyl orthosilicate is added in ethyl alcohol and is dissolved, then water is added dropwise, then adjusted pH value to 3~4, be then added dropwise molten
Glue a stirs to get colloidal sol b；
S3, it after addition ethyl acetoacetate stirs evenly into ethyl alcohol, adds tetrabutyl titanate progress and once stirs
To sol c；It is added into ethyl alcohol after magnesium nitrate, chromic nitrate and boric acid are mixed uniformly and obtains solution d；Solution d is added dropwise to sol c
In, secondary agitation is then carried out, adds water, then triple mixing, standing obtains colloidal sol e；
S4, colloidal sol b is stirred, colloidal sol e is added dropwise in whipping process and water obtains colloidal sol f；By the stone containing sorbester p18
Wax oil carries out heating water bath, and colloidal sol f is then added dropwise and enters paraffin oil, then stirs, filters, is dried to obtain gel particle；
S5, gel particle is sintered, cooling obtains glass microballoon.
Preferably, in the S1 of the glass microballoon preparation method in modified glass microspheres, by weight by 12~15 parts of nitric acid
After aluminium, 11~12 parts of zirconium nitrates, 2~4 parts of cerous nitrates and the mixing of 0.4~0.8 part of calcium nitrate, be added to the water dissolving obtain mixing it is molten
Sodium hydroxide solution is then added dropwise in liquid, filtering, and filter cake cleaning is placed in water and carries out ultrasonic disperse, then heating water bath, water
The temperature of bath heating is 70~73 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains colloidal sol a.
Preferably, in the S2 of the glass microballoon preparation method in modified glass microspheres, by weight by 22~25 parts of positive silicon
Acetoacetic ester, which is added in 5~5.8 parts of ethyl alcohol, to be dissolved, then 1~1.3 part of water is added dropwise, and is then adjusted pH value to 3~4, is then added dropwise 6~9
Part colloidal sol a, 45~60min of stirring obtain colloidal sol b.
Preferably, in the S3 of the glass microballoon preparation method in modified glass microspheres, second is added into ethyl alcohol by weight
After ethyl acetoacetic acid ethyl ester stirs evenly, adds 155~158 parts of 4~5h of the primary stirring of tetrabutyl titanates progress and obtain sol c；To
It is added in ethyl alcohol after 13~16 parts of magnesium nitrates, 11~14 parts of chromic nitrates and 2~2.5 parts of boric acid are mixed uniformly and obtains solution d；By solution
D is added dropwise in sol c, is then carried out 1~1.5h of secondary agitation, is added water, then 25~28h of triple mixing, and standing 25~
28h obtains colloidal sol e.
Preferably, in the S4 of the glass microballoon preparation method in modified glass microspheres, by weight by 60~70 parts of colloidal sol b
It is stirred, 20~23 parts of colloidal sol e is added dropwise in whipping process and 7~10 parts of water obtain colloidal sol f；By the paraffin oil containing sorbester p18
Heating water bath is carried out, the temperature of heating water bath is 62~65 DEG C, and colloidal sol f is then added dropwise and enters paraffin oil, then stirs, filters, does
It is dry to obtain gel particle.
Preferably, in the S5 of the glass microballoon preparation method in modified glass microspheres, the concrete operations of sintering are：It is warming up to
130~140 DEG C, 2.5~2.8h is kept the temperature, is then warming up to 730~750 DEG C with the heating rate of 1.5~2.5 DEG C/min, heat preservation
40~60min is warming up to 820~830 DEG C, keeps the temperature 20~25min.
Using water or ethyl alcohol as solvent in glass microballoon preparation method, does not interfere with reaction and generate, there is no need to limited amounts；
Acetylacetone,2,4-pentanedione alleviates the hydrolysis rate of butyl titanate as buffer, without limited amount；Paraffin oil containing sorbester p18 is made
For flotation agent, it is not necessarily to limited amount.
In the glass microballoon preparation process of the present invention, SiO is prepared by raw material of ethyl orthosilicate2Colloidal sol, by limiting just
The ratio of silester and ethyl alcohol, makes SiO2Collosol concentration is larger, prevent in the subsequent sintering process microballon volume contraction make greatly
At there is stomata generation inside microballon；The present invention is using aluminum nitrate, zirconium nitrate, cerous nitrate and calcium nitrate as raw material, after lye is added, shape
At corresponding hydroxide sediment, after cleaning, carrying out ultrasonic disperse makes hydroxide sediment be uniformly distributed in water,
Then nitric acid is added dropwise and forms colloidal sol a；Colloidal sol a is added dropwise in colloidal sol b, make teos hydrolysis polycondensation process be complexed aluminium,
Zirconium, cerium, calcium ion；And using butyl titanate as raw material, magnesium nitrate, chromic nitrate and boric acid is added in cooperation, and then hydrolysis obtains
TiO2Colloidal sol, by TiO2Colloidal sol, which is added colloidal sol b and is stirred, makes silester be fully hydrolyzed and be complexed as glass with butyl titanate
Network structure；Colloidal sol f is instilled in paraffin oil, colloidal sol becomes spherical shape in paraffin oil due to the effect of surface tension, in water
Stirred in bath, shorten transformation time of the colloidal sol to gel, using sorbester p18 as dispersant, make spherical sol in paraffin oil almost
Do not occur to reunite and granularity difference is smaller, then filtration drying obtains gel microballon；Since still there is stone on the gel particle surface of acquisition
Wax oil first heats up to remove paraffin oil, prevents paraffin oil on fire and keeps sample temperature excessively high and burst, and then slowly heating prevents
Organic principle volatilization in gel microballon is too fast and leads to that stomata is destroyed or generated inside microballon；The present invention is in glass microballoon
Middle introducing aluminium oxide, zirconium oxide, cerium oxide, calcium oxide, magnesia, chromium oxide and boron oxide cooperate, and improve glass
The chemical stability of microballon makes glass microballoon compact structure obtained by the present invention, and translucency is preferable, refractive index up to 1.8~1.9,
Greatly strengthen reflectorizing of paint performance of the present invention.
Using water-based acrylic resin, waterborne polyurethane resin, water-compatible amino resin as film forming matter in the present invention, greatly
Width improves weather-proof, the water-fast, wear-resisting property of the present invention, and makes that adhesive force of the present invention is good, curing rate is fast；Due to modified glass
Glass microballon, nanomete talc powder, bentonite and gas-phase silica have very high specific surface area, promote the cross-linked structure pole of the present invention
It is close, greatly improves the corrosion resistance of the present invention, and is enriched since nanomete talc powder, bentonite and gas-phase silica have
Surface anticorrosive functional group, further increase the present invention corrosion resistance；Bentonite and gas-phase silica are as the present invention
Thixotropic agent and thickener, moreover it is possible to anti-precipitation, resist sagging；It uses after modified glass microspheres cleaning and is carried out in dipping rare-earth salt solution
Reaction, then fires, makes bead surface deposited oxide yttrium, since microballon is mainly by SiO2And Al2O3Equal oxides composition and table
Face is there are many-OH groups, and the yttrium atom in yttrium compound has very strongly active, can open O-H keys, Si-O keys and Al-O keys
And Y-O keys are generated, while the yttrium atom of bead surface can also open c h bond and generate Y-C keys, it is bright to play the role of bridge joint
The aobvious interface binding power for enhancing modified glass microspheres and film forming matter, and the addition of modified glass microspheres also improves composite wood
The thermal stability of material；Modified glass microspheres, nanomete talc powder, bentonite and gas-phase silica match, dioctyl azelate,
Under phenyl alkylsulfonate auxiliary, can more it be uniformly dispersed in film forming matter, then connect by silane coupling agent and film forming matter
Branch, further increases the compatibility between above-mentioned each raw material；Microencapsulated powder oil is as phosphorus flame retardant, with zinc borate, nanometer
Aluminium hydroxide is used cooperatively, and substantially increases the oxygen index (OI) of the present invention, improves the flame retardant property of the present invention, and zinc borate, nanometer
Aluminium hydroxide can not only absorb a large amount of thermal energy during burning, and go back decomposable asymmetric choice net and generate water, to inhibit in combustion process
Smog formed.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of ageing-resistant reflecting coating proposed by the present invention, raw material include by weight：63 parts of water-based acrylic resin,
28 parts of waterborne polyurethane resin, 12 parts of water-compatible amino resin, 15 parts of modified glass microspheres, 17 parts of nanomete talc powder, bentonite 10
Part, 13 parts of gas-phase silica, 1.8 parts of silane coupling agent, 5 parts of microencapsulated powder oil, 18 parts of zinc borate, nano-aluminum hydroxide 22
Part, 3.8 parts of ABS toughener, 1 part of antifoaming agent, 1.5 parts of mould inhibitor, 12 parts of pigment.
The preparation method of modified glass microspheres is：Glass microballoon is placed in absolute ethyl alcohol and impregnates 2h, then carries out ultrasound
The temperature of cleaning, ultrasonic cleaning is 38 DEG C, and the time of ultrasonic cleaning is 20min, and the power of ultrasonic cleaning is 550w, vacuum drying
Afterwards, it is placed in the mixed solution containing ruthenium ion and impregnates 2h, then heat up 77 DEG C, keep the temperature 3.8h, filter, wash, it is dry, 500 DEG C
It fires 22min and obtains modified glass microspheres；Wherein the mixed solution containing ruthenium ion includes：0.3mol/L yttrium nitrates, 0.8mol/
L triethanolamines, solvent are water.
Above-mentioned glass microballoon preparation method is as follows：
S1, it after by weight mixing 12 parts of aluminum nitrates, 12 parts of zirconium nitrates, 2 parts of cerous nitrates and 0.8 part of calcium nitrate, is added
Dissolving obtains mixed solution in water, and sodium hydroxide solution is then added dropwise, and filters, and filter cake cleaning is placed in water and carries out ultrasound point
It dissipates, then heating water bath, the temperature of heating water bath is 70 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains molten
Glue a；
S2,25 parts of ethyl orthosilicates are added in 5 parts of ethyl alcohol dissolve by weight, then 1.3 parts of water are added dropwise, then adjust pH
Then 6 parts of colloidal sol a are added dropwise to 3~4 in value, stirring 60min obtains colloidal sol b；
S3, be added by weight into ethyl alcohol after ethyl acetoacetate stirs evenly, add 155 parts of tetrabutyl titanates into
The primary stirring 5h of row obtains sol c；It is added after 13 parts of magnesium nitrates, 14 parts of chromic nitrates and 2 parts of boric acid are mixed uniformly and obtains into ethyl alcohol
Solution d；Solution d is added dropwise in sol c, secondary agitation 1.5h is then carried out, adds water, then triple mixing 25h, is stood
28h obtains colloidal sol e；
S4,60 parts of colloidal sol b are stirred by weight, be added dropwise 23 parts of colloidal sol e in whipping process and 7 parts of water obtain it is molten
Glue f；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 65 DEG C, and colloidal sol f is then added dropwise and enters paraffin
Then oil stirs, filtering is dried to obtain gel particle；
S5, gel particle is warming up to 130 DEG C, keeps the temperature 2.8h, is then warming up to 750 with the heating rate of 1.5 DEG C/min
DEG C, 40min is kept the temperature, is warming up to 830 DEG C, keeps the temperature 20min, cooling obtains glass microballoon.
Embodiment 2
A kind of ageing-resistant reflecting coating proposed by the present invention, raw material include by weight：66 parts of water-based acrylic resin,
25 parts of waterborne polyurethane resin, 15 parts of water-compatible amino resin, 10 parts of modified glass microspheres, 20 parts of nanomete talc powder, bentonite 7
Part, 16 parts of gas-phase silica, 1.5 parts of silane coupling agent, 10 parts of microencapsulated powder oil, 15 parts of zinc borate, nano-aluminum hydroxide 25
Part, 2.3 parts of ABS toughener, 2 parts of antifoaming agent, 1.2 parts of mould inhibitor, 15 parts of pigment.
The preparation method of modified glass microspheres is：Glass microballoon is placed in absolute ethyl alcohol and impregnates 1h, then carries out ultrasound
The temperature of cleaning, ultrasonic cleaning is 41 DEG C, and the time of ultrasonic cleaning is 16min, and the power of ultrasonic cleaning is 580w, vacuum drying
Afterwards, it is placed in the mixed solution containing ruthenium ion and impregnates 1h, then heat up 80 DEG C, keep the temperature 3.5h, filter, wash, it is dry, 530 DEG C
It fires 18min and obtains modified glass microspheres；Wherein the mixed solution containing ruthenium ion includes：0.6mol/L yttrium nitrates, 0.5mol/
L triethanolamines, solvent are water.
Above-mentioned glass microballoon preparation method is as follows：
S1, it after by weight mixing 15 parts of aluminum nitrates, 11 parts of zirconium nitrates, 4 parts of cerous nitrates and 0.4 part of calcium nitrate, is added
Dissolving obtains mixed solution in water, and sodium hydroxide solution is then added dropwise, and filters, and filter cake cleaning is placed in water and carries out ultrasound point
It dissipates, then heating water bath, the temperature of heating water bath is 73 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains molten
Glue a；
S2,22 parts of ethyl orthosilicates are added in 5.8 parts of ethyl alcohol dissolve by weight, then 1 part of water is added dropwise, then adjust pH
Then 9 parts of colloidal sol a are added dropwise to 3~4 in value, stirring 45min obtains colloidal sol b；
S3, be added by weight into ethyl alcohol after ethyl acetoacetate stirs evenly, add 158 parts of tetrabutyl titanates into
The primary stirring 4h of row obtains sol c；It is added after 16 parts of magnesium nitrates, 11 parts of chromic nitrates and 2.5 parts of boric acid are mixed uniformly and obtains into ethyl alcohol
To solution d；Solution d is added dropwise in sol c, secondary agitation 1h is then carried out, adds water, then triple mixing 28h, is stood
25h obtains colloidal sol e；
S4,70 parts of colloidal sol b are stirred by weight, 20 parts of colloidal sol e is added dropwise in whipping process and 10 parts of water obtain
Colloidal sol f；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 62 DEG C, and colloidal sol f is then added dropwise and enters paraffin
Then oil stirs, filtering is dried to obtain gel particle；
S5, gel particle is warming up to 140 DEG C, keeps the temperature 2.5h, is then warming up to 730 with the heating rate of 2.5 DEG C/min
DEG C, 60min is kept the temperature, is warming up to 820 DEG C, keeps the temperature 25min, cooling obtains glass microballoon.
Embodiment 3
A kind of ageing-resistant reflecting coating proposed by the present invention, raw material include by weight：65 parts of water-based acrylic resin,
26 parts of waterborne polyurethane resin, 14 parts of water-compatible amino resin, 12 parts of modified glass microspheres, 19 parts of nanomete talc powder, bentonite 8
Part, 15 parts of gas-phase silica, 1.6 parts of silane coupling agent, 8 parts of microencapsulated powder oil, 16 parts of zinc borate, nano-aluminum hydroxide 24
Part, 2.8 parts of ABS toughener, 1.8 parts of antifoaming agent, 1.3 parts of mould inhibitor, 14 parts of pigment.
The preparation method of modified glass microspheres is：Glass microballoon is placed in absolute ethyl alcohol and impregnates 1.3h, is then surpassed
Sound cleans, and the temperature of ultrasonic cleaning is 40 DEG C, and the time of ultrasonic cleaning is 17min, and the power of ultrasonic cleaning is 570w, and vacuum is dry
It after dry, be placed in the mixed solution containing ruthenium ion and impregnate 1.5h, then heat up 79 DEG C, keep the temperature 3.6h, filter, wash, it is dry,
It fires 19min for 520 DEG C and obtains modified glass microspheres；Wherein the mixed solution containing ruthenium ion includes：0.5mol/L yttrium nitrates,
0.6mol/L triethanolamines, solvent are water.
Above-mentioned glass microballoon preparation method is as follows：
S1, after 14 parts of aluminum nitrates, 11.3 parts of zirconium nitrates, 3.4 parts of cerous nitrates and 0.5 part of calcium nitrate are mixed by weight,
It is added to the water dissolving and obtains mixed solution, sodium hydroxide solution is then added dropwise, filter, filter cake cleaning is placed in water and is surpassed
Sound disperses, then heating water bath, and the temperature of heating water bath is 72 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains
To colloidal sol a；
S2,23 parts of ethyl orthosilicates are added in 5.6 parts of ethyl alcohol dissolve by weight, then 1.1 parts of water are added dropwise, then adjusted
Then 8 parts of colloidal sol a are added dropwise to 3~4 in pH value, stirring 50min obtains colloidal sol b；
S3, be added by weight into ethyl alcohol after ethyl acetoacetate stirs evenly, add 157 parts of tetrabutyl titanates into
The primary stirring 4h of row obtains sol c；It is added after 15 parts of magnesium nitrates, 12 parts of chromic nitrates and 2.3 parts of boric acid are mixed uniformly and obtains into ethyl alcohol
To solution d；Solution d is added dropwise in sol c, secondary agitation 1.2h is then carried out, adds water, then triple mixing 27h, it is quiet
It sets 26h and obtains colloidal sol e；
S4,68 parts of colloidal sol b are stirred by weight, be added dropwise 21 parts of colloidal sol e in whipping process and 9 parts of water obtain it is molten
Glue f；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 63 DEG C, and colloidal sol f is then added dropwise and enters paraffin
Then oil stirs, filtering is dried to obtain gel particle；
S5, gel particle is warming up to 138 DEG C, keeps the temperature 2.6h, is then warming up to 735 with the heating rate of 2.2 DEG C/min
DEG C, 55min is kept the temperature, is warming up to 822 DEG C, keeps the temperature 23min, cooling obtains glass microballoon.
Embodiment 4
A kind of ageing-resistant reflecting coating proposed by the present invention, raw material include by weight：64 parts of water-based acrylic resin,
27 parts of waterborne polyurethane resin, 13 parts of water-compatible amino resin, 14 parts of modified glass microspheres, 18 parts of nanomete talc powder, bentonite 9
Part, 14 parts of gas-phase silica, 1.7 parts of silane coupling agent, 6 parts of microencapsulated powder oil, 17 parts of zinc borate, nano-aluminum hydroxide 23
Part, 3.2 parts of ABS toughener, 1.6 parts of antifoaming agent, 1.4 parts of mould inhibitor, 13 parts of pigment.
The preparation method of modified glass microspheres is：Glass microballoon is placed in absolute ethyl alcohol and impregnates 1.7h, is then surpassed
Sound cleans, and the temperature of ultrasonic cleaning is 39 DEG C, and the time of ultrasonic cleaning is 18min, and the power of ultrasonic cleaning is 560w, and vacuum is dry
It after dry, be placed in the mixed solution containing ruthenium ion and impregnate 1.8h, then heat up 78 DEG C, keep the temperature 3.7h, filter, wash, it is dry,
It fires 20min for 510 DEG C and obtains modified glass microspheres；Wherein the mixed solution containing ruthenium ion includes：0.4mol/L yttrium nitrates,
0.7mol/L triethanolamines, solvent are water.
Above-mentioned glass microballoon preparation method is as follows：
S1, after 13 parts of aluminum nitrates, 11.5 parts of zirconium nitrates, 2.6 parts of cerous nitrates and 0.6 part of calcium nitrate are mixed by weight,
It is added to the water dissolving and obtains mixed solution, sodium hydroxide solution is then added dropwise, filter, filter cake cleaning is placed in water and is surpassed
Sound disperses, then heating water bath, and the temperature of heating water bath is 71 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains
To colloidal sol a；
S2,24 parts of ethyl orthosilicates are added in 5.3 parts of ethyl alcohol dissolve by weight, then 1.2 parts of water are added dropwise, then adjusted
Then 7 parts of colloidal sol a are added dropwise to 3~4 in pH value, stirring 55min obtains colloidal sol b；
S3, be added by weight into ethyl alcohol after ethyl acetoacetate stirs evenly, add 156 parts of tetrabutyl titanates into
The primary stirring 5h of row obtains sol c；It is added after 14 parts of magnesium nitrates, 13 parts of chromic nitrates and 2.2 parts of boric acid are mixed uniformly and obtains into ethyl alcohol
To solution d；Solution d is added dropwise in sol c, secondary agitation 1.4h is then carried out, adds water, then triple mixing 26h, it is quiet
It sets 27h and obtains colloidal sol e；
S4,65 parts of colloidal sol b are stirred by weight, be added dropwise 22 parts of colloidal sol e in whipping process and 8 parts of water obtain it is molten
Glue f；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 64 DEG C, and colloidal sol f is then added dropwise and enters paraffin
Then oil stirs, filtering is dried to obtain gel particle；
S5, gel particle is warming up to 135 DEG C, keeps the temperature 2.7h, is then warming up to 745 with the heating rate of 1.8 DEG C/min
DEG C, 45min is kept the temperature, is warming up to 828 DEG C, keeps the temperature 21min, cooling obtains glass microballoon.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of ageing-resistant reflecting coating, which is characterized in that its raw material includes by weight：Water-based acrylic resin 63~66
Part, 25~28 parts of waterborne polyurethane resin, 12~15 parts of water-compatible amino resin, 10~15 parts of modified glass microspheres, nano-talc
17~20 parts of powder, 7~10 parts of bentonite, 13~16 parts of gas-phase silica, 1.5~1.8 parts of silane coupling agent, microencapsulated powder oil
5~10 parts, 15~18 parts of zinc borate, 22~25 parts of nano-aluminum hydroxide, 2.3~3.8 parts of ABS toughener, 1~2 part of antifoaming agent,
1.2~1.5 parts of mould inhibitor, 12~15 parts of pigment；
The preparation method of modified glass microspheres is：Glass microballoon is placed in absolute ethyl alcohol and is impregnated, is then cleaned by ultrasonic, very
It after sky is dry, is placed in the mixed solution containing ruthenium ion and impregnates, then heat up, keep the temperature, filter, wash, dry, firing is changed
Property glass microballoon；
Glass microballoon preparation method in modified glass microspheres is as follows：
S1, after mixing aluminum nitrate, zirconium nitrate, cerous nitrate and calcium nitrate, it is added to the water dissolving and obtains mixed solution, be then added dropwise
Filter cake cleaning is placed in water and carries out ultrasonic disperse, then heating water bath by sodium hydroxide solution, filtering, heating water bath process
Middle dropwise addition nitric acid obtains colloidal sol a to pH=3~4；
S2, ethyl orthosilicate is added in ethyl alcohol and is dissolved, then water is added dropwise, then adjusted pH value to 3~4, colloidal sol a is then added dropwise,
Stir to get colloidal sol b；
S3, be added into ethyl alcohol after ethyl acetoacetate stirs evenly, add tetrabutyl titanate once stirred to get it is molten
Glue c；It is added into ethyl alcohol after magnesium nitrate, chromic nitrate and boric acid stir evenly and obtains solution d；Solution d is added dropwise in sol c,
Then secondary agitation is carried out, adds water, then triple mixing, standing obtains colloidal sol e；
S4, colloidal sol b is stirred, colloidal sol e is added dropwise in whipping process and water obtains colloidal sol f；By the paraffin oil containing sorbester p18
Heating water bath is carried out, colloidal sol f is then added dropwise and enters paraffin oil, then stirs, filters, is dried to obtain gel particle；
S5, gel particle is sintered, cooling obtains glass microballoon.
2. ageing-resistant reflecting coating according to claim 1, which is characterized in that in the preparation method of modified glass microspheres, contain
The mixed solution of ruthenium ion includes：0.3~0.6mol/L yttrium nitrates, 0.5~0.8mol/L triethanolamines, solvent are water.
3. ageing-resistant reflecting coating according to claim 1 or claim 2, which is characterized in that in the preparation method of modified glass microspheres,
The temperature of ultrasonic cleaning is 38~41 DEG C, and the time of ultrasonic cleaning is 16~20min, and the power of ultrasonic cleaning is 550~580w.
4. ageing-resistant reflecting coating according to claim 1 or claim 2, which is characterized in that in the preparation method of modified glass microspheres,
Glass microballoon is placed in 1~2h of immersion in absolute ethyl alcohol, is then cleaned by ultrasonic, after vacuum drying, is placed in containing ruthenium ion
1~2h is impregnated in mixed solution, is then heated up 77~80 DEG C, 3.5~3.8h is kept the temperature, is filtered, and is washed, it is dry, 500~530 DEG C
It fires 18~22min and obtains modified glass microspheres.
5. ageing-resistant reflecting coating according to claim 1 or claim 2, which is characterized in that the glass microballoon in modified glass microspheres
In the S1 of preparation method, by weight by 12~15 parts of aluminum nitrates, 11~12 parts of zirconium nitrates, 2~4 parts of cerous nitrates and 0.4~0.8
After part calcium nitrate mixing, it is added to the water dissolving and obtains mixed solution, sodium hydroxide solution is then added dropwise, filter, filter cake is cleaned
It is placed in water and carries out ultrasonic disperse, then heating water bath, the temperature of heating water bath is 70~73 DEG C, is dripped during heating water bath
Add nitric acid to pH=3~4, obtains colloidal sol a.
6. ageing-resistant reflecting coating according to claim 1 or claim 2, which is characterized in that the glass microballoon in modified glass microspheres
In the S2 of preparation method, 22~25 parts of ethyl orthosilicates is added in 5~5.8 parts of ethyl alcohol dissolves by weight, then it is added dropwise 1~
1.3 parts of water then adjust pH value to 3~4, and 6~9 parts of colloidal sol a are then added dropwise, and 45~60min of stirring obtains colloidal sol b.
7. ageing-resistant reflecting coating according to claim 1 or claim 2, which is characterized in that the glass microballoon in modified glass microspheres
In the S3 of preparation method, after addition ethyl acetoacetate stirs evenly by weight into ethyl alcohol, 155~158 parts of titaniums are added
Sour N-butyl carries out 4~5h of primary stirring and obtains sol c；13~16 parts of magnesium nitrates, 11~14 parts of chromic nitrates are added into ethyl alcohol
Solution d is obtained after being mixed uniformly with 2~2.5 parts of boric acid；Solution d is added dropwise in sol c, 1~1.5h of secondary agitation is then carried out,
Water is added, then 25~28h of triple mixing, stands 25~28h and obtain colloidal sol e.
8. ageing-resistant reflecting coating according to claim 1 or claim 2, which is characterized in that the glass microballoon in modified glass microspheres
In the S4 of preparation method, 60~70 parts of colloidal sol b are stirred by weight, 20~23 parts of colloidal sol e are added dropwise in whipping process
Colloidal sol f is obtained with 7~10 parts of water；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 62~65 DEG C,
Then colloidal sol f is added dropwise and enters paraffin oil, then stirs, filters, be dried to obtain gel particle.
9. ageing-resistant reflecting coating according to claim 1 or claim 2, which is characterized in that the glass microballoon in modified glass microspheres
In the S5 of preparation method, the concrete operations of sintering are：130~140 DEG C are warming up to, 2.5~2.8h is kept the temperature, then with 1.5~2.5
DEG C/heating rate of min is warming up to 730~750 DEG C, keeps the temperature 40~60min, it is warming up to 820~830 DEG C, heat preservation 20~
25min。
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| CN106519754A (en) * | 2016-11-08 | 2017-03-22 | 佛山佳牧乐科技有限公司 | Anti-corrosion reflective coating |
| CN106995642A (en) * | 2017-05-22 | 2017-08-01 | 安徽三义和能源科技有限公司 | A kind of environmental protection aging resistant coating |
| CN107236455A (en) * | 2017-07-26 | 2017-10-10 | 合肥华盖光伏科技有限公司 | It is a kind of for anti-aging paint of street lamp and preparation method thereof |
| CN108659694B (en) * | 2018-06-15 | 2020-10-23 | 惠州学院 | Polyurethane wood lacquer |
| CN111909578A (en) * | 2020-07-17 | 2020-11-10 | 张贞霞 | Semitransparent multifunctional water-based paint |
| CN111849407A (en) * | 2020-07-28 | 2020-10-30 | 浙江伟星实业发展股份有限公司 | Glue suitable for zipper, waterproof zipper and preparation method of waterproof zipper |
| CN113248956A (en) * | 2021-05-08 | 2021-08-13 | 温州银田交通标牌有限公司 | Traffic sign reflecting paint and preparation method thereof |
| CN116515190B (en) * | 2023-05-29 | 2024-03-08 | 重庆维斯顿实业有限公司 | Ageing-resistant low-migration polyethylene pipe and preparation method thereof |
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| CN102020877A (en) * | 2010-10-13 | 2011-04-20 | 天津大学 | Rear-earth surface-modified hollow glass microsphere and preparation method thereof |
| CN103602188A (en) * | 2013-11-28 | 2014-02-26 | 王立明 | Water-based paint applied in aluminum-plastic plates and color steel coiled material |
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