CN103421357B - A kind of preparation technology with the Study On Mica of high durable performance - Google Patents
A kind of preparation technology with the Study On Mica of high durable performance Download PDFInfo
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Abstract
The present invention relates to a kind of preparation technology with the Study On Mica of high durable performance, it for base material, adopts SiO with the pearly pigment of the certain series made at the metal oxide such as mica surface cladding titanium dioxide, ferric oxide with certain grain size distribution
2, Al
2o
3, CeO
2carry out surface coverage etc. light stability material to base material, recycle silicon alkane coupling agent KH570 carries out organic modification to surface of pigments, through the Study On Mica with high-weatherability that suction filtration, washing, drying obtain.The present invention is reasonable in design, simple to operate, equipment cost and energy consumption is low, color and glossiness is good, the preparation technology with the Study On Mica of high durable performance that is suitable for scale operation, is applicable to automobile, boats and ships, exterior decoration etc. and requires higher occasion to weathering resistance.
Description
Technical field
The present invention relates to a kind of preparation technology with the Study On Mica of high durable performance, it can prepare the Study On Mica with high durable performance, belongs to the preparation of the weather resistant pearl pigment based on the weather-proof cladding process of multilayer inorganic-organic hybrid compound.
Background technology
Pearly pigment take mica sheet as base material, deposits one or more layers thin layer of metal oxide and the micro mist that formed in its surface chemistry, is the high performance material as improving product value added.Compared with other pigment, pearly pigment has special surface tissue, higher refractive index and good transparency, and in transparent medium, pearly pigment can create the effect identical with pearliness.At present, pearly pigment is widely applied in various fields such as coating, ink, plastics, printing, makeup and food product pack.
Along with socioeconomic development, the Application Areas of pearly pigment has expanded to the changeable occasion of the environment such as automotive lacquer, outdoor architecture decoration gradually.But due to most of pearly pigment employing TiO
2carry out coated, and TiO
2there is photochemical activity, highly active atomic oxygen can be released under the irradiation of light, destroy various organic coupling material, double bond in macromolecular chain is ruptured, cause the efflorescence of paint film or other connection materials, thus affect the work-ing life of macromolecular material, such as, when using in automobile finish without the pearly pigment of weather-proof process, within 1 year, the phenomenon such as variable color, loss of gloss will be there is.Therefore, improve the weathering resistance of pearly pigment, with the weather condition adapting to constantly change, there is important production practice meaning.
Du pont company first successfully develops the TiO with superpower weathering resistance
2pigment, even and the domestic research to pearly pigment weathering resistance is perfect not.At present, the weathering resistance improving pearly pigment generally can by improving the transformation efficiency of rutile titanium dioxide or mica titanium nacreous material being carried out to the approach such as surface modification treatment and realize.The preparation technology of existing weather resistant pearl pigment mainly contains: at the outer metal that coated one deck light is stable again of titanium dioxide coating or nonmetal oxide protective layer, as cerium oxide, zinc oxide, silicon oxide etc., to block or shielding ultraviolet rays, the photolytic activity of titanium dioxide is reduced; Or modification is carried out to surface of pigments, as coated organic coupling agent etc., improve the method such as pigment and organic avidity.
But at present existing enterprise often adopts single mode to carry out weather-proof level improvement, the such as only inorganic light stability material of coated one deck, or only adopt coupling agent to carry out organic modification.But these preparation technologies effectively can not suppress the photolytic activity of titanium dioxide, obviously can not strengthen the avidity of pigment and resin, and easily cause pearly pigment to lump, the important indicator such as depth of shade, opacifying power, brightness of pigment obviously reduces, and the grade of pearly pigment also can be caused to reduce simultaneously.Therefore coated certain thickness and the multiple inorganic light stability material that adulterates, and to adopt suitable organic coupling agent to carry out surface modification to pigment be improve the principal element of pearly pigment weathering resistance.
Patent at present about pearly pigment preparation technology has a lot, as China Patent Publication No.: 101235227, disclose a kind of preparation method of mica titanium nacreous material, its adopt be partially converted into the titanium tetrachloride of titanyl sulfate, iron(ic) chloride, iron protochloride or titanium tetrachloride and iron(ic) chloride mixed solution as deposition agent, urea is as neutralizing agent, urea adopts and adds in batches, and the mixing salt of hydrolysising titanium salt, molysite or titanium and iron prepares the method for Study On Mica.The method operating procedure is simple, but the decomposition rate due to urea is difficult to be consistent with the hydrolysis rate of titanium salt, be easier to produce free metatitanic acid particle, affect the gloss of pigment, the metatitanic acid particle simultaneously dissociated in a large number can make the filtration of suspension and washing that difficulty occurs, and feeds in raw material because preparation process employing is disposable, can not ensure that deposition agent is coated on mica surface uniformly, the glossiness of pigment is reduced, and reduces the dispersing property of pigment.
And for example China Patent Publication No.: 101517011, disclose a kind of synthetic mica based pearlescent pigments of contain ferrite, it take synthetic mica as substrate, carries out surface treatment, make the method that the reflectivity of pearly pigment and colourity keep stable to the ferrite coating through calcining.But the method is only applicable to synthetic mica, and need in its last handling process to add epoxy silane and aminosilane two kinds of coupling agents, add the production cost of product.
The present invention to have compared with the silvery white mica titanium nacreous material of high-rutile type titanium dioxide transformation efficiency, illusion-colour mica titanium nacreous material, the golden glory series pearly pigment of painted mica ferrotianium and the iron mica metal glory series pearly pigment that obtains at the direct coated iron oxide of mica surface for base material, adopts SiO respectively
2, Al
2o
3, CeO
2carry out surface coverage etc. light stability material to base material, recycle silicon alkane coupling agent KH570 carries out organic modification to surface of pigments, thus prepares the pearly pigment had compared with high-weatherability.This pigment is applicable to automobile, boats and ships, exterior decoration etc. and requires higher occasion to weathering resistance.
The present invention to have compared with the silvery white mica titanium nacreous material of high-rutile type titanium dioxide transformation efficiency, illusion-colour mica titanium nacreous material, the golden glory series pearly pigment of painted mica ferrotianium and the iron mica metal glory series pearly pigment that obtains at the direct coated iron oxide of mica surface for base material, adopts SiO respectively
2, Al
2o
3, CeO
2carry out surface coverage etc. light stability material to base material, recycle silicon alkane coupling agent KH570 carries out organic modification to surface of pigments, thus prepares the pearly pigment had compared with high-weatherability.This pigment is applicable to automobile, boats and ships, exterior decoration etc. and requires higher occasion to weathering resistance.
Summary of the invention
Technical problem to be solved by this invention to overcome in prior art existing above-mentioned deficiency, and provide a kind of reasonable in design, simple to operate, equipment cost and energy consumption is low, color and glossiness is good, the preparation technology with the Study On Mica of high durable performance that is suitable for scale operation.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation technology with the Study On Mica of high durable performance, is characterized in that: its preparation process is:
A. 40g transparent sheet-like base material is dropped into reactor, be made into deionized water the suspension that mass percent concentration is 10%, at the uniform velocity stir and be warming up to 75-85 DEG C, by alkaline solution adjust ph to 8.5-10;
B. by the massfraction of dehydrated alcohol and silicon-dioxide be choose any one kind of them in the methyl silicate of 28%, tetraethoxy or two kinds be made into silicon precursor alcohol mixeding liquid, with constant flow pump, 10-30g silicon precursor alcohol mixeding liquid is pumped in suspension, add in 2h, continue reaction 1h afterwards, obtain mother liquor;
C. mother liquor is filtered, after deionized water wash 4 times, dry 6-8 hour in the baking oven of 100 DEG C, then the pigment obtained after drying is dropped into reactor again, the secondary suspension that mass percent concentration is 10% is made into deionized water, at the uniform velocity stir and be warming up to 75-85 DEG C, by alkaline solution adjust ph to 7-8.5;
D. by a certain proportion of AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3/ CeCl
3mixed aqueous solution, with constant flow pump by 10-20mL AlCl
3/ CeCl
3mixed aqueous solution pumps in secondary suspension, and co-precipitation hydridization is coated on pigment flakes, and uses alkaline solution equilibrium ph, adds in 1h, continues afterwards to stir 20min, obtains secondary mother liquid;
E. secondary mother liquid is filtered, form filter cakes with deionized water rinsing 3 times, then by filter cake again dispersed with stirring in deionized water, obtain three suspension that pigment mass percentage concentration is 10%, at the uniform velocity stir and be warming up to 70-80 DEG C, and by alkaline solution adjust ph to 8.5-9.5;
F. silane coupling agent and dehydrated alcohol are made into silane coupling agent alcohol mixeding liquid, with constant flow pump, 6-20g silane coupling agent alcohol mixeding liquid are pumped in three suspension, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors;
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain that there is the pearly pigment compared with high durable performance.
Transparent sheet-like base material of the present invention is silvery white mica titanium nacreous material, is called for short FWD103, TiO in described silvery white mica titanium nacreous material
2clad ratio be 28-32%.
Transparent sheet-like base material of the present invention is illusion-colour mica titanium nacreous material, is called for short FWD225, TiO in described illusion-colour mica titanium nacreous material
2clad ratio be 50-55%.
Transparent sheet-like base material of the present invention is painted mica ferrotianium golden glory series pearly pigment, is called for short FWD300, TiO in described painted mica ferrotianium golden glory series pearly pigment
2clad ratio be 35-40%, Fe
2o
3clad ratio be 2-5%.
Transparent sheet-like base material of the present invention is iron mica metal glory series pearly pigment, is called for short FWD502, Fe in described iron mica metal glory series pearly pigment
2o
3clad ratio be 40-45%.
The median size of transparent sheet-like base material of the present invention is 10-60 μm.
The median size of transparent sheet-like base material of the present invention is 5-25 μm.
In step a of the present invention and step e, described alkaline solution is ammonia aqueous solution; In described step c and steps d, described alkaline solution is aqueous sodium hydroxide solution.
In step b of the present invention, SiO in described silicon precursor alcohol mixeding liquid
2massfraction be 14%-20%.
In steps d of the present invention, described AlCl
3/ CeCl
3in mixed aqueous solution, AlCl
3concentration be 0.03-0.05kg/L, CeCl
3concentration be 0.03-0.05kg/L.
In step f of the present invention, in silane coupling agent alcohol mixeding liquid, the massfraction of silane coupling agent is 8.5%-12.5%.
In step f of the present invention, silane coupling agent is γ-methacryloxypropyl trimethoxy silane, is called for short KH570.
The present invention adopt liquid makes homogenize material consistent with the feed way combined under liquid be coated on pearly pigment surface, both avoided pigment and affected the interference effect of its laminate structure to light owing to bearing high shear force in preparation process, in turn ensure that the high dispersing of pigment simultaneously, simultaneously, the present invention to natural mica and synthetic mica all applicable, and operating process is simple, production cost is lower.
The present invention compared with prior art, has following positive effect:
1, transparent sheet-like base material used in the present invention has higher rutile TiO
2transformation efficiency, rutile is TiO
2high-temperature-phase, compared to the anatase octahedrite of low-temperature phase, the lattice of rutile titanium dioxide is more stable fine and close, and its photocatalytic activity is lower, and photostabilization, weathering resistance and chemical proofing are all better.
2, first the present invention adopts SiO
2, Al
2o
3, CeO
2etc. light stability material to having optically active coating layer TiO
2surface cover, reduce the contact of itself and resin material, thus reduce UV-light to the impact of pigment; Then with silane coupling agent KH570, organic modification is carried out to surface of pigments, effectively can reduce the intergranular micropore of coating, improve the avidity of pigment and resin, the generation of surface of pigments micro-bubble can be prevented simultaneously, avoid product in use because the frequent variations of envrionment temperature, humidity causes pigment to be separated with organic connection material.Artificial accelerated aging QUV340(2000h is carried out to through the weather-proof coated pearly pigment of multilayer inorganic-organic hybrid compound) test, its color and glossiness are all obviously better than the pearly pigment of unprocessed mistake.
3, it is obvious, easy to operate, with low cost that the weather-proof cladding process of multilayer inorganic-organic hybrid compound that the present invention adopts has improvement effect, and equipment is simple, and the advantages such as condition is not harsh, are suitable for scale operation.
4, adopt in the present invention liquid makes homogenize material consistent with the feed way combined under liquid be coated on pearly pigment surface, both avoid pigment and affected the interference effect of its laminate structure to light owing to bearing high shear force in preparation process, in turn ensure that the high dispersing of pigment simultaneously.
5, the present invention adopts patent No. titanium tetrachloride device for formulating disclosed in 201220395321.2, ensures raw-material stability; Adopt the special PH automatic control system of German general sieve name to ensure the accurate control of pH value in the coated process of hydrolysis simultaneously.
Accompanying drawing explanation
Fig. 1 is that in the present invention, iris interferes the XRD figure of blue FWD225 pigment to be composed.
Fig. 2 is weather-proof coated third layer silane coupling agent KH570 schematic diagram before treatment.
Fig. 3 is the schematic diagram after weather-proof coated third layer silane coupling agent KH570 process.
Fig. 4 is FWD225 and FWD225WR artificial accelerated aging QUV340(2000h) test before schematic diagram.
Fig. 5 is FWD225 and FWD225WR artificial accelerated aging QUV340(2000h) test after schematic diagram.
Embodiment
Below in conjunction with accompanying drawing, also by embodiment, the invention will be further described.
Embodiment 1:
Adopt silvery white mica titanium nacreous material (FWD103) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take silvery white mica titanium nacreous material 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 75 DEG C, by ammonia soln adjust ph to 8.5.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 14%, pumps in reactor, add in 2h with constant flow pump by 15g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 6 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 75 DEG C, by aqueous sodium hydroxide solution adjust ph to 7.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.03kg/L and 0.04kg/L, with constant flow pump by 16mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 70 DEG C, by ammonia soln adjust ph to 8.5.
F. 6.5g is pumped into reactor containing the ethanolic soln constant current that the massfraction of silane coupling agent KH570 is 12.5%, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of silvery white mica titanium nacreous material with high-weatherability, be called for short FWD103WR.
Embodiment 2:
Adopt silvery white mica titanium nacreous material (FWD103) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take silvery white mica titanium nacreous material 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 85 DEG C, by ammonia soln adjust ph to 9.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 20%, pumps in reactor, add in 2h with constant flow pump by 20g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 8 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 85 DEG C, by aqueous sodium hydroxide solution adjust ph to 8.5.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.04kg/L and 0.03kg/L, with constant flow pump by 17mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 70 DEG C, by ammonia soln adjust ph to 9.5.
F. 10g is pumped into reactor containing the ethanolic soln constant current that the massfraction of silane coupling agent KH570 is 8.5%, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of silvery white mica titanium nacreous material with high-weatherability, be called for short FWD103WR.
Embodiment 3:
Adopt silvery white mica titanium nacreous material (FWD103) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take silvery white mica titanium nacreous material 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 80 DEG C, by ammonia soln adjust ph to 9.5.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 18%, pumps in reactor, add in 2h with constant flow pump by 15g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 7 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 80 DEG C, by aqueous sodium hydroxide solution adjust ph to 8.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.035/L and 0.04g/L, with constant flow pump by 15mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 75 DEG C, by ammonia soln adjust ph to 9.
F. massfraction 10g being contained silane coupling agent KH570 is that 10% ethanolic soln constant current pumps into reactor, adds in 30min, continues afterwards to stir insulation reaction 1h, obtains three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of silvery white mica titanium nacreous material with high-weatherability, be called for short FWD103WR.
Table 1 is when adopting silvery white mica titanium nacreous material (FWD103) as transparent sheet-like base material, the quality product examining report obtained.
table 1 FWD103 product information and technical indicator
Embodiment 4:
Adopt illusion-colour mica titanium nacreous material (FWD225) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take illusion-colour mica titanium nacreous material 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 75 DEG C, by ammonia soln adjust ph to 8.5.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 14%, pumps in reactor, add in 2h with constant flow pump by 15g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 6 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 75 DEG C, by aqueous sodium hydroxide solution adjust ph to 7.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.03kg/L and 0.04kg/L, with constant flow pump by 16mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 70 DEG C, by ammonia soln adjust ph to 8.5.
F. 6.5g is pumped into reactor containing the ethanolic soln constant current that the massfraction of silane coupling agent KH570 is 12.5%, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of illusion-colour mica titanium nacreous material with high-weatherability, be called for short FWD225WR.
Embodiment 5:
Adopt illusion-colour mica titanium nacreous material (FWD225) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take illusion-colour mica titanium nacreous material 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 85 DEG C, by ammonia soln adjust ph to 9.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 20%, pumps in reactor, add in 2h with constant flow pump by 20g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 8 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 85 DEG C, by aqueous sodium hydroxide solution adjust ph to 8.5.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.04kg/L and 0.03kg/L, with constant flow pump by 17mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 70 DEG C, by ammonia soln adjust ph to 9.5.
F. 10g is pumped into reactor containing the ethanolic soln constant current that the massfraction of silane coupling agent KH570 is 8.5%, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of illusion-colour mica titanium nacreous material with high-weatherability, be called for short FWD225WR.
Embodiment 6:
Adopt illusion-colour mica titanium nacreous material (FWD225) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take illusion-colour mica titanium nacreous material 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 80 DEG C, by ammonia soln adjust ph to 9.5.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 18%, pumps in reactor, add in 2h with constant flow pump by 15g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 7 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 80 DEG C, by aqueous sodium hydroxide solution adjust ph to 8.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.035/L and 0.04g/L, with constant flow pump by 15mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 75 DEG C, by ammonia soln adjust ph to 9.
F. massfraction 10g being contained silane coupling agent KH570 is that 10% ethanolic soln constant current pumps into reactor, adds in 30min, continues afterwards to stir insulation reaction 1h, obtains three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of illusion-colour mica titanium nacreous material with high-weatherability, be called for short FWD225WR.
Illusion-colour mica titanium nacreous material (FWD225) has higher rutile TiO
2transformation efficiency, as shown in Figure 1.Rutile is TiO
2high-temperature-phase, compared to the anatase octahedrite of low-temperature phase, the lattice of rutile titanium dioxide is more stable fine and close, and its photocatalytic activity is lower, and photostabilization, weathering resistance and chemical proofing are all better.
In FIG, at place'ss (corresponding crystal face is respectively 110,101,111) such as 27.38 °, 35.88 ° and 41.08 °, 2 θ have occurred that rutile-type diffraction peak is composed respectively, and absorption peak is strong.And Detitanium-ore-type 2 θ characteristic peak 25.38 °, 37.90 ° and 48.12 ° (corresponding crystal face is respectively 101,004,200) absorb faint, illustrate in FWD225 containing rutile TiO
2ratio is higher.
First the present invention adopts SiO
2, Al
2o
3, CeO
2etc. light stability material to having optically active coating layer TiO
2surface cover, reduce the contact of itself and resin material, thus reduce UV-light to the impact of pigment; Then with silane coupling agent KH570, organic modification is carried out to surface of pigments, as shown in Figure 2 to 3, effectively can reduce the intergranular micropore of coating, improve the avidity of pigment and resin, the generation of surface of pigments micro-bubble can be prevented simultaneously, avoid product in use because the frequent variations of envrionment temperature, humidity causes pigment to be separated with organic connection material.Artificial accelerated aging QUV340(2000h is carried out to through the weather-proof coated pearly pigment of multilayer inorganic-organic hybrid compound) test, its color and glossiness are all obviously better than the pearly pigment of unprocessed mistake, as shown in Fig. 4 ~ Fig. 5.
Table 2 is when adopting illusion-colour mica titanium nacreous material (FWD225) as transparent sheet-like base material, the quality product examining report obtained.
table 2 FWD225 product information and technical indicator
Embodiment 7:
Adopt golden glory series pearly pigment (FWD300) of painted mica ferrotianium as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take painted mica ferrotianium golden glory series pearly pigment 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 75 DEG C, by ammonia soln adjust ph to 8.5.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 14%, pumps in reactor, add in 2h with constant flow pump by 15g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 6 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 75 DEG C, by aqueous sodium hydroxide solution adjust ph to 7.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.03kg/L and 0.04kg/L, with constant flow pump by 16mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 70 DEG C, by ammonia soln adjust ph to 8.5.
F. 6.5g is pumped into reactor containing the ethanolic soln constant current that the massfraction of silane coupling agent KH570 is 12.5%, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of painted mica ferrotianium golden glory series pearly pigment with high-weatherability, be called for short FWD300WR.
Embodiment 8:
Adopt golden glory series pearly pigment (FWD300) of painted mica ferrotianium as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take painted mica ferrotianium golden glory series pearly pigment 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 85 DEG C, by ammonia soln adjust ph to 9.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 20%, pumps in reactor, add in 2h with constant flow pump by 20g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 8 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 85 DEG C, by aqueous sodium hydroxide solution adjust ph to 8.5.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.04kg/L and 0.03kg/L, with constant flow pump by 17mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 70 DEG C, by ammonia soln adjust ph to 9.5.
F. 10g is pumped into reactor containing the ethanolic soln constant current that the massfraction of silane coupling agent KH570 is 8.5%, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of painted mica ferrotianium golden glory series pearly pigment with high-weatherability, be called for short FWD300WR.
Embodiment 9:
Adopt golden glory series pearly pigment (FWD300) of painted mica ferrotianium as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take painted mica ferrotianium golden glory series pearly pigment 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 80 DEG C, by ammonia soln adjust ph to 9.5.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 18%, pumps in reactor, add in 2h with constant flow pump by 15g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 7 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 80 DEG C, by aqueous sodium hydroxide solution adjust ph to 8.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.035/L and 0.04g/L, with constant flow pump by 15mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 75 DEG C, by ammonia soln adjust ph to 9.
F. massfraction 10g being contained silane coupling agent KH570 is that 10% ethanolic soln constant current pumps into reactor, adds in 30min, continues afterwards to stir insulation reaction 1h, obtains three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of painted mica ferrotianium golden glory series pearly pigment with high-weatherability, be called for short FWD300WR.
Table 3 is when adopting golden glory series pearly pigment (FWD300) of painted mica ferrotianium as transparent sheet-like base material, the quality product examining report obtained.
table 3 FWD300 product information and technical indicator
Embodiment 10:
Adopt iron mica metal glory series pearly pigment (FWD502) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take iron mica metal glory series pearly pigment 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 75 DEG C, by ammonia soln adjust ph to 8.5.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 14%, pumps in reactor, add in 2h with constant flow pump by 15g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 6 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 75 DEG C, by aqueous sodium hydroxide solution adjust ph to 7.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.03kg/L and 0.04kg/L, with constant flow pump by 16mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 70 DEG C, by ammonia soln adjust ph to 8.5.
F. 6.5g is pumped into reactor containing the ethanolic soln constant current that the massfraction of silane coupling agent KH570 is 12.5%, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of iron mica metal glory series pearly pigment with high-weatherability, be called for short FWD502WR.
Embodiment 11:
Adopt iron mica metal glory series pearly pigment (FWD502) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take iron mica metal glory series pearly pigment 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 85 DEG C, by ammonia soln adjust ph to 9.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 20%, pumps in reactor, add in 2h with constant flow pump by 20g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 8 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 85 DEG C, by aqueous sodium hydroxide solution adjust ph to 8.5.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.04kg/L and 0.03kg/L, with constant flow pump by 17mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 70 DEG C, by ammonia soln adjust ph to 9.5.
F. 10g is pumped into reactor containing the ethanolic soln constant current that the massfraction of silane coupling agent KH570 is 8.5%, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of iron mica metal glory series pearly pigment with high-weatherability, be called for short FWD502WR.
Embodiment 12:
Adopt iron mica metal glory series pearly pigment (FWD502) as transparent sheet-like base material, carry out the preparation of pearly pigment.Its preparation process is:
A. take iron mica metal glory series pearly pigment 40g, drop in reactor, add deionized water 450mL, stir and be warming up to 80 DEG C, by ammonia soln adjust ph to 9.5.
B. dehydrated alcohol and methyl silicate are made into containing SiO
2massfraction is the silicon precursor alcohol mixeding liquid of 18%, pumps in reactor, add in 2h with constant flow pump by 15g silicon precursor alcohol mixeding liquid, continues reaction 1h afterwards, obtains mother liquor.
C. mother liquor is filtered, with deionized water wash 4 times, in the baking oven of 100 DEG C dry 7 hours, then the pigment obtained after drying is dropped into reactor again, add deionized water 450mL, at the uniform velocity stir and be warming up to 80 DEG C, by aqueous sodium hydroxide solution adjust ph to 8.
D. by AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3and CeCl
3density be respectively the mixed aqueous solution of 0.035/L and 0.04g/L, with constant flow pump by 15mL AlCl
3/ CeCl
3mixed aqueous solution pumps in reactor, and co-precipitation hydridization is coated on pigment flakes, and uses aqueous sodium hydroxide solution equilibrium ph.Add in 1h, continue afterwards to stir 20min, obtain secondary mother liquid.
E. secondary mother liquid is filtered, form filter cake 3 times with deionized water rinsing, then filter cake is dropped into reactor again, add deionized water 450mL, heat up constant in 75 DEG C, by ammonia soln adjust ph to 9.
F. massfraction 10g being contained silane coupling agent KH570 is that 10% ethanolic soln constant current pumps into reactor, adds in 30min, continues afterwards to stir insulation reaction 1h, obtains three mother liquors.
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain a kind of iron mica metal glory series pearly pigment with high-weatherability, be called for short FWD502WR.
Table 4 is when adopting iron mica metal glory series pearly pigment (FWD502) as transparent sheet-like base material, the quality product examining report obtained.
table 4 FWD502 product information and technical indicator
In addition, it should be noted that, the specific embodiment described in this specification sheets, its formula, title that technique is named etc. can be different.All equivalences of doing according to structure, feature and the principle described in inventional idea of the present invention or simple change, be included in the protection domain of patent of the present invention.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment; only otherwise depart from structure of the present invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
Although the present invention with embodiment openly as above; but it is also not used to limit protection scope of the present invention; any technician being familiar with this technology, not departing from the change and retouching done in the spirit and scope of the present invention, all should belong to protection scope of the present invention.
Claims (7)
1. there is a preparation technology for the Study On Mica of high durable performance, it is characterized in that: its preparation process is:
A. 40g transparent sheet-like base material is dropped into reactor, be made into deionized water the suspension that mass percent concentration is 10%, at the uniform velocity stir and be warming up to 75-85 DEG C, by alkaline solution adjust ph to 8.5-10;
B. by the massfraction of dehydrated alcohol and silicon-dioxide be choose any one kind of them in the methyl silicate of 28%, tetraethoxy or two kinds be made into silicon precursor alcohol mixeding liquid, with constant flow pump, 10-30g silicon precursor alcohol mixeding liquid is pumped in suspension, add in 2h, continue reaction 1h afterwards, obtain mother liquor;
C. mother liquor is filtered, after deionized water wash 4 times, dry 6-8 hour in the baking oven of 100 DEG C, then the pigment obtained after drying is dropped into reactor again, the secondary suspension that mass percent concentration is 10% is made into deionized water, at the uniform velocity stir and be warming up to 75-85 DEG C, by alkaline solution adjust ph to 7-8.5;
D. by a certain proportion of AlCl
3the aqueous solution and CeCl
3aqueous solution also dilution obtains AlCl
3/ CeCl
3mixed aqueous solution, with constant flow pump by 10-20mL AlCl
3/ CeCl
3mixed aqueous solution pumps in secondary suspension, and co-precipitation hydridization is coated on pigment flakes, and uses alkaline solution equilibrium ph, adds in 1h, continues afterwards to stir 20min, obtains secondary mother liquid;
E. secondary mother liquid is filtered, form filter cakes with deionized water rinsing 3 times, then by filter cake again dispersed with stirring in deionized water, obtain three suspension that pigment mass percentage concentration is 10%, at the uniform velocity stir and be warming up to 70-80 DEG C, and by alkaline solution adjust ph to 8.5-9.5;
F. silane coupling agent and dehydrated alcohol are made into silane coupling agent alcohol mixeding liquid, with constant flow pump, 6-20g silane coupling agent alcohol mixeding liquid are pumped in three suspension, add in 30min, continue afterwards to stir insulation reaction 1h, obtain three mother liquors;
G. three mother liquors are filtered, with deionized water rinsing 3 times, in the baking oven of 120 DEG C dry 12 hours, obtain that there is the pearly pigment compared with high durable performance;
In described step a and step e, described alkaline solution is ammonia aqueous solution; In described step c and steps d, described alkaline solution is aqueous sodium hydroxide solution;
In described step b, SiO in described silicon precursor alcohol mixeding liquid
2massfraction be 14%-20%; In described steps d, described AlCl
3/ CeCl
3in mixed aqueous solution, AlCl
3concentration be 0.03-0.05kg/L, CeCl
3concentration be 0.03-0.05kg/L;
In described step f, in silane coupling agent alcohol mixeding liquid, the massfraction of silane coupling agent is 8.5%-12.5%; Silane coupling agent is γ-methacryloxypropyl trimethoxy silane, is called for short KH570.
2. the preparation technology with the Study On Mica of high durable performance according to claim 1, is characterized in that: described transparent sheet-like base material is silvery white mica titanium nacreous material, is called for short FWD103, TiO in described silvery white mica titanium nacreous material
2clad ratio be 28-32%.
3. the preparation technology with the Study On Mica of high durable performance according to claim 1, is characterized in that: described transparent sheet-like base material is illusion-colour mica titanium nacreous material, is called for short FWD225, TiO in described illusion-colour mica titanium nacreous material
2clad ratio be 50-55%.
4. the preparation technology with the Study On Mica of high durable performance according to claim 1, it is characterized in that: described transparent sheet-like base material is painted mica ferrotianium golden glory series pearly pigment, be called for short FWD300, TiO in described painted mica ferrotianium golden glory series pearly pigment
2clad ratio be 35-40%, Fe
2o
3clad ratio be 2-5%.
5. the preparation technology with the Study On Mica of high durable performance according to claim 1, it is characterized in that: described transparent sheet-like base material is iron mica metal glory series pearly pigment, be called for short FWD502, Fe in described iron mica metal glory series pearly pigment
2o
3clad ratio be 40-45%.
6. the preparation technology with the Study On Mica of high durable performance according to claim arbitrary in claim 2 to 5, is characterized in that: the median size of described transparent sheet-like base material is 10-60 μm.
7. the preparation technology with the Study On Mica of high durable performance according to claim arbitrary in claim 2 to 5, is characterized in that: the median size of described transparent sheet-like base material is 5-25 μm.
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