CN109705624A - A kind of preparation method of blue-orange two-color magic pearlescent pigment - Google Patents
A kind of preparation method of blue-orange two-color magic pearlescent pigment Download PDFInfo
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- 239000000049 pigment Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 111
- 239000012065 filter cake Substances 0.000 claims abstract description 56
- 239000011159 matrix material Substances 0.000 claims abstract description 47
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 108
- 238000003756 stirring Methods 0.000 claims description 39
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000004321 preservation Methods 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 25
- 229910021641 deionized water Inorganic materials 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 21
- 239000000498 cooling water Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 18
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 17
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims 5
- 238000001914 filtration Methods 0.000 claims 2
- 238000009413 insulation Methods 0.000 claims 1
- 238000005253 cladding Methods 0.000 abstract description 29
- 238000001354 calcination Methods 0.000 abstract description 9
- 238000001311 chemical methods and process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000010445 mica Substances 0.000 description 8
- 229910052618 mica group Inorganic materials 0.000 description 8
- 238000002791 soaking Methods 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 3
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 description 3
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- WGKMWBIFNQLOKM-UHFFFAOYSA-N [O].[Cl] Chemical compound [O].[Cl] WGKMWBIFNQLOKM-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- MZZSDCJQCLYLLL-UHFFFAOYSA-N Secalonsaeure A Natural products COC(=O)C12OC3C(CC1=C(O)CC(C)C2O)C(=CC=C3c4ccc(O)c5C(=O)C6=C(O)CC(C)C(O)C6(Oc45)C(=O)OC)O MZZSDCJQCLYLLL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Cosmetics (AREA)
Abstract
A kind of preparation method of the double-colored illusion-colour pearlescent pigment of Blue Curacao, its feature the following steps are included: prepare flake matrix material first, it is raw material with soluble zirconates, phosphoric acid and hydrofluoric acid, using conventional fine chemical-process, in atmospheric conditions, reaction temperature be 60~90 DEG C, the reaction time 2~4 hours, flake matrix material；Cladding point 2 progress in flake matrix material surface are filtered, wash after the first subsurface coats, and filter cake is carried out dispersion and carries out second of surface cladding；Then it is filtered, washs, filter cake is dried at 125~140 DEG C, calcining 45 minutes is carried out at 830~860 DEG C, obtains the double-colored illusion-colour pearlescent pigment of Blue Curacao.
Description
Technical field
The present invention relates to a kind of preparation methods of the double-colored illusion-colour pearlescent pigment of Blue Curacao.
Background technique
Illusion-colour pearlescent pigment is further cladding titanium dioxide on the basis of silvery white pearlescent pigment, with clad ratio and
The increase of titanium dioxide multi geometric thickness, the reflection coloured light of pigment chip is successively to yellow, red, purple, blue, green conversion.It is colorful
The pearlescent pigment that changes colour is successful novel magical color pearlescent pigment newly developed in recent years.It is on the basis of monochromatic illusion-colour pearlescent pigment
A kind of illusion-colour pearlescent pigment with multipath reflection coloured light formed and coating various coloring metal ion oxides again.It is real
On border, this pearlescent pigment is the combination of illusion-colour pearlescent pigment and colored nacreous pigment.
Pearlescent pigment has the flash effect of metallic pigments, and can generate the soft color of natural peral, its flash of light effect
Fruit is passively luminous, that is to say, that flash effect can be just shown under conditions of light.The main Types of pearlescent pigment have:
Natural fish scale pearlescent pigment, bismuth oxychloride crystallization pearlescent pigment, mica coat pearlescent pigment.Production is most in the world at present and answers
With widest pearlescent pigment, be using natural mica thin slice as core (for the size of mica from 4m to 120m, thickness is about 0.5m),
By special chemical technology, one or more layers titanium or other metal oxides are coated on its surface.But natural mica conduct
The basis material of pearlescent pigment has its defect: although mica sheet can obtain lesser thickness and biggish radius-thickness ratio, usually
There is wider thickness distribution range (0.2 ~ 1 μm), is easy to influence the stability of plated film in this way, is not easy that the pearl of uniform form and aspect is made
Delustering pigment, after with metal oxide coated mica piece, the level step to be formed and edge gradient thickness are removed due to mica and
Make light that scattering phenomenon occur, reduce pearlescent effect, in addition natural mica foreign ion also coloured containing iron ion etc., needs
These foreign ions are removed using pretreatment process.
A kind of preparation method of the double-colored illusion-colour pearlescent pigment of Blue Curacao, feature the following steps are included: prepare sheet base first
Then body material carries out surface cladding to flake matrix material；The preparation method of flake matrix material: reaction kettle is put into 3000 weights
The deionized water of part is measured, stirring is opened, the solid zirconium oxychloride of 200~250 parts by weight is added into reaction kettle, to solid oxygen chlorine
After change zirconium is completely dissolved, the hydrofluoric acid of 50~80 parts by weight is added into reaction kettle, hydrofluoric acid concentration is 41~42%, stirring 30
Minute, the phosphoric acid of 160~220 parts by weight is added into reaction kettle, phosphoric acid concentration is 90~93%, stirs 30 minutes, starts to rise
Temperature starts to keep the temperature when temperature reaches 60~90 DEG C, and soaking time 2~4 hours, after heat preservation, to temperature of reaction kettle nature
50 DEG C are cooled to hereinafter, be filtered, wash, obtains flake matrix material filter cake；
2 progress of flake matrix material surface cladding point, first time surface coating method: reaction kettle is put into going for 2200 parts by weight
Ionized water, open stirring, be added into reaction kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78
At~82 DEG C, start to keep the temperature, the pH value of system is first adjusted to 1.8~2.0 with titanium tetrachloride solution, then by titanium tetrachloride solution
The sodium hydroxide solution for being 20~25% with concentration is added in reaction kettle simultaneously, and the pH value of system is remained in adition process
It is 850~900 parts by volume for the addition total amount to 1.8~2.0, titanium tetrachloride solution, controls titanium tetrachloride solution and 20~25%
Sodium hydroxide solution the addition time be 5~6 hours, addition finish heat preservation 30 minutes, open cooling water to reaction kettle carry out it is cold
But, when temperature is down to 50 DEG C hereinafter, be filtered, wash, the first subsurface cladding pearlescent pigment filter cake is obtained；
Second of surface coating method: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
It is above-mentioned to obtain the first subsurface cladding pearlescent pigment filter cake, it starts to warm up, when temperature reaches 80~90 DEG C, starts to keep the temperature, first
The pH value of system is adjusted to 3.5~4.5 with liquor ferri trichloridi, the hydrogen for being then 20~25% by liquor ferri trichloridi and concentration
Sodium hydroxide solution is added in reaction kettle simultaneously, remains that the pH value of system is the tri-chlorination to 3.5~4.5 in adition process
The addition total amount of iron liquid be 160~180 parts by volume, control liquor ferri trichloridi and 20~25% sodium hydroxide solution addition
Time be 3~4 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C with
Under, it is filtered, washs, obtain the double-colored illusion-colour pearlescent pigment filter cake of Blue Curacao；
Filter cake is dried at 125~140 DEG C, calcining 45 minutes is then carried out at 830~860 DEG C, it is double to obtain Blue Curacao
Color illusion-colour pearlescent pigment；The concentration of the titanium tetrachloride solution is 1.5 mol/Ls；The concentration of the liquor ferri trichloridi
For 2.0 mol/Ls.
Innovative point of the present invention: using soluble zirconates, phosphoric acid and hydrofluoric acid for raw material, using conventional fine chemical-process,
In atmospheric conditions, reaction temperature is 60~90 DEG C, the reaction time 2~4 hours, obtains flake matrix material, this synthesis side
Flake matrix material diameter and thickness that method obtains is uniformly and controllable, and 3~5 μm of flake matrix material diameter and thickness 50~
70nm keeps the performance of pigment more preferable.
Summary of the invention
A kind of preparation method of the double-colored illusion-colour pearlescent pigment of Blue Curacao, feature the following steps are included: prepare sheet base first
Then body material carries out surface cladding to flake matrix material；The preparation method of flake matrix material: reaction kettle is put into 3000 weights
The deionized water of part is measured, stirring is opened, the solid zirconium oxychloride of 200~250 parts by weight is added into reaction kettle, to solid oxygen chlorine
After change zirconium is completely dissolved, the hydrofluoric acid of 50~80 parts by weight is added into reaction kettle, hydrofluoric acid concentration is 41~42%, stirring 30
Minute, the phosphoric acid of 160~220 parts by weight is added into reaction kettle, phosphoric acid concentration is 90~93%, stirs 30 minutes, starts to rise
Temperature starts to keep the temperature when temperature reaches 60~90 DEG C, and soaking time 2~4 hours, after heat preservation, to temperature of reaction kettle nature
50 DEG C are cooled to hereinafter, be filtered, wash, obtains flake matrix material filter cake；
2 progress of flake matrix material surface cladding point, first time surface coating method: reaction kettle is put into going for 2200 parts by weight
Ionized water, open stirring, be added into reaction kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78
At~82 DEG C, start to keep the temperature, the pH value of system is first adjusted to 1.8~2.0 with titanium tetrachloride solution, then by titanium tetrachloride solution
The sodium hydroxide solution for being 20~25% with concentration is added in reaction kettle simultaneously, and the pH value of system is remained in adition process
It is 850~900 parts by volume for the addition total amount to 1.8~2.0, titanium tetrachloride solution, controls titanium tetrachloride solution and 20~25%
Sodium hydroxide solution the addition time be 5~6 hours, addition finish heat preservation 30 minutes, open cooling water to reaction kettle carry out it is cold
But, when temperature is down to 50 DEG C hereinafter, be filtered, wash, the first subsurface cladding pearlescent pigment filter cake is obtained；
Second of surface coating method: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
It is above-mentioned to obtain the first subsurface cladding pearlescent pigment filter cake, it starts to warm up, when temperature reaches 80~90 DEG C, starts to keep the temperature, first
The pH value of system is adjusted to 3.5~4.5 with liquor ferri trichloridi, the hydrogen for being then 20~25% by liquor ferri trichloridi and concentration
Sodium hydroxide solution is added in reaction kettle simultaneously, remains that the pH value of system is the tri-chlorination to 3.5~4.5 in adition process
The addition total amount of iron liquid be 160~180 parts by volume, control liquor ferri trichloridi and 20~25% sodium hydroxide solution addition
Time be 3~4 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C with
Under, it is filtered, washs, obtain the double-colored illusion-colour pearlescent pigment filter cake of Blue Curacao；
Filter cake is dried at 125~140 DEG C, calcining 45 minutes is then carried out at 830~860 DEG C, it is double to obtain Blue Curacao
Color illusion-colour pearlescent pigment；
The concentration of the titanium tetrachloride solution is 1.5 mol/Ls；
The concentration of the liquor ferri trichloridi is 2.0 mol/Ls.
Specific embodiment
Embodiment 1
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrofluoric acid that concentration is 41% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 200kg
50kg is stirred 30 minutes, and the phosphatase 11 60kg that concentration is 90% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
When reaching 60 DEG C, start to keep the temperature, soaking time 4 hours, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C hereinafter,
It is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 1.8, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 20% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 1.8 in adition process, the addition total amount of titanium tetrachloride solution is 850
Rise, the concentration of titanium tetrachloride solution is 1.5 mol/Ls, control titanium tetrachloride solution and 20% sodium hydroxide solution addition when
Between be 5 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, is added into reaction kettle above-mentioned
Flake matrix material filter cake is obtained, is started to warm up, when temperature reaches 80 DEG C, starts to keep the temperature, first with liquor ferri trichloridi by body
The pH value of system is adjusted to 3.5, and the sodium hydroxide solution that liquor ferri trichloridi and concentration are 20% is then added to reaction kettle simultaneously
In, remain that the pH value of system is to 3.5 in adition process, the addition total amount of liquor ferri trichloridi is 160 liters, ferric trichloride
The concentration of solution be 2.0 mol/Ls, control liquor ferri trichloridi and 20% sodium hydroxide solution the addition time be 3 hours,
Addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, be filtered, wash,
Obtain the double-colored illusion-colour pearlescent pigment filter cake of Blue Curacao；
Filter cake is dried at 125 DEG C, calcining 45 minutes is then carried out at 830 DEG C, obtains the double-colored illusion-colour pearly-lustre of Blue Curacao
Pigment.
Embodiment 2
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrofluoric acid that concentration is 42% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 250kg
80kg is stirred 30 minutes, and the phosphoric acid 220kg that concentration is 93% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
When reaching 90 DEG C, start to keep the temperature, soaking time 2 hours, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C hereinafter,
It is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 82 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 2.0, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 25% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 2.0 in adition process, the addition total amount of titanium tetrachloride solution is 900
Rise, the concentration of titanium tetrachloride solution is 1.5 mol/Ls, control titanium tetrachloride solution and 25% sodium hydroxide solution addition when
Between be 6 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, is added into reaction kettle above-mentioned
Flake matrix material filter cake is obtained, is started to warm up, when temperature reaches 90 DEG C, starts to keep the temperature, first with liquor ferri trichloridi by body
The pH value of system is adjusted to 4.5, and the sodium hydroxide solution that liquor ferri trichloridi and concentration are 25% is then added to reaction kettle simultaneously
In, remain that the pH value of system is to 4.5 in adition process, the addition total amount of liquor ferri trichloridi is 180 liters, ferric trichloride
The concentration of solution be 2.0 mol/Ls, control ferric trichloride and 25% sodium hydroxide solution the addition time be 4 hours, be added
Heat preservation 30 minutes is finished, cooling water is opened and reaction kettle is cooled down, when temperature is down to 50 DEG C hereinafter, be filtered, wash, is obtained
The double-colored illusion-colour pearlescent pigment filter cake of Blue Curacao；
Filter cake is dried at 140 DEG C, calcining 45 minutes is then carried out at 860 DEG C, obtains the double-colored illusion-colour pearly-lustre of Blue Curacao
Pigment.
Embodiment 3
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrogen fluorine that concentration is 41.5% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 230kg
Sour 60kg is stirred 30 minutes, and the phosphatase 11 80kg that concentration is 91% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
Degree starts to keep the temperature, soaking time 3 hours when reaching 70 DEG C, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C with
Under, it is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, to anti-
Answer be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 80 DEG C, start to keep the temperature, first with four
The pH value of system is adjusted to 1.9 by titanium chloride solution, then by titanium tetrachloride solution and concentration be 22% sodium hydroxide solution simultaneously
It is added in reaction kettle, remains that the pH value of system is to 1.9 in adition process, the addition total amount of titanium tetrachloride solution is
880 liters, the concentration of titanium tetrachloride solution is 1.5 mol/Ls, control titanium tetrachloride solution and 22% sodium hydroxide solution plus
The angle of incidence be 5.5 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C with
Under, it is filtered, washs, obtain the first subsurface cladding pearlescent pigment filter cake；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, is added into reaction kettle
It states to obtain flake matrix material filter cake, starts to warm up, start to warm up, when temperature reaches 85 DEG C, start to keep the temperature, first use tri-chlorination
The pH value of system is adjusted to 4.0 by ferrous solution, and then the sodium hydroxide solution that liquor ferri trichloridi and concentration are 23% is added simultaneously
The pH value that system is remained into reaction kettle, in adition process is to 4.0, and the addition total amount of liquor ferri trichloridi is 170 liters,
The concentration of liquor ferri trichloridi be 2.0 mol/Ls, control liquor ferri trichloridi and 23% sodium hydroxide solution the addition time
It is 3.5 hours, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, carrying out
It is filtered, washed, obtains the double-colored illusion-colour pearlescent pigment filter cake of Blue Curacao；
Filter cake is dried at 132 DEG C, calcining 45 minutes is then carried out at 850 DEG C, obtains the double-colored illusion-colour pearly-lustre of Blue Curacao
Pigment.
Embodiment 4
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrogen fluorine that concentration is 41.8% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 240kg
Sour 75kg is stirred 30 minutes, and the phosphoric acid 215kg that concentration is 92.8% is added into reaction kettle, stirs 30 minutes, starts to warm up, when
When temperature reaches 85 DEG C, start to keep the temperature, soaking time 2.5 hours, after heat preservation, naturally cools to 50 DEG C to temperature of reaction kettle
Hereinafter, being filtered, washing, flake matrix material filter cake is obtained；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 82 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 2.0, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 21% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 2.0 in adition process, the addition total amount of titanium tetrachloride solution is 900
Rise, the concentration of titanium tetrachloride solution is 1.5 mol/Ls, control titanium tetrachloride solution and 21% sodium hydroxide solution addition when
Between be 6 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, is added into reaction kettle above-mentioned
Flake matrix material filter cake is obtained, is started to warm up, when temperature reaches 88 DEG C, starts to keep the temperature, first with liquor ferri trichloridi by body
The pH value of system is adjusted to 4.3, and the sodium hydroxide solution that liquor ferri trichloridi and concentration are 21% is then added to reaction kettle simultaneously
In, remain that the pH value of system is to 4.3 in adition process, the addition total amount of liquor ferri trichloridi is 165 liters, ferric trichloride
The concentration of solution is 2.0 mol/Ls, and it is 3.4 small for controlling liquor ferri trichloridi and 21% addition time of sodium hydroxide solution
When, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, being filtered, washing
It washs, obtains the double-colored illusion-colour pearlescent pigment filter cake of Blue Curacao；
Filter cake is dried at 135 DEG C, calcining 45 minutes is then carried out at 890 DEG C, obtains the double-colored illusion-colour pearly-lustre of Blue Curacao
Pigment.
Embodiment 5
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrogen fluorine that concentration is 41.6% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 225kg
Sour 70kg is stirred 30 minutes, and the phosphoric acid 200kg that concentration is 92% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
Degree starts to keep the temperature, soaking time 3 hours when reaching 80 DEG C, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C with
Under, it is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 1.8, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 22% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 1.8 in adition process, the addition total amount of titanium tetrachloride solution is 870
Rise, the concentration of titanium tetrachloride solution is 1.5 mol/Ls, control titanium tetrachloride solution and 22% sodium hydroxide solution addition when
Between be 5 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, is added into reaction kettle above-mentioned
Flake matrix material filter cake is obtained, is started to warm up, when temperature reaches 87 DEG C, starts to keep the temperature, first with liquor ferri trichloridi by body
The pH value of system is adjusted to 3.8, and the sodium hydroxide solution that liquor ferri trichloridi and concentration are 22% is then added to reaction kettle simultaneously
In, remain that the pH value of system is to 3.8 in adition process, the addition total amount of liquor ferri trichloridi is 172 liters, ferric trichloride
The concentration of solution is 2.0 mol/Ls, and it is 3.8 small for controlling liquor ferri trichloridi and 22% addition time of sodium hydroxide solution
When, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, being filtered, washing
It washs, obtains the double-colored illusion-colour pearlescent pigment filter cake of Blue Curacao；
Filter cake is dried at 139 DEG C, calcining 45 minutes is then carried out at 840 DEG C, obtains the double-colored illusion-colour pearly-lustre of Blue Curacao
Pigment.
Embodiment 6
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrofluoric acid that concentration is 42% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 230kg
68kg is stirred 30 minutes, and the phosphatase 11 90kg that concentration is 92% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
When reaching 75 DEG C, start to keep the temperature, soaking time 4 hours, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C hereinafter,
It is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 81 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 2.0, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 24% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 2.0 in adition process, the addition total amount of titanium tetrachloride solution is 860
Rise, the concentration of titanium tetrachloride solution is 1.5 mol/Ls, control titanium tetrachloride solution and 24% sodium hydroxide solution addition when
Between be 6 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, is added into reaction kettle above-mentioned
Flake matrix material filter cake is obtained, is started to warm up, when temperature reaches 82 DEG C, starts to keep the temperature, first with liquor ferri trichloridi by body
The pH value of system is adjusted to 4.2, and the sodium hydroxide solution that liquor ferri trichloridi and concentration are 22% is then added to reaction kettle simultaneously
In, remain that the pH value of system is to 4.2 in adition process, the addition total amount of liquor ferri trichloridi is 178 liters, ferric trichloride
The concentration of solution is 2.0 mol/Ls, and it is 3.1 small for controlling liquor ferri trichloridi and 22% addition time of sodium hydroxide solution
When, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, being filtered, washing
It washs, obtains the double-colored illusion-colour pearlescent pigment filter cake of Blue Curacao；
Filter cake is dried at 137 DEG C, calcining 45 minutes is then carried out at 855 DEG C, obtains the double-colored illusion-colour pearly-lustre of Blue Curacao
Pigment.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5472491A (en) * | 1993-06-24 | 1995-12-05 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Pearlescent pigment for water-borne surface-coating systems |
| WO1998013426A1 (en) * | 1996-09-27 | 1998-04-02 | Merck Patent Gmbh | Modified nacreous lustre pigments for water paint systems |
| CN101547977A (en) * | 2006-12-05 | 2009-09-30 | 西巴控股有限公司 | Surface-modified (effect) pigments |
| CN102181177A (en) * | 2011-03-22 | 2011-09-14 | 华南理工大学 | Method for synthesizing rutile mica titanium pearlescent pigment without calcination |
| CN102260421A (en) * | 2011-06-08 | 2011-11-30 | 四川大学 | Magic-color nacreous aluminum powder pigment and preparation method thereof |
| CN104098931A (en) * | 2014-07-11 | 2014-10-15 | 杭州弗沃德精细化工有限公司 | Preparation method of super interference gold pearlescent pigment |
| CN104327552A (en) * | 2014-09-25 | 2015-02-04 | 广西七色珠光材料股份有限公司 | High temperature resistant pearlescent pigment and preparation method thereof |
-
2019
- 2019-02-25 CN CN201910136515.7A patent/CN109705624A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5472491A (en) * | 1993-06-24 | 1995-12-05 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Pearlescent pigment for water-borne surface-coating systems |
| WO1998013426A1 (en) * | 1996-09-27 | 1998-04-02 | Merck Patent Gmbh | Modified nacreous lustre pigments for water paint systems |
| CN101547977A (en) * | 2006-12-05 | 2009-09-30 | 西巴控股有限公司 | Surface-modified (effect) pigments |
| CN102181177A (en) * | 2011-03-22 | 2011-09-14 | 华南理工大学 | Method for synthesizing rutile mica titanium pearlescent pigment without calcination |
| CN102260421A (en) * | 2011-06-08 | 2011-11-30 | 四川大学 | Magic-color nacreous aluminum powder pigment and preparation method thereof |
| CN104098931A (en) * | 2014-07-11 | 2014-10-15 | 杭州弗沃德精细化工有限公司 | Preparation method of super interference gold pearlescent pigment |
| CN104327552A (en) * | 2014-09-25 | 2015-02-04 | 广西七色珠光材料股份有限公司 | High temperature resistant pearlescent pigment and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 袁潇等: "磷酸锆碟片粒径对提高二氧化钛悬浮液分散稳定性的影响", 《功能材料》 * |
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