CN109943100A - A kind of purple pearlescent pigment, preparation method and application - Google Patents
A kind of purple pearlescent pigment, preparation method and application Download PDFInfo
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- CN109943100A CN109943100A CN201910307192.3A CN201910307192A CN109943100A CN 109943100 A CN109943100 A CN 109943100A CN 201910307192 A CN201910307192 A CN 201910307192A CN 109943100 A CN109943100 A CN 109943100A
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- pearlescent pigment
- layer
- substrate
- purple
- intermediate isolating
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- 239000000049 pigment Substances 0.000 title claims abstract description 107
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000000758 substrate Substances 0.000 claims abstract description 48
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 41
- 239000010941 cobalt Substances 0.000 claims abstract description 41
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 41
- 230000007062 hydrolysis Effects 0.000 claims abstract description 20
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 20
- 239000003973 paint Substances 0.000 claims abstract description 13
- 238000005253 cladding Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 239000004033 plastic Substances 0.000 claims abstract description 10
- 229920003023 plastic Polymers 0.000 claims abstract description 10
- 239000010985 leather Substances 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 230000008021 deposition Effects 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 19
- 238000001354 calcination Methods 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 159000000013 aluminium salts Chemical class 0.000 claims description 8
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 8
- 150000001868 cobalt Chemical class 0.000 claims description 8
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical group [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000003086 colorant Substances 0.000 claims description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000010445 mica Substances 0.000 claims description 6
- 229910052618 mica group Inorganic materials 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 150000002505 iron Chemical class 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011324 bead Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 238000009938 salting Methods 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 229910052788 barium Inorganic materials 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 80
- 238000003756 stirring Methods 0.000 description 17
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- -1 ferrous metal oxide Chemical class 0.000 description 6
- 239000004743 Polypropylene Substances 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- 229920001155 polypropylene Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 3
- 229910001626 barium chloride Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000011775 sodium fluoride Substances 0.000 description 2
- 235000013024 sodium fluoride Nutrition 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000008234 soft water Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- CRHLEZORXKQUEI-UHFFFAOYSA-N dialuminum;cobalt(2+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Co+2].[Co+2] CRHLEZORXKQUEI-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 239000001034 iron oxide pigment Substances 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical class CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a kind of purple pearlescent pigment, preparation method and applications, are related to pearlescent pigment technical field.Purple pearlescent pigment includes substrate, is successively coated with iron oxide layer, intermediate isolating layer and cobalt blue layer from the inside to the outside on substrate；Preferably, the weight ratio of substrate, iron oxide layer, intermediate isolating layer and cobalt blue layer is 100:2-5:1-3:2-10.The preparation method of purple pearlescent pigment includes: successively coated iron oxide layer, intermediate isolating layer and cobalt blue layer on substrate；Preferably, iron oxide layer, intermediate isolating layer and cobalt blue layer are to carry out cladding formation using the hydrolysis of metal salt by way of liquid deposition.The purple pearlescent pigment of high chroma is formed using the structure that the specific combination of colored oxide is superimposed, while there is good high temperature resistance, can be applied in coating, paint, plastics, leather or wallpaper.
Description
Technical field
The present invention relates to pearlescent pigment technical fields, and in particular to a kind of purple pearlescent pigment, preparation method and answer
With.
Background technique
Pearlescent pigment is gradually widely used in traditional organic and inorganic, metallic pigments answer as a kind of novel pigment
Use field.Design feature based on pearlescent pigment, pearlescent pigment not only has the color of traditional inorganic organic pigment, but also has
There is the luster effect of certain metallic pigments.But compared to inorganic pigment, the tinting strength, tinting power of pearlescent pigment is inadequate.
It is commercialized the pearlescent pigment for the TiO 2 series with stronger interference color effect that common two major classes are at present, has
Interference colours and the iron oxide pearlescent pigment for absorbing color.Just because of the spy of the absorption color and interference colours of iron oxide pearlescent pigment
Point becomes and inorganic iron oxide pigment and organic red pigment is replaced to be possibly realized.But it is existing for pearly-lustre face
The research of material is limited only to blue, black, red, still belongs to for absorbing the research of pearlescent pigment of color and interference colours with purple
Blank.
Summary of the invention
The purpose of the present invention is to provide a kind of purple pearlescent pigment, by sequentially formed on substrate iron oxide layer,
Intermediate isolating layer and cobalt blue layer form a kind of pigment of high chroma purple pearly-lustre, and high temperature resistance is excellent.
Another object of the present invention is to provide a kind of preparation method and application of purple pearlescent pigment, method is easy easily
Row is suitable for industrial applications, and the pigment being prepared is a kind of high chroma purple pearlescent pigment, can be in coating, paint, modeling
It is applied in material, leather or wallpaper.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The invention proposes a kind of purple pearlescent pigments, including substrate, are successively coated with oxidation from the inside to the outside on substrate
Iron layer, intermediate isolating layer and cobalt blue layer；
Preferably, the weight ratio of substrate, iron oxide layer, intermediate isolating layer and cobalt blue layer is 100:2-5:1-3:2-10.
The present invention also proposes a kind of preparation method of purple pearlescent pigment, includes the following steps:
The iron oxide layer successively coated from the inside to the outside, intermediate isolating layer and cobalt blue layer are formed on substrate.
Application of the above-mentioned purple pearlescent pigment in coating, paint, plastics, leather or wallpaper.
The beneficial effect that the embodiment of the present invention provides a kind of purple pearlescent pigment is: it is successively wrapped from the inside to the outside on substrate
Iron oxide layer, intermediate isolating layer and cobalt blue layer are covered, forms high chroma using the structure that the specific combination of colored oxide is superimposed
Purple pearlescent pigment, and the purple pearlescent pigment has good high temperature resistance.
The present invention also provides a kind of preparation methods of purple pearlescent pigment, by being alternately coated with non-ferrous metal oxidation
Object forms the purple pearlescent material of bright high chroma by the superposition of iron oxide and cobalt blue solid colour, can coating, paint,
It is applied in plastics, leather or wallpaper.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the pictorial diagram of purple pearlescent pigment and KC9219 pearlescent pigment powder that the embodiment of the present invention is prepared；
Fig. 2 is the purple pearlescent pigment that the embodiment of the present invention is prepared and KC9219 pearlescent pigment powder in PU resin
Effect contrast figure.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
A kind of purple pearlescent pigment provided in an embodiment of the present invention, preparation method and application are carried out specifically below
It is bright.
The embodiment of the present invention proposes a kind of preparation method of purple pearlescent pigment, by the way that successively cladding aoxidizes on substrate
Iron layer, intermediate isolating layer and cobalt blue layer pass through iron oxide and cobalt blue solid colour by being alternately coated with non-ferrous metal oxide
Superposition forms the purple pearlescent material of bright high chroma.
It should be noted that intermediate isolating layer primarily serves the effect of isolation oxidation iron layer and cobalt blue layer, oxygen can be obstructed
Change iron layer and the doping of interlayer occurs in high-temperature burning process in cobalt blue layer, avoids the occurrence of the impure of form and aspect.
Specifically, iron oxide layer, intermediate isolating layer and cobalt blue layer are to be formed to coat by liquid phase method；Wherein, iron oxide
Layer and cobalt blue layer are to hydrolyze to form cladding using metal salt using Liquid-phase hydrolysis, then form metal using calcining and aoxidize
Object；Intermediate isolating layer is to form cladding using liquid phase deposition.Liquid phase deposition is a kind of deposition method of easy regulation, very
It is suitable for preparing the pearlescent pigment of composite material formation, specifically comprises the following steps:
The formation of S1, iron oxide layer
Hydrolysis, which is carried out, after the suspension that substrate and water are formed is mixed with iron salt solutions obtains the first mixed liquor；It is preferred that
Ground, any one or more of molysite in iron chloride, ferric nitrate and ferric sulfate；More preferably iron chloride.Above several iron
Salt is adapted to form metal oxide layer in substrate surface using liquid phase deposition.
Further, the pH value in the hydrolytic process of molysite is 2.5-3.5, and temperature is 70-90 DEG C, hydrolysis time 20-
40min.The hydrolytic process needs of molysite carry out under stronger acid condition, to promote the progress of hydrolysis.Invention human hair
Existing, the hydrolysising condition control of molysite is advisable within the above range, to guarantee hydrolysis rate, shortens the reaction time.
It is highly preferred that in hydrolytic process, using volume fraction for the hydrochloric acid solution of 40-60% and concentration is 25-35%
Sodium hydroxide solution carry out pH value adjusting.Before iron salt solutions are added, use salt acid for adjusting pH for 2.5-3.5, slow
The slow molysite that is added uses sodium hydroxide to keep pH constant later.
Preferably, substrate has red or purple interference colours；It is highly preferred that substrate is selected from natural mica pearlescent pigment, closes
At any one in nacreous mica pigment, alumina bead delustering pigment and glass pearlescent pigment；Further preferably synthetic mica
Pearlescent pigment.The color for being conducive to the pearlescent pigment for making to be prepared using above several substrates is more bright, and has preferable
Dispersibility, the product color fastness being prepared using synthetic mica pearlescent pigment, glossiness are ideal.It requires supplementation with
It is that above-mentioned raw materials such as synthetic mica pearlescent pigment, is commercial products.
Preferably, the partial size of substrate is 1-100 μm, more preferably 3-60 μm, further preferably 10-40 μm.In order to mention
The uniformity of high covering material load, the partial size of substrate should not be too large or too small, can according to need and crush raw material to meet
Particle size requirements.
Further, the weight ratio of substrate and iron oxide layer is 100:2-5, and the covering amount of iron oxide layer should not be too large, if
The load capacity of iron oxide layer crosses conference and thoroughly changes substrate, and form and aspect are mobile toward blue, and influences purple effect.
Preferably, iron oxide layer is the material of high refractive index, and the refractive index of covering material used is 2.5- in iron oxide layer
3.0.Be conducive to make the colour developing of final material more preferable using the iron oxide layer of high refractive index, obtain the material with bright color.
The formation of S2, intermediate isolating layer
Precipitation reaction is carried out after first mixed liquor is mixed with intermediate isolating salting liquid obtains the second mixed liquor；Preferably,
Any one or more of the material of intermediate isolating layer in barium sulfate, calcirm-fluoride and silica, more preferably barium sulfate.
Above several salts are adapted to that iron oxide layer and cobalt blue layer can be obstructed in high-temperature burning process as intermediate isolating material
There is the doping of interlayer, avoids result in the impure problem of form and aspect.
Specifically, barium sulfate, calcirm-fluoride and silica are utilized in the mode formed in solution, if barium sulfate is with chlorine
Change barium and sodium sulphate is raw material；Calcirm-fluoride is using sodium fluoride and calcium chloride as raw material；Silica is original with sodium metasilicate and hydrochloric acid
Material.
Preferably, the pH value in intermediate isolating salt precipitation process is 7-8, and temperature is 70-90 DEG C, sedimentation time 20-
40min.Inventors have found that this one-step hydrolysis is advisable under neutral or weak basic condition, can further mention with this condition
High hydrolysis rate shortens the reaction time.
Equally, during the reaction, the hydrogen that volume fraction is 25-35% for the hydrochloric acid solution of 40-60% and concentration is used
The adjusting of sodium hydroxide solution progress pH value.After first step hydrolysis, first solution ph is adjusted to using sodium hydroxide
7-8, sequential hydrolysis keep pH value constant using the two cooperation in the process.
Specifically, substrate and intermediate isolating layer weight ratio are 100:1-3, the covering amount of intermediate isolating layer compared to other two
Layer is lower, and covering amount can effectively obstruct iron oxide layer and cobalt blue layer when being 1-3%, prevents from occurring during subsequent calcination
Doping problem.
The formation of S3, cobalt blue layer
Hydrolysis is carried out after second mixed liquor is mixed with the mixed liquor of aluminium salt and cobalt salt, is then filtered again, and
The solid being obtained by filtration is calcined.Such as substrate+Fe is formed by calcination process2O3+BaSO4+Co(AlO2)2Structure, had
There is the purple pearlescent pigment of bright color and preferably dispersibility.Wherein, cobalt blue layer shows spinel-type.
Preferably, the pH value in aluminium salt and the hydrolytic process of cobalt salt is 6-7, and temperature is 70-90 DEG C, hydrolysis time 20-
40min.Inventors have found that this one-step hydrolysis is advisable under neutral or solutions of weak acidity, can further mention with this condition
High hydrolysis rate shortens the reaction time.
Equally, in hydrolytic process, the hydrogen that volume fraction is 25-35% for the hydrochloric acid solution of 40-60% and concentration is used
The adjusting of sodium hydroxide solution progress pH value.Second step first uses salt acid for adjusting pH value for 6-7 after the reaction was completed, then subsequent anti-
It should be controlled with sodium hydroxide in the process and keep pH constant.
Further, after aluminium salt and cobalt salt are hydrolyzed and filtered, solid is washed and under the conditions of 50-150 DEG C of temperature
Dry 6-18h, then calcined.The impurity on the surface of solids is further removed by washing and drying, is conducive to by rear
Continuous calcining obtains the purer product of form and aspect.Preferably, calcination temperature is 600-1100 DEG C, calcination time 0.5-3h；More
Preferably, calcination temperature is 700-1000 DEG C.Calcination process control is advisable within the said temperature range, and temperature is excessively high to destroy production
The structure of product is easy to influence the color of product；Temperature is too low or calcining non-uniform phenomenon occurs, is also unfavorable for obtaining having and become clear
The product of color.
Specifically, cobalt salt is selected from cobalt chloride and/or cobalt nitrate；More preferably cobalt chloride；Aluminium salt is selected from alchlor and nitre
Any one or more in sour aluminium, aluminum sulfate；More preferably alchlor.
Specifically, the weight ratio of substrate and cobalt blue layer is 100:2-10, and cobalt blue layer and iron oxide layer are roughly the same, Ke Yilve
Higher than the content of iron oxide layer, the superposition of iron oxide layer and cobalt blue layer is utilized in the case, passes through the covering amount of both control
Bright purple pearlescent pigment can be formed.
Preferably, in the suspension that substrate and water are formed, the concentration of substrate is 40-60g/L, and the concentration of substrate is controlled upper
It states and is conducive to coat iron oxide layer more effectively in range.Improve the uniformity that product is prepared.
Preferably, cobalt blue layer is the material of high refractive index, and the refractive index of covering material used is 2.5-3.0 in cobalt blue layer.
Be conducive to make the colour developing of final material more preferable using the cobalt blue layer of high refractive index, obtain the material with bright color.
The embodiment of the invention also provides a kind of purple pearlescent pigments, including substrate, successively wrap from the inside to the outside on substrate
It is covered with iron oxide layer, intermediate isolating layer and cobalt blue layer.It can be prepared by the preparation method of above-mentioned purple pearlescent pigment.
Preferably, the weight ratio of substrate, iron oxide layer, intermediate isolating layer and cobalt blue layer is 100:2-5:1-3:2-10；It is logical
It crosses the load capacity of each layer, so that iron oxide layer and cobalt blue layer carry out the superposition of solid colour, forms the high purple pearl of brightness
Delustering pigment, while assigning material good high temperature resistance.
The composition of purple pearlescent pigment can indicate are as follows: substrate+Fe2O3+BaSO4+Co(AlO2)2By adjust iron oxide,
Different violet colors can be obtained in the thickness of cobalt aluminate cladding.Above-mentioned purple pearlescent pigment can coating, paint, plastics,
Application in leather or wallpaper, to assign material purple pearl effect.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of preparation methods of purple pearlescent pigment comprising following steps:
Under agitation, to interfere purple synthetic mica pearlescent pigment to be added to 2L the 80g that average grain diameter is about 15 μm soft
In water, and 70 DEG C are heated to, pH value is down to 2.5 with the hydrochloric acid of 1:1, continue the liquor ferri trichloridi of slow 300ml10%, used
The 30% constant pH value of sodium hydroxide solution progress is constant, continues to stir 20min after adding.
After pH value is risen to 7.0, is stirred 10 minutes after 5g barium chloride is added, be then slowly added into the sodium sulphate of 35ml10%
Solution.It keeps 70 DEG C to continue after stirring 20min after adding, pH value is down to 6.0 with the hydrochloric acid of 1:1, continues the three of slow 400ml
The solution of aluminium chloride/cobalt chloride (40g containing alchlor, cobalt chloride 10g), while being controlled with 30% sodium hydroxide and keeping PH
=6.5 is constant.It keeps 70 DEG C to continue after stirring 20min after adding, dries 18 hours after being filtered, washing at 50 DEG C, most
It is calcined 3 hours at 600 DEG C.
Embodiment 2
The present embodiment provides a kind of preparation methods of purple pearlescent pigment comprising following steps:
Under agitation, purple synthetic mica pearlescent pigment is interfered to be added to 2L the 120g that average grain diameter is about 100 μm
In soft water, and 90 DEG C are heated to, pH value are down to 3.5 with the hydrochloric acid of 1:1, continues the liquor ferri trichloridi of slow 30ml10%,
It is constant that constant pH value is carried out with 30% sodium hydroxide solution, continues to stir 40min after adding.
After pH value is risen to 8.0, is stirred 10 minutes after 5g barium chloride is added, be then slowly added into the sodium sulphate of 35ml10%
Solution.It keeps 90 DEG C to continue after stirring 40min after adding, pH value is down to 7.0 with the hydrochloric acid of 1:1, continues the three of slow 40ml
The solution of aluminium chloride/cobalt chloride (4g/1g), while being controlled with 30% sodium hydroxide and keeping PH=6.5 constant.It is protected after adding
It holds 90 DEG C to continue after stirring 40min, be dried at 150 DEG C after being filtered, washing 6 hours, it is most small in 1100 DEG C of calcinings 0.5
When.
Embodiment 3
The present embodiment provides a kind of preparation methods of purple pearlescent pigment comprising following steps:
Under agitation, to interfere purple synthetic mica pearlescent pigment to be added to 2L the 100g that average grain diameter is about 30 μm soft
In water, and 80 DEG C are heated to, pH value is down to 3.0 with the hydrochloric acid of 1:1, continue the liquor ferri trichloridi of slow 300ml10%, used
The 30% constant pH value of sodium hydroxide solution progress is constant, continues to stir half an hour after adding.
After pH value is risen to 7.5, is stirred 10 minutes after 5g barium chloride is added, be then slowly added into the sodium sulphate of 35ml10%
Solution.It keeps 80 DEG C to continue after stirring half an hour after adding, pH value is down to 6.5 with the hydrochloric acid of 1:1, continues slow 400ml's
The solution of alchlor/cobalt chloride (40g/10g), while being controlled with 30% sodium hydroxide and keeping PH=6.5 constant.It adds
It keeps 80 DEG C to continue after stirring half an hour afterwards, dries at 110 DEG C after being filtered, washing 12 hours, most calcined at 700 DEG C
0.5 hour.
Embodiment 4
The present embodiment provides a kind of preparation methods of purple pearlescent pigment comprising following steps:
Under agitation, to interfere purple natural mica pearlescent pigment to be added to 2L the 100g that average grain diameter is about 60 μm soft
In water, and 80 DEG C are heated to, pH value is down to 3.0 with the hydrochloric acid of 1:1, continue the iron nitrate solution of slow 150ml10%, used
The 30% constant pH value of sodium hydroxide solution progress is constant, continues to stir half an hour after adding.
After pH value is risen to 7.5, is stirred 10 minutes after 2g sodium fluoride is added, be then slowly added into the calcium chloride of 27ml10%
Solution.It keeps 80 DEG C to continue after stirring half an hour after adding, pH value is down to 6.5 with the hydrochloric acid of 1:1, continues slow 200ml's
The solution of aluminum nitrate/cobalt nitrate (32g/12g), while being controlled with 30% sodium hydroxide and keeping PH=6.5 constant.After adding
It is kept for 80 DEG C continue after stirring half an hour, is dried at 110 DEG C after being filtered, washing 12 hours, most calcine 0.5 at 1000 DEG C
Hour.
Embodiment 5
The present embodiment provides a kind of preparation methods of purple pearlescent pigment comprising following steps:
Under agitation, purple alumina bead delustering pigment is interfered to be added to 2L soft water the 100g that average grain diameter is about 15 μm
In, and 80 DEG C are heated to, pH value is down to 3.0 with the hydrochloric acid of 1:1, continues the ferrum sulfuricum oxydatum solutum of slow 300ml10%, with 30%
Sodium hydroxide solution to carry out constant pH value constant, continue to stir half an hour after adding.
After pH value is risen to 7.5, is stirred 10 minutes after 2.9g sodium metasilicate is added, be then slowly added into the hydrochloric acid of 17ml10%
Solution.It keeps 80 DEG C to continue after stirring half an hour after adding, pH value is down to 6.5 with the hydrochloric acid of 1:1, continues slow 400ml's
The solution of aluminum nitrate/cobalt nitrate (64g/14g), while being controlled with 30% sodium hydroxide and keeping PH=6.5 constant.After adding
It is kept for 80 DEG C continue after stirring half an hour, is dried at 110 DEG C after being filtered, washing 12 hours, most calcine 0.5 at 1000 DEG C
Hour.
Embodiment 6
The present embodiment provides a kind of preparation methods of purple pearlescent pigment, and specific steps are roughly the same with embodiment 5, no
It is that substrate is that the 100g that average grain diameter is about 30 μm interferes purple glass pearlescent pigment with place.
Comparative example 1
This comparative example provides a kind of preparation method of pigment, and specific steps are roughly the same with embodiment 3, and difference exists
In: cladding sequence is followed successively by cobalt blue layer, intermediate isolating layer and iron oxide layer.
Comparative example 2
This comparative example provides a kind of preparation method of pigment, and specific steps are roughly the same with embodiment 3, and difference exists
In: iron oxide layer thickness is improved, the dosage of 10% ferric trichloride is 1000mL in experimentation.
Test example 1
By taking the sample being prepared in embodiment 3 as an example, the assessment of properties of product is carried out.The quality evaluation of sample is using normal
The method that the coating seen is stamped the card, certain pearlescent pigment is added in resin after mixing evenly, is then coated with, then uses X-Rite
MA68 color difference meter tests color and finish.It is compared with KC9219 form and aspect, test result is shown in Table 1.
1 color of table and finish testing result
As known from Table 1, the sample being prepared in the present invention, close with existing product KC9219 form and aspect (h ° of value represents color
Phase).In similar form and aspect, color saturation (C* value) and brightness (L* value) are improved, especially color saturation (C* value)
It is obviously improved.
Comparative example 3 and comparative example 1-2 are it is found that the sequence of adjustment cladding can generate apparent shadow to the form and aspect of pigment
Ring, due to cobalt blue with the titanium dioxide layer on sheet substrate in conjunction with and finally iron oxide layer cladding, under the conditions of this pH value,
Cobalt oxide/the alumina layer coated before understands some dissolution, and with the hydrolysis of iron ion cladding during, be entrained in oxygen
Change iron layer.In this way, final form and aspect can retreat, and can blackening.The excessive iron oxide layer that will lead to of the load capacity of iron oxide layer has coated
Formed afterwards it is golden, and then after coating cobalt blue, the form and aspect of entire pearly-lustre can partially bluish-green phase, cannot get purple pearly-lustre.
Test example 2
The purple pearlescent pigment and KC9219 pearlescent pigment powder that the embodiment of the present invention 3 is prepared compare, as a result
Such as Fig. 1.Left side is purple pearlescent pigment in Fig. 1, and right side is KC9219 pearlescent pigment powder, and KC9219 pearlescent pigment powder is white
Color, and the pearlescent pigment that the embodiment of the present invention is prepared is purple, after gray scale is adjusted as shown in fig. 1.
The pearlescent pigment that the embodiment of the present invention is prepared can be applied to paint, coating, plastics, colored leather, wallpaper,
The fields such as powdery paints.Such as pearlescent pigment of the invention is added in paint or plastics, very excellent color can be shown
And color effect.
(1) by taking paint spraying as an example
The pearlescent pigment being prepared in 4.00 grams of embodiments 3 of precise, adds 4.0 grams of butyl acetates and 8.0 grams poly-
Ester car paint resin is placed under blender and is dispersed with stirring 10 minutes, continues 84.0 grams of car paint resin system stirrings 5 of addition
Minute.The viscosity of coating is first adjusted before spraying to Ford4 cup 14-15 seconds.Temperature when spraying between control spraying is 25 Celsius
Degree, relative humidity 60%.Twice of spraying, dodges dry cover varnish after ten minutes, is dodged after doing again and toasts 30 points in 140 degrees Celsius
Clock.
Effect of the purple pearlescent pigment and KC9219 pearlescent pigment powder that the embodiment of the present invention 3 is prepared in PU resin
Fruit compares, and as a result sees Fig. 2.Find out as can be seen from Figure 2, the purple pearlescent pigment being prepared in the embodiment of the present invention is in PU tree
It is purple after being adulterated in rouge, the state in Fig. 2 is showed after gray scale is adjusted.
(2) by taking injection molding application as an example
It accurately weighs polypropylene (PP) dried at 200 grams 105 DEG C to expect in plastic sealing bag, 1 milliliter of light is added
Oily (being also dispersed oil) is then vibrated, and gloss oil is allowed to be sufficiently mixed with polypropylene material.4.000 grams of reality is weighed with assay balance preparation
The pearl powder applied in example 3 is added in plastic sealing bag, vibrates again, rubs, makes pearl powder full and uniform dispersion in PP particle.
Barrel temperature reaches after setting value (usually 180 DEG C~200 DEG C), and the polypropylene material for preparing is added inside hopper, using penetrating
Glue and melten gel function squeeze out clout original in barrel, until squeezing out virgin material, squeeze out virgin material and answer glossy, free from admixture, nothing
Stain, without burn, bubble-free；Meanwhile nozzle should be without clogging when injection.After two panels is no different before and after plastic sheet wait come out,
The plastic sheet that reproduction comes out is to stablize qualified product, can enter automatically normal production.
In conclusion a kind of purple pearlescent pigment provided by the invention, the successively cladding oxidation from the inside to the outside on substrate
Iron layer, intermediate isolating layer and cobalt blue layer form the purple pearl of high chroma using the structure that the specific combination of colored oxide is superimposed
Delustering pigment, and the purple pearlescent pigment has good high temperature resistance.
A kind of preparation method of purple pearlescent pigment provided by the invention, by being alternately coated with non-ferrous metal oxide,
By the superposition of iron oxide and cobalt blue solid colour, the purple pearlescent material of bright high chroma is formed, which can be with
It is applied in coating, paint, plastics, leather or wallpaper.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of purple pearlescent pigment, which is characterized in that including substrate, be successively coated with oxidation from the inside to the outside on the substrate
Iron layer, intermediate isolating layer and cobalt blue layer；
Preferably, the weight ratio of the substrate, the iron oxide layer, the intermediate isolating layer and the cobalt blue layer is 100:2-5:
1-3:2-10；
Preferably, the iron oxide layer, the intermediate isolating layer and the cobalt blue layer are to be formed to coat by liquid phase method；Its
In, the iron oxide layer and the cobalt blue layer are to be hydrolyzed to form cladding using Liquid-phase hydrolysis using metal salt, then utilized
Calcining forms metal oxide；The intermediate isolating layer is to form cladding using liquid phase deposition.
2. purple pearlescent pigment according to claim 1, which is characterized in that the refractive index of the iron oxide layer is 2.5-
3.0；
Preferably, the refractive index of the cobalt blue layer is 2.5-3.0.
3. according to claim 1 or purple pearlescent pigment described in 2, which is characterized in that the substrate has red interference color
Or purple interference colours；Preferably, the substrate is selected from natural mica pearlescent pigment, synthetic mica pearlescent pigment, aluminium oxide pearly-lustre
Any one in pigment and glass pearlescent pigment；Preferably synthetic nacreous mica pigment；
Preferably, the substrate has laminated structure；
Preferably, the partial size of the substrate is 1-100 μm, more preferably 3-60 μm, further preferably 10-40 μm.
4. purple pearlescent pigment according to claim 1, which is characterized in that the material of the intermediate isolating layer is selected from sulfuric acid
Any one or more in barium, calcirm-fluoride and silica, more preferably barium sulfate.
5. the preparation method of purple pearlescent pigment described in any one of -4 according to claim 1, which is characterized in that including as follows
Step:
The iron oxide layer successively coated from the inside to the outside, intermediate isolating layer and cobalt blue layer are formed on substrate；
Preferably, the substrate has red interference color or purple interference colours；It is highly preferred that the substrate is selected from natural mica pearl
Any one in delustering pigment, synthetic mica pearlescent pigment, alumina bead delustering pigment and glass pearlescent pigment；Further preferably
Synthetic mica pearlescent pigment；
Preferably, the partial size of the substrate is 1-100 μm, more preferably 3-60 μm, further preferably 10-40 μm.
6. the preparation method of purple pearlescent pigment according to claim 5, which comprises the steps of:
Hydrolysis, which is carried out, after the suspension that substrate and water are formed is mixed with iron salt solutions obtains the first mixed liquor；
Precipitation reaction is carried out after first mixed liquor is mixed with intermediate isolating salting liquid obtains the second mixed liquor；
Hydrolysis is carried out after second mixed liquor is mixed with the mixed liquor of aluminium salt and cobalt salt, is then filtered again, and
The solid being obtained by filtration is calcined；
Preferably, the cobalt salt is selected from cobalt chloride and/or cobalt nitrate；More preferably cobalt chloride；
Preferably, any one or more of the aluminium salt in alchlor, aluminum nitrate and aluminum sulfate；More preferably trichlorine
Change aluminium；
Preferably, any one or more of the molysite in iron chloride, ferric nitrate and ferric sulfate；More preferably chlorination
Iron；
Preferably, the intermediate isolating layer is any one or more to be formed in barium sulfate, calcirm-fluoride and silica, more excellent
It is selected as barium sulfate.
7. the preparation method of purple pearlescent pigment according to claim 6, which is characterized in that the hydrolytic process of the molysite
In pH value be 2.5-3.5, temperature be 70-90 DEG C, hydrolysis time 20-40min；
Preferably, the pH value in the intermediate isolating salt precipitation process is 7-8, and temperature is 70-90 DEG C, sedimentation time 20-
40min；
Preferably, the pH value in the aluminium salt and the hydrolytic process of the cobalt salt is 6-7, and temperature is 70-90 DEG C, and hydrolysis time is
20-40min；
It is highly preferred that during the reaction, the hydrogen that volume fraction is 25-35% for the hydrochloric acid solution of 40-60% and concentration is used
The adjusting of sodium hydroxide solution progress pH value.
8. the preparation method of purple pearlescent pigment according to claim 6, which is characterized in that the substrate, the oxidation
The weight ratio of iron layer, the intermediate isolating layer and the cobalt blue layer is 100:2-5:1-3:2-10；
Preferably, in the suspension that substrate and water are formed, the concentration of substrate is 40-60g/L.
9. the preparation method of purple pearlescent pigment according to claim 7 or 8, which is characterized in that in the aluminium salt and
After the cobalt salt is hydrolyzed and filtered, by solid washing and dry 6-18h under the conditions of 50-150 DEG C of temperature, then calcined；
Preferably, calcination temperature is 600-1100 DEG C, calcination time 0.5-3h；It is highly preferred that calcination temperature is 700-1000
℃。
10. preparation side described in any one of purple pearlescent pigment of any of claims 1-4 or claim 5-9
Application of the purple pearlescent pigment that method is prepared in coating, paint, plastics, leather or wallpaper.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111454590A (en) * | 2020-04-07 | 2020-07-28 | 上海毅旺塑胶颜料有限公司 | Special flow-mark-free pearlescent pigment for plastics and preparation method thereof |
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| CN1622981A (en) * | 2001-07-12 | 2005-06-01 | 默克专利股份有限公司 | Multilayer pigments based on glass flakes |
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