CN113717549A - Green pearlescent pigment and preparation method and application thereof - Google Patents
Green pearlescent pigment and preparation method and application thereof Download PDFInfo
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- CN113717549A CN113717549A CN202111156770.1A CN202111156770A CN113717549A CN 113717549 A CN113717549 A CN 113717549A CN 202111156770 A CN202111156770 A CN 202111156770A CN 113717549 A CN113717549 A CN 113717549A
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- 239000000049 pigment Substances 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 95
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000000576 coating method Methods 0.000 claims abstract description 46
- 239000002131 composite material Substances 0.000 claims abstract description 40
- 229910000410 antimony oxide Inorganic materials 0.000 claims abstract description 34
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims abstract description 34
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000001056 green pigment Substances 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 16
- 238000000151 deposition Methods 0.000 claims abstract description 15
- 230000007062 hydrolysis Effects 0.000 claims abstract description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 14
- 239000007791 liquid phase Substances 0.000 claims abstract description 14
- 239000003973 paint Substances 0.000 claims abstract description 6
- 239000004033 plastic Substances 0.000 claims abstract description 6
- 229920003023 plastic Polymers 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000010985 leather Substances 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims abstract description 4
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 54
- 239000000243 solution Substances 0.000 claims description 50
- 239000000758 substrate Substances 0.000 claims description 48
- 239000000463 material Substances 0.000 claims description 45
- 239000011248 coating agent Substances 0.000 claims description 37
- 239000000377 silicon dioxide Substances 0.000 claims description 27
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical group [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- CVNKFOIOZXAFBO-UHFFFAOYSA-J tin(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Sn+4] CVNKFOIOZXAFBO-UHFFFAOYSA-J 0.000 claims description 18
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 17
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 17
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 17
- 229910001887 tin oxide Inorganic materials 0.000 claims description 17
- 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 16
- 235000012239 silicon dioxide Nutrition 0.000 claims description 16
- 239000004115 Sodium Silicate Substances 0.000 claims description 15
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 15
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 15
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical group Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 13
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims description 11
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical group [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 11
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical group Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 9
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 9
- 150000001844 chromium Chemical class 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 241000276425 Xiphophorus maculatus Species 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000010445 mica Substances 0.000 claims description 6
- 229910052618 mica group Inorganic materials 0.000 claims description 6
- 150000001462 antimony Chemical class 0.000 claims description 4
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical group C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 150000003608 titanium Chemical class 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 238000005253 cladding Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims 1
- 230000005012 migration Effects 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 72
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000004408 titanium dioxide Substances 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 7
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 238000005507 spraying Methods 0.000 description 6
- 239000004743 Polypropylene Substances 0.000 description 5
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- 239000012071 phase Substances 0.000 description 5
- 229920001155 polypropylene Polymers 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 230000003301 hydrolyzing effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- -1 stirring uniformly Substances 0.000 description 4
- LJAOOBNHPFKCDR-UHFFFAOYSA-K chromium(3+) trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Cr+3] LJAOOBNHPFKCDR-UHFFFAOYSA-K 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- UYTPUPDQBNUYGX-UHFFFAOYSA-N guanine Chemical compound O=C1NC(N)=NC2=C1N=CN2 UYTPUPDQBNUYGX-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 239000008234 soft water Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 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
- 239000007788 liquid Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- ALHBQZRUBQFZQV-UHFFFAOYSA-N tin;tetrahydrate Chemical compound O.O.O.O.[Sn] ALHBQZRUBQFZQV-UHFFFAOYSA-N 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to the technical field of pigments, and discloses a green pearlescent pigment, and a preparation method and application thereof. The preparation method of the green pearlescent pigment comprises the following steps: adopting a liquid phase deposition method, and leading antimony oxide and titanium oxide to be coated on the surfaces of the green particles through hydrolysis of metal salt to form a titanium oxide-doped antimony oxide composite layer to obtain a semi-finished pigment; and drying and calcining the semi-finished pigment. The green pearlescent pigment comprises green pigment particles and a titanium oxide and antimony oxide doped composite layer coated on the outer layer of the green pigment particles from inside to outside. The green pearlescent pigment has the advantages of high chromaticity and glossiness, good high-temperature resistance, good color fastness and good color migration resistance, and is suitable for being applied to coatings, paints, plastics, leather or wallpaper.
Description
Technical Field
The invention relates to the technical field of pigments, in particular to a green pearlescent pigment and a preparation method and application thereof.
Background
One of the two types of pearlescent pigments is a green effect pearlescent pigment with interference color formed according to the thickness change of a coating layer, such as single coated iron oxide and iron oxide, which is not bright enough in color and can show the effect only by matching with a certain colored substrate; secondly, the green pearlescent pigment is formed by compounding the green organic pigment and the pearlescent pigment with interference green, and the color concentration of the green pearlescent pigment is brighter than that of the green pearlescent pigment with single interference color, but the problems of color migration, low temperature resistance and the like exist. Based on the characteristics of the products in the two modes, the use method, the effect and the application field of the product are limited.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a green pearlescent pigment, and a preparation method and application thereof.
The invention is realized by the following steps:
in a first aspect, the present invention provides a method for preparing a green pearlescent pigment, comprising:
adopting a liquid phase deposition method, and leading antimony oxide and titanium oxide to be coated on the surfaces of the green particles through hydrolysis of metal salt to form a titanium oxide-doped antimony oxide composite layer to obtain a semi-finished pigment;
and calcining the semi-finished pigment.
In an optional embodiment, the temperature of a solution system dispersed with the apparent green particles is controlled to be 55-78 ℃, the pH value is 1.5-2.0, then a mixed solution containing antimony salt and titanium salt is added into the solution system, the pH value is kept unchanged in the adding process, and the generated antimony oxide and titanium oxide are coated on the apparent green particles to form a composite layer.
In an alternative embodiment, the antimony salt is antimony trichloride and the titanium salt is titanium tetrachloride.
In an alternative embodiment, the green-appearing particle comprises a substrate and a color-developing layer coated outside the substrate; the mass ratio of the composite layer to the substrate is 53-75%.
In an alternative embodiment, the ratio of the mass of antimony oxide to the mass of titanium oxide in the composite layer is 1.2 to 1.7%.
In an alternative embodiment, the substrate is a sheet substrate.
In an alternative embodiment, the platy substrate is at least one of natural mica, synthetic mica, glass flakes, and alumina.
In an alternative embodiment, the platelet-shaped substrate is synthetic mica having a particle size of 5 to 100 μm, preferably 10 to 40 μm.
In an alternative embodiment, the surface of the greenish-appearing particles is coated with a layer of silica, the coating of the layer of silica being prior to the coating of the composite layer.
In an alternative embodiment, the coating method of the silicon dioxide layer is as follows: the generated silicon dioxide is loaded on the surface of the green-appearing particle by hydrolyzing sodium metasilicate by adopting a liquid phase deposition method.
In an alternative embodiment, the silicon dioxide layer coating is: adding sodium metasilicate into the solution dispersed with the green-appearing particles, and then keeping the pH of the solution system at 6.5-7.5 by using acid and keeping the temperature at 75-85 ℃ to ensure that the generated silicon dioxide is coated on the surfaces of the flaky substrate particles.
In an alternative embodiment, the ratio of the mass of the silica layer to the mass of the platelet-shaped substrate is between 50% and 100%.
In an alternative embodiment, the color developing layer is a chromium hydroxide layer, and the green-developing particles are obtained by coating the surface of the base particles with the chromium hydroxide layer.
In an alternative embodiment, the coating method of the chromium hydroxide layer is as follows: the generated chromium hydroxide is coated on the surface of the flaky substrate particles by adopting a liquid phase deposition method and hydrolyzing chromium salt.
In an alternative embodiment, the chromium hydroxide layer cladding is: controlling the pH value of the solution dispersed with the flaky substrate particles to be 6.5-7.5 and the temperature to be 75-85 ℃, and then adding chromium salt into the solution system to enable chromium hydroxide generated by the reaction to be coated on the surfaces of the flaky substrate particles.
In an optional embodiment, the calcined chromium hydroxide is decomposed into chromium oxide, and the mass ratio of the formed chromium oxide layer to the flaky base material is 22-35%.
In an alternative embodiment, the chromium salt is chromium chloride.
In an alternative embodiment, a tin hydroxide coating is further included before the chromium hydroxide coating is coated on the surface of the base material particles.
In an alternative embodiment, the tin hydroxide coating method is as follows: the liquid phase deposition method is adopted, and the generated tin hydroxide is coated on the surfaces of the flaky substrate particles through hydrolysis of tin salt.
In an alternative embodiment, the tin hydroxide coating is: controlling the pH value of the solution dispersed with the flaky substrate particles to be 1.5-2.0 and the temperature to be 55-78 ℃, and then adding a tin salt solution into the solution system to ensure that tin hydroxide generated by hydrolysis is coated on the surfaces of the flaky substrate particles.
In an alternative embodiment, the calcined tin hydroxide is decomposed to tin oxide, and the mass ratio of the formed tin oxide layer to the sheet-like base material is 1.2 to 1.7%.
In an alternative embodiment, the tin salt is tin chloride.
In an alternative embodiment, the calcination temperature is 800 to 1000 ℃.
In an alternative embodiment, the step of drying the intermediate pigment before calcining is further included.
In a third aspect, the embodiments of the present invention provide a green pearlescent pigment, which is prepared by the preparation method provided in any one of the foregoing embodiments.
In a fourth aspect, an embodiment of the present invention provides a green pearlescent pigment, where the structure of the green pearlescent pigment particle includes, from inside to outside, a green pigment particle and a composite layer of titanium oxide doped with antimony oxide coated on an outer layer of the green pigment particle.
In an alternative embodiment, the ratio of the mass of antimony oxide to the mass of titanium oxide in the composite layer is 1.2 to 1.7%; more preferably, the core of the green pigment particle is a base material, and the mass ratio of the titanium oxide in the composite layer to the base material is 53-75%; preferably, the substrate is a sheet-like substrate.
In an alternative embodiment, a silica layer is further included between the green pigment particles and the composite layer, and the ratio of the mass of the silica layer to the mass of the substrate is 50% to 100%.
In an optional embodiment, the green pigment particles comprise a chromium oxide layer coated outside the flaky base material, and the mass ratio of the chromium oxide layer to the base material is 22-35%.
In an optional embodiment, a tin oxide layer is further included between the base material and the chromium oxide layer, and the mass ratio of the tin oxide layer to the base material is 1.2-1.7%.
In an alternative embodiment, the platy substrate is at least one of natural mica, synthetic mica, glass flakes, and alumina; more preferably, the sheet-like base material is synthetic mica having a particle diameter of 5 to 100 μm, preferably 10 to 40 μm.
In a fifth aspect, the present invention provides the use of a green pearlescent pigment according to the previous embodiments in coatings, paints, plastics, leather or wallpaper.
The invention has the following beneficial effects:
the titanium dioxide is coated outside the pigment particles, so that the high-temperature resistance of the pigment can be improved, and the color fastness and the dispersibility of the pigment are improved; and doping of antimony oxide increases the grey blue phase of titanium oxide and can increase the crystallinity of titanium dioxide. Therefore, the coating of the composite layer can improve the chroma and the glossiness of the pigment, so that the pigment has better high-temperature resistance and better color fastness.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a diagram of a physical product obtained in application example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The green pearlescent pigment and the preparation method thereof provided by the embodiments of the present invention are specifically described below.
According to the green pearlescent pigment provided by the embodiment of the invention, the structure of the green pearlescent pigment particles comprises the green pigment particles and a titanium oxide doped antimony oxide composite layer coated on the outer layer of the green pigment particles from inside to outside.
The titanium dioxide is coated outside the pigment particles, so that the high-temperature resistance of the pigment can be improved, and the color fastness and the dispersibility of the pigment are improved; and doping of antimony oxide increases the grey blue phase of titanium oxide and can increase the crystallinity of titanium dioxide. Therefore, the coating of the composite layer can improve the chroma and the glossiness of the pigment, so that the pigment has better high-temperature resistance and better color fastness.
The specific structure of the green pearlescent pigment from inside to outside is as follows:
the flaky base material is a core, and a tin oxide layer, a chromium oxide layer, a silicon dioxide layer and a composite layer are sequentially coated outside the flaky base material.
The coating of tin oxide is mainly to activate the surface of the sheet-like base material; the chromium oxide layer is colored and coated on the surface of the flaky base material to form absorption color; the silicon dioxide layer can form a low refractive index layer with a certain optical thickness to play a role in optically enhancing the brightness and the chromaticity; the composite layer coating can improve the chromaticity, the luster, the dispersibility, the color fastness and the high temperature resistance of the green pearlescent pigment. In conclusion, the multilayer coating structure of the pigment can realize that the green pearlescent pigment has high photochromic degree and brightness and good high temperature resistance and color migration resistance.
Preferably, in order to enable the prepared green pearlescent pigment to have more excellent performance, the mass ratio of the tin oxide layer to the flaky substrate is 1.2-1.7%; the mass ratio of the chromium oxide layer to the flaky base material is 22-35%; the mass ratio of the silicon dioxide layer to the flaky substrate is 50-100%; the mass ratio of antimony oxide to titanium oxide in the composite layer is 1.2-1.7%; the mass ratio of the titanium oxide in the composite layer to the flaky base material is 53-75%.
Preferably, the platy substrate is at least one of natural mica, synthetic mica, glass flake and alumina; more preferably, the sheet-like base material is synthetic mica having a particle diameter of 5 to 100 μm, preferably 10 to 40 μm.
The preparation method of the green pearlescent pigment provided by the embodiment of the application comprises the following steps:
adopting a liquid phase deposition method, and leading antimony oxide and titanium oxide to be coated on the surfaces of the green particles through hydrolysis of metal salt to form a titanium oxide-doped antimony oxide composite layer to obtain a semi-finished pigment; and calcining the semi-finished pigment.
By the preparation method provided by the embodiment of the application, the green pearlescent pigment with the surface coated with the antimony oxide and titanium oxide composite layer can be prepared, the gray blue phase of titanium oxide is increased by antimony oxide in the composite layer, and the crystallinity of titanium dioxide can be increased by antimony oxide. Therefore, the composite layer of the outer layer of the green pearlescent pigment can improve the chromaticity and the luster of the green pearlescent pigment, and the coated titanium dioxide can enable the pigment to have high temperature resistance and improve the color fastness and the dispersibility of the pigment.
The preparation method specifically comprises the following steps:
s1, coating with tin hydroxide layer
The liquid phase deposition method is adopted, and the generated tin hydroxide is coated on the surfaces of the flaky substrate particles through hydrolysis of tin salt.
The method specifically comprises the following steps: controlling the pH of the solution dispersed with the flaky substrate particles to be 1.5-2.0 and the temperature to be 55-78 ℃ (such as 55 ℃, 60 ℃, 70 ℃ or 78 ℃), and then adding a tin salt solution into the solution system to coat the surfaces of the flaky substrate particles with tin hydroxide generated by hydrolysis. Preferably, the tin salt is tin tetrachloride.
More specifically:
suspending the flaky base material in water, raising the temperature of the water to 55-78 ℃, adding hydrochloric acid into the water to reduce the pH value of the aqueous solution to 1.5-2.0, then adding stannic chloride into the aqueous solution system to hydrolyze the stannic chloride, keeping the pH value of the system unchanged by using a sodium hydroxide solution in the process, stirring for half an hour after the stannic chloride is added, and completely hydrolyzing the stannic chloride to generate stannic hydroxide to coat the surface of the flaky base material.
The mass ratio of the added amount of the tin tetrachloride to the sheet-shaped base material is 1.2-1.7% based on the amount of tin oxide generated by calcining tin hydroxide.
S2, coating with chromium hydroxide layer
Adopting a liquid phase deposition method, and leading the generated chromium hydroxide to be coated on the surfaces of the flaky substrate particles through the hydrolysis of chromium salt;
the method comprises the following steps:
the chromium hydroxide layer coating comprises the following components: controlling the pH value of the solution dispersed with the flaky base material particles to be 6.5-7.5 and the temperature to be 75-85 ℃ (for example, 75 ℃, 80 ℃ or 85 ℃), and then adding chromium salt into the solution system to coat the chromium hydroxide generated by the reaction on the surfaces of the flaky base material particles to obtain green-appearing particles. The green-appearing particles herein correspond to the aforementioned green pigment particles after calcination, and the coated chromium hydroxide layer is a color-developing layer. Preferably, the chromium salt is chromium chloride.
More specifically:
and after the step S1 is completed, raising the temperature of the solution system to 75-85 ℃, adjusting the pH to 6.5-7.5 by adopting a sodium hydroxide solution, slowly adding a chromium chloride solution into the solution system, and adjusting the pH to be unchanged by the sodium hydroxide solution in the process of adding the chromium chloride until the target coating amount is reached.
Preferably, the addition amount of the chromium chloride is 22-35% of the mass ratio of the chromium chloride to the flaky substrate, wherein the chromium chloride is calculated by decomposing the calcined chromium hydroxide into chromium oxide.
S3, coating with silicon dioxide layer
The generated silicon dioxide is loaded on the surface of the green-appearing particle by hydrolyzing sodium metasilicate by adopting a liquid phase deposition method.
The method comprises the following steps: adding sodium metasilicate to a solution in which the flaky substrate particles are dispersed, and then maintaining the pH of the solution system at 6.5 to 7.5 with an acid at a temperature of 75 to 85 ℃ (for example, 75 ℃, 80 ℃ or 85 ℃) to coat the surface of the flaky substrate particles with the generated silica.
More specifically:
and (S2) after the step is completed, keeping the temperature and the pH value of the solution system unchanged, adding sodium metasilicate into the solution system, and keeping the pH value unchanged by using hydrochloric acid in the process of adding the sodium metasilicate. Stirring for half an hour after the sodium metasilicate is added to ensure that the generated silicon dioxide is completely coated.
Preferably, the ratio of the mass of the silica layer to the mass of the sheet-like base material is 50% to 100%.
S4 composite layer coating
And coating antimony oxide and titanium oxide on the surfaces of the green particles by adopting a liquid phase deposition method through hydrolysis of metal salt to obtain the semi-finished pigment.
The method comprises the following steps:
controlling the temperature of a solution system dispersed with the apparent green particles to be 55-78 ℃ (such as 55 ℃, 60 ℃, 70 ℃ or 78 ℃) and the pH to be 1.5-2.0, then adding a mixed solution containing antimony trichloride and titanium tetrachloride into the solution system, and keeping the pH unchanged in the adding process, so that the generated antimony oxide and titanium oxide are coated on the apparent green particles to form a composite layer.
More specifically:
and S3, after the reaction is completed, reducing the temperature of the solution system to 55-78 ℃, controlling the pH value to 1.5-2.0 by hydrochloric acid, slowly adding a mixed solution of antimony trichloride and titanium tetrachloride into the solution system, and keeping the pH value unchanged by using a sodium hydroxide solution in the adding process until the reaction is completed.
Preferably, the mass ratio of antimony oxide to titanium oxide in the composite layer is 1.2 to 1.7%.
Preferably, the ratio of the mass of antimony oxide in the composite layer to the mass of the sheet-like base material is 53 to 75%.
Preferably, the platy substrate is at least one of natural mica, synthetic mica, glass flakes, and alumina.
Preferably, the platy substrate is synthetic mica with a particle size of 5 to 100 μm, preferably 10 to 40 μm.
S5 calcination
And (S4) filtering after the step is finished, drying the solid particles at 110 ℃ for 12h, calcining the dried particles at 800-1000 ℃ for 30min to decompose tin hydroxide into tin oxide and chromium hydroxide into chromium oxide, and thus obtaining the green pearlescent pigment.
In the present application, a green-appearing particle is a pigment particle that appears green after calcination or that itself appears green. For example, in the examples, the greenish particles are particles coated with a layer of chromium hydroxide and decomposed into chromium oxide after calcination to appear green. It should be noted that, in other embodiments of the present application, the green-appearing particles may also be particles that have been decomposed by calcination to produce chromium oxide or pigment particles that have been obtained by a method other than liquid deposition to exhibit a green color. Whether the green pigment particles are not required to be calcined or the particles which are required to be calcined into the green pigment are coated by the composite layer and then calcined, and the green pigment particles are obtained after calcination, the technical scheme is included in the technical scheme provided by the application.
The other green pearlescent pigment provided by the embodiment of the application is prepared by the preparation method provided by the embodiment of the application.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
Under the condition of stirring, 100g of synthetic mica with the particle size range of 5-45 mu m (the average particle size is 27 mu m) is added into 2L of soft water, the soft water is heated to 65 ℃, the pH value of a solution system is reduced to 1.5 by hydrochloric acid with the mass concentration of 50%, tin tetrachloride with the mass ratio of 1.5 percent to the synthetic mica calculated by tin oxide is continuously and slowly added, the constant pH value is kept unchanged by sodium hydroxide solution with the mass concentration of 30 percent, the stirring is continuously carried out for half an hour after the addition is finished, then the temperature is increased to 78 ℃, the pH value is increased to 6.5, 500ml of chromium chloride solution prepared by 100g of chromium chloride hexahydrate is continuously and slowly added, and the pH value is controlled and kept unchanged by sodium hydroxide with the mass concentration of 30 percent. After the addition, the stirring was continued for half an hour, 2000ml of sodium metasilicate solution prepared from 200g of sodium metasilicate was continuously added, and the pH was kept constant with hydrochloric acid. After the completion of the addition, stirring was continued for half an hour, then the pH was raised to 1.5, and 600ml of a titanium tetrachloride solution having a titanium tetrachloride concentration of 160g/L (which contained 1.5% by mass of antimony chloride based on the amount of antimony oxide formed relative to the amount of titanium dioxide formed) was further slowly added, and the pH was kept constant with a 30% by mass sodium hydroxide solution. After the reaction is finished, the mixture is dried for 12 hours at 110 ℃ after being filtered and washed, and finally calcined for 0.5 hour at 800 ℃. The green pearlescent pigment is obtained.
Example 2
This embodiment is substantially the same as embodiment 1 except that: the synthetic mica has a particle size in the range of 10-30 μm (average particle size of 15 μm); 600ml of chromium chloride solution, made up of 120g of chromium chloride hexahydrate, was added, 1500ml of sodium metasilicate solution, made up of 150g of sodium metasilicate.
Example 3
This embodiment is substantially the same as embodiment 1 except that: the mass ratio of the tin chloride to the flaky base material is 1.2 percent, wherein the tin chloride is added in terms of tin oxide obtained by reaction; adding 600ml of chromium chloride solution prepared by 120g of chromium chloride hexahydrate; adding 1800ml sodium metasilicate solution prepared by 180g sodium metasilicate; the titanium tetrachloride was added in an amount of 500ml in which antimony chloride was mixed in an amount of 1.2% by mass in terms of antimony oxide to titanium dioxide produced.
Example 4
This embodiment is substantially the same as embodiment 1 except that: the mass ratio of the tin chloride to the flaky base material is 1.7 percent, wherein the tin chloride is added in terms of tin oxide obtained by reaction; the titanium tetrachloride was added in an amount of 700ml, in which antimony chloride was mixed in a mass ratio of 1.7% based on the amount of antimony oxide formed to the amount of titanium dioxide formed.
Example 5
This embodiment is substantially the same as embodiment 1 except that: the amount of antimony chloride in the titanium tetrachloride solution added was 2.5% in terms of antimony oxide formed compared with titanium dioxide formed.
Example 6
This embodiment is substantially the same as embodiment 1 except that: the tin hydroxide layer was not coated. The pigment particles obtained do not contain a tin oxide layer.
Comparative example 1
In this comparative example, in comparison with example 1, the titanium tetrachloride solution used was not doped with antimony chloride.
Comparative example 2
Compared with the embodiment 1, the comparative example is dried and calcined without coating the composite layer after coating the silicon dioxide layer.
Experimental example 1
The green pearlescent pigments of examples 1 to 6 and comparative examples 1 to 2 were subjected to performance evaluation in a specific manner of:
the quality of the sample is evaluated by a common method of coating a scratch card or a spray plate. Adding a certain pearlescent pigment into resin or paint, stirring uniformly, coating or spraying a plate, and testing the color and the smoothness by using an X-Rite MA68 color difference instrument. As shown in the following table:
TABLE 1 Alice test color data
As can be seen from the above table, the pigment prepared in each example has similar hue (h DEG value represents hue), and the color saturation (C value) and brightness (L value) are remarkably improved compared with the prior product KC 8235. In particular, the color saturation (C value) is significantly improved.
Comparing example 1 and example 5, the saturation and brightness of example 5 were found to be slightly worse, demonstrating the better technical effect when the antimony oxide doping level is within the range claimed in the present application. Comparing example 1 with comparative example 1, the saturation and brightness are both significantly better, which shows that doping antimony chloride can improve the saturation of the pigment and further shows that doping antimony chloride can increase the grey blue phase of titanium oxide; comparing example 1 with comparative example 2, comparative example 2 does not coat the composite layer, and the brightness is much worse than example 1, which shows that for green pearlescent pigment, the brightness can be obviously improved by coating the composite layer.
Experimental example 2
Application example 1: taking paint spraying as an example
4.00 g of the pearlescent pigment from example 1 was weighed out accurately, 4.0 g of butyl acetate and 8.0 g of polyester automotive coating resin were added, the mixture was stirred and dispersed for 10 minutes in a stirrer, and 84.0 g of the automotive coating resin system was added and stirred for 5 minutes. The viscosity of the coating was adjusted to 14-15 seconds for Ford 4 cup before spraying. And during spraying, the temperature of a spraying room is controlled to be 25 ℃, and the relative humidity is controlled to be 60%. Spraying twice, flashing for 10 minutes, covering with varnish, flashing again, and baking at 140 ℃ for 30 minutes. The painting results are shown in fig. 1, and it can be seen that they have very excellent color and color effects.
Application example 2: taking injection molding applications as an example:
200g of polypropylene (PP) material dried at 105 ℃ is accurately weighed into a plastic sealing bag, 1 ml of gloss oil (also called dispersing oil) is added, and then the mixture is shaken to fully mix the gloss oil and the polypropylene material. 4.000 g of the pearl essence of example 1 was weighed into a plastic sealed bag by using an analytical balance preparation, and the bag was shaken and kneaded again to sufficiently and uniformly disperse the pearl essence in the PP particles. After the temperature of the charging barrel reaches a set value (usually 180-200 ℃), adding the prepared polypropylene material into a hopper, extruding the original residual material in the charging barrel by using the functions of injecting glue and melting glue until a new material is extruded, wherein the extruded new material has luster, no impurities, no black spots, no scorching and no bubbles; meanwhile, the nozzle is not blocked during glue injection. After the front and the rear plastic sheets are not different, the produced plastic sheets are stable and qualified products, and can enter automatic normal production.
In conclusion, the green pearlescent pigment and the preparation method thereof provided by the invention have the advantages that titanium dioxide is coated outside the pigment particles, so that the high temperature resistance of the pigment can be improved, and the color fastness and the dispersibility of the pigment are improved; and doping of antimony oxide increases the grey blue phase of titanium oxide and can increase the crystallinity of titanium dioxide. Therefore, the coating of the composite layer can improve the chroma and the glossiness of the pigment and improve the high-temperature resistance and the color fastness of the pigment. Therefore, the green pearlescent pigment provided by the application has the advantages of high chromaticity and glossiness, good high temperature resistance, good color fastness and good color migration resistance, and is suitable for being applied to coatings, paints, plastics, leather or wallpaper.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a green pearlescent pigment is characterized by comprising the following steps:
adopting a liquid phase deposition method, and leading antimony oxide and titanium oxide to be coated on the surfaces of the green particles through hydrolysis of metal salt to form a titanium oxide-doped antimony oxide composite layer to obtain a semi-finished pigment;
and calcining the semi-finished pigment.
2. The method for preparing a green pearlescent pigment according to claim 1, wherein the temperature of the solution system in which the green particles are dispersed is controlled to 55 to 78 ℃ and the pH is 1.5 to 2.0, and then a mixed solution containing antimony salt and titanium salt is added to the solution system, and the pH is maintained during the addition process, so that the generated antimony oxide and titanium oxide are coated on the green particles to form the composite layer;
preferably, the antimony salt is antimony trichloride, and the titanium salt is titanium tetrachloride.
3. The method for producing a green pearl pigment according to claim 1 or 2, wherein the green-appearing particle comprises a substrate and a color-developing layer coated outside the substrate; the mass ratio of the composite layer to the base material is 53-75%;
preferably, the mass ratio of antimony oxide to titanium oxide in the composite layer is 1.2-1.7%;
preferably, the substrate is a sheet-like substrate;
preferably, the platy substrate is at least one of natural mica, synthetic mica, glass flake and alumina,
preferably, the sheet-like base material is synthetic mica, and the particle size of the synthetic mica is 5-100 μm, preferably 10-40 μm.
4. The method for producing a green pearl pigment according to claim 3, wherein a silica layer is coated on the surface of the green-appearing particle, and the silica layer is coated before the coating of the composite layer;
preferably, the coating method of the silicon dioxide layer is as follows: adopting a liquid phase deposition method, and loading the generated silicon dioxide on the surfaces of the green particles through sodium metasilicate hydrolysis;
further preferably, the silica layer coating is: adding sodium metasilicate into the solution dispersed with the apparent green particles, and then keeping the pH of the solution system at 6.5-7.5 by using acid and the temperature at 75-85 ℃ to ensure that the generated silicon dioxide is coated on the surfaces of the flaky substrate particles;
preferably, the ratio of the mass of the silica layer to the mass of the sheet-like base material is 50% to 100%.
5. The process for producing a green pearl pigment according to claim 3, wherein the color-developing layer is a chromium hydroxide layer, and the green-developing particles are obtained by coating a chromium hydroxide layer on the surface of the base particles;
preferably, the cladding method of the chromium hydroxide layer comprises the following steps: adopting a liquid phase deposition method, and coating the generated chromium hydroxide on the surfaces of the flaky substrate particles through the hydrolysis of chromium salt;
more preferably, the chromium hydroxide layer coating is: controlling the pH value of the solution dispersed with the flaky substrate particles to be 6.5-7.5 and the temperature to be 75-85 ℃, and then adding chromium salt into the solution system to enable chromium hydroxide generated by reaction to be coated on the surfaces of the flaky substrate particles;
preferably, the calcined chromium hydroxide is decomposed into chromium oxide, and the mass ratio of the formed chromium oxide layer to the flaky base material is 22-35%;
preferably, the chromium salt is chromium chloride.
6. The method for preparing a green pearlescent pigment according to claim 4, which further comprises coating a tin hydroxide layer before coating the chromium hydroxide layer on the surface of the base material particles;
preferably, the tin hydroxide coating method is as follows: coating the surfaces of the flaky substrate particles with the generated tin hydroxide by adopting a liquid phase deposition method through hydrolysis of tin salt;
more preferably, the tin hydroxide coating is: controlling the pH value of the solution dispersed with the flaky substrate particles to be 1.5-2.0 and the temperature to be 55-78 ℃, and then adding a tin salt solution into the solution system to ensure that tin hydroxide generated by hydrolysis is coated on the surfaces of the flaky substrate particles;
preferably, the calcined tin hydroxide is decomposed into tin oxide, and the mass ratio of the formed tin oxide layer to the flaky base material is 1.2-1.7%;
preferably, the tin salt is tin chloride.
7. The method for preparing a green pearlescent pigment according to claim 1, characterized in that the calcination temperature is 800 to 1000 ℃;
preferably, the step of drying the semi-finished pigment before calcining is also included.
8. A green pearlescent pigment, characterized by being produced by the production method according to any one of claims 1 to 7.
9. The green pearlescent pigment is characterized in that the structure of green pearlescent pigment particles comprises green pigment particles and a titanium oxide doped antimony oxide composite layer coated on the outer layer of the green pigment particles from inside to outside;
preferably, the mass ratio of antimony oxide to titanium oxide in the composite layer is 1.2-1.7%; more preferably, the core of the green pigment particle is a base material, and the mass ratio of the titanium oxide in the composite layer to the base material is 53-75%; preferably, the substrate is a sheet-like substrate;
preferably, a silicon dioxide layer is further included between the green pigment particles and the composite layer, and the mass ratio of the silicon dioxide layer to the substrate is 50-100%;
preferably, the green pigment particles comprise a chromium oxide layer coated outside the flaky base material, and the mass ratio of the chromium oxide layer to the base material is 22-35%;
preferably, a tin oxide layer is further arranged between the base material and the chromium oxide layer, and the mass ratio of the tin oxide layer to the base material is 1.2-1.7%;
preferably, the platy substrate is at least one of natural mica, synthetic mica, glass flake and alumina; more preferably, the sheet-like base material is synthetic mica having a particle diameter of 5 to 100 μm, preferably 10 to 40 μm.
10. Use of the green pearlescent pigment of claim 8 or 9 in coatings, paints, plastics, leather or wallpaper.
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