CN106349799B - A kind of preparation method of coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate package cadmium pigment - Google Patents
A kind of preparation method of coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate package cadmium pigment Download PDFInfo
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- CN106349799B CN106349799B CN201610838456.4A CN201610838456A CN106349799B CN 106349799 B CN106349799 B CN 106349799B CN 201610838456 A CN201610838456 A CN 201610838456A CN 106349799 B CN106349799 B CN 106349799B
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- 239000011248 coating agent Substances 0.000 title claims abstract description 27
- 238000000576 coating method Methods 0.000 title claims abstract description 27
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000000919 ceramic Substances 0.000 title claims abstract description 26
- 238000007641 inkjet printing Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000001030 cadmium pigment Substances 0.000 title claims abstract description 14
- 239000000049 pigment Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 9
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 239000012467 final product Substances 0.000 claims abstract description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical group CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 39
- 229910052793 cadmium Inorganic materials 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 8
- 239000011669 selenium Substances 0.000 claims description 8
- 150000001447 alkali salts Chemical class 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 6
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 6
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 claims description 5
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 230000020477 pH reduction Effects 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 150000002898 organic sulfur compounds Chemical class 0.000 claims description 4
- -1 phosphate compound Chemical class 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims 2
- OSNIIMCBVLBNGS-UHFFFAOYSA-N 1-(1,3-benzodioxol-5-yl)-2-(dimethylamino)propan-1-one Chemical compound CN(C)C(C)C(=O)C1=CC=C2OCOC2=C1 OSNIIMCBVLBNGS-UHFFFAOYSA-N 0.000 claims 1
- 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 1
- 235000005979 Citrus limon Nutrition 0.000 abstract description 5
- 238000000498 ball milling Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000012798 spherical particle Substances 0.000 abstract description 3
- 229910052714 tellurium Inorganic materials 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 2
- 244000248349 Citrus limon Species 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 239000011701 zinc Substances 0.000 description 5
- 244000131522 Citrus pyriformis Species 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 244000061458 Solanum melongena Species 0.000 description 3
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 2
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 2
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 239000001052 yellow pigment Substances 0.000 description 2
- 239000004246 zinc acetate Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000170916 Paeonia officinalis Species 0.000 description 1
- 235000006484 Paeonia officinalis Nutrition 0.000 description 1
- ZXRRHFSTAFVGOC-UHFFFAOYSA-N [AlH3].[K] Chemical compound [AlH3].[K] ZXRRHFSTAFVGOC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000000003 hoof Anatomy 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 150000002641 lithium Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of preparation method of coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate package cadmium pigment.This method presses certain molar ratio first and the corresponding each raw material of Zr, Si, Cd, S, Se, Te, Zn, Al, P is carried out ingredient, and then to reaction conditions such as each raw material strict control combination, hybrid mode, orders of addition, final product is made.Method of the invention reduces the process that tradition needs ball milling, and calcination temperature also reduces 100 degree, generates apparent energy-saving effect.Gained pigment meso-position radius of the invention can achieve 0.6-1.2 micron, D97 be 2 microns, almost spherical particle and there is outstanding advantages of good mobility, high temperature resistant, good weatherability, environmental protection, and color can be distributed in lemon yellow-it is yellow-red-aubergine, be able to satisfy different field coating/ceramic ink jet printing requirement.
Description
Technical field
The invention belongs to a kind of coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicates to wrap up cadmium pigment
Preparation method, in particular to a kind of coating use/ceramic ink jet printing wraps up cadmium system face with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of material.
Background technique
Pigment is indispensable one of the ingredient of various coating, and pigment not only acts as the effect of color and decoration, especially heavy
What is wanted is that it can improve painting film strength, anti-corrosion, fast light, weather resistance and other effects.Cadmium pigment is a weight in inorganic pigment
Want kind.Two class of yellow class and red colour system can be substantially divided by being divided to by color.Yellow class is the solid solution of CdS and CdS with ZnS,
Its form and aspect gradually switch to lemon yellow with the increase of ZnS content.Since cadmium pigment acid resistance is poor, in certain item
Under part, can dissociate cadmium ion out, pollute environment, be unfavorable for being widely applied.Cadmium pigment is wrapped in using zirconium silicate crystal
Wherein, since zirconium silicate matrix has the Optimalities such as high-temperature stability is good, chemical stability is good, the transparency is good, corrosion resistance is strong
Can, it not only can solve cadmium yellow high-temperature discoloration and the pollution problem to environment, but also further expansion cadmium yellow pigment is used into model
It encloses.And traditional zirconium silicate wraps up cadmium system technique, can only produce meso-position radius at 4-8 microns, maximum particle diameter is at 20 microns or more, no
Can be suitably used for coating use/ceramic ink jet printing to use, and be distributed on particle tiny pin hole, dispersibility not enough, therefore, performance is not
It is good.
Summary of the invention
It is an object of the invention to improve the deficiency of prior art zirconium silicate package cadmium system technique, provide a kind of coating use/
The preparation method of ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate package cadmium pigment, its almost spherical particle and tool
Have good mobility, high temperature resistant, environmental protection, good weatherability, particle meso-position radius can achieve 0.6-1.2 microns, D97 be 2 microns
And color development it is strong the advantages that, be able to satisfy the requirement of different field coating and ceramic ink jet printing.
In order to achieve the above object, the technical scheme is that
A kind of preparation side of coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate package cadmium pigment
Method, it is characterised in that include the following steps:
(1) Zr:Si:Cd:S:Se:Te:Zn:Al:P=(0.6~0.8) is pressed: (0.5~0.9): (0.04~0.06):
(0.04~0.06): (0.001~0.02): (0.0001~0.002): (0.001~0.005): (0.0005~0.005):
The molar ratio (i.e. the mass ratio of the material) of (.0001~0.008) weighs the corresponding raw material of each element respectively；
(2) metal salt of Zr, Cd, Zn and aluminum contained compound (the corresponding compound of Al) are dissolved in organic solvent, are denoted as
A；
(3) by organic sulfur compound (the corresponding raw material of S), selenium simple substance (the corresponding raw material of Se), Te simple substance (the corresponding original of Te
Material) and alkali or basic salt be dissolved in organic solvent, be denoted as B；
(4) organosilicon is taken, C is denoted as；
(5) acid is taken, D is denoted as；
(6) phosphorus-containing compound dissolution in a solvent, is denoted as J；
(7) A is mixed in a manner of total drop with B, is kept stirring, while J being added dropwise in the process, is denoted as E；
(8) after E stirs 0.5~2h, C, D is dripped in E altogether, is kept stirring, and control pH, is denoted as F；
(9) it until F being washed to no ion wash-off, is dried with drying box, smashes it through 100~1000 meshes, be denoted as G；
(10) G is uniformly mixed with fluorine-containing mineralizer, is denoted as H；
(11) H is fitted into crucible and is calcined；
(12) by calcined product acidification, soda boiling, rinsing and drying, I, i.e. final product coating use/ceramic ink jet printing are denoted as
Cadmium pigment is wrapped up with high temperature environment-friendly type time nanometer zirconium silicate.
It is because the partial size of resulting materials of the present invention is 0.6- it is worth noting that there is " secondary nanometer " in title herein
1.2 microns, the upper limit is more bigger than general nanometer concept (the general nanometer upper limit to hundreds of nanometers), and lower limit is again than general
Micron it is small (micron refers generally to several to more than ten micron), therefore to be expressed as " secondary nanometer ".
Further, the metal salt of Zr, Cd, Zn of step (2) are the organic metal salt or inorganic metal salt of Zr, Cd, Zn,
The preferably acetate of Zr, Cd, Zn or the corresponding chloride of metal.
Further, the aluminum contained compound preferably sulfuric acid aluminium potassium or aluminium chloride of step (2).
Further, the preferred ammonium sulfide of organic sulfur compound or thiocarbamide of step (3).
Further, step (2), the preferred propylene glycol of organic solvent of step (3), dimethylformamide, dimethyl sulfoxide
One or more of.
Further, the alkali of step (3) or basic salt preferred NaOH, Na2CO3、NaHCO3One or more of.
Further, the preferred ethyl orthosilicate of organosilicon of step (4).
Further, the sour preferably sulfuric acid or hydrochloric acid of step (5).
Further, the preferred metaphosphoric acid of phosphorus-containing compound or polymer phosphate compound of step (6).
Further, the pH value range of step (8) is 7.0~8.5.
Further, the drying box temperature range of step (9) is 100~150 DEG C.
Further, in the fluorine-containing mineralizer preferred fluorinated lithium, ammonium fluosilicate, ammonium fluoride, ammonium fluoroborate of step (10)
The ratio between amount of substance of one or more, fluorine-containing mineralizer and Zr is 1:0.8~1.2.
Further, the calcining of step (11), temperature are 600~800 DEG C, and the time is 10~30 minutes.
The beneficial effects of the present invention are:
(1) the resulting zirconium silicate package cadmium pigment of preparation method of the invention is that (i.e. small size is micro- for time nanostructure
Rice structure), almost spherical particle, meso-position radius can achieve 0.6-1.2 micron, D97 be 2 microns, significantly improve the prior art
The inadequate problem of zirconium silicate package cadmium pigment dispersibility, have that color development is strong, good fluidity, high temperature resistant, environmental protection, good weatherability
The advantages of.
(2) preparation method of the invention reduces tradition and needs the process of ball milling, calcination temperature also reduce 100 degree with
On, produce apparent energy-saving effect.
(3) present invention not only can control the phenomenon that presoma colloid increases but also also provide for react under hot conditions and generates
With gaseous chemical component, avoids high temperature easy-sintering from increasing to particle, do not need ball-milling technology, and color can be distributed in
Lemon yellow-is yellow-red-aubergine, it can satisfy requirement of the different field as coating/ceramic ink jet printing.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention；
Fig. 2 is that coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate prepared by embodiment 1 wraps up cadmium system
The TEM of lemon yellow pigment detects photo；
Fig. 3 is that coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate prepared by embodiment 2 wraps up cadmium system
The TEM of aubergine pigment detects photo；
Fig. 4 is that coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate prepared by embodiment 3 wraps up cadmium system
The TEM of aubergine pigment detects photo.
Specific embodiment
The present invention will be further described in detail combined with specific embodiments below, but embodiments of the present invention are not limited to
This can refer to routine techniques progress to not specified technological parameter.
Embodiment 1
Step 1: by basic zirconium chloride 0.6mol, caddy 0.06mol, zinc chloride 0.002mol and aluminium chloride 0.004mol
It is dissolved in propylene glycol and is configured to the solution that total mass fraction is 35%, be denoted as A；
Step 2: by sodium hydroxide 0.14mol, ammonium sulfide 0.06mol, selenium simple substance 0.01mol and tellurium simple substance 0.001mol
It is dissolved in propylene glycol and is configured to the solution that total mass fraction is 11%, be denoted as B；
Step 3: 0.6mol ethyl orthosilicate is taken to be dissolved in propylene glycol, it is denoted as C；
Step 4: by 30ml diluting concentrated sulfuric acid at 500ml sulfuric acid solution (H2SO4, 98wt%), it is denoted as D；
Step 5: in a solvent by metaphosphoric acid 0.001mol dissolution, being denoted as J；
Step 6: dripping A and B in propylene glycol altogether, it is kept stirring, while J being added dropwise in the process, is denoted as E；
Step 7: C, D are dripped in E altogether, is kept stirring, and control pH=7.5, is denoted as F after E stirs 1h；
Step 8: until F is washed to no ion wash-off, excessively 100 after dry, pulverize under 150 DEG C of temperature environment~
1000 meshes, are denoted as G；
Step 9: G is uniformly mixed with 16g (0.6mol) lithium fluoride, it is denoted as H；
Step 10: H is fitted into crucible, calcined at 800 DEG C and keeps the temperature 30 minutes；
Step 11: product acidification, soda boiling, rinsing and drying are finally denoted as I.
Gained pigment color is peony, and meso-position radius is 0.8 micron.
Embodiment 2
Step 1: zirconium acetate 0.6mol, cadmium acetate 0.06mol, zinc acetate 0.001mol and aluminium chloride 0.002mol is molten
It is configured to the solution that mass concentration is 35% in propylene glycol, is denoted as A；
Step 2: by sodium hydroxide 0.14mol, ammonium sulfide 0.06mol, selenium simple substance 0.01mol and tellurium simple substance 0.0008mol
It is dissolved in propylene glycol and is configured to the solution that mass concentration is 11%, be denoted as B；
Step 3: 0.6mol ethyl orthosilicate is taken to be dissolved in propylene glycol, it is denoted as C；
Step 4: 100mL concentrated hydrochloric acid is taken to be diluted to 300ml hydrochloric acid solution (HCl, 37.5wt%), it is denoted as D；
Step 5: in a solvent by metaphosphoric acid 0.002mol dissolution, being denoted as J；
It mixes, is kept stirring step 6: A is dripped altogether with B, while J being added dropwise in the process, be denoted as E；
Step 7: by C, D drop in E, being kept stirring, and control pH=8 after E stirs 1h, being denoted as F；
Step 8: until F is washed to no ion wash-off, excessively 100 after dry, pulverize under 150 DEG C of temperature environment~
1000 meshes, are denoted as G；
Step 9: G is uniformly mixed with 16g (0.6mol) lithium fluoride, it is denoted as H；
Step 10: H is fitted into crucible, calcined at 800 DEG C and keeps the temperature 30 minutes；
Step 11: product acidification, soda boiling, rinsing and drying are finally denoted as I.
Gained pigment color is lemon yellow, and meso-position radius is 0.6 micron.
Embodiment 3
Step 1: zirconium acetate 0.8mol, cadmium acetate 0.04mol, zinc acetate 0.005mol and aluminium chloride 0.004mol is molten
It is configured to the solution that mass concentration is 35% in propylene glycol, is denoted as A；
Step 2: by sodium hydroxide 0.12mol, ammonium sulfide 0.04mol, selenium simple substance 0.008mol and hoof simple substance 0.002mol
It is dissolved in propylene glycol and is configured to the solution that mass concentration is 11%, be denoted as B；
Step 3: 0.9mol ethyl orthosilicate is taken to be dissolved in propylene glycol, it is denoted as C；
Step 4: 100mL concentrated hydrochloric acid is taken to be diluted to 300ml hydrochloric acid solution (HCl, 37.5wt%), it is denoted as D；
Step 5: in a solvent by metaphosphoric acid 0.006mol dissolution, being denoted as J；
It mixes, is kept stirring step 6: A is dripped altogether with B, while J being added dropwise in the process, be denoted as E；
Step 7: by C, D drop in E, being kept stirring, and control pH=7 after E stirs 1h, being denoted as F；
Step 8: until F is washed to no ion wash-off, excessively 100 after dry, pulverize under 150 DEG C of temperature environment~
1000 meshes, are denoted as G；
Step 9: G is uniformly mixed with 0.9mol ammonium fluoride, it is denoted as H；
Step 10: H is fitted into crucible, calcined at 800 DEG C and keeps the temperature 30 minutes；
Step 11: product acidification, soda boiling, rinsing and drying are finally denoted as I.
Gained pigment color is aubergine, and meso-position radius is 1.0 microns.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of coating use/ceramic ink jet printing preparation method of high temperature environment-friendly type time nanometer zirconium silicate package cadmium pigment,
It is characterized by comprising the following steps:
(1) Zr:Si:Cd:S:Se:Te:Zn:Al:P=(0.6 ~ 0.8): (0.5 ~ 0.9): (0.04 ~ 0.06) is pressed: (0.04 ~
0.06): (0.001 ~ 0.02): (0.0001 ~ 0.002): (0.001 ~ 0.005): (0.0005 ~ 0.005): (0.001 ~ 0.008)
Molar ratio weigh the corresponding raw material of each element respectively；
(2) metal salt of Zr, Cd, Zn and aluminum contained compound are dissolved in organic solvent, are denoted as A；
(3) organic sulfur compound, selenium simple substance, Te simple substance and alkali or basic salt are dissolved in organic solvent, are denoted as B；
(4) organosilicon is taken, C is denoted as；
(5) acid is taken, D is denoted as；
(6) phosphorus-containing compound dissolution in a solvent, is denoted as J；
(7) A is mixed in a manner of total drop with B, is kept stirring, while J being added dropwise in the process, is denoted as E；
(8) after E stirs 0.5 ~ 2h, C, D is dripped in E altogether, is kept stirring, and control pH, is denoted as F；
(9) it until F being washed to no ion wash-off, is dried with drying box, smashes it through 100 ~ 1000 meshes, be denoted as G；
(10) G is uniformly mixed with fluorine-containing mineralizer, is denoted as H；
(11) H is fitted into crucible and is calcined；
(12) by calcined product acidification, soda boiling, rinsing and drying, it is denoted as I, i.e. final product coating use/ceramic ink jet printing is high
Temperature environmental-friendly time nanometer zirconium silicate wraps up cadmium pigment, wherein secondary nanometer indicates that the partial size of resulting materials is 0.6-1.2 microns.
2. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the metal salt of Zr, Cd, Zn of step (2) are the organic metal salt or nothing of Zr, Cd, Zn
Machine metal salt；The aluminum contained compound of step (2) is aluminum aluminum sulfate or aluminium chloride；Step (2) organic solvent is propylene glycol, dimethyl
One or more of formamide, dimethyl sulfoxide.
3. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the organic sulfur compound of step (3) is ammonium sulfide or thiocarbamide；The organic solvent of step (3)
For one or more of propylene glycol, dimethylformamide, dimethyl sulfoxide.
4. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the alkali or basic salt of step (3) are NaOH, Na2CO3、NaHCO3One of or two
Kind or more.
5. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the organosilicon of step (4) is ethyl orthosilicate.
6. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the acid of step (5) is sulfuric acid or hydrochloric acid.
7. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the phosphorus-containing compound of step (6) is metaphosphoric acid or polymer phosphate compound.
8. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the pH value range of step (8) is 7.0 ~ 8.5；The drying box temperature of step (9) is 100
~150℃。
9. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the fluorine-containing mineralizer of step (10) is lithium fluoride, ammonium fluosilicate, ammonium fluoride, fluoboric acid
The ratio between amount of substance of one or more of ammonium, fluorine-containing mineralizer and Zr is 1:0.8 ~ 1.2.
10. coating use/ceramic ink jet printing according to claim 1 wraps up cadmium system with high temperature environment-friendly type time nanometer zirconium silicate
The preparation method of pigment, which is characterized in that the calcining of step (11), temperature are 600 ~ 800 DEG C, and the time is 10 ~ 30 minutes.
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| CN113072839B (en) * | 2021-03-11 | 2023-01-03 | 龙南鑫坤无机新材料有限公司 | Bright bright scarlet coating pigment for ceramic ink-jet printing and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1403470A (en) * | 1972-05-05 | 1975-08-28 | Degussa | Ceramci pigments based on zirconium silicate |
| CN101182236A (en) * | 2007-11-15 | 2008-05-21 | 广东东鹏陶瓷股份有限公司 | Zirconium silicate coated ceramic pigment and method for making same |
| CN101786902A (en) * | 2010-03-04 | 2010-07-28 | 陕西科技大学 | Preparation method for extended red ZrSiO_4-Cd (S_xSe_(1-x)) pigment |
| CN102515853A (en) * | 2011-12-30 | 2012-06-27 | 江苏拜富科技有限公司 | Preparation method of zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment |
-
2016
- 2016-09-21 CN CN201610838456.4A patent/CN106349799B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1403470A (en) * | 1972-05-05 | 1975-08-28 | Degussa | Ceramci pigments based on zirconium silicate |
| CN101182236A (en) * | 2007-11-15 | 2008-05-21 | 广东东鹏陶瓷股份有限公司 | Zirconium silicate coated ceramic pigment and method for making same |
| CN101786902A (en) * | 2010-03-04 | 2010-07-28 | 陕西科技大学 | Preparation method for extended red ZrSiO_4-Cd (S_xSe_(1-x)) pigment |
| CN102515853A (en) * | 2011-12-30 | 2012-06-27 | 江苏拜富科技有限公司 | Preparation method of zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment |
Non-Patent Citations (1)
| Title |
|---|
| 溶胶_共沉淀法合成硅酸锆包裹硫硒化镉色料的研究;刘华锋;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20160131;第13，43,52页 |
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