CN109651846A - A kind of post-processing approach of rare-earth sulfide - Google Patents
A kind of post-processing approach of rare-earth sulfide Download PDFInfo
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- CN109651846A CN109651846A CN201811622624.1A CN201811622624A CN109651846A CN 109651846 A CN109651846 A CN 109651846A CN 201811622624 A CN201811622624 A CN 201811622624A CN 109651846 A CN109651846 A CN 109651846A
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- China
- Prior art keywords
- rare
- earth sulfide
- primary powder
- quality
- oxide
- Prior art date
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- -1 rare-earth sulfide Chemical class 0.000 title claims abstract description 51
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 47
- 238000012805 post-processing Methods 0.000 title claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- 239000012065 filter cake Substances 0.000 claims description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000003350 kerosene Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 230000001476 alcoholic effect Effects 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 239000011787 zinc oxide Substances 0.000 claims description 9
- 239000000428 dust Substances 0.000 claims description 8
- 239000008396 flotation agent Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- MMXSKTNPRXHINM-UHFFFAOYSA-N cerium(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[Ce+3].[Ce+3] MMXSKTNPRXHINM-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000004220 aggregation Methods 0.000 claims description 6
- 230000002776 aggregation Effects 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 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 5
- 239000002253 acid Substances 0.000 claims description 5
- 238000003682 fluorination reaction Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 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 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229910001515 alkali metal fluoride Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- OLXOEPPPBAHCOC-UHFFFAOYSA-N cerium(3+) lanthanum(3+) trisulfide Chemical compound [S-2].[La+3].[Ce+3].[S-2].[S-2] OLXOEPPPBAHCOC-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000002283 diesel fuel Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- 150000003951 lactams Chemical class 0.000 claims description 2
- YTYSNXOWNOTGMY-UHFFFAOYSA-N lanthanum(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[La+3].[La+3] YTYSNXOWNOTGMY-UHFFFAOYSA-N 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- 239000000230 xanthan gum Substances 0.000 claims description 2
- 229920001285 xanthan gum Polymers 0.000 claims description 2
- 235000010493 xanthan gum Nutrition 0.000 claims description 2
- 229940082509 xanthan gum Drugs 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims 1
- CGBRHEMTHVMXEI-UHFFFAOYSA-L dicalcium oxygen(2-) sulfate Chemical compound [O-2].[Ca+2].S(=O)(=O)([O-])[O-].[Ca+2] CGBRHEMTHVMXEI-UHFFFAOYSA-L 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- GVGCUCJTUSOZKP-UHFFFAOYSA-N nitrogen trifluoride Chemical compound FN(F)F GVGCUCJTUSOZKP-UHFFFAOYSA-N 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- 239000002243 precursor Substances 0.000 claims 1
- 239000000049 pigment Substances 0.000 abstract description 14
- 239000000126 substance Substances 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical class Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000485 pigmenting effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- GOLXNESZZPUPJE-UHFFFAOYSA-N spiromesifen Chemical compound CC1=CC(C)=CC(C)=C1C(C(O1)=O)=C(OC(=O)CC(C)(C)C)C11CCCC1 GOLXNESZZPUPJE-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010792 warming Methods 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
- 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
-
- 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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- 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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
-
- 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
-
- 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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- 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
- C09C3/12—Treatment with organosilicon compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention provides a kind of post-processing approach of rare-earth sulfide, and the method passes through the rare-earth sulfide primary powder arrived that will be prepared after step processing of the invention, and bright-coloured as pigment color, tinting strength, tinting power, strong covering power, chemical stability is good, heat-resist.
Description
Technical field
The present invention relates to chemical technology fields, and in particular to a kind of post-processing approach of rare-earth sulfide.
Background technique
Increasingly serious with International Environmental Protection situation, many countries make stringent regulation limitation or forbid making in recent years
With the toxic pigment polluted the environment, the colour containing toxic heavy metals such as cadmium, chromium and lead being just widely used in the market
Inorganic pigment will all be eliminated.The nineties in last century, the national legislations such as America and Europe provide the marking paint on road must be it is unleaded,
Last year European Union provides that all red and yellow uitramarines must not contain cadmium again.So developing green non-poisonous free of contamination high quality red
It is extremely urgent with yellow uitramarine.
Rare earth sulfide pigment is a kind of environment friendly inorganic pigment without heavy metal, and not soluble in water and strong base solution is readily soluble
In acid and hydrogen sulfide gas is released, its chemical stability in inert gas and reducing atmosphere is being aoxidized up to 1500 DEG C
Up to 350 DEG C in atmosphere.In recent years, due to rare earth sulfide pigment have chromatic colour, good weatherability and by as one kind
The color pigment of environmental protection is applied to the fields such as plastics, coating, to replace toxic heavy metal pigment.
There are two types of the most widely used preparation methods of rare earth sulfide pigment: one is to consolidate synthetic method, the other is gas
Gu synthetic method.The rare earth sulfide pigment of either which kind of method synthesis suffers from that color power, covering power are poor, and thermal stability is not high,
The poor disadvantage of acid resistance.
Summary of the invention
Therefore, the purpose of the present invention is under the premise of not influencing rare earth sulfide pigment intrinsic colour, obtain nonhazardous,
Good dispersion, and the pigment rare-earth sulfide that tinting strength, tinting power, covering power, thermal stability and acid resistance are all improved.
Above-mentioned purpose of the invention is achieved through the following technical solutions:
A kind of post-processing approach of rare-earth sulfide, method includes the following steps:
(1) rare-earth sulfide primary powder is mixed with water, obtains mixed solution；Then flotation agent is added into mixed liquor,
The ground and mixed in colloid mill removes the aggregation of floating during grinding, filter cake is then obtained by filtration.
(2) filter cake that step (1) obtains is washed with alcoholic solution, the filter cake after then making washing is mixed with alcoholic solution to be stirred
It mixes, dispersing agent is added during stirring, then in the absence of oxygen, be ground to the rare-earth sulfide in mixed solution
Partial size is 100-3000nm；
(3) after step (2), fluorization agent is added into mixed liquor and carries out fluorination treatment；
(4) after the fluorination treatment of step (3), zinc oxide and catalyst are added into mixed solution；
(5) after step (4), transparent oxide presoma is added, and into mixed solution immediately with 100-1000g/
The speed of min adds, and stirs 1-3h；
(6) after step (5), filtering, alcohol are washed and are dried, and obtain dry rare-earth sulfide；
(7) rare-earth sulfide by the drying that step (6) obtains is sieved through screen centrifuge, obtains product.
Preferably, in step (1), the rare-earth sulfide primary powder is cerium sulphide, lanthanum sulfide, lanthanum cerium sulfide or sulphur
Change the primary powder of samarium；It is highly preferred that the rare-earth sulfide primary powder is cerium sulphide primary powder；
Preferably, in step (1), the mass ratio of the rare-earth sulfide primary powder and water is 1:1-5；
Preferably, in step (1), the flotation agent is kerosene, diesel oil, vegetable oil；
Preferably, in step (1), the quality of the flotation agent is the 3%-9% of rare-earth sulfide primary powder quality,
More preferably 5%；
Preferably, in step (1), the aggregation of the floating is the aggregation of the carbon dust and flotation agent in primary powder
Object；
Preferably, in step (2), the alcoholic solution is selected from methanol, ethyl alcohol or butanol, more preferably 99% ethyl alcohol；
Preferably, in step (2), described mixed with filter cake with the quality of alcoholic solution is rare-earth sulfide primary powder matter
2-10 times of amount, more preferably 3 times；
Preferably, in step (2), the dispersing agent is the polymerization of non-ionic water-soluble either organic solvent-soluble
Object；More preferably cellulose and its derivates, polyvinyl lactam, polyethylene oxide, polyethylene glycol, polyoxyethylated polyoxypropylene
Glycol, polyacrylate, polyoxyethylated acid esters, polyoxyethylenated alkylphenol, polyvinyl alcohol, alkanolamide, polyethylene pyrrole
Pyrrolidone or compound based on xanthan gum, more preferably polyvinylpyrrolidone；
Preferably, in step (2), the quality of the dispersing agent is the 0.5%- of rare-earth sulfide primary powder quality
5%, more preferably 2%；
Preferably, in step (2), the partial size is 300-800nm, it is therefore preferable to 500nm；
Preferably, in step (3), the fluorization agent is solid, liquid or gaseous fluorinated dose, more preferably liquid or gas
Body fluorization agent；
Preferably, in step (3), the fluorization agent is selected from fluorine gas, hydrofluoric acid, ammonium fluoride, alkali metal fluoride or fluorine
Change nitrogen, more preferably ammonium fluoride；
Preferably, in step (3), the quality of the fluorization agent is the 1%- of rare-earth sulfide primary powder quality
20%, more preferably 5%；
Preferably, in step (4), the partial size of the zinc oxide is less than 40 μm, more preferably 500nm；
Preferably, in step (4), the quality of the zinc oxide is the 1%- of rare-earth sulfide primary powder quality
15%；More preferably 5%；
Preferably, in step (4), the catalyst be ammonium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, more preferably
For ammonium hydroxide；
Preferably, in step (4), the quality of the catalyst is the 5%- of rare-earth sulfide primary powder quality
60%；More preferably 25%；
Preferably, in step (5), the transparent oxide presoma is selected from silester (corresponding silica), sulphur
Sour aluminium (corresponding aluminium oxide), zirconium sulfate (corresponding zirconium oxide), calcium sulfate (corresponding calcium oxide) or sulfuric acid rare earth (corresponding rare earth metal
Oxide) one of or it is a variety of；It is highly preferred that the transparent oxide presoma is selected from silester；
Preferably, in step (5), the quality of the transparent oxide presoma is rare-earth sulfide primary powder quality
5%-50%；More preferably 15%；
Preferably, during carrying out step (5), maintaining temperature is 10-40 DEG C, more preferably 25 DEG C；Maintenance pH is 8-
10, more preferably 9；
Preferably, in step (7), centrifugal screen aperture is 10-100 μm, more preferably 45 μm.
In a specific embodiment, the fluorination treatment of step (3) is carried out using the following conditions:
Ce2S3Concentration of slurry (refers to the mixture obtained after step (2) processing, that is, refers to rare-earth sulfide+alcoholic solution+dispersion
Agent): 300~500g/L；
NH4F solution concentration: 120~180g/L；
Handle PH:> 8-10；
Treatment temperature: > 20-30 DEG C；
Handle the time: 100-120min.
In another specific embodiment, carries out 2 times in step (5) or repeatedly carry out again step (6) later, and work as
When step (5) carries out 2 times or repeatedly carries out step (6) again later, transparent oxide forerunner used by each implementation steps (5)
Body may be the same or different.
In another specific embodiment, step (6) are carried out again after step (5) carry out 2 times, wherein real for the first time
Applying transparent oxide presoma used by step (5) is silester (corresponding silica), second of implementation steps (5) institute
The transparent oxide presoma used is aluminum sulfate (corresponding aluminium oxide).
The rare earth sulfide pigment that post-processing approach through the invention obtains is bright-colored, and carbon particle impurity is few, material
Middle no larger particles, even particle size distribution improve pigmenting power, covering power, improve anti-ultraviolet property, improve
Weatherability, products obtained therefrom chemical stability is good, heat-resist, is that organic red pigment is incomparable, is free of heavy metal, green
Environmental protection.
Specific embodiment
The present invention is further described in detail With reference to embodiment, and the embodiment provided is only for explaining
The bright present invention, the range being not intended to be limiting of the invention.
Unless otherwise instructed, rare-earth sulfide primary powder described in following embodiment is prepared by following steps:
1) rare earth compound is uniformly mixed with additive, is fitted into reaction vessel, wherein rare earth compound is cerous carbonate,
Additive is sodium carbonate, and the additional proportion of additive is that the molar ratio of Na/Ce is 0.8；
2) it is passed through inert gas into reaction vessel, displaces the air in reactor, hydrogen sulfide, two is passed through after 30min
The mix sulphur source gas of nitric sulfid, it is 3 that wherein the additional proportion of gas sulphur source, which is the molar ratio of S/Ce,；
3) it is heated up 50 minutes to 500 DEG C by room temperature with 10 DEG C/min of speed, keeps the temperature 60 minutes, then with 10 DEG C/min
Speed is warming up to 900 DEG C, keeps the temperature 120 minutes.
Embodiment 1
(1) by 400g cerium sulphide primary powder and 1200g water mixed grinding in colloid mill, then it is added 20g kerosene, 5
Kerosene and carbon dust are pulled out after minute, until mixed liquor surface is floated without kerosene and carbon dust, then filter to obtain filter cake；
(2) 95% ethanol washing of the filter cake for obtaining step (1), then presses the filter cake after washing with 95% ethyl alcohol
The mass ratio of 1:2 mixes, and 8g PVP (polyvinylpyrrolidone) dispersing agent is added, and under nitrogen protection with sand mill by pigment
Partial size is reduced to 500nm；
(3) 20g ammonium fluoride is then added into mixed liquor under conditions of 20-30 DEG C, reacts 2h；
(4) 20g zinc oxide, 200g ammonium hydroxide are then added into mixed liquor；
(5) 60g ethyl orthosilicate is added into mixed liquor in 2h, stirs 2 hours；
(6) it then filters, washs and dry；
(7) material after drying is crossed into 45 μm of screen centrifuges, obtains product.
Embodiment 2
(1) by 400g cerium sulphide primary powder and 1200g water mixed grinding in colloid mill, then it is added 20g kerosene, 5
Kerosene and carbon dust are pulled out after minute, until mixed liquor surface is floated without kerosene and carbon dust, then filter to obtain filter cake；
(2) 95% ethanol washing of the filter cake for obtaining step (1), then presses the filter cake after washing with 95% ethyl alcohol
The mass ratio of 1:2 mixes, and 8g PVP dispersing agent is added, and be under nitrogen protection reduced to pigment particle size with sand mill
4000nm；
Step (3)-(7) are same as Example 1.
Embodiment 3
(1) by 400g cerium sulphide primary powder and 1200g water mixed grinding in colloid mill, then it is added 20g kerosene, 5
Kerosene and carbon dust are pulled out after minute, until mixed liquor surface is floated without kerosene and carbon dust, then filter to obtain filter cake；
(2) 95% ethanol washing of the filter cake for obtaining step (1), then presses the filter cake after washing with 95% ethyl alcohol
The mass ratio of 1:2 mixes, and 8g PVP dispersing agent is added, and be under nitrogen protection reduced to pigment particle size with sand mill
2000nm；
Step (3)-(7) are same as Example 1.
The tinting strength, tinting power of product prepared by embodiment 1-3 is measured, as a result as shown in the table:
| Embodiment | Tinting strength, tinting power |
| 1 | 100 |
| 2 | 50 |
| 3 | 80 |
Embodiment 4
Step (1)-(3) are same as Example 1；
It carries out that 20g zinc oxide is only added into mixed liquor when step (4), ammonium hydroxide is not added；
Step (5)-(7) are same as Example 1.
Embodiment 5
Step (1)-(3) are same as Example 1；
20g zinc oxide, 50g ammonium hydroxide are added into mixed liquor for step (4)；
Step (5)-(7) are same as Example 1.
Embodiment 6
Step (1)-(4) are same as Example 1；
It is only stirred when step (5) 2 hours, ethyl orthosilicate is not added；
Step (6)-(7) are same as Example 1.
Embodiment 7
Step (1)-(4) are same as Example 1；
28g ethyl orthosilicate is added in step (5) in 2h into mixed liquor, stirs 2 hours；
Step (6)-(7) are same as Example 1.
Measure the heat resistance and H of embodiment 1 and 4-7 products obtained therefrom2S burst size, as a result as shown in the table:
| Embodiment | Heatproof (DEG C) | H2S burst size (ppm) |
| 1 | 320 | 95 |
| 4 | 240 | 505 |
| 5 | 280 | 280 |
| 6 | 240 | 610 |
| 7 | 280 | 290 |
Claims (8)
1. a kind of post-processing approach of rare-earth sulfide, method includes the following steps:
(1) rare-earth sulfide primary powder is mixed with water, obtains mixed solution；Then flotation agent is added into mixed liquor, in glue
Body grinds interior ground and mixed, and the aggregation of floating is removed during grinding, filter cake is then obtained by filtration；
(2) filter cake that step (1) obtains being washed with alcoholic solution, the filter cake and alcoholic solution after then making washing are mixed,
Dispersing agent is added during stirring, then in the absence of oxygen, is ground to the partial size of the rare-earth sulfide in mixed solution
For 100-3000nm；
(3) after step (2), fluorization agent is added into mixed liquor and carries out fluorination treatment；
(4) after the fluorination treatment of step (3), zinc oxide and catalyst are added into mixed solution；
(5) after step (4), transparent oxide presoma is added, and into mixed solution immediately with 100-1000g/min's
Speed adds, and stirs 1-3h；
(6) it after step (5), is filtered, washed and dries, obtain dry rare-earth sulfide；
(7) rare-earth sulfide by the drying that step (6) obtains is sieved through screen centrifuge, obtains product.
2. according to the method described in claim 1, wherein in step (1), the rare-earth sulfide primary powder be cerium sulphide,
The primary powder of lanthanum sulfide, lanthanum cerium sulfide or samaric sulfide；It is highly preferred that the rare-earth sulfide primary powder is that cerium sulphide is primary
Powder.
3. method according to claim 1 or 2, wherein in step (1), the rare-earth sulfide primary powder and water
Mass ratio is 1:1-5；
Preferably, the flotation agent is kerosene, diesel oil, vegetable oil；
Preferably, the quality of the flotation agent be rare-earth sulfide primary powder quality 3%-9%, more preferably 5%；
Preferably, in step (1), the aggregation of the floating is the aggregation of the carbon dust and flotation agent in primary powder.
4. method according to any one of claim 1-3, wherein the alcoholic solution is selected from methanol, second in step (2)
Alcohol or butanol, more preferably 99% ethyl alcohol；
Preferably, in step (2), described mixed with filter cake with the quality of alcoholic solution is rare-earth sulfide primary powder quality
2-10 times, more preferably 3 times；
Preferably, in step (2), the dispersing agent is the polymer of non-ionic water-soluble either organic solvent-soluble；
More preferably cellulose and its derivates, polyvinyl lactam, polyethylene oxide, polyethylene glycol, polyoxyethylated polyoxypropylene two
Alcohol, polyacrylate, polyoxyethylated acid esters, polyoxyethylenated alkylphenol, polyvinyl alcohol, alkanolamide, polyvinyl pyrrole
Alkanone or compound based on xanthan gum, more preferably polyvinylpyrrolidone；
Preferably, in step (2), the quality of the dispersing agent is the 0.5%-5% of rare-earth sulfide primary powder quality；More
Preferably 2%；
Preferably, in step (2), the partial size is 300-800nm, preferably 500nm.
5. method according to any of claims 1-4, wherein the fluorization agent is solid, liquid in step (3)
Or gaseous fluorinated dose, more preferably liquid or gaseous fluorinated dose；
Preferably, in step (3), the fluorization agent is selected from fluorine gas, hydrofluoric acid, ammonium fluoride, alkali metal fluoride or nitrogen fluoride,
More preferably ammonium fluoride；
Preferably, in step (3), the quality of the fluorization agent is the 1%-20% of rare-earth sulfide primary powder quality, more
Preferably 5%.
6. method according to any one of claims 1-5, wherein the partial size of the zinc oxide is less than in step (4)
40 μm, more preferably 500nm；
Preferably, in step (4), the quality of the zinc oxide is the 1%-15% of rare-earth sulfide primary powder quality；More
Preferably 5%；
Preferably, in step (4), the catalyst is ammonium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, more preferably ammonia
Water；
Preferably, in step (4), the quality of the catalyst is the 5%-60% of rare-earth sulfide primary powder quality；More
Preferably 25%.
7. method according to claim 1 to 6, wherein in step (5), the transparent oxide presoma
It is (corresponding selected from silester (corresponding silica), aluminum sulfate (corresponding aluminium oxide), zirconium sulfate (corresponding zirconium oxide), calcium sulfate
Calcium oxide) or one of sulfuric acid rare earth (corresponding rare-earth oxide) or a variety of；It is highly preferred that before the transparent oxide
It drives body and is selected from silester；
Preferably, during carrying out step (5), maintaining temperature is 10-40 DEG C, more preferably 25 DEG C；Maintenance pH is 8-10, more
Preferably 9；
Preferably, in step (7), centrifugal screen aperture is 10-100 μm, more preferably 45 μm.
8. method according to any one of claims 1-7, wherein carrying out 2 times in step (5) or repeatedly carrying out again later
Step (6), and when step (5) carry out 2 times or repeatedly carry out step (6) again later, used by each implementation steps (5)
Transparent oxide presoma can be identical or not identical；
Preferably, step (6) are carried out again after step (5) carry out 2 times, wherein used by first time implementation steps (5) thoroughly
Bright oxide precursor is silester (corresponding silica), before transparent oxide used by second of implementation steps (5)
Drive body is aluminum sulfate (corresponding aluminium oxide).
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| CN110591414A (en) * | 2019-10-14 | 2019-12-20 | 包头中科世纪科技有限责任公司 | Rare earth sulfide and/or rare earth oxysulfide colorant and preparation method thereof |
| CN112625464A (en) * | 2020-12-01 | 2021-04-09 | 景德镇陶瓷大学 | PEG (polyethylene glycol) and carbon powder refined cristobalite coated gamma-Ce2S3Preparation method of red pigment and product prepared by preparation method |
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