CN109260037A - A kind of multifunctional rare-earth colorant and preparation method thereof - Google Patents

A kind of multifunctional rare-earth colorant and preparation method thereof Download PDF

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Publication number
CN109260037A
CN109260037A CN201811292051.0A CN201811292051A CN109260037A CN 109260037 A CN109260037 A CN 109260037A CN 201811292051 A CN201811292051 A CN 201811292051A CN 109260037 A CN109260037 A CN 109260037A
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Prior art keywords
rare
zinc
earth
colorant
multifunctional
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Inventor
傅继澎
董伟
李成宇
王滨
池建义
张洪杰
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Baotou Rare Earth R&d Center Chinese Academy Of Sciences
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Baotou Rare Earth R&d Center Chinese Academy Of Sciences
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27—Zinc; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/23—Sulfur; Selenium; Tellurium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/58—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • A61K8/585—Organosilicon compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms

Abstract

The present invention relates to a kind of preparation methods of multifunctional rare-earth colorant, and precipitating reagent and surfactant to be added later, the rare-earth colorant of oxide coated by zinc is sufficiently made after reaction by the way that first rare-earth colorant first product is added in zinc salt solvent；Next, first dispersing the rare-earth colorant of the oxide coated by zinc in water or ethanol water, then pH is adjusted, siloxanes is added, and sufficiently reacted under agitation, product is centrifuged, washs to get multifunctional rare-earth colorant；In the method for the present invention, first colorant is coated using zinc oxide, upper hydrophobic coating is modified except zinc oxide coated layer again, multifunctional rare-earth colorant not only strong coloring force is finally prepared, ultraviolet absorbability is good, thermal stability is high, and there is bigger compatibility between organic substrate, can be suitable for the demand of organic system.

Description

A kind of multifunctional rare-earth colorant and preparation method thereof
Technical field
The present invention relates to the technical fields of rare-earth colorant, and in particular to a kind of multifunctional rare-earth colorant and its preparation side Method.
Background technique
For many years, the colorant that heavy metal base inorganic pigment always generally uses.But heavy metal base inorganic pigment pair Environment has very big harm, while endangering the health of the mankind.
In order to avoid the heavy metal in heavy metal base inorganic pigment endangers mankind's bring, the producer of colorant and make User, which has been working hard, develops new colorant.
Rare-earth sulfide is as a kind of environmentally protective colorant, it is considered to be safe and reliable novel inorganic colorant, Therefore rare-earth sulfide colorant uses just especially suitable in chemical product, but in face of acid-base property, sunlight irradiation in chemical product To requirements such as sun-proof, thermal stability, existing rare-earth colorant is not able to satisfy daily use chemicals for equal complex environments and chemical product The use demand of product.
Summary of the invention
In order to solve the above problems existing in the present technology, the present invention provides a kind of strong coloring forces, sun protection good, hot steady Qualitative high, multifunctional rare-earth colorant that safety is good and preparation method thereof.More kinetic energy rare-earth colorants of the present invention and day Change and there is bigger compatibility between the matrix of articles, demand can be fitted.
The technical scheme adopted by the invention is as follows:
A kind of preparation method of multifunctional rare-earth colorant, includes the following steps:
(1) rare-earth colorant first product is taken, be added in zinc solution and be sufficiently mixed uniformly, precipitating reagent is added later And surfactant, it is sufficiently reacted under agitation, after product is centrifuged, washs, obtains oxide coated by zinc Rare-earth colorant；
(2) it disperses the rare-earth colorant of step (1) described oxide coated by zinc in water or ethanol water, pH tune is added later It saves agent and adjusts pH value, add siloxanes, sufficiently reacted under stirring condition, product is centrifuged, washs to get described Multifunctional rare-earth colorant.
Zinc oxide has excellent UV screening ability, covers the full scope of UVA and UVB wavelength.In rare-earth sulfide Surface cladding, realizes the nanoscale of zinc oxide thickness level, improves UV absorption efficiency.In addition, since integral particle is micro- Metrical scale, and flocculation of reuniting caused by preventing scale too small, and prevent that its absorbability on the skin, it is in cellular level On capability of influence and their intrinsic toxicity in terms of compared with its macroscopical component the problem of.
Zinc oxide material itself be it is hydrophilic, this prevents with Zinc oxide coating particle from makeup or sun-proof being answered Organic solvent, oil and the ductile material wetting of matrix are commonly used as in.In addition, zinc oxide has high photolytic activity, this may Lead to detrimental effect caused by the reaction as metal oxide and between other components in sun-screening agent or cosmetics.
General acceptable method for overcoming these problems be to metal oxide particle carry out surface coating, thus It becomes hydrophobic.In the trial for overcoming the problems, such as this, organo-silicon compound such as siloxanes and polysiloxanes for pair Metal oxide powder is handled.Organosilicon is the polymer that the rule with-Si-O- repeats main chain, and this polymer Side group containing different degrees of functionality.Most significantly, using contain epoxy group, amido, hydroxyl, hydrogen-based, vinyl, pendent alkyl groups Organo-silicon compound.In addition, the side group of organo-silicon compound can choose to match selected matrix, so as to obtain Bigger compatibility between surface treated powder and matrix.
In step (1), the rare-earth colorant first product is rare-earth sulfide, rare-earth oxide sulfate, rare earth aluminate, Pr- ZrSiO4、YIn1-xMnxO3One or more of mixture.The rare-earth colorant first product passes through well known in the art any Method obtains, such as solid-gas phase reaction, solid-solid reaction, and metallorganic pyrolysis, plasma-deposited, CVD, PVD, magnetic control splash It penetrates, melting etc..Then by mechanical or chemical method, selected particles are formed.
The zinc salt is zinc acetate, trbasic zinc phosphate, zinc dihydrogen phosphate, zinc nitrate, zinc chloride, zinc sulfate, zinc stearate, grape The mixture of one or more of saccharic acid zinc, zinc oxalate, amino-acid zinc, zinc citrate, meta-sodium zincate；
The solvent of the zinc solution is alcohol-water mixture or water, and the concentration of zinc salt is 0.1- in the zinc solution 2.5mol/L。
The precipitating reagent is potassium hydroxide, in sodium hydroxide, ammonium hydroxide, hexamethylenetetramine, 2-methylimidazole, diethanol amine One or more of mixtures；
The molar ratio of the zinc salt and the precipitating reagent is 20:1-1:5.
The surfactant is diethylene glycol (DEG), ten alkyl benzene sulphonates, 18/16/dodecyl sodium sulfate, 18/ten Six/neopelex, 18/16/dodecyl trimethyl ammonium bromide, 18/16/trimethyl chlorine Change ammonium, ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, 18/16/lauryl amine, poly- second Glycol-polyglycerol-polyethylene glycol triblock copolymer, P123, F127,18/16/calcium dodecyl benzene sulfonate, castor Sesame oil polyoxyethylene ether, PVP, PVA, anionic polyacrylamide, polyoxyethylene, polyvinyl alcohol, lauryl sulfosuccinate list Rouge disodium, single Tryfac 5573,18/16/1-isobutyl-3,5-dimethylhexylphosphoric acid potassium, laurel alcohol ether phosphate AEO3, AEO9, fat Alcohol polyoxyethylene ether, laurel alcohol ether phosphate potassium, lauric acid amide of ethanol, dodecanamide propyl decil lactones, polyoxy Ethylene monoalkyl phosphoric acid esters, polyoxyethylene bisalkyl phosphate, dioctyl phenyl phosphate ester, dioctyl sodium sulphosuccinate, two One of (2- ethylhexyl) Disodium sulfosuccinate, polyacrylamide, citric acid, L-cysteine, sodium tartrate are several The mixture of kind；
The molar ratio of the zinc salt and the surfactant is 10:1-1:10.
In step (1), the temperature for carrying out the reaction is 20-90 DEG C, and the time for carrying out the stirring is 0.5-20h.
The pH adjusting agent is ammonium chloride, potassium tetroxalate, potassium hydrogen tartrate, disodium hydrogen phosphate, potassium dihydrogen phosphate, boric acid Sodium, sodium tetraphenylborate, calcium hydroxide, ammonium carbonate, mixture one or several kinds of in acetic acid；
Adjusting the pH value is 4-10.
The siloxanes is dimethyl siloxane, methyl hydrogen siloxane, triethoxy octyl siloxanes, methyl triethoxy Siloxanes, trifluoromethyl trimethicone, n-octyl siloxanes, positive decyl siloxanes, dimethylformamide dimethyl oxygroup siloxanes, six Tetramethyldisiloxane, hexam ethylcyclotrisiloxane, 1,1,3,3 ,-tetramethyl disiloxane, 2- (3,4- epoxycyclohexyl) ethyl three Methoxy silane, 2- (3,4- epoxycyclohexyl) ethyl triethoxysilane, 3- (2,3 the third oxygen of epoxy) propyl-triethoxysilicane Alkane, 3- (2,3 the third oxygen of epoxy) hydroxypropyl methyl diethoxy silane, hexamethyldisiloxane, dimethyldichlorosilane, prestox ring Tetrasiloxane, dodecyltrimethoxysilane, hexadecyl trimethoxy silane, γ-chloropropyl trichloro-silane, γ-chlorine third Base trichlorosilane, gamma-aminopropyl-triethoxy-silane (KH550), n-octytriethoxysilane, γ-aminopropyl trimethoxy Silane (KH551), γ-aminopropyltriethoxy diethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, KH602, One or several kinds of mixture in KH792, KH560, KH570, KH590, KH571, KH151, KH171, KH792；
The molar ratio of the rare-earth colorant of the additional amount of the siloxanes and the oxide coated by zinc is 1:20-2:1.
In step (2), the temperature for carrying out the reaction is 20-80 DEG C, and the time for carrying out the stirring is 0.5-20h.
The material can it is compatible with following substance be used together, and be suitable for mouth, nose, skin contact hydrophobicity liquid Body.Surfactant, super fatting agent, oil, emulsifier, consistency modifiers, thickener, polymer, stabilizer, biological source activity at Point, sweller, other UV light protective agents, antioxidant, hydrotropic agent, preservative, solubilizer, aromatic oil, bacterial inhibitor, Matrix and their mixture.
Matrix is selected from double glyceride or glyceryl ester, be based on C6-C18 fatty acid double glyceride or glyceryl ester and By the reaction modifying (caprylic/capric glyceryl ester, wheat germ glycerides etc.) with other alcohol, the aliphatic ester of polyglycereol (gathers sweet Oil-n such as -4 decylate of polyglycereol, -2 isostearate of polyglycereol etc.) or castor oil, hydrogenated vegetable oil, Sweet Almond Oil, wheat Bud oil, sesame oil, cotmar, coconut oil, avocado oil, corn oil, rilanit special, sher butter, cupu oil, soya-bean oil, Ermine oil, sunflower oil, safflower oil, macadimia nut oil, olive oil, h-tallow, Pericarppium Armeniacae Amarum oil, hazelnut oil and borage oil；Liquid Body organosilicon or polysiloxane, mineral oil, Parleam, poly decene, alkane, at least ten carbon atom Isoparaffin, and aliphatic or aromatics ester oil (such as isopropyl myristate, myristic acid Lauryl Ester, palmitinic acid are different Propyl diester, diisopropyl sebacate, adipic acid diisopropyl ester or C8-C18 alkyl benzoate), coco glycerides are pungent Acid/capric acid glyceryl ester, sad propylheptyl ester, carbonic acid dioctyl ester, ethylhexyl palmitate, and sad ethylhexyl Ester.Water is also included in the range of matrix.
The invention has the benefit that
The preparation method of multifunctional rare-earth colorant of the present invention, by the way that zinc salt first is added in rare-earth colorant first product In solvent, precipitating reagent and surfactant are added later, the rare-earth colorant of oxide coated by zinc is sufficiently made after reaction；It connects down Come, first disperse the rare-earth colorant of the oxide coated by zinc in water or ethanol water, adds pH adjusting agent and adjust pH, be added Siloxanes, and sufficiently reacted under agitation, product is centrifuged, washs to get multifunctional rare-earth colorant；This In inventive method, first colorant is coated using zinc oxide, then modifies upper hydrophobic coating except zinc oxide coated layer, most The strong coloring force of multifunctional rare-earth colorant is prepared eventually, sun protection good, thermal stability is high, and safety is good, and with it is organic There is bigger compatibility between matrix, the demand of organic system can be suitable for.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with It obtains other drawings based on these drawings.
Fig. 1 is the SEM figure of 1 gained multifunctional rare-earth sulfide colorant of the embodiment of the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work Other embodiment belongs to the range that the present invention is protected.
Embodiment 1
The present embodiment provides a kind of preparation methods of multifunctional rare-earth lanthanum sulfide, include the following steps:
(1) 200g rare earth lanthanum sulfide first product is weighed, is added in the acetic acid zinc solution of the 1.5mol/L of 500ml and is filled Divide and be uniformly mixed, 5.5g hexamethylenetetramine, 12g cetyl trimethylammonium bromide is added later, under 90 DEG C, stirring condition Sufficiently reaction 1.5h is carried out, after product is centrifuged, washs, obtains the rare earth lanthanum sulfide of oxide coated by zinc；
(2) it disperses the rare earth lanthanum sulfide of step (1) described oxide coated by zinc in 500ml water, 5g carbonic acid is added later It is 8 that ammonium, which adjusts pH value, adds 50g dimethyl siloxane, abundant to carry out under the conditions of 2000r/min in 30 DEG C, stirring rate 2h is reacted, product is centrifuged, washs to get the multifunctional rare-earth lanthanum sulfide.
Embodiment 2
The present embodiment provides a kind of preparation methods of multifunctional rare-earth sulphur samarium oxide, include the following steps:
(1) 200g rare earth sulphur samarium oxide first product is weighed, is added in the zinc nitrate solution of the 1.0mol/L of 500ml and carries out It is sufficiently mixed uniformly, 3g potassium hydroxide, 12g diethylene glycol (DEG) is added later, sufficiently reaction 1h is carried out under 85 DEG C, stirring condition, is produced After object is centrifuged, washs, the rare earth sulphur samarium oxide of oxide coated by zinc is obtained；
(2) it disperses the rare earth sulphur samarium oxide of step (1) described oxide coated by zinc in 500ml water, 2ml tetra- is added later Potassium oxalate adjust pH value be 5, add 45g hexamethyldisiloxane, 80 DEG C, stirring rate be 1000r/min under the conditions of into Row sufficiently reaction 30min, product are centrifuged, wash to get the multifunctional rare-earth sulphur samarium oxide.
Embodiment 3
The present embodiment provides a kind of preparation methods of multifunctional rare-earth cerium sulphide samarium, include the following steps:
(1) 200g rare earth cerium sulphide first product is weighed, is added in the zinc phosphate solution of the 1.3mol/L of 500ml and is filled Divide and be uniformly mixed, 1.8g sodium hydroxide, 22.6g disodium ethylene diamine tetraacetate are added later, is filled under 20 DEG C, stirring condition Divide reaction 20h, after product is centrifuged, washs, obtains the rare earth cerium sulphide of oxide coated by zinc；
(2) it disperses the rare earth cerium sulphide of step (1) described oxide coated by zinc in 500ml water, di(2-ethylhexyl)phosphate is added later Hydrogen sodium adjust pH value be 6, add 48g methyl hydrogen siloxane, 20 DEG C, stirring rate be 1500r/min under the conditions of filled Divide reaction 20h, product is centrifuged, washs to get the multifunctional rare-earth cerium sulphide.
Multifunctional rare-earth cerium sulphide described in the present embodiment is used for the anti-Sai sun screen of UV, the specific operation method is as follows: prepared Appropriate deionized water, tetra- sodium of multifunctional rare-earth cerium sulphide 12g, 0.1gEDTA, 3g glycerol, 5g lauric acid hexyl ester, 8g oneself Diacid dibutyl ester, begins to warm up 75-80 DEG C, 0.5g xanthan gum, 2g octadecyl alcolol polyethers -25,2g octadecyl alcolol, 1.2gPEG- 8,5g glycerol caprylates, 5g octyl methoxycinnamate, 4g castor oil, 2g titanium dioxide are heated to 70-80 DEG C, use spiral shell Propeller mixer merges mixing homogenizing 1-3 minutes.It is cooled to room temperature, is then stopped, through detecting, the sun-proof finger of the suncream Number SPF is 30.
Embodiment 4
The present embodiment provides a kind of preparation methods of multifunctional rare-earth sulphur cerium oxide, include the following steps:
(1) 200g rare earth cerium sulphide first product is weighed, is added in the liquor zinci chloridi of the 1.3mol/L of 500ml and is filled Divide and be uniformly mixed, 1.8g ammonium hydroxide, 22.6g polyethylene glycol glycerine-polyethylene glycol triblock copolymer are added later, 20 DEG C, sufficiently reaction 20h is carried out under stirring condition, after product is centrifuged, wash, the rare earth for obtaining oxide coated by zinc vulcanizes Cerium；
(2) it disperses the rare earth cerium sulphide of step (1) described oxide coated by zinc in 500ml water, hydroxide is added later It is 10 that calcium, which adjusts pH value, adds 55g 3- aminopropyl triethoxysilane, is 1500r/min condition in 20 DEG C, stirring rate Lower progress sufficiently reaction 20h, product are centrifuged, wash to get the multifunctional rare-earth cerium sulphide.
Embodiment 5
The present embodiment provides a kind of preparation methods of multifunctional rare-earth lanthanum cerium sulfide, include the following steps:
(1) 200g rare earth cerium sulphide first product is weighed, is added in the solution of zinc sulfate of the 1.3mol/L of 500ml and is filled Divide and be uniformly mixed, 1.8g 2-methylimidazole, 22.6g polyvinyl alcohol are added later, is carried out under 20 DEG C, stirring condition sufficiently anti- After answering 20h, product to be centrifuged, wash, the rare earth cerium sulphide of oxide coated by zinc is obtained；
(2) it disperses the rare earth cerium sulphide of step (1) described oxide coated by zinc in 500ml water, tartaric acid is added later It is 5 that potassium, which adjusts pH value, adds 60gKH560, in 20 DEG C, stirring rate to carry out sufficiently reaction 20h under the conditions of 1500r/min, Product is centrifuged, washs to get the multifunctional rare-earth cerium sulphide.
Embodiment 6
The present embodiment provides a kind of preparation methods of multifunctional rare-earth sulphur cerium oxide samarium, include the following steps:
(1) 200g rare earth cerium sulphide first product is weighed, is added in the zinc stearate solution of the 1.3mol/L of 500ml and carries out It is sufficiently mixed uniformly, 1.8g diethanol amine, 22.6g laurel alcohol ether phosphate potassium is added later, is carried out under 20 DEG C, stirring condition Sufficiently reaction 20h, after product is centrifuged, washs, obtains the rare earth cerium sulphide of oxide coated by zinc；
(2) it disperses the rare earth cerium sulphide of step (1) described oxide coated by zinc in 500ml water, acetic acid tune is added later Saving pH value is 4, adds 60g KH590, in 20 DEG C, stirring rate to carry out sufficiently reaction 20h under the conditions of 1500r/min, is produced Object is centrifuged, washs to get the multifunctional rare-earth cerium sulphide.
Embodiment 7
The present embodiment provides the preparation methods of a kind of multifunctional rare-earth sulphur samarium oxide and samaric sulfide mixture, including walk as follows It is rapid:
(1) 200g rare earth cerium sulphide first product is weighed, is added in the zinc stearate solution of the 1.3mol/L of 500ml and carries out It is sufficiently mixed uniformly, 1.8g 2-methylimidazole, 22.6g polyacrylamide is added later, is filled under 20 DEG C, stirring condition Divide reaction 20h, after product is centrifuged, washs, obtains the rare earth cerium sulphide of oxide coated by zinc；
(2) it disperses the rare earth cerium sulphide of step (1) described oxide coated by zinc in 500ml water, Boratex is added later Adjusting pH value is 9, adds 60g KH792, in 20 DEG C, stirring rate to carry out sufficiently reaction 20h under the conditions of 1500r/min, Product is centrifuged, washs to get the multifunctional rare-earth cerium sulphide.
Embodiment 8
The present embodiment provides a kind of preparation methods of multifunctional rare-earth cerium aluminate, include the following steps:
(1) 200g cerium aluminate first product is weighed, be added in the acetic acid zinc solution of the 1.5mol/L of 500ml and is carried out is sufficiently mixed It closes uniformly, 1.5g sodium hydroxide, 12g cetyl trimethylammonium bromide is added later, carried out under 90 DEG C, stirring condition abundant 1.5h is reacted, after product is centrifuged, washs, obtains the rare earth aluminic acid cerium of oxide coated by zinc；
(2) it disperses the rare earth aluminic acid cerium of step (1) described oxide coated by zinc in 500ml water, acetic acid tune is added later Saving pH value is 5, adds 30g phenyltrimethoxysila,e, abundant to carry out under the conditions of 2000r/min in 30 DEG C, stirring rate 2h is reacted, product is centrifuged, washs to get the multifunctional rare-earth cerium aluminate.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.

Claims (10)

1. a kind of preparation method of multifunctional rare-earth colorant, which comprises the steps of:
(1) rare-earth colorant first product is taken, be added in zinc solution and be sufficiently mixed uniformly, precipitating reagent and table are added later Face activating agent, is sufficiently reacted under agitation, after product is centrifuged, washs, obtains the rare earth of oxide coated by zinc Colorant；
(2) it disperses the rare-earth colorant of step (1) described oxide coated by zinc in water or ethanol water, pH adjusting agent is added later PH value is adjusted, siloxanes is added, is sufficiently reacted under stirring condition, product is centrifuged, washs to get more function It can rare-earth colorant.
2. the preparation method of multifunctional rare-earth colorant according to claim 1, which is characterized in that described in step (1) Rare-earth colorant first product is rare-earth sulfide, rare-earth oxide sulfate, rare earth aluminate, Pr-ZrSiO4、YIn1-xMnxO3In one Kind or several mixtures.
3. the preparation method of multifunctional rare-earth colorant according to claim 1, which is characterized in that described in step (1) Zinc salt is zinc acetate, trbasic zinc phosphate, zinc dihydrogen phosphate, zinc nitrate, zinc chloride, zinc sulfate, zinc stearate, zinc gluconate, oxalic acid The mixture of one or more of zinc, amino-acid zinc, zinc citrate, meta-sodium zincate；
The solvent of the zinc solution is alcohol-water mixture or water, and the concentration of zinc salt is 0.1-2.5mol/ in the zinc solution L。
4. the preparation method of multifunctional rare-earth colorant according to claim 1, which is characterized in that the precipitating reagent is hydrogen The mixture of one or more of potassium oxide, sodium hydroxide, ammonium hydroxide, hexamethylenetetramine, 2-methylimidazole, diethanol amine；
The molar ratio of the zinc salt and the precipitating reagent is 20:1-1:5.
5. the preparation method of multifunctional rare-earth colorant according to claim 1, which is characterized in that the surfactant For diethylene glycol (DEG), ten alkyl benzene sulphonates, 18/16/dodecyl sodium sulfate, 18/16/neopelex, ten Eight/16/dodecyl trimethyl ammonium bromide, 18/16/dodecyl trimethyl ammonium chloride, ethylenediamine tetra-acetic acid, second two Amine tetraacethyl disodium, tetrasodium ethylenediamine tetraacetate, 18/16/lauryl amine, polyethylene glycol glycerine-poly- second two Alcohol triblock copolymer, P123, F127,18/16/calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether, PVP, PVA, Anionic polyacrylamide, polyoxyethylene, polyvinyl alcohol, lauryl sulfosuccinate monoester disodium, single Tryfac 5573, ten Eight/16/1-isobutyl-3,5-dimethylhexylphosphoric acid potassium, laurel alcohol ether phosphate AEO3, AEO9, fatty alcohol polyoxyethylene ether, lauryl alcohol phosphorus Acid esters potassium, lauric acid amide of ethanol, dodecanamide propyl decil lactones, polyoxyethylene monoalkyl phosphoric acid esters, polyoxy second Alkene bisalkyl phosphate, dioctyl phenyl phosphate ester, dioctyl sodium sulphosuccinate, two (2- ethylhexyl) succinate sulfonic acid The mixture of one or more of sodium, polyacrylamide, citric acid, L-cysteine, sodium tartrate；
The molar ratio of the zinc salt and the surfactant is 10:1-1:10.
6. the preparation method of multifunctional rare-earth colorant according to claim 1, which is characterized in that in step (1), carry out The temperature of the reaction is 20-90 DEG C, and the time for carrying out the stirring is 0.5-20h.
7. the preparation method of multifunctional rare-earth colorant according to claim 1, which is characterized in that the pH adjusting agent is Ammonium chloride, potassium tetroxalate, potassium hydrogen tartrate, disodium hydrogen phosphate, potassium dihydrogen phosphate, Boratex, sodium tetraphenylborate, calcium hydroxide, One or several kinds of mixture in ammonium carbonate；
Adjusting the pH value is 4-10.
8. the preparation method of multifunctional rare-earth colorant according to claim 1, which is characterized in that the siloxanes is two Methylsiloxane, methyl hydrogen siloxane, triethoxy octyl siloxanes, methyltriethoxy silane oxygen alkane, trifluoromethyl trimethyl Siloxanes, n-octyl siloxanes, positive decyl siloxanes, dimethylformamide dimethyl oxygroup siloxanes, hexamethyldisiloxane, hexamethyl three Siloxanes, 1,1,3,3 ,-tetramethyl disiloxane, 2- (3,4- epoxycyclohexyl) ethyl trimethoxy silane, 2- (3,4- epoxy Cyclohexyl) ethyl triethoxysilane, 3- (2,3 the third oxygen of epoxy) propyl-triethoxysilicane, 3- (2,3 the third oxygen of epoxy) propyl first Base diethoxy silane, hexamethyldisiloxane, dimethyldichlorosilane, octamethylcy-clotetrasiloxane, dodecyl trimethoxy Base silane, hexadecyl trimethoxy silane, γ-chloropropyl trichloro-silane, γ-chloropropyl trichloro-silane, three second of γ-aminopropyl Oxysilane, n-octytriethoxysilane, γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxy diethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, KH602, KH792, KH560, KH570, KH590, KH571, KH151, One or several kinds of mixture in KH171, KH792；
The molar ratio of the rare-earth colorant of the additional amount of the siloxanes and the oxide coated by zinc is 1:20-2:1.
9. the preparation method of multifunctional rare-earth colorant according to claim 1, which is characterized in that in step (2), carry out The temperature of the reaction is 20-80 DEG C, and the time for carrying out the stirring is 0.5-20h.
10. the multifunctional rare-earth colorant that any one of claim 1-9 the method is prepared.
CN201811292051.0A 2018-10-31 2018-10-31 A kind of multifunctional rare-earth colorant and preparation method thereof Pending CN109260037A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1426376A (en) * 2000-03-30 2003-06-25 罗狄亚稀土公司 Composition based on rare earth metal sulplide with improved chemical stability, its preparation method and use as pigment thereof
CN101522818A (en) * 2006-10-05 2009-09-02 西巴控股公司 Method for the hydrophobic treatment of pigment particles and the personal care compositions comprising said pigment particles
CN103819934A (en) * 2014-02-25 2014-05-28 内蒙古大学 Method for preparing coated rare earth sulfide pigment
EP3211043B1 (en) * 2016-02-23 2020-05-13 Merck Patent GmbH Effect pigments based on al2o3-flakes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1426376A (en) * 2000-03-30 2003-06-25 罗狄亚稀土公司 Composition based on rare earth metal sulplide with improved chemical stability, its preparation method and use as pigment thereof
CN101522818A (en) * 2006-10-05 2009-09-02 西巴控股公司 Method for the hydrophobic treatment of pigment particles and the personal care compositions comprising said pigment particles
CN103819934A (en) * 2014-02-25 2014-05-28 内蒙古大学 Method for preparing coated rare earth sulfide pigment
EP3211043B1 (en) * 2016-02-23 2020-05-13 Merck Patent GmbH Effect pigments based on al2o3-flakes

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