CN103333528A - Preparation method of pearlescent pigment having fluorescent effect - Google Patents
Preparation method of pearlescent pigment having fluorescent effect Download PDFInfo
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- CN103333528A CN103333528A CN2013102592714A CN201310259271A CN103333528A CN 103333528 A CN103333528 A CN 103333528A CN 2013102592714 A CN2013102592714 A CN 2013102592714A CN 201310259271 A CN201310259271 A CN 201310259271A CN 103333528 A CN103333528 A CN 103333528A
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Abstract
The invention relates to a preparation method of a pearlescent pigment having a fluorescent effect. According to the method, a mica-titanium pearlescent pigment is prepared from mica, which comprises the following process: throwing the mica into water to form a suspension 1, and evenly stirring to obtain a reaction mother solution 1; dropwisely adding a titanium tetrachloride solution into the reaction mother solution 1, regulating the pH value of the system, and stirring to obtain a product suspension 2; performing solid-liquid separation, and drying to obtain a mica-titanium pearlescent pigment material; throwing the prepared mica-titanium pearlescent pigment into water to form a reactant suspension 3, thus obtaining a reaction mother solution; dropwisely adding a mixed solution of a calcium solution and water-soluble salt of transition metal M into the reaction mother solution, and continually stirring to obtain a product suspension 3; and performing solid-liquid separation, drying, and then thoroughly roasting to obtain the pearlescent pigment having a fluorescent effect. The method provided by the invention is simple in preparation process, low in raw material cost and easy to popularize.
Description
Technical field
The present invention relates to a kind of preparation method of pearly pigment, particularly relate to a kind of preparation method with pearly pigment of fluorescent effect.
Background technology
Composite Double coating mica titanium nacreous material elder generation in mica surface, plays coated by titanium dioxide interference effect and produces pearl effect, has reasonable nacreous lustre.Coat other metal oxides or the nonmetallic substance with property again on the mica titanium nacreous material surface, make pearly pigment not only have good pearly-lustre characteristic but also some special performances are arranged.
Several big class materials such as that red fluorescence material comprises is sulfide-based, oxysulfide class, oxide-based and metatitanic acid salt, the red illuminating material that titanates of alkali-earth metals is a class stable chemical performance, purity of color is high that the rare earth ion praseodymium mixes.The praseodymium ion doped calcium titanate is a kind of desirable high-visibility pigment, its cie color coordinate x=0.680, y=0.311, and emmission spectrum is pure, very near desirable ruddiness, bigger application prospect is arranged.
Praseodymium doped calcium titanate Preparation of Fluorescent Material method is also more numerous, at present domestic and international known have high temperature solid-state method, combustion method, sol-gel method etc.High temperature solid-state method has its special advantages as a kind of method of the synthesizing luminescent material that generally uses, and production process is comparatively simple, technical maturity and constantly perfect.Chinese patent CN 101544886 B(praseodymium doped calcium titanate luminescent powder and preparations thereof) in conjunction with spray pyrolysis and high temperature solid-state method, with a certain amount of CaCO
3And Pr
6O
11Solid is dissolved in rare nitric acid, heated and stirred is driven excessive acid out of, reach after 2 ~ 3 in the pH value of solution value, again solution is heated to molten molten shape, the cooling back adds tetrabutyl titanate, water-ethanol solution, citric acid and polyoxyethylene glycol, stirring obtains presoma, and high-temperature roasting obtains praseodymium doped calcium titanate fluorescent material after the spraying drying.The method of Chinese patent CN 101899298 an A(fast synthesizing luminescent material), be dissolved in the deionized water than taking by weighing nitrocalcite, zinc nitrate, butyl (tetra) titanate, yellow soda ash, citric acid and polyoxyethylene glycol according to metering, taking by weighing Praseodymium trioxide is dissolved in the concentrated nitric acid, burning is not to firing in retort furnace after mixing, and aftertreatment namely obtains praseodymium doped calcium titanate fluorescent material.
Relevant research has been done to the preparation of doped strontium aluminate fluorescence mica powder by Wuhan University of Technology, uses coprecipitation method and combustion method to prepare europium, dysprosium adulterated al hydrochlorate fluorescent material.Use coprecipitation method to prepare doped strontium aluminate fluorescence mica powder, the factor of consumption, aspects such as reaction pH etc. of selection, consumption, temperature of reaction, activator and the auxiliary of precipitation agent of having studied is to (the high Huimin of fluorescent material Effect on Performance, pigments, mica preparation and mechanism research [D] thereof. Wuhan: Wuhan University of Technology, 2010.).But the fluorescence mica powder of preparation need make pearl effect not good by just having more excellent fluorescence intensity than higher maturing temperature.
The report of studying the pearly pigment with fluorescent effect is less, and pearly-lustre characteristic and the fluorescent materials effect of comprehensive pearly pigment also are development needs, can bring reasonable economic benefit, false proof usefulness, decorative effect.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with pearly pigment of fluorescent effect.
To achieve these goals, the technical solution used in the present invention is:
1, the pre-preparation of mica titanium nacreous material
A. mica 50g mica is dropped in the 500mL water and form suspension liquid, and regulate suspension liquid pH value to 2.0 with the hydrochloric acid of 6.0mol/L, stir, get reaction mother liquor 1;
B. the 100mL titanium tetrachloride solution is added drop-wise in 78 ℃ of reaction mother liquors 1 under the water bath condition, be 2.0 by 4.0mol/L sodium hydroxide regulation system pH value, constantly stir simultaneously, homogeneous reaction in the promotion system between each component, after treating that liquid feeding is finished, continue to stir 30 min, get product suspension liquid 1.
C. product suspension liquid 1 is implemented solid-liquid separation, and dry gained solid matter is the mica titanium nacreous material raw material that secondary coats.
Described titanium tetrachloride solution, solubility are 2mol/L;
Described dropping is to carry out under the 0.3mL/min;
Described stirring, its speed is 400r/min.
2, the preparation of pearly pigment
A. mica titanium nacreous material is dropped into to stir in the water than the ratio of 10 ml waters according to 1 gram mica titanium nacreous material and form reactant suspension liquid 2, with sodium hydroxide solution adjusting suspension liquid pH value to 10 ~ 11, stir, get reaction mother liquor 2;
B. under 70 ~ 80 ℃ of temperature condition, adopt measure control equipment that the mixing solutions of the water-soluble salt of calcium liquid and the transition metal M speed with 0.040 ~ 0.12mL/min is joined in the above-mentioned reaction mother liquor, speed with 400 r/min keeps mechanical stirring constantly simultaneously, with the homogeneous reaction between each component in the promotion system;
C. after solution to be mixed is added dropwise to complete, continue to stir 30 min, get product suspension liquid 3;
D. product suspension liquid 3 is implemented solid-liquid separation, and dry gained solid matter;
E. under 600 ~ 1000 ℃, the solid matter that thorough roasting is dry cools off, and gets the fluorescent effect pearly pigment.
Described calcium liquid refers to ca nitrate soln or calcium chloride solution;
M in the described transition metal M water-soluble salt refers to praseodymium, europium, zinc or cerium;
The water-soluble salt of described transition metal M refers to the nitrate of praseodymium, europium, zinc or cerium, or the muriate of praseodymium, europium, zinc or cerium, or the mixing solutions of the water-soluble salt of the transition metal M of two kinds of arbitrary proportions;
Described mixing solutions, wherein the integral molar quantity of transition metal M praseodymium, europium, zinc or cerium is 1～6:1000 with calcium molar weight ratio in the calcium liquid;
Described mica titanium nacreous material is that technical scheme 1 described method is by the homemade silvery white type pearly pigment of the present invention.Described homemade mica titanium nacreous material has different form and aspect according to different clad ratios, along with the increase of clad ratio presents silvery white, Huang, red, blue, green coloured light change effect successively.Self-control process substrate material mica can be natural, also can be synthetic, and preferred sheet directly is 10～60 μ m, and radius-thickness ratio is the mica more than 45, and the synthetic fluorophlogopite that has this sheet footpath and thickness is then better;
Concentration of hydrochloric acid of the present invention is 6.0mol/L, and naoh concentration is 2.0～4.0mol/L.
The inventive method preparation is simple, and raw materials cost the is easy to apply.
Description of drawings
Excitation spectrum and the emmission spectrum of the pearly pigment that Fig. 1 obtains for the present invention;
The XRD spectra of the pearly pigment that Fig. 2 obtains for the present invention;
The photo of pearly pigment under natural light that Fig. 3 obtains for the present invention;
Fig. 4 is the serial SEM figure with fluorescent effect pearly pigment of different pH values, temperature of reaction, liquid feeding speed and maturing temperature preparation.
Embodiment
For the understanding of the present invention better, existing in conjunction with the accompanying drawings and embodiments, the present invention is described further.
Fig. 1 is pH value 10.5, and 75 ℃ of temperature of reaction, liquid feeding speed are 0.080mL/min, excitation spectrum and the emmission spectrum figure of the fluorescent effect pearly pigment that obtains after 800 ℃ of roastings.
A among Fig. 2, b, c is respectively mica titanium nacreous material, not the XRD spectra of roasting fluorescent effect pearly pigment and 800 ℃ of roasting fluorescent effect pearly pigments.
It is photo under the fluorescent effect pearly pigment natural light among Fig. 3.
A is that the pH value is 11.0 among Fig. 4, and 70 ℃ of temperature of reaction, liquid feeding speed are 0.12mL/min, fluorescent effect pearly pigment SEM figure after 1000 ℃ of roastings.
B is that the pH value is 10.0 among Fig. 4, and 80 ℃ of temperature of reaction, liquid feeding speed are 0.080mL/min, fluorescent effect pearly pigment SEM figure after 600 ℃ of roastings.
C is that the pH value is 10.5 among Fig. 4, and 75 ℃ of temperature of reaction, liquid feeding speed are 0.080mL/min, fluorescent effect pearly pigment SEM figure after 800 ℃ of roastings.
D is that the pH value is 10.5 among Fig. 4, and 75 ℃ of temperature of reaction, liquid feeding speed are 0.040mL/min, fluorescent effect pearly pigment SEM figure after 800 ℃ of roastings.
Embodiment 1
1, the pre-preparation of mica titanium nacreous material
A. the 50g mica is dropped into and form suspension liquid 1 in the 500mL water, and regulate suspension liquid pH value to 2.0 with the hydrochloric acid of 6.0mol/L, stir, get reaction mother liquor 1.
B. the titanium tetrachloride solution 100mL with 2mol/L joins in 78 ℃ of reaction mother liquors 1 under the water bath condition with 0.3mL/min, be 2.0 by 4.0mol/L sodium hydroxide regulation system pH value, constantly stir with 400r/min simultaneously, homogeneous reaction in the promotion system between each component, after treating that liquid feeding is finished, continue to stir 30 min, get product suspension liquid 2.
C. product suspension liquid 2 is implemented solid-liquid separation, and dry gained solid matter is the mica titanium nacreous material raw material that secondary coats.
2, the preparation of pearly pigment
A. the mica titanium nacreous material with the 40g pre-preparation drops into stirring formation reactant suspension liquid 2 in the 400mL water, and with the pH value to 11.0 that the sodium hydroxide of 3.0mol/L is regulated suspension liquid 2, stirs, and gets reaction mother liquor 2.
Praseodymium nitrate and the 2mol/L calcium chloride solution that b. will contain 0.008mol/L are mixed into the 20mL mixed solution, speed with 0.12mL/min is added dropwise to mixed solution in 70 ℃ of reaction mother liquors under the water bath condition, by 3.0mol/L sodium hydroxide system pH is adjusted to 11.0, constantly stir with 400r/min simultaneously, homogeneous reaction in the promotion system between each component, drop to be mixed add finish after, continue to stir 30 min, get product suspension liquid 3.
C. product suspension liquid 3 is implemented solid-liquid separation, and dry gained solid matter.
D. at 1000 ℃ of following baked solid materials, obtain the fluorescent effect pearly pigment that has of the present invention through cooling.The pearly pigment that present embodiment is prepared, SEM figure is shown in a among Fig. 4.
Embodiment 2
1, the pre-preparation of mica titanium nacreous material
The method of pre-preparation is with embodiment 1.
2, the preparation of pearly pigment
A. the 40g mica titanium nacreous material is dropped into and stir formation reactant suspension liquid 2 in the 400mL water, and with the pH value to 10.0 that the sodium hydroxide of 2.0mol/L is regulated suspension liquid 2, stir, get reaction mother liquor 2.
B. will contain the europium nitrate of 0.012mol/L and the ca nitrate soln of 2mol/L and be mixed into the 20mL mixed solution, speed with 0.080mL/min is added drop-wise to mixed solution in 80 ℃ of reaction mother liquors 2 under the water bath condition, by the adjusting of 2.0mol/L sodium hydroxide system pH is adjusted to 10, constantly stir with 400r/min simultaneously, homogeneous reaction in the promotion system between each component, drop to be mixed add finish after, continue to stir 30 min, get product suspension liquid 3.
C. product suspension liquid 3 is implemented solid-liquid separation, and dry gained solid matter.
D. at 600 ℃ of following baked solid materials, obtain pearly pigment of the present invention through cooling.The pearly pigment that present embodiment is prepared, SEM figure is shown in the b among Fig. 4.
Embodiment 3
1, the pre-preparation of mica titanium nacreous material
The method of pre-preparation is with embodiment 1.
2, the preparation of pearly pigment
A. the 40g mica titanium nacreous material is dropped into and stir formation reactant suspension liquid 2 in the 400mL water, and with the pH value to 10.5 that the sodium hydroxide of 2.0mol/L is regulated suspension liquid 2, stir, get reaction mother liquor 2.
B. will contain the praseodymium chloride of 0.001mol/L, the cerous nitrate of 0.001mol/L and the calcium chloride solution of 2mol/L and be mixed into the 20mL mixed solution, speed with 0.080mL/min is added dropwise to mixed solution in 75 ℃ of reaction mother liquors under the water bath condition, by 2.0mol/L sodium hydroxide system pH is adjusted to 10.5, constantly stir with 400r/min simultaneously, homogeneous reaction in the promotion system between each component, drop to be mixed add finish after, continue to stir 30 min, get product suspension liquid 3.
C. product suspension liquid 3 is implemented solid-liquid separation, and dry gained solid matter.
D. at 800 ℃ of following baked solid materials, obtain pearly pigment of the present invention through cooling.The pearly pigment that present embodiment is prepared, SEM figure is shown in the c among Fig. 4.
Embodiment 4
1, the pre-preparation of mica titanium nacreous material
The method of pre-preparation is with embodiment 1.
2, the preparation of pearly pigment
A. the 40g mica titanium nacreous material is dropped into and stir formation reactant suspension liquid 2 in the 400mL water, and with the pH value to 10.5 that the sodium hydroxide of 2.0mol/L is regulated suspension liquid 2, stir, get reaction mother liquor 2.
The ca nitrate soln that b. will contain praseodymium nitrate, 0.002mol/L zinc chloride and the 2mol/L of 0.002mol/L is mixed into the 20mL mixed solution, speed with 0.040mL/min is added dropwise to mixed solution in 75 ℃ of reaction mother liquors 2 under the water bath condition, by 2.0mol/L sodium hydroxide regulation system pH value is adjusted to 10.5, constantly stir with 400r/min simultaneously, homogeneous reaction in the promotion system between each component, drop to be mixed add finish after, continue to stir 30 min, get product suspension liquid 3.
C. product suspension liquid 3 is implemented solid-liquid separation, and dry gained solid matter.
D. at 800 ℃ of following baked solid materials, obtain pearly pigment of the present invention through cooling.The pearly pigment that present embodiment is prepared, SEM figure is shown in the d among Fig. 4.
Claims (8)
1. the preparation method with pearly pigment of fluorescent effect at first is to utilize mica that mica titanium nacreous material is carried out pre-preparation, and the homemade mica titanium nacreous material of recycling is prepared pearly pigment, it is characterized in that:
1) pre-preparation of mica titanium nacreous material
A. mica is dropped into and form suspension liquid in the water, and regulate suspension liquid pH value to 2.0 with the hydrochloric acid of 6.0mol/L, stir, get reaction mother liquor 1;
B. the 100mL titanium tetrachloride solution is added drop-wise in 78 ℃ of reaction mother liquors 1 under the water bath condition, be 2.0 by 4.0mol/L sodium hydroxide regulation system pH value, constantly stir simultaneously, homogeneous reaction in the promotion system between each component, after treating that liquid feeding is finished, continue to stir 30 min, get product suspension liquid 1;
C. the product suspension liquid is implemented solid-liquid separation, and dry gained solid matter is the mica titanium nacreous material raw material that secondary coats;
2) preparation of pearly pigment
A. mica titanium nacreous material is dropped into and form reactant suspension liquid 2 in the water, the pH value of regulating suspension liquid 2 with sodium hydroxide solution is 10 ~ 11, stirs, and gets reaction mother liquor 2;
B. under 70 ~ 80 ℃ of temperature condition, the mixing solutions of the water-soluble salt of calcium liquid and transition metal M is added drop-wise in the reaction mother liquor 2, keep mechanical stirring constantly simultaneously;
C. after solution interpolation to be mixed is finished, continue to stir 30 min, get product suspension liquid 3;
D. product suspension liquid 3 is implemented solid-liquid separation, and dry gained solid matter;
E. under 600 ~ 1000 ℃, the solid matter that thorough roasting is dry cools off, and gets the fluorescent effect pearly pigment.
2. a kind of preparation method with pearly pigment of fluorescent effect according to claim 1 is characterized in that described titanium tetrachloride solution, and solubility is 2mol/L; Described dropping is to carry out under the 0.3mL/min; Described mechanical stirring, stirring velocity are 400r/min.
3. a kind of preparation method with pearly pigment of fluorescent effect according to claim 1 is characterized in that described reactant suspension liquid 1 is than the proportional arrangement of 10 ml waters according to 1 gram mica titanium nacreous material.
4. a kind of preparation method with pearly pigment of fluorescent effect according to claim 1 is characterized in that described dropping, and its speed is 0.040 ~ 0.12mL/min; Described mechanical stirring, stirring velocity are 400 r/min.
5. a kind of preparation method with pearly pigment of fluorescent effect according to claim 1 is characterized in that described calcium liquid refers to ca nitrate soln or calcium chloride solution.
6. a kind of preparation method with pearly pigment of fluorescent effect according to claim 1, the water-soluble salt that it is characterized in that described transition metal M refers to the nitrate of praseodymium, europium, zinc or cerium, or the muriate of praseodymium, europium, zinc or cerium, or the mixing solutions of the arbitrary proportion of the water-soluble salt of two kinds of transition metal M.
7. a kind of preparation method with pearly pigment of fluorescent effect according to claim 8 is characterized in that the integral molar quantity of praseodymium, europium, zinc or cerium in the water-soluble salt of described transition metal M and calcium molar weight ratio in the calcium liquid are 1～6:1000.
8. a kind of preparation method with pearly pigment of fluorescent effect according to claim 1 is characterized in that described concentration of hydrochloric acid is 6.0mol/L, and naoh concentration is 2.0～4.0mol/L.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103773085A (en) * | 2014-01-10 | 2014-05-07 | 浙江瑞成珠光颜料有限公司 | Functional mica pigment processing technique |
| CN107629782A (en) * | 2017-09-06 | 2018-01-26 | 瑞彩科技股份有限公司 | A kind of preparation method of the photochromic pearlescent pigment of tungsten oxide mica and its dispersion liquid |
| CN112662201A (en) * | 2020-12-21 | 2021-04-16 | 江西善纳新材料科技有限公司 | Preparation method of mica-based fluorescent pearlescent pigment |
| CN113583479A (en) * | 2021-06-29 | 2021-11-02 | 福建师范大学 | Method for preparing silver pearlescent pigment by using solid waste generated in process of processing inkstone pot |
| CN113637478A (en) * | 2021-08-13 | 2021-11-12 | 河北师范大学 | Europium-doped barium tetrasilicon mica fluorescent powder and preparation method and application thereof |
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| US20080279796A1 (en) * | 2007-03-05 | 2008-11-13 | Carsten Handrosch | Transition metal-containing effect pigments |
| CN101544886A (en) * | 2009-05-07 | 2009-09-30 | 哈尔滨工程大学 | Praseodymium-doped calcium titanate luminescent powder and preparation method thereof |
| CN103013186A (en) * | 2012-12-21 | 2013-04-03 | 福建师范大学 | Composite coloring pearlescent pigment and preparation thereof |
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2013
- 2013-06-26 CN CN2013102592714A patent/CN103333528A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20080279796A1 (en) * | 2007-03-05 | 2008-11-13 | Carsten Handrosch | Transition metal-containing effect pigments |
| CN101544886A (en) * | 2009-05-07 | 2009-09-30 | 哈尔滨工程大学 | Praseodymium-doped calcium titanate luminescent powder and preparation method thereof |
| CN103013186A (en) * | 2012-12-21 | 2013-04-03 | 福建师范大学 | Composite coloring pearlescent pigment and preparation thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103773085A (en) * | 2014-01-10 | 2014-05-07 | 浙江瑞成珠光颜料有限公司 | Functional mica pigment processing technique |
| CN107629782A (en) * | 2017-09-06 | 2018-01-26 | 瑞彩科技股份有限公司 | A kind of preparation method of the photochromic pearlescent pigment of tungsten oxide mica and its dispersion liquid |
| CN107629782B (en) * | 2017-09-06 | 2020-09-11 | 瑞彩科技股份有限公司 | Preparation method of tungsten oxide-mica photochromic pearlescent pigment and dispersion liquid thereof |
| CN112662201A (en) * | 2020-12-21 | 2021-04-16 | 江西善纳新材料科技有限公司 | Preparation method of mica-based fluorescent pearlescent pigment |
| CN112662201B (en) * | 2020-12-21 | 2021-10-22 | 江西善纳新材料科技有限公司 | Preparation method of mica-based fluorescent pearlescent pigment |
| CN113583479A (en) * | 2021-06-29 | 2021-11-02 | 福建师范大学 | Method for preparing silver pearlescent pigment by using solid waste generated in process of processing inkstone pot |
| CN113637478A (en) * | 2021-08-13 | 2021-11-12 | 河北师范大学 | Europium-doped barium tetrasilicon mica fluorescent powder and preparation method and application thereof |
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Application publication date: 20131002 |