CN102795657A - Preparation method of white hydrotalcite-like compound - Google Patents
Preparation method of white hydrotalcite-like compound Download PDFInfo
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- CN102795657A CN102795657A CN2012102819225A CN201210281922A CN102795657A CN 102795657 A CN102795657 A CN 102795657A CN 2012102819225 A CN2012102819225 A CN 2012102819225A CN 201210281922 A CN201210281922 A CN 201210281922A CN 102795657 A CN102795657 A CN 102795657A
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Abstract
The invention relates to a preparation method of a white hydrotalcite-like compound, comprising the following steps: firstly respectively preparing a solution A by mixedly dissolving sodium meta aluminate and sodium hydroxide in deionized water, preparing a solution B by mixed dissolving magnesium chloride and zinc chloride in deionized water, preparing a solution C by respectively dissolving europia and terbium oxide with dilute hydrochloric acid and pouring into the solution B, and preparing a mixed slurry D by dissolving the mixed ligand in sodium stearate; under the effect of strong stirring or supersonic waves, simultaneously adding the solution A and the solution C in the mixed slurry D, uniformly stirring, then adjusting the pH value of the mixed slurry, aging, washing sediments, then conducting pumping filtration, and drying the filter cake to obtain the white hydrotalcite-like compound. According to the invention, the single matrix white material can be synthesized by one step method under mild conditions. The white hydrotalcite-like compound disclosed herein has excellent luminescent property of metal complex and thermostability of inorganic substance, and has a latent application prospect in the field of photoelectricity.
Description
Technical field
The invention belongs to the photovaltaic material technical field, be specifically related to a kind of preparation method of the houghite that emits white light.
Technical background
White light LEDs is low as a kind of energy consumption, luminous efficiency is high, the life-span is long, pollution-free, compact construction, little, the lightweight environmental protection novel solid of volume light source, is showing and lighting field has great application prospect.1997, Japanese Ri Ya chemical company was with blue light GaN tube core LD pumped YAG: Ce
3+Yellow fluorescent powder has been developed white light LEDs, but has problems such as colour temperature is high, colour rendering index is low.In order to address the above problem, adopt ultraviolet-near ultraviolet (350-410 nm) tube core to excite three primary colors fluorescent powder to realize that white light LEDs becomes one of focus of this area research, be considered to the leading of White-light LED illumination of new generation.But at present; The white emitting fluorescent powder that is complementary with ultraviolet and near ultraviolet chip lacks; And it is more serious that the ubiquity white light emission is unstable, synthesis temperature is high, product is reunited, shortcoming such as during preparation technology's energy charge, and also this white emitting fluorescent powder generally adopts the method for mixture of red, green, blue three kinds of primary colours fluorescent material to make; Because exist color to absorb and proportioning regulation and control problem between the mixture, luminous efficiency etc. are a greater impact again.In addition, numerous patents of these fluorescent material are monopolized by offshore company for a long time, and this type of fluorescent material on the existing market is mostly all from Japan, the U.S. and Taiwan, expensive.Therefore, development single-matrix white luminescent material that can be complementary with the ultraviolet chip, that preparation condition is gentle is significant.
(hydrotalcite-like compounds HTlc) is one type and has hydrotalcite (Layered double hydroxides, LDHs) mixed metal hydroxides of layered crystal structure by what divalence and trivalent metal ion were formed houghite.But its laminate metal modulation, interlayer anion has the intercalation assembleability, can be as required, with various inorganic and organic anions, with between many and interposed layer such as heteropolyanion and title complex negatively charged ion, assembling obtains the target material of supramolecular structure.So far, the various countries investigator is to synthetic, the preparation method of LDHs and HTLc, and carried out broad research at aspects such as IX, absorption, separation, catalysis, medicine and explored with using.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the houghite that emits white light; Utilize the orientation effect of the controlled and veneer structure of intercalation property, the laminate of hydrotalcite stratified material; According to the three primary colours superposition theorem will be rubescent respectively, green, the europium of blue light, terbium, Zn complex mix with hydrotalcite by a certain percentage, synthesizes the white light houghite fluorescent material Eu/Tb/Zn-HTlc of single-matrix.
The present invention is with the luminescence center ion (Eu of an amount of europium, terbium, Zn complex
3+, Tb
3+, Zn
2+) part replaces the trivalent aluminium ion (Al in the magnesium aluminum-hydrotalcite flaggy
3+) and divalence mg ion (Mg
2+); Use the tensio-active agent StNa with thenoyltrifluoroacetone, 2 simultaneously; Oleophilicity mixed ligands such as 2-dipyridyl are brought the magnesium aluminum-hydrotalcite interlayer into, make mixed ligand and disperse to be embedded in the luminescence center ion coordination on the magnesium aluminum-hydrotalcite oxyhydroxide flaggy, send red, green, blue simultaneously; Three kinds of light mix the formation white light, obtain a kind of white light houghite fluorescent material of single-matrix.
For realizing that the technical scheme that the object of the invention adopts is:
1, the preformulation of reactant
With sodium metaaluminate (AlNaO
2) be dissolved in respectively in the deionized water with sodium hydroxide (NaOH), be mixed with solution A;
With magnesium chloride (MgCl
2) and zinc chloride (ZnCl
2) be dissolved in respectively in the deionized water, remix becomes solution B;
Europium sesquioxide and terbium sesquioxide respectively with pouring into behind the diluted hydrochloric acid dissolution in the solution B, are mixed with solution C;
Molten the mixing of mixed ligand is mixed with mixed serum D in StNa.
In the described solution A, the sodium metaaluminate mass percent accounts for 20%, and the sodium hydroxide mass percent accounts for 10%.
In the described solution B, Mg
2+: Zn
2+Mol ratio be 1:0.18～0.3.
Mg in the described solution B
2+With the Al in the solution A
3+Mol ratio be 1:0.1～0.27.
Described solution C is according to Eu
3+: Tb
3+: Zn
2+Mol ratio be the ratio preparation of 1:7.8～9.5:18～24.
Described mixed ligand is meant that with a kind of in the beta-diketon class of thenoyltrifluoroacetone (TTA), benzoyltrifluoroacetone(BTA (BTA), benzoyl acetone (BA), trifluoroacetylacetone (TFA), diphenylpropane-1,3-dione(DPPO) (DBM) or methyl ethyl diketone (acac) or two kinds be first part; 2; 2-dipyridyl (2; 2-biby) or 1; A kind of in the 10-phenanthroline (o-phen) is second part, and is three or the quaternary mixed ligand that the 3rd part is formed with a kind of in Xaxa, para-aminosalicylic acid, Whitfield's ointment or the wintergreen oil.The consumption of mixed ligand is to decide according to the amount of luminescence center, wherein: (Eu
3++ Tb
3+): first part: the mol ratio of second part is 1:2.5～3.8:0.8～1.5; Zn
2+: the mol ratio of the 3rd part is 1:1.69～2.3.
Dissolve the mixing in advance of said mixed ligand is meant in advance the mixed ligand dissolving or is dispersed in the tensio-active agent StNa.Dissolving the purpose of mixing in advance only is to make mixed ligand dissolve diffusing getting final product, and is to make oil loving mixed ligand more be prone to insert the magnesium aluminum-hydrotalcite interlayer in the process in order to prepare in coprecipitation method.Mg ion in the solution B: the mol ratio of StNa is 1:0.17～0.27 among the mixed serum D.
2, preparation
Under violent stirring or UW effect, simultaneously solution A and solution C are dropwise added among the mixed serum D, the back that stirs becomes the reaction mixed serum, with aqueous sodium hydroxide solution conditioned reaction mixed serum to pH=9
～13, in 60
～80 ℃ of following ageings 10
～12 hours; With the reaction mixed serum suction filtration after the ageing, the water washing leaching cake to the pH=7 that filtrates～8, once more the deposition, suction filtration; The filter cake that obtains behind the suction filtration is in 100
～110 ℃ of oven dry down promptly obtain the houghite Eu/Tb/Zn-HTlc that emits white light of the present invention.
Description of drawings
Fig. 1 is the fluorescence emission spectrum of Eu/Tb/Zn-HTlc under 365 nm excite of the embodiment of the invention 1 preparation.
Fig. 2 is the FT-IR spectrogram of the Eu/Tb/Zn-HTlc of the embodiment of the invention 1 preparation.
Fig. 3 is the MgAl-LDHs (a) of the embodiment of the invention 1 preparation and the X-ray diffractogram of Eu/Tb/Zn-HTlc (b), and illustration is little angle XRD among the figure.
Embodiment
Below white light houghite of the present invention and preparation method thereof is described further, will helps understanding of the present invention with indefiniteness embodiment, and not as to qualification of the present invention,
Embodiment 1
1, takes by weighing 0.02 gram NaAlO
2, 0.01 the gram NaOH together be dissolved in the deionized water, this is a solution A;
2, take by weighing 0.18 gram MgCl
2, 0.054 the gram ZnCl
2Be dissolved in respectively in the deionized water, be mixed into mixing solutions B after the dissolving;
3, take by weighing 0.003 gram Eu
2O
3With 0.03 gram Tb
4O
7, with adding in the solution B behind the diluted hydrochloric acid dissolution, this is a solution C;
4, take by weighing 0.01 gram thenoyltrifluoroacetone, 0.04 gram methyl ethyl diketone, 0.03 gram 1 respectively, 10-phenanthroline and 0.1 gram Whitfield's ointment with together pouring into behind the anhydrous alcohol solution in the aqueous solution that contains 0.1 gram StNa, are mixed with mixed serum D respectively.
5, under the high degree of agitation that continues, simultaneously solution A and solution C are dropwise splashed among the mixed serum D, process mixed serum after molten fully the mixing; With aqueous sodium hydroxide solution conditioned reaction mixed serum to pH=11; In 80 ℃ of following ageings 12 hours, suction filtration, water washing filter cake were to the pH=7-8 that filtrates, with suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate; Filter cake obtains white light houghite (Eu/Tb/Zn-HTlc) in 100 ℃ of oven dry down.
As shown in Figure 1, under the 365nm ultraviolet excitation, sample has located to occur respectively the characteristic emission peak of europium, terbium, Zn complex at 614nm, 545nm, 490nm etc.; Stack spectrum for RGB; Use ColorCoordinate.exe chromaticity coordinates computed in software, getting chromaticity coordinates is (0.346,0.339); Approach the chromaticity coordinates (0.33,0.33) of the pure white light that provides of International Commission on Illumination (CIE) in 1931.
As shown in Figure 2, free ligand o-phen is positioned at 1561 (ν
C=C+C=N), 854 (δ
C-H) and 739 cm
-1(δ
C-H) charateristic avsorption band, red shift to 1519,848 respectively, 723 cm in sample spectra
-1, show that metals ion forms title complex (Cong Y., Fu J., Cheng Z.Y., et al. with o-phen
J. Poly. Sc.:Part B:Poly. Phys.2005,43:2181-2189); Free ligand Hacac is positioned at 624 cm
-1(ν
C=O) charateristic avsorption band, also red shift to 1573 cm in sample spectra
-1, show metals ion with acac
-Form title complex; Be positioned at 1642 cm
-1The ν of free ligand HTTA
C=OVibration peak appears at 1600 cm in sample spectra
-1, this provides strong evidence (Xiao L. R., Gao F., Tang J. Y., et al. with its formation title complex for metals ion
Spectrosc. Spect. Anal.,2004,24 (6): 756-761); In addition, 1456 (ν
AsCOO -) and 1392 cm
-1(ν
S COO -) appearance of absorption peak shows that Whitfield's ointment has formed title complex with metals ion.
As shown in Figure 3, after mixed ligand got into hydrotalcite layers, its laminate spacing increased to 4.42nm by the 0.78nm of magnesium aluminum-hydrotalcite; (003) diffraction peak broadens and dies down; Simultaneously other senior diffraction peak also dies down or disappears, show add mixed ligand after, along with the increase of the amount that gets into interlayer; Laminate is supportted De Gengkai, and the existing part of Eu/Tb/Zn-HTlc laminate is peeled off.
Embodiment 2
1, takes by weighing 0.024 gram NaAlO
2, 0.012 the gram NaOH together be dissolved in the deionized water, this is a solution A;
2, take by weighing 0.18 gram MgCl
2, 0.0527 the gram ZnCl
2Be dissolved in respectively in the deionized water, be mixed into solution B after the dissolving;
3, take by weighing 0.003 gram Eu
2O
3With 0.025 gram Tb
4O
7, with adding in the solution B behind the diluted hydrochloric acid dissolution, this is a solution C;
4, take by weighing 0.04 gram trifluoroacetylacetone, 0.08 gram diphenylpropane-1,3-dione(DPPO), 0.023 gram 2 respectively, 2-dipyridyl and 0.11 gram wintergreen oil, with together pouring into behind the anhydrous alcohol solution in the aqueous solution that contains 0.11 gram StNa, this is mixed serum D respectively.
5, under the UW effect that continues; Simultaneously water solution A and solution C are dropwise splashed among the mixed serum D, with aqueous sodium hydroxide solution conditioned reaction mixed serum to pH=11, in 80 ℃ of following ageings 11 hours; Suction filtration, water washing filter cake are to the pH=8 that filtrates; With suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter cake obtains white light houghite (Eu/Tb/Zn-HTlc) in 110 ℃ of oven dry down
Embodiment 3
1, takes by weighing 0.029 gram NaAlO
2, 0.015 the gram NaOH together be dissolved in the deionized water, this is a solution A;
2, take by weighing 0.14 gram MgCl
2, 0.05 the gram ZnCl
2Be dissolved in respectively in the deionized water, be mixed into solution B after the dissolving;
3, take by weighing 0.003 gram Eu
2O
3With 0.026 gram Tb
4O
7, with adding in the solution B behind the diluted hydrochloric acid dissolution, this is a solution C;
4, take by weighing 0.027 gram benzoyltrifluoroacetone(BTA, 0.04 gram methyl ethyl diketone, 0.027 gram 2 respectively; 2-dipyridyl and 0.11 gram para-aminosalicylic acid; With together pouring into behind the anhydrous alcohol solution in the aqueous solution that contains 0.12 gram StNa, this is mixed serum D respectively.
5, under the high degree of agitation that continues; Simultaneously water solution A and solution C are dropwise splashed among the mixed serum D, with aqueous sodium hydroxide solution conditioned reaction mixed serum to pH=10, in 60 ℃ of following ageings 10 hours; Suction filtration, water washing filter cake are to the pH=7 that filtrates; With suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter cake obtains white light houghite (Eu/Tb/Zn-HTlc) in 105 ℃ of oven dry down
Embodiment 4
1, takes by weighing 0.034 gram NaAlO
2, 0.017 the gram NaOH together be dissolved in the deionized water, this is a solution A;
2, take by weighing 0.18 gram MgCl
2, 0.047 the gram ZnCl
2Be dissolved in respectively in the deionized water, be mixed into solution B after the dissolving;
3, take by weighing 0.003 gram Eu
2O
3With 0.0279 gram Tb
4O
7, with adding in the solution B behind the diluted hydrochloric acid dissolution, this is a solution C;
4, take by weighing 0.04 gram thenoyltrifluoroacetone, 0.04 gram methyl ethyl diketone, 0.046 gram 1 respectively; 10-phenanthroline and 0.13 gram Xaxa; With together pouring into behind the anhydrous alcohol solution in the aqueous solution that contains 0.132 gram StNa, this is mixed serum D respectively.
5, under the high degree of agitation that continues; Simultaneously water solution A and solution C are dropwise splashed among the mixed serum D, with aqueous sodium hydroxide solution conditioned reaction mixed serum to pH=13, in 70 ℃ of following ageings 12 hours; Suction filtration, water washing filter cake are to the pH=7 that filtrates; With suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter cake obtains white light houghite (Eu/Tb/Zn-HTlc) in 100 ℃ of oven dry down.
Embodiment 5
1, takes by weighing 0.04 gram NaAlO
2, 0.02 the gram NaOH together be dissolved in the deionized water, this is a solution A;
2, take by weighing 0.18 gram MgCl
2, 0.045 the gram ZnCl
2Be dissolved in respectively in the deionized water, be mixed into solution B after the dissolving;
3, take by weighing 0.003 gram Eu
2O
3With 0.029 gram Tb
4O
7, with adding in the solution B behind the diluted hydrochloric acid dissolution, this is a solution C;
4, take by weighing 0.05 gram benzoyl acetone, 0.08 gram diphenylpropane-1,3-dione(DPPO), 0.049 gram 1 respectively; 10-phenanthroline and 0.115 gram para-aminosalicylic acid; With together pouring into behind the anhydrous alcohol solution in the aqueous solution that contains 0.147 gram StNa, this is mixed serum D respectively.
5, under the UW effect that continues; Simultaneously water solution A and solution C are dropwise splashed among the mixed serum D, with aqueous sodium hydroxide solution conditioned reaction mixed serum to pH=9, in 80 ℃ of following ageings 11 hours; Suction filtration, water washing filter cake are to the pH=8 that filtrates; With suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter cake obtains white light houghite (Eu/Tb/Zn-HTlc) in 105 ℃ of oven dry down.
Claims (8)
1. the preparation method of a houghite that emits white light is characterized in that
1) preformulation of reactant
Sodium metaaluminate and sodium hydroxide are dissolved in respectively in the deionized water, are mixed with solution A;
Magnesium chloride and zinc chloride are dissolved in respectively in the deionized water, and remix becomes solution B;
Europium sesquioxide and terbium sesquioxide respectively with pouring into behind the diluted hydrochloric acid dissolution in the solution B, are mixed with solution C;
Molten the mixing of mixed ligand is mixed with mixed serum D in StNa;
2) preparation
Under violent stirring or UW effect, simultaneously solution A and solution C are dropwise added among the mixed serum D, the back that stirs becomes the reaction mixed serum, with aqueous sodium hydroxide solution conditioned reaction mixed serum to pH=9
～13, in 60
～80 ℃ of following ageings 10
～12 hours; With the reaction mixed serum suction filtration after the ageing, the water washing leaching cake to the pH=7 that filtrates～8, once more the deposition, suction filtration; The filter cake that obtains behind the suction filtration is in 100
～110 ℃ of oven dry down promptly obtain the houghite Eu/Tb/Zn-HTlc that emits white light of the present invention.
2. the preparation method of a kind of houghite that emits white light according to claim 1 is characterized in that the sodium metaaluminate mass percent accounts for 20% in the described solution A preparation, and mass percent accounts for 20%, and the sodium hydroxide mass percent accounts for 10%.
3. the preparation method of a kind of houghite that emits white light according to claim 1 is characterized in that in the described solution B preparation Mg
2+: Zn
2+Mol ratio be 1:0.18～0.3.
4. the preparation method of a kind of houghite that emits white light according to claim 1 is characterized in that the Mg in the described solution B
2+With the Al in the solution A
3+Mol ratio be 1:0.1～0.27.
5. the preparation method of a kind of houghite that emits white light according to claim 1 is characterized in that in the solution C preparation Eu
3+: Tb
3+: Zn
2+Mol ratio be 1:7.8～9.5:18～24.
6. the preparation method of a kind of houghite that emits white light according to claim 1; It is characterized in that mixed ligand of the present invention is meant that with a kind of in the beta-diketon class of thenoyltrifluoroacetone, benzoyltrifluoroacetone(BTA, benzoyl acetone, trifluoroacetylacetone, diphenylpropane-1,3-dione(DPPO) or methyl ethyl diketone or two kinds be first part; 2; 2-dipyridyl (2; 2-biby) or 1, a kind of in the 10-phenanthroline (o-phen) is second part, and is three or the quaternary mixed ligand that the 3rd part is formed with a kind of in Xaxa, para-aminosalicylic acid, Whitfield's ointment or the wintergreen oil.
7. the preparation method of a kind of houghite that emits white light according to claim 6, the consumption that it is characterized in that mixed ligand mixed ligand of the present invention is to decide according to the amount of luminescence center, wherein: (Eu
3++ Tb
3+): first part: the mol ratio of second part is 1:2.5～3.8:0.8～1.5; Zn
2+: the mol ratio of the 3rd part is 1:1.69～2.3.
8. the preparation method of a kind of houghite that emits white light according to claim 1 is characterized in that mg ion in the solution B of the present invention: the mol ratio of StNa is 1:0.17～0.27 among the mixed serum D.
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Cited By (5)
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|---|---|---|---|---|
| CN103408682A (en) * | 2013-07-23 | 2013-11-27 | 福建师范大学 | White-light-type hydrotalcite nano composite material and application thereof for LED light source |
| CN105329934A (en) * | 2014-08-15 | 2016-02-17 | 广东先导稀材股份有限公司 | Preparation method of hydrotalcite-like compound used for electrophoretic paint |
| CN105377973A (en) * | 2013-03-01 | 2016-03-02 | 苏米特·库马尔 | Hybrid composite nanomaterials |
| CN109231899A (en) * | 2018-09-14 | 2019-01-18 | 吉林建筑大学 | A kind of high-intensitive alkali-activated carbonatite gel rubber material can be applied to particular surroundings |
| CN109259740A (en) * | 2018-10-23 | 2019-01-25 | 湖州市中医院 | A kind of anti-low temperature scald skin temperature Indicator Paper |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105377973A (en) * | 2013-03-01 | 2016-03-02 | 苏米特·库马尔 | Hybrid composite nanomaterials |
| JP2016520987A (en) * | 2013-03-01 | 2016-07-14 | クマール, スミートKUMAR, Sumeet | Hybrid composite nanomaterial |
| CN105377973B (en) * | 2013-03-01 | 2018-09-18 | 苏米特·库马尔 | Hybridization compounding nano material |
| CN103408682A (en) * | 2013-07-23 | 2013-11-27 | 福建师范大学 | White-light-type hydrotalcite nano composite material and application thereof for LED light source |
| CN105329934A (en) * | 2014-08-15 | 2016-02-17 | 广东先导稀材股份有限公司 | Preparation method of hydrotalcite-like compound used for electrophoretic paint |
| CN109231899A (en) * | 2018-09-14 | 2019-01-18 | 吉林建筑大学 | A kind of high-intensitive alkali-activated carbonatite gel rubber material can be applied to particular surroundings |
| CN109259740A (en) * | 2018-10-23 | 2019-01-25 | 湖州市中医院 | A kind of anti-low temperature scald skin temperature Indicator Paper |
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Application publication date: 20121128 |