CN101249974A - Aluminized hydrotalcite having strong fluorescence and preparation method thereof - Google Patents
Aluminized hydrotalcite having strong fluorescence and preparation method thereof Download PDFInfo
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- CN101249974A CN101249974A CNA2007101440136A CN200710144013A CN101249974A CN 101249974 A CN101249974 A CN 101249974A CN A2007101440136 A CNA2007101440136 A CN A2007101440136A CN 200710144013 A CN200710144013 A CN 200710144013A CN 101249974 A CN101249974 A CN 101249974A
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Abstract
The invention relates to a group of strong fluorescent hydrotalcite containing aluminium which has the simplest chemical formula of (M2+1-xAl3x(OH)-12)An-x/nx/mzB) and a process for preparation. The steps comprise reducing the content of aluminium ion (Al3+) in hydroxide lamellar of the hydrotalcite containing aluminium such as magnesium aluminium hydrotalcite and zinc aluminum hudrotalcite to an appropriate value and simultaneously coordinating ligand which is dissolved or dispersed in interlayer hydrophobicity anion, thereby effectively preventing fluorescence quenching of the aluminium ion (Al3+) which is utilized as a luminous center. And a special combining structure of the ligand or mixed ligand which is mixed in the interlayer anion and the aluminium ion (Al3+) which is embedded on the lamellar increases the dissymmetry of the coordinating aluminium ion (Al3+) which is utilized as the luminous center, simultaneously because the protective action of the hydrotalcite laminate structure, the heat stability of (Al-LLDHs) is increased, thereby obtaining a group of novel high fluorescent hydrotalcite containing aluminium which can emit relative aluminium coordination chelate strong fluorescence is different from the normal hydrotalcite containing aluminium without fluorescence.
Description
Technical field:
The present invention relates to a class and have aluminized hydrotalcite of hyperfluorescence and preparation method thereof
Background technology:
The simplest general formula is [M
2+ 1-xM
3+ x(OH)
2] A
N- X/n.yH
2O] hydrotalcite (layered double hydroxi-des, LDHs), M in its flaggy
2+Be divalent cations such as Mg, Ni, Cu or Zn, M
3+Be isomorphous Tricationic such as Al
3+Deng, A
N-Be interlayer anion such as CO
3 2-, Cl
-, SO
4 2-, NO
3 -Or other organic anion.Because M
2+Partly by M
3+Make the hydrotalcite flaggy positively charged behind the isomorphous substitution, the negatively charged ion between interposed layer links to each other with flaggy with weak chemical bond, with positive charge excessive on the balance flaggy, and is filled into interlayer with the water molecules of some amount.Because the cationic substitutability of flaggy of LDHs and the commutability of interlayer anion, can be with various inorganic with organic anion, with in many and the interposed layer such as heteropolyanion and title complex negatively charged ion, assembling obtains the stratiform thing of supramolecular structure, or Tricationic (Al
3+) be that other the isomorphous or nearly isomorphous Tricationic replaces, can obtain thus different series intercalation houghite material (hydrotalcite-like compound, LLDHs).So far, the various countries investigator is to synthetic, the preparation method of LDHs and LLDHs, and the broad research of having carried out at aspects such as ion-exchange, absorption, separation, catalysis, medicine is explored with using.
In recent years, the preparation of various functional houghites and characteristic research particularly receive publicity.Because the rare earth of special electron structure of tool and various multivalence, the transition metal that appraises at the current rate have functions such as various light, electricity, magnetic, catalysis, therefore rare earth and multivalence, the transition metal ion that appraises at the current rate are introduced in the hydrotalcite structure to obtain functional houghite, become one of focus of hydrotalcite research field.People such as Duan Xue in 2005 propose the patent application (number of patent application: 200510012245.7 of " having rare earth compounding intercalated houghite of fluorescent characteristic and preparation method thereof "; Publication number: CN1715365A), tie up to hydrotalcite layers and introduce the ammonia carboxylic title complex of rare earth ion such as Eu by ion-exchange to obtain the epipolic hydrotalcite of tool.In addition, L.Latterini etc. insert hydrotalcite layers with azo class and other dyestuff by ion-exchange, and acquisition has the hybrid material of light, electric work energy.
As everyone knows, has good thermostability, the oxine aluminium (Alq of wide excitation band and high fluorescence efficiency
3) wait aluminium coordination inner complex, fluorescence metal title complex as a class excellent combination property, be used for one of fluorescent material of luminous or display device by first-selection always, but it is difficult to problems such as big area film forming, cost height and is still its difficult problem of further using of puzzlement so far, and becomes the focus that the investigator pays close attention to.
Summary of the invention:
Based on above research background, the present invention contains trivalent aluminium ion (Al in the aluminum hydrotalcite with magnesium aluminum-hydrotalcite, zinc-aluminium hydrotalcite etc.
3+) content reduce, parts such as oxine with metering are dissolved or dispersed in the lipophilicity negatively charged ion such as stearate radical that contain the aluminum hydrotalcite interlayer simultaneously, make itself and the trivalent aluminium ion coordination that is uniformly distributed on the divalent metal oxyhydroxide flaggy of hydrotalcite, so, part such as oxine because of with aluminum ion (Al
3+) coordination and " suspension " on divalent metal oxyhydroxide flaggy surface and each unit be fixed thereon by isolated, thereby assembling, a kind of special ligand complex structure that is different from aluminium coordination inner complexs such as oxine aluminium fully of formation, because this special construction has the bigger structural asymmetries of aluminium coordination inner complex such as oxine aluminium of specific ionization or " freedom ", thereby can improve the fluorescence efficiency of its luminescence center; In addition, because trivalent aluminium ion (Al wherein
3+) be homodisperse, be fixed on the flaggy, thereby can effectively prevent the quenching of fluorescence that each luminescence unit causes because of reunion; Owing to the provide protection of such hydrotalcite layered structure, improved the thermostability of material simultaneously.Thereby obtain and the common non-blooming novel high fluorescence aluminized hydrotalcite that the different class of aluminum hydrotalcite can be sent corresponding aluminium coordination inner complex intense fluorescence that contains.
Particular content of the present invention is as follows:
1, a class that the present invention relates to has the aluminized hydrotalcite (Al-LLDHs) of hyperfluorescence, has following simplest formula:
[M
2+ 1-xAl
3+ x(OH)
-1 2]A
n- x/nD
x/mzB]，
M wherein
2+Be the divalent metal of magnesium, zinc, copper, nickel; Al
3+Be trivalent aluminium ion, be scattered in the divalent metal oxyhydroxide laminate of this houghite; OH
-1Be monovalence hydroxide radical anion, A
N-Be interlayer anion or mixed anion, its flat fare n=1～2; D is part or mixed ligand, its average coordination number m=2～3; B is the contained neutral molecule of houghite, and z is the neutral molecule number; X is Al
3+/ (M
2++ Al
3+) molar ratio, x=0.165-0.05; Part D is molten to be mixed in interlayer anion A
N-Among, and with laminate on Al
3+Coordination.
2. the aluminized hydrotalcite (Al-LLDHs) with hyperfluorescence of the present invention, its simplest formula
[M2+1-xAl3+x (OH)-12] An-x/n Dx/mzB] in Al
3+Content x is not as common magnalium hydrotalcite
The Al of aluminium zinc hydrotalcite
3+Content x=0.33-0.25, and will be that the x value is reduced to x=0.165-0.05.
3. the aluminized hydrotalcite (Al-LLDHs) with hyperfluorescence of the present invention, wherein D is oxine, 3,5 Dibromosalicylaldehydes contract 8 quinolylamines and 5 or 2 substitutive derivatives; The beta-diketon class of methyl ethyl diketone (acac), diphenylpropane-1,3-dione(DPPO) (DBM); Schiff's base or two Schiff's base; Hydroxyanthraquinone (alizarin), carbazole, porphyrin or derivatives thereof, Quercetin (QCT Quercetin), morin (Morin), chrome azurol S, fluorone or its mixture.
4. the aluminized hydrotalcite (Al-LLDHs) with hyperfluorescence of the present invention, wherein part D is the molten in advance C of being mixed in
12-20Sodium soap, C
12-20Fat sodium sulfonate, C
0-12Alkylbenzoic acid sodium, C
0-12In sodium alkyl benzene sulfonate, sodium salicylate or its mixture, thus the R for preparing by coprecipitation method
ePart D is molten among the-LLDHs mixes in interlayer anion A
N-Among, simultaneously with the divalent metal oxyhydroxide laminate that is scattered in houghite on Al
3+Coordination.
5. the aluminized hydrotalcite (Al-LLDHs) with hyperfluorescence of the present invention, wherein molten mixing in C
12-20Sodium soap, C
12-20Part D content in fat sodium sulfonate, Sodium Benzoate, benzene sulfonic acid sodium salt, sodium salicylate or its mixture is trivalent aluminium ion Al wherein
3+/ 2nd to 1/3rd of a molar content x.
6. as mentioned above, be reduced to the trivalent aluminium ion content (x) in the oxyhydroxide flaggy in the houghite a certain amount of, simultaneously part such as an amount of oxine or molten the mixing of its mixed ligand are scattered in the lipophilicity negatively charged ion of hydrotalcite or houghite interlayer, and with the trivalent Al that disperses to be embedded on the oxyhydroxide flaggy
3+Ion coordination had both prevented the trivalent Al as luminescence center
3+Ionic may fluorescence essence go out, and molten oxine part or its mixed ligand and the trivalent Al that is embedded on the oxyhydroxide flaggy that mixes in interlayer anion
3+The specific group assembling structure that ion coordination forms has improved the coordination Al as luminescence center
3+Asymmetry, thereby obtain and the common non-blooming novel high fluorescence aluminized hydrotalcite that the different class of aluminum hydrotalcite can be sent corresponding aluminium coordination inner complex intense fluorescence that contains.
7. has simplest formula [M
2+ 1-xAl
3+ x(OH)
-1 2] A
N- X/nD
X/mZB] the aluminized hydrotalcite (Al-LLDHs) of hyperfluorescence, be to implement preparation by coprecipitation method.The concrete steps that coprecipitation method preparation method takes are: preparation contains the water solution A of aluminum soluble salt and an amount of NaOH of xmol; Preparation contains the aqueous solution B of (1-x) mol solubility magnesium salts; Preparation contains the lipophilicity organic acid sodium of (x/n) mol, the part of (x/m) mol or the aqueous solution C of mixed ligand.In violent stirring, or ultrasonic wave, or under the microwave action, simultaneously solution A and B are dropwise added C solution, the aqueous sodium hydroxide solution conditioned reaction mixed serum of using proper concn is to PH=9～13, in 60～80 ℃ of following ageings 6～12 hours, suction filtration, water washing filter Pie are to filtering PH=7 at night～8, suction filtration behind the throw out, filter Pie was dried 2 hours down in 100～110 ℃, obtained the aluminized hydrotalcite (Al-LLDHs) of hyperfluorescence.
Embodiment:
Below rear earth containing hydrotalcite of high fluorescence of the present invention and preparation method thereof is described further, will helps understanding the present invention and advantage thereof with indefiniteness embodiment, and not as a limitation of the invention,
Embodiment 1.
Preparation contains 1.65 * 10
-2The NaAlO of mol
2With 1.65 * 10
-2The molNaOH aqueous solution (A); Preparation contains 1.0 * 10
-1The MgCl of mol
2The aqueous solution (B); Preparation contains 1.65 * 10
-2Mol sodium stearate, 0.825 * 10
-2The aqueous solution of mol oxine (C).Under violent stirring, simultaneously with solution (A) with (B) dropwise add (C) solution, with 20% aqueous sodium hydroxide solution conditioned reaction mixed serum to PH=11, in 80 ℃ of following ageings 12 hours, suction filtration, water washing filter Pie are to filtering PH=7 at night～8, with suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter Pie was dried 2 hours down in 105 ± 5 ℃, obtained the aluminized hydrotalcite sample (Al-LLDHS) of hyperfluorescence.With ultraviolet excitation, send oxine aluminium strong feature blue-greenish colour fluorescence (487nm), fluorescence intensity is 3.9 * 10
3(a.u.), fluorescence lifetime is 21.24ns, and quantum yield is 67%, and the fluorescence quantum yield that records pure oxine aluminium under with condition is 57%.
Embodiment 2.
Preparation contains 5.0 * 10
-3The NaAlO of mol
2With 5.0 * 10
-3The mol molNaOH aqueous solution (A); Preparation contains 1.0 * 10
-1The MgCl of mol
2The aqueous solution (B); Preparation contains 5.0 * 10
-3Mol 16 carbon fatty acid sodium, 0.25 * 10
-3The aqueous solution of mol oxine (C).Under the ultrasonic wave effect, simultaneously with solution (A) with (B) dropwise add (C) solution, with 20% aqueous sodium hydroxide solution conditioned reaction mixed serum to PH=11, in 80 ℃ of following ageings 12 hours, suction filtration, water washing filter Pie were to filtering PH=7 at night～8, with suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter Pie was dried 2 hours down in 105 ± 5 ℃, obtained the aluminized hydrotalcite sample (Al-LLDH of hyperfluorescence
S).With ultraviolet excitation, send oxine aluminium strong feature blue-greenish colour fluorescence (487nm), fluorescence intensity reaches 4.7 * 10
4(a.u.).
Embodiment 3.
Preparation contains 1.0 * 10
-2The NaAlO of mol
2With 1.0 * 10
-2The mol NaOH aqueous solution (A); Preparation contains 1.0 * 10
-1The MgCl of mol
2The aqueous solution (B); Preparation contains 1.0 * 10
-2Mol Sodium dodecylbenzene sulfonate, 0.5 * 10
-2The aqueous solution of mol oxine (C).Under the violent stirring of not stopping, simultaneously with solution (A) with (B) dropwise add (C) solution, with 20% aqueous sodium hydroxide solution conditioned reaction mixed serum to PH=11, in 80 ℃ of following ageings 12 hours, suction filtration, water washing filter Pie are to filtering PH=7 at night～8, with suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter Pie was dried 2 hours down in 105 ± 5 ℃, obtained the aluminized hydrotalcite sample (Al-LLDH of hyperfluorescence
S).With ultraviolet excitation, send oxine aluminium strong feature blue-greenish colour fluorescence (487nm), fluorescence intensity reaches 6.7 * 10
3(a.u.).
Embodiment 4.
Preparation contains 5.0 * 10
-3The NaAlO of mol
2With 5.0 * 10
-3The mol molNaOH aqueous solution (A); Preparation contains 1.0 * 10
-1The MgCl of mol
2The aqueous solution (B); Preparation contains 5.0 * 10
-3Mol tetradecacarbon fatty acid sodium, 0.25 * 10
-3The contract aqueous solution (C) of 8 quinolylamines ((DBSAQ)) of mol 3,5 Dibromosalicylaldehydes.Under the ultrasonic wave effect, simultaneously with solution (A) with (B) dropwise add (C) solution, with 20% aqueous sodium hydroxide solution conditioned reaction mixed serum to PH=11, in 80 ℃ of following ageings 12 hours, suction filtration, water washing filter Pie were to filtering PH=7 at night～8, with suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter Pie was dried 2 hours down in 105 ± 5 ℃, obtained the aluminized hydrotalcite sample (Al-LLDH of hyperfluorescence
S).With the 430nm ultraviolet excitation, send aluminium blue-fluorescence (535nm), fluorescence intensity reaches 1.1 * 10
4(a.u.).
Embodiment 5.
Preparation contains 5.0 * 10
-3The NaAlO of mol
2With 5.0 * 10
-3The mol molNaOH aqueous solution (A); Preparation contains 1.0 * 10
-1The MgCl of mol
2The aqueous solution (B); Preparation contains 5.0 * 10
-3Mol tetradecacarbon fatty acid sodium, 0.25 * 10
-3The alcohol-water mixing solutions (C) of mol chrome azurol S (CAS).Under the ultrasonic wave effect, simultaneously with solution (A) with (B) dropwise add (C) solution, with 20% aqueous sodium hydroxide solution conditioned reaction mixed serum to PH=11, in 80 ℃ of following ageings 12 hours, suction filtration, water washing filter Pie were to filtering PH=7 at night～8, with suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter Pie was dried 2 hours down in 105 ± 5 ℃, obtained the aluminized hydrotalcite sample (Al-LLDH of hyperfluorescence
S).With the 430nm ultraviolet excitation, send the fluorescence (620nm) that aluminium and chrome azurol S (CAS) complexing forms 1: 2 title complex, fluorescence intensity reaches 2.1 * 10
3(a.u.).
Embodiment 6.
Preparation contains 5.0 * 10
-3The NaAlO of mol
2With 5.0 * 10
-3The mol molNaOH aqueous solution (A); Preparation contains 1.0 * 10
-1The MgCl of mol
2The aqueous solution (B); Preparation contains 5.0 * 10
-3Mol 12 carbon fatty acid sodium, 0.25 * 10
-3The alcohol-water mixing solutions (C) of mol Quercetin (QCT Quercetin).Under the ultrasonic wave effect, simultaneously with solution (A) with (B) dropwise add (C) solution, with 20% aqueous sodium hydroxide solution conditioned reaction mixed serum to PH=11, in 80 ℃ of following ageings 12 hours, suction filtration, water washing filter Pie were to filtering PH=7 at night～8, with suction filtration behind a small amount of soaked in absolute ethyl alcohol, the washing precipitate, filter Pie was dried 2 hours down in 105 ± 5 ℃, obtained the aluminized hydrotalcite sample (Al-LLDH of hyperfluorescence
S).With the 365nm ultraviolet excitation, (490～500nm), fluorescence intensity reaches 7.4 * 10 to send the fluorescence of Quercetin aluminum complex
4(a.u.).
Claims (6)
1. a class has aluminized hydrotalcite of hyperfluorescence and preparation method thereof, it is characterized in that the aluminized hydrotalcite (Al-LLDHs) of described high fluorescence has following simplest formula:
[M
2+ 1-xAl
3+ x(OH)
-1 2]A
n- x/n?D
x/mzB]
M wherein
2+Be magnesium, zinc, copper, nickel divalent metal; Al
3+Be trivalent aluminium ion, be scattered in the divalent metal oxyhydroxide laminate of this houghite; OH
-1Be monovalence hydroxide radical anion, A
N-Be negatively charged ion or mixed anion, its flat fare n=1～2; D is part or mixed ligand, molten mixing in interlayer anion A
N-Among, and with laminate on Al
3+Coordination, its average coordination number m=2～3; B is the contained neutral molecule of houghite, and z is the neutral molecule number; X is Al
3+/ (M
2++ Al
3+) molar ratio; A
N-Be interlayer anion.
2. by described aluminized hydrotalcite of claim 1 and preparation method thereof with hyperfluorescence,, it is characterized in that Al
3+Content is in the 0.165-0.05 interval.
3. by described aluminized hydrotalcite of claim 1 and preparation method thereof, it is characterized in that D is oxine, 3,5 Dibromosalicylaldehydes contract 8 quinolylamines and 5 or 2 substitutive derivatives with hyperfluorescence; The beta-diketon class of methyl ethyl diketone or diphenylpropane-1,3-dione(DPPO); Schiff's base or two Schiff's base; Hydroxyanthraquinone, carbazole, porphyrin or derivatives thereof, Quercetin, morin, chrome azurol S or fluorone or its mixture.
4. by described aluminized hydrotalcite of claim 1 and preparation method thereof, it is characterized in that D is the molten in advance C of being mixed in hyperfluorescence
12-20Sodium soap, C
12-20Fat sodium sulfonate, C
0-12Alkylbenzoic acid sodium, C
0-12In sodium alkyl benzene sulfonate or sodium salicylate or its mixture, mix in interlayer anion A thereby part D is molten among the Al-LLDHs for preparing by coprecipitation method
N-Among, simultaneously with the divalent metal oxyhydroxide laminate that is scattered in houghite on Al
3+Coordination.
5. by described aluminized hydrotalcite of claim 1 and preparation method thereof, it is characterized in that wherein molten mixing in C with hyperfluorescence
12-20Sodium soap, C
12-20D content in fat sodium sulfonate, Sodium Benzoate, benzene sulfonic acid sodium salt, sodium salicylate or its mixture is trivalent aluminium ion (Al wherein
3+) molar content x 1/2nd to 1/3rd.
6. by described aluminized hydrotalcite of claim 1 and preparation method thereof, it is characterized in that Al-LLDHs implements preparation by coprecipitation method with hyperfluorescence.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449691A (en) * | 2014-10-21 | 2015-03-25 | 淄博职业学院 | Polyvinyl carbazole intercalated hydrotalcite fluorescent film and preparation method thereof |
| CN104556097A (en) * | 2015-01-14 | 2015-04-29 | 苏州大学 | Method for preparing hydrotalcite-like compounds and zeolites by using blast furnace slag |
| WO2016078220A1 (en) * | 2014-11-17 | 2016-05-26 | 京东方科技集团股份有限公司 | Blue light polarizing thin film and preparation method therefor, as well as blue light backlight source and liquid crystal display device |
| CN107022115A (en) * | 2017-05-10 | 2017-08-08 | 北京化工大学 | It is a kind of for intercalated houghite anti-ultraviolet ageing agent of rubber and preparation method thereof and application method |
-
2007
- 2007-12-14 CN CNA2007101440136A patent/CN101249974A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449691A (en) * | 2014-10-21 | 2015-03-25 | 淄博职业学院 | Polyvinyl carbazole intercalated hydrotalcite fluorescent film and preparation method thereof |
| WO2016078220A1 (en) * | 2014-11-17 | 2016-05-26 | 京东方科技集团股份有限公司 | Blue light polarizing thin film and preparation method therefor, as well as blue light backlight source and liquid crystal display device |
| CN104556097A (en) * | 2015-01-14 | 2015-04-29 | 苏州大学 | Method for preparing hydrotalcite-like compounds and zeolites by using blast furnace slag |
| CN107022115A (en) * | 2017-05-10 | 2017-08-08 | 北京化工大学 | It is a kind of for intercalated houghite anti-ultraviolet ageing agent of rubber and preparation method thereof and application method |
| CN107022115B (en) * | 2017-05-10 | 2019-08-13 | 北京化工大学 | A kind of intercalated houghite anti-ultraviolet ageing agent for rubber and preparation method thereof and application method |
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Open date: 20080827 |