CN1566260A - Photochromic nitrate type hydrotalcite and method for producing the same - Google Patents

Photochromic nitrate type hydrotalcite and method for producing the same Download PDF

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Publication number
CN1566260A
CN1566260A CN03148426.3A CN03148426A CN1566260A CN 1566260 A CN1566260 A CN 1566260A CN 03148426 A CN03148426 A CN 03148426A CN 1566260 A CN1566260 A CN 1566260A
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CN
China
Prior art keywords
hydrotalcite
metal ion
nitrate
divalent
photochromic
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Pending
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CN03148426.3A
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Chinese (zh)
Inventor
段雪
周彤
王戈
王治强
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Priority to CN03148426.3A priority Critical patent/CN1566260A/en
Priority to PCT/CN2003/000615 priority patent/WO2005002724A1/en
Priority to AU2003248228A priority patent/AU2003248228A1/en
Publication of CN1566260A publication Critical patent/CN1566260A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/028—Beta-aluminas
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
    • C09K9/02—Organic tenebrescent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/007—Mixed salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/75—Cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/755—Nickel
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/20—Two-dimensional structures
    • C01P2002/22—Two-dimensional structures layered hydroxide-type, e.g. of the hydrotalcite-type
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)

Abstract

The invention relates to a photochromic nitrate type hydrotalcite and method for producing the same, wherein a laminate containing bivalent transient metal is used the main body to introduce the nitrate anion foreign body into the interlamination, thus obtaining the hydrotalcite whose interlaminar anion is nitrate anion, its constitutional formula is M2+[1-x]M3+[x]NO3-[x]*mH2O, wherein 0.1<=x<=0.33, m=3-6.

Description

A kind of nitrate radical type hydrotalcite and preparation method thereof with photochromic characteristic
Affiliated field: the present invention relates to a kind of nitrate radical intercalated houghite and preparation method thereof with photochromic characteristic.
Background technology: document H.Tagaya, S.Sato, T.Kuwahara, J.Kadokawa, K.Masa and K.Chiba, J.Mater.Chem., 1994,4,1907 and T.Kuwahara, H.Tagaya and K.Chiba, Microporous Mater.1995,4,247, all adopt ion exchange method, based on magnesium aluminum-hydrotalcite, the organic photochromic species are introduced interlayer, preparation inorganic-organic hybridization photochromic material.The weak point of this kind method is: hydrotalcite is just as the solid media that improves organic photochromic material in this material, it does not participate in photochromic in essence, and be subjected to the photosensitive property of intercalation object self, the influence of factor such as electrically charged and ion configuration.
From (S.Miyata in 1975, Clays and Clay minerals, 1975,23,369) report of the hydrotalcite of the synthetic magnalium nitrate radical type of coprecipitation method is just arranged, the also synthetic peroxy-nitric acid root type hydrotalcite of the investigator in most thereafter hydrotalcites field, and these work just with the hydrotalcite of nitrate radical type as precursor, it is the bigger anionic intercalated houghite of volume that method by ion-exchange obtains interlayer, and the hydrotalcite of nitrate radical type is not the purpose product.Gianni A.Caravaggio, Christian Detellier and Zbigniew Wronski, J.Mater.Chem., 2001,11,912, adopt coprecipitation method to synthesize the nickel aluminium nitrate radical type hydrotalcite of different nickel aluminum ratios and studied its chemical property, but do not relate to photochromic characteristic as cell positive material.
Summary of the invention: the present invention directly is matrix with the hydrotalcite, and the molecule Modulatory character and the intercalation that are had according to hydrotalcite itself carry out molecular designing, prepare a kind of photochromic material with specific photosensitive property.Thereby this material is subjected to uv-radiation and laminate divalent transition metal element generation coordination with the interlayer anion nitrate radical and follow transfer transport to produce photochromism, overcome traditional photochromic material and be confined to a certain photosensitive property, can realize that photo-thermal is reversible, and be free of contamination inorganic-the inorganic hybridization system.
This photochromic material is that interlayer anion is the hydrotalcite of nitrate radical, and be laminate structure: its structural formula is:
[M 2+ 1-xM 3+ x]NO 3x -·mH 2O，
0.1≤x≤0.33 wherein, m=3-6 is an interlayer crystal water molecule number,
M 2+Representing divalent-metal ion, can be Ni 2+, Co 2+Or Fe 2+Any, M 2+Preferred Ni 2+
M 3+Representing trivalent metal ion, can be Co 3+, Fe 3+, Al 3+Or Ga 3+Any, M 3+Preferred Al 3+
This hydrotalcite has photochromic properties, and promptly when high voltage mercury lamp radiation 10-60 minute that uses 200W-1000W, the color of hydrotalcite changed, and after 60-100 ℃ of heating, color restoration, and this photo-thermal process is reversible.
This nitrate radical type hydrotalcite prepares with method once,
A. prepare the mixing solutions of solubility divalent metal nitrate and solubility trivalent metal nitrate, wherein divalent-metal ion concentration is 0.2-1.2M, and divalence, trivalent metal ion mol ratio are 2-4: 1; Divalent-metal ion can be Ni 2+, Co 2+Or Fe 2+Any, preferred Ni 2+Trivalent metal ion can be Co 3+, Fe 3+, Al 3+Or Ga 3+Any one, preferred Al 3+
B. compound concentration is NaOH or the KOH alkaline solution of 1.0-4.0M;
C. the nitrate mixed solution with the steps A preparation is added drop-wise in the alkaline solution of step B preparation lentamente, and vigorous stirring is 8-10 until the pH scope, drip to finish, 50 ℃-90 ℃ crystallization 12-70 hour, filter, wash neutrality, 60 ℃ of-100 ℃ of dryings 24 hours obtain nitrate radical type hydrotalcite.
The hydrotalcite that obtains is carried out XRD, IR, elemental analysis demonstration, and nitrate radical is the unique negatively charged ion of interlayer.
Above-mentioned hydrotalcite is placed down irradiation 10-60 minute of high voltage mercury lamp under the 200W-1000W, and the color of hydrotalcite changes, and solid violet is characterized by the increase of optical density outward, and after 60-100 ℃ of heating, color restoration, and this photo-thermal process is reversible.
Advantage of the present invention is:
1. synthesized hydrotalcite first with photochromic characteristic;
2. the preparation method's technology that is adopted is simple, and cost is low, and reaction is easy to carry out;
3. kind and the mol ratio by divalence and trivalent metal ion in the control solution, the photochromic properties of adjustable hydrotalcite.
Laminate contain the nitrate radical type hydrotalcite of transition metal be a kind of inorganic-the inorganic composite photochromic material, more traditional organic or inorganic one organic photochromic material prepares simple and pollution-free.
Embodiment: embodiment 1:
Steps A: with the solid Ni (NO of 21.76g (0.1mol) 3) 26H 2Solid Al (the NO of O and 14g (0.05mol) 3) 39H 2O is dissolved in the 100ml water.
Step B: 12gNaOH is dissolved in the alkaline solution that is made into 3.0M in the 100ml water.
Step C: vigorous stirring on one side, on one side salts solution is slowly dropped in the alkaline solution, regulating pH=9 and drip and finish, 65 ℃ of crystallization 24h filter, wash to the pH value and are about 7,65 ℃ of dry 24h, obtain nickel aluminium nitrate radical type hydrotalcite material.
By XRD spectra, IR spectrogram and ultimate analysis as can be known, the hydrotalcite layers negatively charged ion that obtains is a nitrate radical all, is the LDHs material that a kind of crystalline phase is single, structure is consistent.
Place the high voltage mercury lamp of 250W to shine 20 minutes down this LDHs, its color is by the light blue Dark grey that becomes, and through 65 ℃ of heating for some time, it is light blue that color reverts to again, and this process is reversible.
Embodiment 2:
Steps A: with the solid Co (NO of 11.64g (0.04mol) 3) 26H 2Solid Al (the NO of O and 7.5g (0.02mol) 3) 39H 2O is dissolved in the 100ml water.
Step B: 8gNaOH is dissolved in the alkaline solution that is made into 2.0M in the 100ml water.
Step C: vigorous stirring on one side, on one side salts solution is slowly dropped in the alkaline solution, regulating pH=8 and drip and finish, 80 ℃ of crystallization 24h filter, wash to the pH value and are about 7,80 ℃ of dry 24h, obtain cobalt aluminium nitrate radical type hydrotalcite material.
By XRD spectra, IR spectrogram and ultimate analysis as can be known, the hydrotalcite layers negatively charged ion that obtains is a nitrate radical all, is the LDHs material that a kind of crystalline phase is single, structure is consistent.
Place the high voltage mercury lamp of 500W to shine 30 minutes down this product, its color becomes light red by pink colour, and this process photo-thermal is reversible.

Claims (4)

1. nitrate radical type hydrotalcite with photochromic characteristic, it is a laminate structure, it is characterized in that structural formula is:
[M 2+ 1-xM 3+ x]NO 3 - x·mH 2O，
0.1≤x≤0.33 wherein, m=3-6 is an interlayer crystal water molecule number, M 2+Representing divalent-metal ion, can be Ni 2+, Co 2+Or Fe 2+Any; M 3+Representing trivalent metal ion, can be Co 3+, Fe 3+, Al 3+Or Ga 3+Any;
This hydrotalcite has photochromic properties, and promptly when high voltage mercury lamp radiation 10-60 minute that uses 200W-1000W, the color of hydrotalcite changed, and after 60-100 ℃ of heating, color restoration, and this photo-thermal process is reversible.
2. the nitrate radical type hydrotalcite with photochromic characteristic according to claim 1 is characterized in that divalent metal is from M 2+Preferred Ni 2+, trivalent metal ion M 3+Preferred Al 3+
3. preparation method with nitrate radical type hydrotalcite of photochromic characteristic, its preparation process is as follows:
A. prepare the mixing solutions of solubility divalent metal nitrate and solubility trivalent metal nitrate, wherein divalent-metal ion concentration is 0.2-1.2M, and divalence, trivalent metal ion mol ratio are 2-4: 1; Divalent-metal ion can be Ni 2+, Co 2+Or Fe 2+Any, trivalent metal ion can be Co 3+, Fe 3+, Al 3+Or Ga 3+Any one;
B. compound concentration is NaOH or the KOH alkaline solution of 1.0-4.0M;
C. the nitrate mixed solution with the steps A preparation is added drop-wise in the alkaline solution of step B preparation lentamente, and vigorous stirring is 8-10 until the pH scope, drip to finish, 50 ℃-90 ℃ crystallization 12-70 hour, filter, wash neutrality, 60 ℃ of-100 ℃ of dryings 24 hours obtain nitrate radical type hydrotalcite.
4. the preparation method with nitrate radical type neatly of photochromic characteristic according to claim 3 is characterized in that divalent metal is from Ni 2+, the preferred Al of trivalent metal ion 3+
CN03148426.3A 2003-07-01 2003-07-01 Photochromic nitrate type hydrotalcite and method for producing the same Pending CN1566260A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN03148426.3A CN1566260A (en) 2003-07-01 2003-07-01 Photochromic nitrate type hydrotalcite and method for producing the same
PCT/CN2003/000615 WO2005002724A1 (en) 2003-07-01 2003-08-01 The nitrate radical-type hidrotalcite with photochronism and the process for preparing it
AU2003248228A AU2003248228A1 (en) 2003-07-01 2003-08-01 The nitrate radical-type hidrotalcite with photochronism and the process for preparing it

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CN03148426.3A CN1566260A (en) 2003-07-01 2003-07-01 Photochromic nitrate type hydrotalcite and method for producing the same

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100382886C (en) * 2005-05-26 2008-04-23 天津大学 Adsorption material for removing copper and lead from plant medicine and preparation method thereof
CN100463858C (en) * 2006-04-12 2009-02-25 北京化工大学 Ultra-hydrophobic lamellar dihydroxyl composite metal oxide thin film and preparing method thereof
CN107651712A (en) * 2017-09-13 2018-02-02 太原理工大学 It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105688212A (en) * 2016-03-03 2016-06-22 北京化工大学 Compound with bimodule imaging and synergy therapy functions and preparing method thereof
CN110755617B (en) * 2019-11-27 2021-11-02 东华大学 Layered double hydroxide nano drug-loaded compound and preparation and application thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4843168A (en) * 1987-12-22 1989-06-27 Amoco Corporation Catalysis using pillared hydrotalcites
GB9512727D0 (en) * 1995-06-22 1995-08-23 Bp Chem Int Ltd Synthesis of glycol ethers

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100382886C (en) * 2005-05-26 2008-04-23 天津大学 Adsorption material for removing copper and lead from plant medicine and preparation method thereof
CN100463858C (en) * 2006-04-12 2009-02-25 北京化工大学 Ultra-hydrophobic lamellar dihydroxyl composite metal oxide thin film and preparing method thereof
CN107651712A (en) * 2017-09-13 2018-02-02 太原理工大学 It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs
CN107651712B (en) * 2017-09-13 2019-06-18 太原理工大学 It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs

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