CN106281301B - A kind of organic phosphoric acid zinc photochromic material and preparation method thereof - Google Patents
A kind of organic phosphoric acid zinc photochromic material and preparation method thereof Download PDFInfo
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- CN106281301B CN106281301B CN201610648624.3A CN201610648624A CN106281301B CN 106281301 B CN106281301 B CN 106281301B CN 201610648624 A CN201610648624 A CN 201610648624A CN 106281301 B CN106281301 B CN 106281301B
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- 239000000463 material Substances 0.000 title claims abstract description 42
- OXHXATNDTXVKAU-UHFFFAOYSA-N phosphoric acid zinc Chemical compound [Zn].OP(O)(O)=O OXHXATNDTXVKAU-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 16
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 15
- 239000010935 stainless steel Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 13
- 239000011574 phosphorus Substances 0.000 claims abstract description 13
- 229910001868 water Inorganic materials 0.000 claims abstract description 13
- 239000011701 zinc Substances 0.000 claims abstract description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000009415 formwork Methods 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000002447 crystallographic data Methods 0.000 claims abstract description 3
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 4
- 125000004437 phosphorous atom Chemical group 0.000 claims description 4
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 230000005588 protonation Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 125000000339 4-pyridyl group Chemical group N1=C([H])C([H])=C([*])C([H])=C1[H] 0.000 description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 150000007513 acids Chemical class 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 230000002441 reversible effect Effects 0.000 description 4
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical class [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 244000178870 Lavandula angustifolia Species 0.000 description 1
- 235000010663 Lavandula angustifolia Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004941 influx Effects 0.000 description 1
- 229910052816 inorganic phosphate Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 230000005945 translocation Effects 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/3804—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)] not used, see subgroups
- C07F9/3808—Acyclic saturated acids which can have further substituents on alkyl
-
- 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
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/188—Metal complexes of other metals not provided for in one of the previous groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to photochromic material and its preparing technical fields, it is related to a kind of organic phosphoric acid zinc photochromic material and preparation method thereof, zinc source, organic phosphorus sources, organic formwork agent and water are fitted into after mixing in the stainless steel high-pressure reaction vessel with ptfe autoclave, the good light yellow crystal of crystallinity is obtained within 5~8 days in 145-160 DEG C of crystallization；Gained light yellow crystal is successively through deionized water washing, suction filtration again, and is dried at room temperature for that organic phosphoric acid zinc photochromic material is prepared, and molecular formula is [H3TPT][Zn3(CH3C(O)(PO3)2)(CH3C(O)(PO3)2H)]·H2O, molecular weight 950.48, crystallographic data areZ=2, space group P-1；Preparation method is simple, easy to operate, at low cost, environmental-friendly, reproducible.
Description
Technical field：
The invention belongs to photochromic material and its preparing technical fields, are related to a kind of novel transition metal organic phosphate
Reversible color material and its preparation process, especially a kind of organic phosphoric acid zinc photochromic material and preparation method thereof.
Background technology：
Photochromic refers to the transformation of compound molecular structure under certain wavelength or intensity illumination effect, causes it to light
Absorption peak corresponding change, i.e. the variation of color.Photochromic material is meant by color can occur after light source activation
A kind of material of variation, because its reality or potential application in numerous areas such as anti-fake, storage, switching devices causes researcher pole
Big interest.Molecule base photochromic material has the function of structure controllability and the advantage of Scalability.Metal tripolyphosphate salt system
By researcher extensive concern and deeply probe into, to metal tripolyphosphate salt system introduce suitable short of electricity subbase group contribute to it is photic
The preparation of off-color material.Metal tripolyphosphate salt system, can be to conduct under illumination or other shooting conditions as electron donor
The group of electron deficient receptor transmits electronics, and Intramolecular electron transfer occurs, induces the generation of photochromic behavior.
So far, phosphorus source is mostly Phos (phosphoric acid or phosphorous acid) in the metal phosphate reported, organic phosphoric acid
Study it is relatively fewer, this is because：On the one hand, compared to inorganic phosphate, the component more diversification of organic phosphoric acid, and easy function
Dough is convenient for the regulation and control of material structure, and metal-organophosphorus acid investigation of materials, which is more conducive to, obtains novel molecular base photolytic activity material
Material；On the other hand, the reasonable selection of electron acceptor and introducing are the key that photochromic material is constructed.To metal tripolyphosphate salt system
It is middle to introduce more pyridine organic groups, it will help the preparation of photochromic material.2,4,6- tri- (4- pyridyl groups) -1,3,5- triazines
With more pyridine groups and short of electricity subbase group, it is expected to be used for constructing for photochromic material.Therefore, a kind of organic phosphoric acid zinc of demand
It is photochromic to construct molecule base by selecting suitable electron donor and electron acceptor for photochromic material and preparation method thereof
Material, by organic phosphoric acid (electron donor) and more pyridine ligands 2,4,6- tri- (4- pyridyl groups) -1,3,5-triazines (electronics by
Body) and source metal assembling research, design and prepare the photochromic new material of an example molecule base.
Invention content：
Present invention aims to overcome that disadvantage of the existing technology, seeks design and provides a kind of organic phosphoric acid zinc light-induced variable
Color material and preparation method thereof, by 1-hydroxy ethylidene-1,1-diphosphonic acid (electron donor), 2,4,6- tri- (4- pyridyl groups) -1,3,5- tri-
The assembling of piperazine (electron acceptor) and zinc oxide is studied, and the photochromic crystalline material with quick effect is prepared, and is realized and is divided
Subbase photochromic material is constructed, and guidance is provided for the design synthesis and application study of such material.
To achieve the goals above, organic phosphoric acid zinc photochromic material of the present invention has two-dimensional layered structure,
Middle zinc atom has two kinds of coordination modes of four-coordination and hexa-coordinate, and each phosphorus atoms and three oxygen of surrounding on organophosphor are matched
Position, organophosphor replaces with zinc atom connects and composes two-dimensional layered structure, the active force that organic amine molecule of protonation passes through hydrogen bond
Between the layers, molecular formula is [H for filling3TPT][Zn3(CH3C(O)(PO3)2)(CH3C(O)(PO3)2H)]·H2O, molecule
Amount is 950.48, and crystallographic data is
Z=2, space group P-1.
The detailed process that the present invention prepares organic phosphoric acid zinc photochromic material is：
(1), zinc source, organic phosphorus sources, organic formwork agent and water are uniformly mixed and obtain mixture, wherein organic phosphorus sources and zinc
The molar ratio in source is 0.63：1, the molar ratio of organic formwork agent and phosphorus source is 0.24：1, the molar ratio of organic formwork agent and zinc source
It is 0.15：1, the molar ratio of water and phosphorus source is 49：1.
(2), the mixture for obtaining step (1) is packed into the stainless steel high-pressure reaction vessel with ptfe autoclave
In, obtain within 5~8 days the good light yellow crystal of crystallinity in 145-160 DEG C of crystallization；
(3), it by light yellow crystal obtained by step (2) successively through deionized water washing, suction filtration, and is dried at room temperature for, i.e.,
Organic phosphoric acid zinc photochromic material is prepared.
Zinc source of the present invention is zinc oxide；Organic phosphorus sources are 1-hydroxy ethylidene-1,1-diphosphonic acid；Organic formwork agent is 2,4,6-
Three (4- pyridyl groups) -1,3,5- triazines；The volume of stainless steel high-pressure reaction vessel is 25mL or 30mL.
Compared with prior art, the present invention preparing a kind of organophosphor with ability of reverse photochromism performance having not been reported
Color occurs for sour zinc photochromic material, photochromic material 5min after visible light or 325nm ultra violet lamps by yellowish
Color to purple transformation；And purple takes off after the crystal for translating into purple heats 30min in 90 DEG C of baking ovens, is returned to light
Yellow, and crystal shape is kept not to be changed, fatigue resistance is good；Preparation method is simple, easy to operate, at low cost, environment
Close friend, it is reproducible.
Description of the drawings：
Fig. 1 is that the coordination environment of zinc atom and phosphorus atoms shows in organic phosphoric acid zinc photochromic material crystal of the present invention
It is intended to.
Fig. 2 is two that organic phosphoric acid zinc photochromic material of the present invention is total to that oxygen is formed by connecting by phosphorus atoms and zinc atom
Tie up layer structure figure.
Fig. 3 is accumulation graph of the organic phosphoric acid zinc photochromic material of the present invention in ac planes, wherein what is protonated has
Machine amine is filled between the layers by the active force of hydrogen bond.
Fig. 4 is the infrared spectrogram of organic phosphoric acid zinc photochromic material of the present invention.
Fig. 5 is the XRD spectra and monocrystalline fitting spectrogram of organic phosphoric acid zinc photochromic material powder of the present invention, wherein
Experimental indicates that XRD spectra, simulated indicate that monocrystalline is fitted spectrogram.
Fig. 6 is the epr signal figure of organic phosphoric acid zinc photochromic material of the present invention under ultraviolet light.
Fig. 7 is the faint yellow sample (above) of organic phosphoric acid zinc photochromic material for preparing of the present invention in visible light or ultraviolet
Become deep ultraviolet (lower left figure), lavender (lower right figure) under light irradiation.
Specific implementation mode：
The invention will be further described by way of example and in conjunction with the accompanying drawings.
Embodiment 1：
0.08g zinc oxide and 0.05g 2,4,6- tri- (4- pyridyl groups) -1,3,5- triazines are added to 25mL by the present embodiment
0.15ml 1-hydroxy ethylene-1,1-diphosphonics are added after stirring 15min to use 5mL water dissolutions in the stainless steel cauldron of lining in polytetrafluoroethylene (PTFE)
Acid continues stirring 2 hours at room temperature, forms uniform reaction solution, then seals the stainless steel cauldron equipped with reaction solution,
Crystallization 7 days in 160 DEG C of baking oven wait that stainless steel cauldron is taken out natural cooling at room temperature after the completion of reacting, will be stainless
The crystal generated in steel reaction kettle is removed and is cleaned repeatedly with deionized water 5 times, and drying at room temperature obtains faint yellow flat crystal,
As organic phosphoric acid zinc photochromic material.
The present embodiment carries out monocrystalline experiment to obtained faint yellow flat crystal, and experiment proves, in the ultraviolet light and heats of 325nm
The reversible transformation of color can be realized under disposition, and monocrystalline keeps shape and crystallinity constant in colourshifting process, this
Organic phosphoric acid zinc photochromic material prepared by the embodiment color presentation before illumination is faint yellow, under the irradiation of ultraviolet light,
Maximum absorption wavelength changes, and color gradually becomes purple；When being heated to 90 DEG C, the color of monocrystalline is changed into yellowish again
The mechanism of color, discoloration is under the irradiation of 325nm ultraviolet lights, and the electron acceptor of protonation obtains electronics shape from electron donor
At 2,4,6- tri- (4- pyridyl groups) -1,3,5-triazines free radicals, make its influx and translocation at ultraviolet light 325nm, purple is presented.
Compound monocrystal has reversible photochromic behavior with ultra violet lamp in distilled water in air, and has good thermostabilization
Property.
Embodiment 2：
0.10g zinc oxide is added in the stainless steel cauldron that 25mL polytetrafluoroethylene (PTFE) is lining by the present embodiment, to not
The steel reaction kettle that becomes rusty is interior to be added 5mL water and 0.18ml 1-hydroxy ethylidene-1,1-diphosphonic acids, stirs 20 minutes at room temperature, after forming uniform solution
Above-mentioned solution is added in 0.08g 2,4,6- tri- (4- pyridyl groups) -1,3,5-triazines, is put after finally sealing stainless steel cauldron
It is reacted 6 days into 160 DEG C of baking ovens, obtains faint yellow flat crystal, by cooling down, being filtered, washed and dried in such as embodiment 1
Method, obtain target product items characterization and result it is same as Example 1.
Embodiment 3：
0.08g zinc oxide is added in the stainless steel cauldron that 30mL polytetrafluoroethylene (PTFE) is lining by the present embodiment, then
5mL water, 0.15ml 1-hydroxy ethylidene-1,1-diphosphonic acids and 0.05g 2,4,6- tri- (4- pyridyl groups) -1,3,5-triazines is added and stirs 1.5h,
Finally the stainless steel cauldron equipped with reaction solution is sealed, crystallization obtains faint yellow flake crystalline in 145 DEG C of baking oven after 8 days
Body, by method that is cooling in such as embodiment 1, being filtered, washed and dried, obtained target product items characterization and result and reality
It is identical to apply example 1.
Embodiment 4：
0.08g zinc oxide is added to the polytetrafluoroethyl-ne alkene reaction equipped with 4mL water, 1mL methanol mixed solutions by the present embodiment
It in kettle, stirs 30 minutes at room temperature, reactant adds 0.15ml 1-hydroxy ethylidene-1,1-diphosphonic acids and stirs 30 minutes after mixing, connects
It addition 0.05g 2,4,6- tri- (4- pyridyl groups) -1,3,5-triazines and continues stirring 1~1.5 hour, by polytetrafluoroethyl-ne alkene reaction
Kettle is fitted into stainless steel high-pressure reaction vessel and seals, and crystallization obtains faint yellow flat crystal in 7 days at 155 DEG C, by such as embodiment 1
Middle cooling, the method being filtered, washed and dried, obtained target product items characterization and result are same as Example 1.
Embodiment 5：
0.12g zinc oxide is added in the stainless steel cauldron that 30mL polytetrafluoroethylene (PTFE) is lining by the present embodiment, then
4.5mL water, 0.20ml 1-hydroxy ethylidene-1,1-diphosphonic acids and 0.06g 2,4,6- tri- (4- pyridyl groups) -1,3,5-triazines is added and stirs 2h,
Finally the stainless steel cauldron equipped with reaction solution is sealed, crystallization obtains faint yellow flake crystalline in 145 DEG C of baking oven after 7 days
Body, by method that is cooling in such as embodiment 1, being filtered, washed and dried, obtained target product items characterization and result and reality
It is identical to apply example 1.
Claims (1)
1. a kind of preparation method of organic phosphoric acid zinc photochromic material, it is characterised in that specifically preparation process is：
(1), zinc source, organic phosphorus sources, organic formwork agent and water are uniformly mixed and obtain mixture, wherein organic phosphorus sources and zinc source
Molar ratio is 0.63：1, the molar ratio of organic formwork agent and phosphorus source is 0.24：1, organic formwork agent and the molar ratio in zinc source are
0.15：1, the molar ratio of water and phosphorus source is 49：1；
(2), the mixture that step (1) obtains is fitted into the stainless steel high-pressure reaction vessel with ptfe autoclave,
145-160 DEG C of crystallization obtains the good light yellow crystal of crystallinity for 5~8 days；
(3), it by light yellow crystal obtained by step (2) successively through deionized water washing, suction filtration, and is dried at room temperature for, that is, prepares
Obtain organic phosphoric acid zinc photochromic material；
The zinc atom for the organic phosphoric acid zinc photochromic material being prepared has two kinds of coordination modes of four-coordination and hexa-coordinate, organic
Each phosphorus atoms and three oxygen of surrounding on phosphorus are coordinated, and organophosphor replaces with zinc atom connects and composes two-dimensional layered structure,
Organic amine molecule of protonation is filled between the layers by the active force of hydrogen bond, and molecular formula is [H3TPT][Zn3(CH3C
(O)(PO3)2)(CH3C(O)(PO3)2H)]·H2O, molecular weight 950.48, crystallographic data are Z=2, space group are
P-1；
The zinc source is zinc oxide；Organic phosphorus sources are 1-hydroxy ethylidene-1,1-diphosphonic acid；Organic formwork agent TPT is (the 4- pyrroles of 2,4,6- tri-
Piperidinyl) -1,3,5- triazines；The volume of stainless steel high-pressure reaction vessel is 25mL or 30mL.
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| CN108409783B (en) * | 2018-03-08 | 2020-05-29 | 青岛大学 | Long-chain flexible fatty amine-guided organic cobalt phosphonate material and preparation method thereof |
| CN108690056B (en) * | 2018-06-26 | 2020-12-29 | 青岛大学 | Photochromic material with quick response time and wide response range and preparation method thereof |
| CN109336913B (en) * | 2018-10-12 | 2021-01-15 | 青岛大学 | Electron transfer type hybrid photochromic material and preparation method thereof |
| CN111116615B (en) * | 2019-10-18 | 2023-08-18 | 青岛大学 | Metal phosphonate material with room temperature demagnetizing effect and preparation method thereof |
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