CN104086603A - Structure and preparation method of imidazole modified phosphotungstate compound - Google Patents

Structure and preparation method of imidazole modified phosphotungstate compound Download PDF

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CN104086603A
CN104086603A CN201410319723.8A CN201410319723A CN104086603A CN 104086603 A CN104086603 A CN 104086603A CN 201410319723 A CN201410319723 A CN 201410319723A CN 104086603 A CN104086603 A CN 104086603A
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himi
equal
compound
imidazoles
modified
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杨艳艳
曲小姝
娄大伟
赵文卓
罗亚楠
于丽颖
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Jilin Institute of Chemical Technology
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Jilin Institute of Chemical Technology
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Abstract

The invention discloses a monocrystalline structure and a preparation method of an imidazole modified phosphotungstate compound and relates to the field of inorganic chemistry. The crystal has the chemical formula of [Na2(Himi)2(H2O)2](Himi)2[P2W18O62].6H2O(imi= C3N2H4; Himi= C3N2H5),C12N8H32Na2P2W18O70, has the molecular weight of 4845.6, has the space group of P-1 and belongs to a triclinic system, wherein a is equal to 1.41164(10)nm, b is equal to 1.48792(11)nm, c is equal to 2.26166(17)nm, alpha is equal to 72.1320(10) degrees, beta is equal to 81.3340(10) degrees, gamma is equal to 62.5800(10) degrees, V is equal to 4.013(5)nm<3>, Z is equal to 2, F(000) is equal to 4144, R1 is equal to 0.00955, and wR2 is equal to 0.1872. The crystal is prepared by adopting a normal-temperature aqueous solution synthesis method; the prepared compound is clear in composition and structure and has a potential drug application value.

Description

Suanphosphotungstate compound structure and preparation method that a kind of imidazoles is modified
Technical field
The invention belongs to inorganic polyacid technical field of chemistry, relate to the synthetic of Dawson structure Suanphosphotungstate compound that benzotriazole modifies, say so more specifically [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) preparation method and the structure of compound.
Background technology
In recent years, polyoxometalates has received concern [1-2] in the application prospect aspect material, catalysis and medicine, and it is one of them very active research field that organic molecule is modified polyacid compound.Because molybdenum atom in silicomolybdate has variable oxidation state, also have variable coordination configuration, this make it have various just more with potential function, for example: ion-exchange, absorption, pharmaceutical chemistry and catalysis etc.
Imidazoles is a kind of important fine chemical material, is mainly used in the solidifying agent of the synthetic and epoxy resin of medicine and agricultural chemicals.In medicine, for imidazoles antifungal drug, be miconazole, econazole, KETOKONAZOL, one of main raw material of the medicines such as clotrimazole, is also widely used for the sanitas of fruit.As epoxy curing agent, as the rust-preventive agent of copper, medicine, pesticide material, also as raw material and the organic synthesis intermediate of urea formaldehyde resin curing agent, photography medicine, tackiness agent, coating, vulcanizer, antistatic agent etc.
Synthesize a Suanphosphotungstate compound [Na that imidazoles is modified herein 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5), by ultimate analysis, infrared spectra and X-diffraction single crystal structure characterize this compound.This compound composition is clear and definite, has potential drug value.
Reference.
[1]?Gumez-Garcia?C.?J.,?Ouahab?L.,?Gimene-?Saiz?C.?et?al?.?.?Angew.?Chem.?Int.?Ed.?Engl.?[J],?1994,?33:?223。
[2]?Judd?D.?A.,?Nettles?J.?H.,?Nevins?N.?et?al.?.?J.?Am.?Chem.?Soc.?[J]?,2001,?123:?886。
Summary of the invention
The present invention relates to [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) (1) compound crystal structure.
The present invention relates to [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) preparation method of (1) compound crystal, the research of take off data and data.
The present invention relates to [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) application of (1) compound aspect medicine.
For achieving the above object, the invention provides following technical scheme:
There is the Suanphosphotungstate compound of the imidazoles modification of following chemical general formula: [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) (1)
The silicomolybdate compound that morpholine of the present invention is modified, wherein monocrystalline is collected with Bruker Smart CCD Apex (II) diffractometer, adopts Mo-K α (λ=0.71073), room temperature 293 (2) K.Use SHELX 97 programs to resolve and revise crystalline structure by direct method and complete matrix method of least squares.Record main crystal data as follows: molecular formula is C 12n 8h 32na 2p 2w 18o 70, molecular weight 4845.6, crystal belongs to triclinic(crystalline)system, p-1spacer, a=1.41164 (10) nm, b=1.48792 (11) nm, c=2.26166 (17) nm, α=72.1320 (10) °, β=81.3340 (10) °, γ=62.5800 (10) °, v=4.013 (5) nm 3, z=2, f(000)=4144, r 1 =0.00955, wR 2 =0.1872.
The present invention further discloses [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) preparation method of compound: get 0.17g K 6p 2w 18o 62material dissolution, in the NaAc-HAc buffered soln of 20 mL pH=4.50, in the situation that continuing to stir, drips 1 mL NiSO 4solution (1 mol/L), adds 0.05g imidazoles, adds 0.5gNaCI solid, and solution presents light green, without precipitation, stops stirring static crystallization.
Brief description of the drawings
Fig. 1 is [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) molecular structure of (1) compound.
Fig. 2 is [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) accumulation graph of (1) compound.
Embodiment
Silicomolybdate compound [the Na that a kind of imidazoles is modified 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) (1) and preparation method thereof and condition: get 0.17g K 6p 2w 18o 62material dissolution, in the NaAc-HAc buffered soln of 20 mL pH=4.50, in the situation that continuing to stir, drips 1 mL NiSO 4solution (1 mol/L), adds 0.05g imidazoles, adds 0.5gNaCI solid, and solution presents light green, without precipitation, stops stirring static crystallization.After one day, grow green bulk crystals.This crystal records its structure by X-single crystal diffractometer and corresponding software.At compound [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) comprise [P in the crystal of (1) 2w 18o 62] 6-negatively charged ion, (Hmorph) +positively charged ion, Na +positively charged ion and 2 crystal water molecules, (Hmorph) +positively charged ion, Na +positively charged ion and crystal water molecule interconnect by electrostatic force and hydrogen bond.
Compound [Na 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) 1089.6,960.0,912.8 and 785.1cm -1the strong absorption peak at place is Dawson structure [P 2w 18o 62] 6-the charateristic avsorption band of negatively charged ion, pointed out respectively for ν as(W-O t), ν as(W-O b-W), ν as(P-O a) and ν as(W-O c-W). at 1635.3 cm -1with 1585.4 cm -1the strong absorption peak at place belongs to protonated imidazole molecule stretching vibration peak.
Embodiment
Get 0.17g K 6p 2w 18o 62material dissolution, in the NaAc-HAc buffered soln of 20 mL pH=4.50, in the situation that continuing to stir, drips 1 mL NiSO 4solution (1 mol/L), adds 0.05g imidazoles, adds 0.5gNaCI solid, and solution presents light green, without precipitation, stops stirring static crystallization.

Claims (4)

1. the Suanphosphotungstate compound [Na that imidazoles is modified 2(Himi) 2(H 2o) 2] (Himi) 2[P 2w 18o 62] 6H 2o (imi=C 3n 2h 4; Himi=C 3n 2h 5) preparation and structure.
2. a monocrystalline for the Suanphosphotungstate compound that imidazoles claimed in claim 1 is modified, is characterized in that: molecular formula is C 12n 8h 32na 2p 2w 18o 70, molecular weight 4845.6, crystal belongs to triclinic(crystalline)system, p-1spacer, a=1.41164 (10) nm, b=1.48792 (11) nm, c=2.26166 (17) nm, α=72.1320 (10) °, β=81.3340 (10) °, γ=62.5800 (10) °, v=4.013 (5) nm 3, z=2, f(000)=4144, r 1 =0.00955, wR 2 =0.1872.
3. the method for the Suanphosphotungstate compound that described in claim 1, imidazoles is modified, is characterized in that: get 0.17g K 6p 2w 18o 62material dissolution, in the NaAc-HAc buffered soln of 20 mL pH=4.50, in the situation that continuing to stir, drips 1 mL NiSO 4solution (1 mol/L), adds 0.05g imidazoles, adds 0.5gNaCI solid, and solution presents light green, without precipitation, stops stirring static crystallization.
4. the Suanphosphotungstate compound that described in claim 1, imidazoles is modified is prepared the application aspect medicine.
CN201410319723.8A 2014-07-08 2014-07-08 Structure and preparation method of imidazole modified phosphotungstate compound Pending CN104086603A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105080608A (en) * 2014-05-06 2015-11-25 东北师范大学 Application of novel polyacid catalyst in cellulose hydrolyzation
CN107141259A (en) * 2017-05-12 2017-09-08 昆明学院 A kind of imidazoles with many wolframic acid cocrystallization super molecular compounds and preparation method thereof
CN110423252A (en) * 2019-06-25 2019-11-08 扬州大学 Krebs type polyacid compound and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
杨艳艳: "Na2(Himi)2(H2O)2](Himi)2[P2W18O62]• 6H2O的合成与晶体结构", 《吉林化工学院学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105080608A (en) * 2014-05-06 2015-11-25 东北师范大学 Application of novel polyacid catalyst in cellulose hydrolyzation
CN105080608B (en) * 2014-05-06 2018-02-23 东北师范大学 A kind of application of more acid catalysts in cellulose hydrolysis
CN107141259A (en) * 2017-05-12 2017-09-08 昆明学院 A kind of imidazoles with many wolframic acid cocrystallization super molecular compounds and preparation method thereof
CN110423252A (en) * 2019-06-25 2019-11-08 扬州大学 Krebs type polyacid compound and preparation method thereof

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Application publication date: 20141008