CN104230994A - Benzotriazole and chromium modified polyacid compound structure and preparation method thereof - Google Patents

Benzotriazole and chromium modified polyacid compound structure and preparation method thereof Download PDF

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CN104230994A
CN104230994A CN201410444955.6A CN201410444955A CN104230994A CN 104230994 A CN104230994 A CN 104230994A CN 201410444955 A CN201410444955 A CN 201410444955A CN 104230994 A CN104230994 A CN 104230994A
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benzotriazole
equal
bta
crystal
compound
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CN104230994B (en
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杨艳艳
谭乃迪
曲小姝
于丽颖
赵文卓
张苗苗
冯素阳
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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 relates to a benzotriazole and chromium modified polyacid compound single-crystal structure and a preparation method thereof in the field of inorganic chemistry. The chemical formula of the crystal is [Cr(H2O)6][BTA]3[P2W18O62].12H2O (BTA refers to C6H5N3, benzotriazole), the molecular weight of the crystal is 5096.9, and the crystal belongs to a hexagonal crystal system in a P-62c space group, wherein a is equal to 1.67436(5)nm, b is equal to 1.67436(5)nm, c is equal to 3.12155(14)nm, gamma is equal to 120(10) degrees, V is equal to 7.5788(5)nm<3>, Z is equal to 1, F(000) is equal to 5543.43, R1 is equal to 0.0524, and wR2 is equal to 0.0965. The crystal is prepared from a normal-temperature aqueous solution by using a synthetic method. The prepared compound disclosed by the invention is clear in composition and structure, and has potential pharmaceutical application values.

Description

The polyacid compound structure that benzotriazole, chromium are modified and preparation method
Technical field
The invention belongs to inorganic polyacid technical field of chemistry, relate to a benzotriazole, the synthesis of Dawson structure polyacid compound that chromium is modified, be [Cr (H in particular 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(BTA=C 6h 5n 3, benzotriazole) and the preparation method of compound and structure.
Background technology
In recent years, the application prospect of polyoxometalates in material, catalysis and medicine receives concern [1-2], and it is one of them very active research field that organic molecule modifies polyacid compound.Because polyatom in polyacid compound has variable oxidation state, also have variable coordination configuration, this make it have various just more with potential function, such as: ion-exchange, absorption, pharmaceutical chemistry and catalysis etc. [3-4].
Benzotriazole is widely used in circulating water treatment agent, in slushing oil, lipid product, is also applied to the vapour-phase inhibitor of Copper and its alloy, lubricating oil additive [5-6].Benzotriazole can coordinate with multiple inhibiter, improves corrosion mitigating effect.Also can with multiple Scale inhibitors, Biocidal algae-killing agent with the use of, especially excellent to closed recirculating cooling water system corrosion mitigating effect, in automobile antifreeze glycol and water, add benzotriazole in coating and can to volatilize the effect of protecting materials.Benzotriazole also can be used as analytical reagent, share with ammoniacal liquor and ethylenediamine tetraacetic acid (EDTA), can be used for optionally measuring silver, copper, zinc.Also can be used as photography antifoggant and organic synthesis intermediate.
Synthesize the phosphorus tungsten polyacid compound [Cr (H of a benzotriazole and chromium metal modification herein 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o (BTA=C 6h 5n 3, benzotriazole), 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]?Zhang?PP,?Peng?J,?Pang?HJ,?Sha?JQ,?Zhu?M,?Wang?DD,?Liu?MG?(2011)?Cryst?Eng?Comm?13:?3832
[2]?Fu?H,?Li?YG,?Lu?Y,?Chen?WL,?Wu?Q,?Meng?JX,?Wang?XL,?Zhang?ZM,?Wang?EB?(2011)?Cryst?Growth?Des?11(2):?459
[3]?Shi?ZY,?Peng?J,?Zhang?ZY,?Yu?X,?Alimaje?K,?Wang?X?(2013)?Inorg?Chem?Commun?33:?105
[4]?Guo?H,?Yu?K,?Su?ZH,?Wang?CM,?Wang?CX,?Zhou?BB?(2013)?Inorg?Chem?Commun?27:?43
[5]?Wang?J,?Li?FB,?Cheng?SY?(2008)?J?Coord?Chem?61:?2122
[6]?Katritzky?AR,?Lan?X,?Yang?JZ,?Denisko?OV?(1998)?Chem?Rev?98:?409
[7]?Kokoszka?GF,?Baranowski?J,?Goldstein?C,?Orsini?J,?Mighell?AD,?Himes?VL,?Siedle?AR?(1983)?J?Am?Chem?Soc?105:?5627。
Summary of the invention
The present invention relates to [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(1) compound crystal structure.
The present invention relates to [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(1) preparation method of compound crystal, the research of take off data and data.
The present invention relates to [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(1) application of compound in medicine.
For achieving the above object, the invention provides following technical scheme:
There is the benzotriazole of following chemical general formula and the Suanphosphotungstate compound of chromium modification: [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(1)
The Suanphosphotungstate compound that benzotriazole of the present invention and chromium are modified, wherein collects diffraction data, Mo under monocrystalline Brucker SMART-CCD diffractometer kalpha-ray ( λ=0. 071 073 nm).SHELX 97 program is used to be resolved by direct method and complete matrix method of least squares and revise crystalline structure.All non-hydrogen atoms all use anisotropy thermal parameter to revise, and obtain all non-hydrogen atom coordinates.This crystal belongs to hexagonal system, p-6 2c spacers, a=1.67436 (5) nm, b=1.67436 (5) nm, c=3.12155 (14) nm, γ=120 (10) °, v=7.5788 (5) nm 3, z=1, f(000)=5543.43, r 1 =0.0524, wR 2 =0.0965.
The present invention further discloses [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(1) preparation method of compound: typical synthetic method is get 1.5g K 6[P 2w 18o 62] 14H 2o is dissolved in 50 mL water, under agitation adds chromium chloride solution 100 mL of 0.01 mol/L, regulates pH=4.20, add 0.2 g benzotriazole under rapid stirring, first generate white precipitate, stir lower disappearance, solution presents blackish green solution, stops stirring, static crystallization.Dark brown bulk crystals is grown after one day.
Accompanying drawing explanation
Fig. 1 is [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(1) molecular structure of compound
Fig. 2 is [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(1) accumulation graph of compound.
Embodiment
Phosphomolybdate compound [Cr (the H that a kind of benzotriazole, chromium are modified 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o(1) and preparation method thereof and condition: get 1.5g K 6[P 2w 18o 62] 14H 2o is dissolved in 50 mL water, under agitation adds chromium chloride solution 100 mL of 0.01 mol/L, regulates pH=4.20, add 0.2 g benzotriazole under rapid stirring, first generate white precipitate, stir lower disappearance, solution presents blackish green solution, stops stirring, static crystallization.Dark brown bulk crystals is grown after one day.This crystal records its structure by X-single crystal diffractometer and corresponding software.Polyanionic [the P of 1 Dawson structure 2w 18o 62] 6-, 3 protonated benzotriazole molecules, the counter cation Cr of 16 water coordination 3+and crystalline water molecules is formed.Valence link calculates and shows, the benzotriazole molecular in title compound is all protonated.Cr in this compound 3+ligancy be 6,6 water moleculess and Cr 3+coordination, Cr-Ow bond distance is 0.1922 (11)-0.1975 (11) nm.In the crystalline structure of compound, protonated benzotriazole molecule and the Cr of 6 water coordinations 3+make counter cation, multi-metal oxygen cluster anions band 6 negative charges, between zwitterion, form ionic compound by electrostatic attraction effect.
Compound [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2the IR figure spectrum wavelength of O is at 400-1000 cm -1in scope, have a large broad peak clearly, this is polyoxoanion [P 2w 18o 62] 6-charateristic avsorption band.Wavelength is at 1000-1700 cm -1in scope, have several spike, this is organic charateristic avsorption band, and this is comprising the absorption peak of C=C key, C=O key and C=N key.Wavelength is at 1700-4000 cm -1in scope, there is a shape very large, and the peak that peak shape is relatively delayed, this is the charateristic avsorption band of water molecules.
Embodiment
Get 1.8g K 6[P 2w 18o 62] 14H 2o is dissolved in 50 mL water, under agitation adds chromium chloride solution 100 mL of 0.01 mol/L, regulates pH=4.30, add 0.3 g benzotriazole under rapid stirring, first generate white precipitate, stir lower disappearance, solution presents blackish green solution, stops stirring, static crystallization.

Claims (4)

1. a polyacid compound for benzotriazole and chromium modification, its chemical formula is [Cr (H 2o) 6] [BTA] 3[P 2w 18o 62] 12H 2o (BTA=C 6h 5n 3, benzotriazole), molecular weight is 5096.9.
2. a monocrystalline for the phosphomolybdate compound of benzotriazole modification according to claim 1, its constitutional features is: molecular formula is C 18h 51crN 9o 80p 2w 18, molecular weight is 5096.9, and this crystal belongs to hexagonal system, p-6 2c spacers, a=1.67436 (5) nm, b=1.67436 (5) nm, c=3.12155 (14) nm, γ=120 (10) °, v=7.5788 (5) nm 3, z=1, f(000)=5543.43, r 1 =0.0524, wR 2 =0.0965.
3. the synthetic method of the polyacid compound of benzotriazole described in claim 1 and chromium modification, is characterized in that: get 1.5g K 6[P 2w 18o 62] 14H 2o is dissolved in 50 mL water, under agitation adds chromium chloride solution 100 mL of 0.01 mol/L, regulates pH=4.20, add 0.2 g benzotriazole under rapid stirring, first generate white precipitate, stir lower disappearance, solution presents blackish green solution, stops stirring, static crystallization.
4. the preparation method of polyacid compound of benzotriazole described in claim 1 and chromium modification and the application in medicine.
CN201410444955.6A 2014-09-03 2014-09-03 Benzotriazole, the polyacid compound structure and preparation method of chromium modification Expired - Fee Related CN104230994B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110423252A (en) * 2019-06-25 2019-11-08 扬州大学 Krebs type polyacid compound and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
JIAN-ZHEN LIAO等,: "Polyoxometalate anion-π interaction-directed assembly of a three-dimensional hydrogen-bonded supramolecular framework with nanoscale porosity", 《CRYSTENGCOMM》 *
Z. V. SLOBODYAN等,: "REALIZATION OF SYNERGISM IN 1-, 2-, 3-BENZOTRIAZOLE TRIMOLYBDATE, TUNGSTATE, AND CHROMATE CORROSION INHIBITORS", 《MATERIALS SCIENCE》 *
杨艳艳等,: "苯并三氮唑修饰的磷钨酸盐化合物合成及性质研究", 《中国化学会第五届全国多酸化学学术研讨会》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110423252A (en) * 2019-06-25 2019-11-08 扬州大学 Krebs type polyacid compound and preparation method thereof

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