CN103601743A - Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives - Google Patents
Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives Download PDFInfo
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- CN103601743A CN103601743A CN201310579614.5A CN201310579614A CN103601743A CN 103601743 A CN103601743 A CN 103601743A CN 201310579614 A CN201310579614 A CN 201310579614A CN 103601743 A CN103601743 A CN 103601743A
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- compound
- btec
- nitro
- magnesium
- carbon disulfide
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Abstract
The present invention provides the compounds and its preparation and use to carbon disulfide and nitro explosive with highly sensitive fluorescence response. The compound molecule formula are as follows: Mg5 (OH) 2 (BTEC) 2 (H2O) 411H2O, wherein H4BTEC be
Compound category anorthic system, space group P-1, cell parameter are as follows: a=7.3742 (3), b=11.4011 (6), c=11.6706 (6)
α=89.666 (4), β=76.813 (4), γ=74.971 (4) °,
Z=1. The compound is for the detection to CS2 and nitro explosive.
Description
Technical field
The present invention relates to prepare under hydrothermal condition a kind of to poisonous high solvent flashing dithiocarbonic anhydride (CS
2) and the high quick-fried thing hazardous substance of nitro there is the magnesium basigamy compound of sensitive fluorescence response performance.This compound is at CS
2and nitro phenenyl concentration is while being only 0.8vol% and 0.04vol%, just shows the sensitive response of the complete cancellation of fluorescence; According to same method to 10
-3mol/L2, when 4-dinitraniline, 4-N-methyl-p-nitroaniline and o-Nitraniline detect, shows high-sensitive fluorescent quenching response, is expected to accomplish something at environmental pollution monitoring and secure context.
Background technology
Title complex based on transition metal and rare earth ion (metal organic frame compound over the past two years, MOF), in heavy metal ion, organic molecule and the high quick-fried thing context of detection of nitro, show excellent performance, and there is highly sensitive, highly selective and be convenient to the advantages such as preparation.Dithiocarbonic anhydride (CS
2) as high volatile volatile hazardous solvent, people's long-term exposure even can induction neurotoxic, arteriosclerosis in the environment of lower concentration etc. disease.In addition as the raw material of producing regenerated fiber, CS
2extensive application also make it can produce SO
2etc. main air pollutant.Nitro benzene and its derivative is also high malicious organic solvent, and many nitro-compounds whiles or the main component of explosive substance, easily cause safety problem.The at present detection of these materials relies on complicated meticulous analytical instrument substantially, develops a kind of efficient, sensitive and test material is extremely urgent easily.
Summary of the invention
The present invention has prepared a kind of metal organic frame compound based on light metal magnesium ion, and its molecular formula is: Mg
5(OH)
2(BTEC)
2(H
2o)
411H
2o, wherein H
4bTEC is
(Pyromellitic Acid), this compound has three-dimensional spacious skeleton construction, has carbonic acid gas adsorption selectivity under normal temperature.Fluorescence property research shows that this compound is to CS
2, oil of mirbane and many nitro-compounds have sensitive fluorescence response, be expected for CS
2, the high quick-fried thing of oil of mirbane and many nitros detection.
The present invention adopts following technical scheme:
The present invention discloses a kind of magnesium basigamy compound dithiocarbonic anhydride and nitro explosive substance to fluorescence response, and its molecular formula is: Mg
5(OH)
2(BTEC)
2(H
2o)
411H
2o, wherein H
4bTEC is
belong to triclinic(crystalline)system, spacer is P-1, and cell parameter is: a=7.3742 (3)
b=11.4011 (6)
c=11.6706 (6)
α=89.666 (4) °, β=76.813 (4) °, γ=74.971 (4) °,
z=1.Compound has the novel secondary construction unit of five core magnesium, by pyromellitic acid bridging, forms three-dimensional tridimensional structure.
The invention provides compound Mg
5(OH)
2(BTEC)
2(H
2o)
411H
2the preparation method of O, comprises the steps: (the NO by Mg
3)
26H
2o, H
4bTEC, NaHCO
3according to mol ratio 1:1:2, and 10mL H
2o is mixed to join in the 20mL stainless steel cauldron that liner is tetrafluoroethylene, in 170 ℃ of solvent thermal reactions, within 4 days, obtains this compound.
Fluorescence property research shows that, under 322nm wavelength excites, compound has strong fluorescent emission at the 435nm place in UV-light region.Be dispersed in tetrahydrofuran solvent for detection of lower concentration CS compound is ultrasonic
2, oil of mirbane and many nitros compound, show sensitive fluorescence response.In addition, this compound can direct-detection oil of mirbane steam, and fluorescence intensity cancellation 50% in 60s, shows highly sensitive detection performance.This compound is expected for to CS
2, oil of mirbane and many nitros the detection of compound.
Accompanying drawing explanation
Fig. 1. the crystalline structure schematic diagram of compound.
Fig. 2. compound is to CS
2the fluorescence response figure of solvent.
Fig. 3. compound is to 10
-3mol/L2, the fluorescence response figure of 4-dinitrobenzene amine aqueous solution.
Fig. 4. under compound normal temperature to CO
2selective adsorption figure.
Embodiment
Embodiment 1:
Mg
5(OH)
2(BTEC)
2(H
2o)
411H
2o's is synthetic
By Mg (NO
3)
26H
2o (1mmol), H
4bTEC (1mmol), NaHCO
3(2mmol) and 10mLH
2o is mixed into settled solution, in the 20mL stainless steel cauldron that inclosure liner is tetrafluoroethylene, in 170 ℃ of isothermal reactions 4 days, be then naturally cooled to room temperature, to choose by hand colourless rhabdolith (target product) 75mg(productive rate 30.4% after absolute ethanol washing).
Embodiment 2:
To CS
2, oil of mirbane and many nitros compound fluorescence detection method
Be distributed in 5mL tetrahydrofuran (THF) 5mg compound is ultrasonic, make stable suspension liquid, suspension liquid is added drop-wise in the wide quartz colorimetric utensil of 1cm and carries out fluoroscopic examination.
By CS
2with liquid-transfering gun, be dropwise added drop-wise to above-mentioned suspension liquid 1uL/ time, with fluorescence detector, record fluorescence intensity at every turn, until CS is recorded in cancellation completely
2consumption;
Oil of mirbane fluorescence detection method is the same; Compound is ground, and solid-state lower fluorescence intensity, is placed in oil of mirbane steam fast, and rapid detection after stop certain hour, records fluorescence intensity, and be recorded in the time in nitrobenzene vapor, until fluorescence intensity no longer declines;
2,4-dinitraniline, 2-N-methyl-p-nitroaniline, 4-N-methyl-p-nitroaniline are configured to 10 with dehydrated alcohol
-3mol/L solution, adopts and detects CS
2method is carried out fluorescence response detection.
Claims (3)
1. pair dithiocarbonic anhydride and nitro explosive substance have the compound of highly sensitive fluorescence response, and its molecular formula is: Mg
5(OH)
2(BTEC)
2(H
2o)
411H
2o, wherein H4BTEC is
compound belongs to triclinic(crystalline)system, and spacer is P-1, and cell parameter is: a=7.3742 (3), b=11.4011 (6), c=11.6706 (6)
α=89.666 (4), β=76.813 (4), γ=74.971 (4) °,
z=1.
2. the synthetic method of compound described in claim 1, is characterized in that: by Mg (NO
3)
26H
2o, H
4bTEC, NaHCO
3according to mol ratio, be 1:1:2, and 10mL H
2o is mixed to join in the 20mL stainless steel cauldron that liner is tetrafluoroethylene, in 170 ℃ of solvent thermal reactions, within 4 days, obtains compound.
3. described in claim 1, compound is used for CS
2and the detection of nitro explosive substance.
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CN201310579614.5A CN103601743A (en) | 2013-11-18 | 2013-11-18 | Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives |
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CN201310579614.5A CN103601743A (en) | 2013-11-18 | 2013-11-18 | Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107099036A (en) * | 2017-03-13 | 2017-08-29 | 中国科学院长春应用化学研究所 | Fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro and its preparation method and application |
CN107216345A (en) * | 2017-05-04 | 2017-09-29 | 中国科学院福建物质结构研究所 | Magnesium transition metal different metal base fluorescence is with polymers probe material and preparation method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103333183A (en) * | 2013-06-25 | 2013-10-02 | 南昌航空大学 | Non-center cadmium metal complex and synthetizing method and application thereof |
-
2013
- 2013-11-18 CN CN201310579614.5A patent/CN103601743A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103333183A (en) * | 2013-06-25 | 2013-10-02 | 南昌航空大学 | Non-center cadmium metal complex and synthetizing method and application thereof |
Non-Patent Citations (3)
Title |
---|
ZHAO-FENG WU等: "A magnesium MOF as a sensitivefluorescence sensor for CS2and nitroaromatic compounds", 《J. MATER. CHEM. A》 * |
吴兆锋: "若干镁基金属有机框架化合物的合成与表征", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
吴兆锋等: "三例镁基金属有机框架化合物的合成与表征", 《中国化学会第28届学术年会第8分会场摘要集》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107099036A (en) * | 2017-03-13 | 2017-08-29 | 中国科学院长春应用化学研究所 | Fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro and its preparation method and application |
CN107216345A (en) * | 2017-05-04 | 2017-09-29 | 中国科学院福建物质结构研究所 | Magnesium transition metal different metal base fluorescence is with polymers probe material and preparation method thereof |
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