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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
compound
btec
nitro
magnesium
carbon disulfide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201310579614.5A
Other languages
Chinese (zh)
Inventor
吴兆锋
谭彬
冯美玲
兰安建
黄小荥
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujian Institute of Research on the Structure of Matter of CAS
Original Assignee
Fujian Institute of Research on the Structure of Matter of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fujian Institute of Research on the Structure of Matter of CAS filed Critical Fujian Institute of Research on the Structure of Matter of CAS
Priority to CN201310579614.5A priority Critical patent/CN103601743A/en
Publication of CN103601743A publication Critical patent/CN103601743A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

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
Figure DDA0000416865640000011
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)
Figure DDA0000416865640000012
α=89.666 (4), β=76.813 (4), γ=74.971 (4) °,
Figure DDA0000416865640000013
Figure DDA0000416865640000014
Z=1. The compound is for the detection to CS2 and nitro explosive.

Description

Magnesium basigamy compound dithiocarbonic anhydride and nitro explosive substance to fluorescence response
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
Figure BDA0000416865620000011
(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
Figure BDA0000416865620000021
belong to triclinic(crystalline)system, spacer is P-1, and cell parameter is: a=7.3742 (3)
Figure BDA0000416865620000022
b=11.4011 (6)
Figure BDA0000416865620000023
c=11.6706 (6)
Figure BDA0000416865620000024
α=89.666 (4) °, β=76.813 (4) °, γ=74.971 (4) °,
Figure BDA0000416865620000025
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
Figure FDA0000416865610000011
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) °,
Figure FDA0000416865610000013
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.
CN201310579614.5A 2013-11-18 2013-11-18 Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives Pending CN103601743A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310579614.5A CN103601743A (en) 2013-11-18 2013-11-18 Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310579614.5A CN103601743A (en) 2013-11-18 2013-11-18 Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives

Publications (1)

Publication Number Publication Date
CN103601743A true CN103601743A (en) 2014-02-26

Family

ID=50120023

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310579614.5A Pending CN103601743A (en) 2013-11-18 2013-11-18 Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives

Country Status (1)

Country Link
CN (1) CN103601743A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
Zhu et al. Enhanced luminescence of NH2-UiO-66 for selectively sensing fluoride anion in water medium
Kumar et al. Calixarenes based materials for gas sensing applications: A review
Wang et al. Eu3+-functionalized covalent organic framework hybrid material as a sensitive turn-on fluorescent switch for levofloxacin monitoring in serum and urine
Xu et al. Eu (III) functionalized Zr-based metal-organic framework as excellent fluorescent probe for Cd2+ detection in aqueous environment
Zhang et al. Ultrasensitive detection of Cr (VI)(Cr2O72−/CrO42−) ions in water environment with a fluorescent sensor based on metal-organic frameworks combined with sulfur quantum dots
Lee et al. Excitation–emission spectra and fluorescence quantum yields for fresh and aged biogenic secondary organic aerosols
Yan et al. Speciation and sources of brown carbon in precipitation at Seoul, Korea: insights from excitation–emission matrix spectroscopy and carbon isotopic analysis
An et al. Zinc-adeninate metal− organic framework for aqueous encapsulation and sensitization of near-infrared and visible emitting lanthanide cations
Hou et al. Highly selective and sensitive detection of Pb2+ and UO22+ ions based on a carboxyl-functionalized Zn (II)-MOF platform
Vellingiri et al. Luminescent metal-organic frameworks for the detection of nitrobenzene in aqueous media
Wei et al. Ultrasensitive and highly selective detection of formaldehyde via an adenine-based biological metal–organic framework
Hou et al. ZnMOF-74 responsive fluorescence sensing platform for detection of Fe3+
Quezada-Novoa et al. Building a shp: a rare-earth metal–organic framework and its application in a catalytic photooxidation reaction
Pang et al. Real‐time in situ volatile organic compound sensing by a dual‐emissive polynuclear Ln‐MOF with pronounced LnIII luminescence response
Ren et al. Water-stable lanthanide-based metal-organic frameworks for rapid and sensitive detection of nitrobenzene derivatives
Shu et al. A New Three‐Dimensional Cd (II) Metal‐Organic Framework for Highly Selective Sensing of Fe3+ as well as Nitroaromatic Compounds
Nikhar et al. Biological metal organic framework (Bio-MOF) for detection of voltaic organic compounds (VOC’s)
Chai et al. Five Mesoporous Lanthanide Metal–Organic Frameworks: Syntheses, Structures, and Fluorescence Sensing of Fe3+, Cr2O72–, and H2O2 and Electrochemical Sensing of Trinitrophenol
Liu et al. A dual-emission Acf@ bioMOF-1 platform as fluorescence sensor for highly efficient detection of inorganic ions
Abuzalat et al. Facile and rapid synthesis of functionalized Zr-BTC for the optical detection of the blistering agent simulant 2-chloroethyl ethyl sulfide (CEES)
Tian et al. Visible light‐driven, one‐pot amide synthesis catalyzed by the B12 model complex under aerobic conditions
Zhang et al. Dandelion-like covalent organic frameworks with high-efficiency fluorescence for ratiometric sensing and visual tracking-by-detection of Fe3+
Li et al. A luminescent pillar-layer Zn (II) metal–organic framework for the ultrasensitive detection of nitroaniline
CN103601743A (en) Magnesium-based complex having fluorescent response to carbon disulfide and nitro explosives
Ghosh et al. Ultrafast and nanomolar level detection of H 2 S in aqueous medium using a functionalized UiO-66 metal–organic framework based fluorescent chemosensor

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20140226

WD01 Invention patent application deemed withdrawn after publication