CN112444514A - Detection test paper based on metal-organic framework and preparation method thereof - Google Patents

Detection test paper based on metal-organic framework and preparation method thereof Download PDF

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CN112444514A
CN112444514A CN202011297306.XA CN202011297306A CN112444514A CN 112444514 A CN112444514 A CN 112444514A CN 202011297306 A CN202011297306 A CN 202011297306A CN 112444514 A CN112444514 A CN 112444514A
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paper
metal
organic framework
mofs
test paper
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朱小平
骆明亮
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Jiangsu Antai Safety Technology Co ltd
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Jiangsu Antai Safety Technology Co ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
    • C08G83/008—Supramolecular polymers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/7756—Sensor type
    • G01N2021/7759—Dipstick; Test strip

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  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
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Abstract

The invention discloses a detection test paper based on a metal-organic framework, which comprises detection test paper, wherein the detection test paper is damaged by the metal-organic framework MOFs and lead acetate; the preparation process comprises the following steps: preparation of paper-based MOFs: reacting 5-azido isophthalic acid H2IPA‑N3Ligand, AlCl3Adding the solution and the bleached paper pulp into N, N-dimethylformamide DMF, uniformly mixing, naturally cooling to room temperature, filtering, collecting precipitate, washing with an organic solvent, and drying to obtain paper-based MOFs; and (3) taking the light yellow paper-based MOFs in the step one, dispersing the light yellow paper-based MOFs in a lead acetate solution, adding a polyvinyl acetate emulsion, and stirring to obtain a uniform mixture. And (3) draining water by using a screen, extruding by using a pressing roller, drying and cutting to obtain the light yellow lead acetate detection test paper, wherein the test paper turns black when encountering hydrogen sulfide gas. The invention utilizes the selective adsorption and porous negative of metal-organic frameworkThe carrier property can realize quick and effective detection of hydrogen sulfide gas, and the safety of people is guaranteed.

Description

Detection test paper based on metal-organic framework and preparation method thereof
Technical Field
The invention relates to detection test paper based on a metal-organic framework and a preparation method thereof, belonging to the field of environmental detection.
Background
Hydrogen sulfide is a flammable acidic gas, colorless, smelly egg odor at low concentrations, and even low concentrations of hydrogen sulfide can also damage human olfactory senses. At high concentrations there is no smell on the contrary (since high concentrations of hydrogen sulfide can paralyze the olfactory nerve). The use of the nose as a means of detecting such gases is fatal. And explosion can occur when hydrogen sulfide is mixed with air in appropriate proportions.
In recent years, with the progress of chemical detection and analysis techniques, the detection of hydrogen sulfide has been rapidly developed, and for example, hydrogen sulfide can be detected by gas chromatography, spectrophotometry, gas tube detection, or the like, but instruments and analysis professionals are required, and it is not appropriate to meet the demand for knowing the presence or absence of hydrogen sulfide at any time on site. Thus, a sensitive and simple detection method is still lacking.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the detection test paper based on the metal-organic framework and the preparation method thereof, the hydrogen sulfide can be quickly adsorbed by utilizing the selective adsorbability and the porous loading property of the metal-organic framework, and the detection is carried out by combining a common detection means. The hydrogen sulfide gas is rapidly and effectively detected, and the safety of people is guaranteed.
In order to achieve the purpose, the invention adopts the technical scheme that: the detection test paper based on the metal-organic framework comprises detection test paper, wherein the detection test paper is damaged and provided with metal-organic framework MOFs and lead acetate; the metal-organic framework MOFs and the lead acetate are loaded on the paper base.
Further, the concentration of the lead acetate solution is 3-10%.
A preparation method of detection test paper based on a metal-organic framework comprises the following preparation steps:
the method comprises the following steps: preparation of paper-based MOFs: reacting 5-azido isophthalic acid H2IPA-N3Ligand, AlCl3Adding the solution and the bleached paper pulp into N, N-dimethylformamide DMF, uniformly mixing, reacting at 80-120 ℃ for 12-24 h, naturally cooling to room temperature, filtering, collecting precipitate, washing with an organic solvent, and drying to obtain paper-based MOFs;
step two: and (3) lead acetate treatment: and (3) taking the light yellow paper-based MOFs in the step one, dispersing the light yellow paper-based MOFs in a lead acetate solution, adding a polyvinyl acetate emulsion, and stirring to obtain a uniform mixture. And (3) draining water by using a screen, extruding by using a pressing roller, drying and cutting to obtain the light yellow lead acetate detection test paper, wherein the test paper turns black when encountering hydrogen sulfide gas.
Further, in the first step, 5-azidoisophthalic acid H2IPA-N3Ligand: AlCl3Solution: drying paper pulp: the mass ratio of the N, N-dimethylformamide is 20-40: 45-60: 2-6: 500-700.
Further, in the first step, 5-azidoisophthalic acid H2IPA-N3Ligand: al (Al)3+The mass ratio of substances is 1: 1.
further, in the first step, AlCl is adopted3The concentration of the solution is 2-4 mol/L.
Further, the organic solvent in the first step includes one of ethanol and methanol.
Further, the drying temperature in the first step is 110-120 ℃.
Further, in the second step, the paper-based MOFs: lead acetate solution: the mass ratio of the polyvinyl acetate emulsion is 45-55: 300-400: 0.1 to 0.3.
Further, the drying temperature in the second step is 100-110 ℃.
The invention has the beneficial effects that: the detection test paper takes paper pulp as a raw material, is simple in preparation process, adopts a simple papermaking process, embeds the metal-organic framework into the test paper, utilizes the excellent adsorption performance of metal-organic frameworks (MOFs) to adsorb hydrogen sulfide gas, and combines the hydrogen sulfide gas with lead acetate in the test paper to realize the on-site rapid detection of gases such as hydrogen sulfide.
Drawings
FIG. 1 is a schematic diagram of quality index of hydrogen sulfide test paper of the present invention;
FIG. 2 is a flow chart of the test paper manufacturing process of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in the specification of the present invention are for the purpose of describing particular embodiments only and are not intended to limit the present invention.
As shown in fig. 1 and 2, the metal-organic framework-based test strip comprises a test strip body, wherein the test strip body is provided with metal-organic framework MOFs and lead acetate; the metal-organic framework MOFs and the lead acetate are loaded on the paper base.
Preferably, the concentration of the lead acetate solution is 3-10%.
The preparation method of the detection test paper based on the metal-organic framework comprises the following preparation steps:
the method comprises the following steps: preparation of paper-based MOFs: reacting 5-azido isophthalic acid H2IPA-N3Ligand, AlCl3Adding the solution and the bleached paper pulp into N, N-dimethylformamide DMF, uniformly mixing, reacting at 80-120 ℃ for 12-24 h, naturally cooling to room temperature, filtering, collecting precipitate, washing with an organic solvent, and drying to obtain paper-based MOFs;
step two: and (3) lead acetate treatment: and (3) taking the light yellow paper-based MOFs in the step one, dispersing the light yellow paper-based MOFs in a lead acetate solution, adding a polyvinyl acetate emulsion, and stirring to obtain a uniform mixture. And (3) draining water by using a screen, extruding by using a pressing roller, drying and cutting to obtain the light yellow lead acetate detection test paper, wherein the test paper turns black when encountering hydrogen sulfide gas.
In the first step, 5-azido isophthalic acid H2IPA-N3Ligand: AlCl3Solution: drying paper pulp: the mass ratio of the N, N-dimethylformamide is 20-40: 45-60: 2-6: 500-700.
Preferably, in step one, 5-azidoisophthalic acid H2IPA-N3Ligand: al (Al)3+The mass ratio of substances is 1: 1.
preferably, AlCl is used in the first step3The concentration of the solution is 2-4 mol/L.
Preferably, the organic solvent in the first step includes one of ethanol and methanol.
Preferably, the drying temperature in the first step is 110-120 ℃.
Preferably, in step two, the paper-based MOFs: lead acetate solution: the mass ratio of the polyvinyl acetate emulsion is 45-55: 300-400: 0.1 to 0.3.
Preferably, the drying temperature in the second step is 100 ℃.
In this embodiment, specifically:
20 g H2IPA-N3Ligand (19.4mmol), 48 mL AlCl3Solution (Al)3+ 19.4mmol) and 2 g of bleached and dried paper pulp are added into 500 g of DMF, and the mixture is uniformly mixed, reacted for 15 h at 120 ℃, naturally cooled to room temperature, filtered, collected and precipitated, washed by ethanol and dried at 110 ℃ to obtain paper-based MOFs;
taking 15 g of the paper-based MOFs, dispersing the paper-based MOFs in 90 mL of 5% lead acetate solution, adding 0.06 g of polyvinyl acetate emulsion, and stirring to obtain a uniform mixture. And (3) draining water by using a screen, extruding by using a squeezing roller, drying at 100 ℃, and cutting to obtain the lead acetate test paper, wherein the test paper turns black when encountering gases such as hydrogen sulfide and the like.
The MOFs test paper produced by the process has the specification of 1.2 cm multiplied by 5 cm and the content of detected hydrogen sulfide of 10mmg/m3The results are shown in the table of FIG. 1.
Metal-organic frameworks (MOFs) are a porous inorganic-organic material, a novel functional material, and have been widely used in the fields of gas storage/separation, sensing, biomedicine, clean energy, etc. due to their customizable molecular structure, good thermal stability, and uniform nanoscale cavities. As an adsorption material, the molecular structure can be designed to realize the selectivity of the molecular sieve, and analytes can be concentrated in MOFs matrix in advance, so that effective host-guest interaction is realized.
If the selective adsorption property and the porous loading property of the metal-organic framework can be utilized, the hydrogen sulfide can be quickly adsorbed, and the detection is carried out by combining a common detection means. The hydrogen sulfide gas is rapidly and effectively detected, and the safety of people is guaranteed.
The invention aims to overcome the defects of difficult field operation, low sensitivity and the like existing in the detection of flammable gases such as hydrogen sulfide and the like at present, and the MOFs is combined with lead acetate and loaded on paper to prepare the sensitive and easily-operated detection test paper based on metal-organic frameworks (MOFs).
The technical principle of the invention is as follows: with 5-azidoisophthalic acid (H)2IPA-N3) Is an organic ligand, Al3+The method is characterized in that MOFs is synthesized by taking the MOFs as a central coordination ion, the MOFs is combined with lead acetate, the hydrogen sulfide gas can be rapidly adsorbed by utilizing the porous adsorbability of the MOFs, the hydrogen sulfide gas is concentrated, and the lead acetate in the MOFs cavity is utilized to achieve the purpose of rapidly detecting the hydrogen sulfide. MOFs and lead acetate are loaded on a paper base through a papermaking process, and the MOFs detection test paper with simple operation and high sensitivity is prepared.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The detection test paper based on the metal-organic framework comprises detection test paper and is characterized in that the detection test paper is damaged by the metal-organic framework MOFs and lead acetate; the metal-organic framework MOFs and the lead acetate are loaded on the paper base.
2. The metal-organic framework-based detection test paper according to claim 1, wherein the concentration of the lead acetate solution is 3-10%.
3. A preparation method of detection test paper based on a metal-organic framework is characterized by comprising the following preparation steps:
the method comprises the following steps: preparation of paper-based MOFs: reacting 5-azido isophthalic acid H2IPA-N3Ligand, AlCl3Adding the solution and the bleached paper pulp into N, N-dimethylformamide DMF, uniformly mixing,reacting at 80-120 ℃ for 12-24 h, naturally cooling to room temperature, filtering, collecting precipitate, cleaning with an organic solvent, and drying to obtain paper-based MOFs;
step two: and (3) lead acetate treatment: taking the light yellow paper-based MOFs in the step one, dispersing the light yellow paper-based MOFs in a lead acetate solution, adding a polyvinyl acetate emulsion, and stirring to obtain a uniform mixture; and (3) draining water by using a screen, extruding by using a pressing roller, drying and cutting to obtain the light yellow lead acetate detection test paper, wherein the test paper turns black when encountering hydrogen sulfide gas.
4. The metal-organic framework-based test strip of claim 3, wherein in the first step, 5-azido isophthalic acid H is2IPA-N3Ligand: AlCl3Solution: drying paper pulp: the mass ratio of the N, N-dimethylformamide is 20-40: 45-60: 2-6: 500-700.
5. The metal-organic framework-based test strip of claim 3, wherein in the first step, 5-azido isophthalic acid H is2IPA-N3Ligand: al (Al)3+The mass ratio of substances is 1: 1.
6. the metal-organic framework-based test strip of claim 3, wherein AlCl is adopted in the first step3The concentration of the solution is 2-4 mol/L.
7. The metal-organic framework-based test strip of claim 3, wherein the organic solvent in the first step comprises one of ethanol and methanol.
8. The metal-organic framework-based test strip of claim 3, wherein the drying temperature in the first step is 110-120 ℃.
9. The metal-organic framework-based test strip according to claim 3, wherein in the second step, the ratio of paper-based MOFs: lead acetate solution: the mass ratio of the polyvinyl acetate emulsion is 45-55: 300-400: 0.1 to 0.3.
10. The test paper based on metal-organic framework as claimed in claim 3, wherein the drying temperature in the second step is 100-110 ℃.
CN202011297306.XA 2020-11-19 2020-11-19 Detection test paper based on metal-organic framework and preparation method thereof Pending CN112444514A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313733A (en) * 2010-07-05 2012-01-11 中国石油集团川庆钻探工程有限公司川东钻探公司 Method for rapid testing hydrogen sulfide content in drilling fluid
CN105833662A (en) * 2016-05-17 2016-08-10 浙江大学 Method for adsorbing and separating sulfur-containing acid gas
CN108619917A (en) * 2018-03-22 2018-10-09 浙江大学 A kind of hydrogen sulfide sensing metal-organic framework base mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313733A (en) * 2010-07-05 2012-01-11 中国石油集团川庆钻探工程有限公司川东钻探公司 Method for rapid testing hydrogen sulfide content in drilling fluid
CN105833662A (en) * 2016-05-17 2016-08-10 浙江大学 Method for adsorbing and separating sulfur-containing acid gas
CN108619917A (en) * 2018-03-22 2018-10-09 浙江大学 A kind of hydrogen sulfide sensing metal-organic framework base mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
AMVROSIOS G. GEORGIADIS ET AL: "《"Hydrogen Sulfide (H2S) Removal via MOFs》", 《MATERIALS》 *
SOUTICK NANDI ET AL: "《Rapid and highly sensitive detection of extracellular and intracellular H2S by an azide-functionalized Al(III)-based metal–organic framework》", 《DALTON TRANSACTIONS》 *

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Application publication date: 20210305