CN110186882B - Fluorescent test paper for detecting nitro compound and preparation method thereof - Google Patents
Fluorescent test paper for detecting nitro compound and preparation method thereof Download PDFInfo
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- CN110186882B CN110186882B CN201910421262.8A CN201910421262A CN110186882B CN 110186882 B CN110186882 B CN 110186882B CN 201910421262 A CN201910421262 A CN 201910421262A CN 110186882 B CN110186882 B CN 110186882B
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6447—Fluorescence; Phosphorescence by visual observation
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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Abstract
The invention relates to a fluorescent test paper for detecting nitro compounds and a preparation method thereof, which comprises the steps of weighing (N, N' - ((2, 5-dihydroxy-1, 4-phenylene) di (methylene)) bisacrylamide, polyethylene glycol monomethyl ether, anhydrous tetrahydrofuran, hexamethylene diisocyanate and 1, 4-diazabicyclo [2.2.2] octane, adding the weighed materials into a dry container, mixing the materials into a uniform solution, heating the solution at 60-80 ℃ for 6-8 hours, adding diethyl ether after the solution is viscous, carrying out vacuum drying to obtain fluorescent polyurethane, dissolving the fluorescent polyurethane into a mixed solution of acetonitrile and water, infiltrating and drying a cut paper sheet to obtain the fluorescent test paper for detecting the nitro compounds, wherein the preparation method is simple, raw materials are easy to obtain, the fluorescent test paper is contacted with the nitro compounds and disappears, and has high sensitivity to TNP, the invention provides an option for low cost detection of hazardous materials.
Description
Technical Field
The invention relates to a fluorescent test paper and a preparation method thereof, in particular to a fluorescent test paper for detecting nitro compounds and a preparation method thereof, belonging to the field of organic compound detection.
Background
The detection of explosives by simple and practical methods has become a crucial problem. Nitro-chemical combination is the main component of explosives, of which 2,4, 6-Trinitrophenol (TNP) (picric acid) is an extremely dangerous substance, a compound with a greater explosive power than other nitro-compounds such as 2-nitrotoluene (oNT), Nitrobenzene (NB) and 2,4, 6-trinitrotoluene (TNT). TNP is also used in industrial dyes and as a clinical chemical agent, which can cause serious pollution of irrigated land and groundwater supply, harmful to human health, and therefore, rapid and efficient detection of nitro compounds is required. At present, although various explosive detection technologies, such as gas chromatography spectroscopy (GC-MS), Surface Enhanced Raman Spectroscopy (SERS) and electrochemical methods, can accurately detect explosives, the methods have the disadvantages of expensive instruments, complex operation, inconvenience in carrying and the like.
Disclosure of Invention
The invention aims to provide the fluorescent test paper for detecting the nitro compound, which has simple preparation method and easily obtained raw materials, and can observe fluorescence under an ultraviolet lamp by naked eyes and the preparation method thereof.
The invention aims to provide the fluorescence test paper for detecting the nitro compound, which is prepared by the following steps:
the method comprises the following steps: preparing fluorescent polyurethane: weighing 0.5-1 g of N, N' - ((2, 5-dihydroxy-1, 4-phenylene) bis (methylene)) bisacrylamide, 1-2 g of polyethylene glycol monomethyl ether, 20-25 mL of anhydrous tetrahydrofuran, 1-2 g of hexamethylene diisocyanate, and 0.1-0.5 g of 1, 4-diazabicyclo [2.2.2] octane into a dry container and mixing to obtain a uniform solution; then heating the solution at 60-80 ℃ for 6-8 hours; adding ether after the solution is viscous, and performing vacuum drying to obtain fluorescent polyurethane;
step two: dissolving 0.1-0.3 g of fluorescent polyurethane in a mixed solution of acetonitrile and water, and then infiltrating and drying a cut paper sheet to obtain fluorescent test paper for detecting nitro compounds;
the invention also includes such features:
1. the ratio of acetonitrile to water is 1: 1 to 1.5;
2. soaking the paper sheet for 2-5 minutes;
3. the size of the paper sheet is 1-3cm multiplied by 2-5 cm.
A preparation method of fluorescent test paper for detecting nitro compounds comprises the following steps:
the method comprises the following steps: preparing fluorescent polyurethane: weighing 0.5-1 g of N, N' - ((2, 5-dihydroxy-1, 4-phenylene) bis (methylene)) bisacrylamide, 1-2 g of polyethylene glycol monomethyl ether, 20-25 mL of anhydrous tetrahydrofuran, 1-2 g of hexamethylene diisocyanate, and 0.1-0.5 g of 1, 4-diazabicyclo [2.2.2] octane into a dry container and mixing to obtain a uniform solution; then heating the solution at 60-80 ℃ for 6-8 hours; adding ether after the solution is viscous, and performing vacuum drying to obtain fluorescent polyurethane;
step two: dissolving 0.1-0.3 g of fluorescent polyurethane in a mixed solution of acetonitrile and water, and then infiltrating and drying a cut paper sheet to obtain fluorescent test paper for detecting nitro compounds;
the ratio of acetonitrile to water is 1: 1 to 1.5;
soaking the paper sheet for 2-5 minutes;
the size of the paper sheet is 1-3cm multiplied by 2-5 cm.
Compared with the prior art, the invention has the beneficial effects that:
the fluorescent test paper prepared by the invention has the advantages of simple preparation method and easily obtained raw materials, can observe fluorescence by naked eyes under an ultraviolet lamp, is contacted with a nitro compound, has no fluorescence, has high sensitivity to TNP, and provides a choice for detecting dangerous goods at low cost.
Drawings
FIG. 1 is a graph showing the fluorescence response of the test strip of example 1 at different concentrations of NP and TNP.
Detailed Description
The present invention will be described in detail with reference to specific examples. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
A fluorescent test paper for detecting nitro compounds and a preparation method thereof, the preparation steps are as follows:
step 1, preparing fluorescent polyurethane, weighing p-HABAN, N' - ((2, 5-dihydroxy-1, 4-phenylene) di (methylene)) diacrylamide, 0.5-1 g), polyethylene glycol monomethyl ether (1-2 g), anhydrous tetrahydrofuran (20-25 mL), hexamethylene diisocyanate (1-2 g) and 1, 4-diazabicyclo [2.2.2] octane (0.1-0.5 g) according to a certain mass ratio, and adding the mixture into a dry two-neck round-bottom flask. The solution is heated at 60-80 ℃ for 6-8 hours under nitrogen. After the clear solution became very viscous, the product precipitated from excess ether and was then dried under vacuum for some time to give the product.
Step 2, dissolve the product (0.1-0.3 g) in acetonitrile: and (2) soaking a paper sheet cut into a size of (1-3) cm x (2-5) cm in a solution of a water (1: 1-1.5 v/v) solution in acetonitrile containing a product: taking out and drying the paper after 2-5min in the mixed solution of water to obtain the fluorescent paper.
Example 1:
p-HABA (0.72g), polyethylene glycol monomethyl ether (1.19g), anhydrous tetrahydrofuran (24mL), hexamethylene diisocyanate (1.80g) and 1, 4-diazabicyclo [2.2.2] octane (0.35g) were weighed into a dry two-necked round-bottomed flask. The solution was heated at 75 ℃ for 8 hours under nitrogen atmosphere. After the clear solution became very viscous, the product precipitated from excess ether and was then dried under vacuum for 24h to give the product.
0.11g of the product was dissolved in acetonitrile: in a solution of aqueous solution (1: 1v/v) (10mM), then a paper sheet cut to a size of 1 cm. times.4 cm was soaked in acetonitrile containing the product: and (3) taking out and drying the mixed solution of water (10mM) after 3min to obtain a fluorescent paper sheet.
FIG. 1 is a graph showing fluorescence response behavior of test strips prepared according to example 1 of the present invention at different concentrations of NP and TNP. It can be obviously seen that the fluorescence of the test paper is weaker and weaker along with the increase of the concentration of the nitro compound, and the test paper has higher sensitivity to TNP.
Example 2:
p-HABA (0.72g), polyethylene glycol monomethyl ether (1.19g), anhydrous tetrahydrofuran (24mL), hexamethylene diisocyanate (1.80g) and 1, 4-diazabicyclo [2.2.2] octane (0.35g) were weighed into a dry two-necked round-bottomed flask. The solution was heated at 75 ℃ for 8 hours under nitrogen atmosphere. After the clear solution became very viscous, the product precipitated from excess ether and was then dried under vacuum for 24h to give the product.
0.11g of the product was dissolved in acetonitrile: in a solution of aqueous solution (1: 1.5v/v) (10mM), then a paper sheet cut to a size of 1cm × 4cm was soaked in acetonitrile containing the product: and (3) taking out and drying the mixed solution of water (10mM) after 3min to obtain a fluorescent paper sheet.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The fluorescent test paper for detecting the nitro compound is characterized by being prepared by the following steps:
the method comprises the following steps: preparing fluorescent polyurethane: weighing 0.5-1 g of N, N' - ((2, 5-dihydroxy-1, 4-phenylene) bis (methylene)) bisacrylamide, 1-2 g of polyethylene glycol monomethyl ether, 20-25 mL of anhydrous tetrahydrofuran, 1-2 g of hexamethylene diisocyanate, and 0.1-0.5 g of 1, 4-diazabicyclo [2.2.2] octane into a dry container and mixing to obtain a uniform solution; then heating the solution at 60-80 ℃ for 6-8 hours; adding ether after the solution is viscous, and performing vacuum drying to obtain fluorescent polyurethane;
step two: 0.1-0.3 g of fluorescent polyurethane is dissolved in a mixed solution of acetonitrile and water, and then a cut paper sheet is soaked and dried to obtain the fluorescent test paper for detecting the nitro compound.
2. The fluorescence test paper for detecting nitro compounds according to claim 1, wherein the ratio of acetonitrile to water is 1: 1 to 1.5.
3. The fluorescence test paper for detecting nitro compounds according to claim 1 or 2, wherein the paper is soaked for 2 to 5 minutes.
4. The fluorescence test paper for detecting a nitro compound according to claim 1 or 2, wherein the size of the paper sheet is 1 to 3cm x 2 to 5 cm.
5. The fluorescence test paper for detecting nitro compounds according to claim 3, wherein the size of the paper sheet is 1 to 3cm x 2 to 5 cm.
6. A preparation method of fluorescent test paper for detecting nitro compounds is characterized by comprising the following steps:
the method comprises the following steps: preparing fluorescent polyurethane: weighing 0.5-1 g of N, N' - ((2, 5-dihydroxy-1, 4-phenylene) bis (methylene)) bisacrylamide, 1-2 g of polyethylene glycol monomethyl ether, 20-25 mL of anhydrous tetrahydrofuran, 1-2 g of hexamethylene diisocyanate, and 0.1-0.5 g of 1, 4-diazabicyclo [2.2.2] octane into a dry container and mixing to obtain a uniform solution; then heating the solution at 60-80 ℃ for 6-8 hours; adding ether after the solution is viscous, and performing vacuum drying to obtain fluorescent polyurethane;
step two: 0.1-0.3 g of fluorescent polyurethane is dissolved in a mixed solution of acetonitrile and water, and then a cut paper sheet is soaked and dried to obtain the fluorescent test paper for detecting the nitro compound.
7. The method for preparing a fluorescence test paper for detecting nitro compounds according to claim 6, wherein the ratio of acetonitrile to water is 1: 1 to 1.5.
8. The method for preparing a fluorescence test paper for detecting nitro compounds according to claim 6 or 7, wherein the paper is soaked for 2-5 minutes.
9. The method of producing a fluorescent test paper for the detection of nitro compounds according to claim 6 or 7, wherein the size of the paper sheet is 1 to 3cm x 2 to 5 cm.
10. The method of claim 8, wherein the size of the paper is 1-3cm x 2-5 cm.
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