CN113776978A - Tripropion triperoxide detection sensor and preparation method thereof - Google Patents
Tripropion triperoxide detection sensor and preparation method thereof Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000003380 quartz crystal microbalance Methods 0.000 claims abstract description 60
- 239000000463 material Substances 0.000 claims abstract description 27
- XJHMOGCOFPLTNG-UHFFFAOYSA-N 2,2-dihydroperoxypropane Chemical compound OOC(C)(C)OO XJHMOGCOFPLTNG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 150000002978 peroxides Chemical class 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 28
- 229910052782 aluminium Inorganic materials 0.000 claims description 28
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000412 dendrimer Substances 0.000 claims description 9
- 229920000736 dendritic polymer Polymers 0.000 claims description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 8
- -1 2, 3, 4, 5-tetraphenyl-phenyl Chemical group 0.000 claims description 7
- 238000004528 spin coating Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical group [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 3
- 238000006467 substitution reaction Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 238000010586 diagram Methods 0.000 description 15
- 239000007789 gas Substances 0.000 description 9
- ZTLXICJMNFREPA-UHFFFAOYSA-N 3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexaoxonane Chemical compound CC1(C)OOC(C)(C)OOC(C)(C)OO1 ZTLXICJMNFREPA-UHFFFAOYSA-N 0.000 description 7
- 239000002360 explosive Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000001871 ion mobility spectroscopy Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
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Abstract
The invention relates to a triacetoneperoxide detection sensor and a preparation method thereof, wherein the sensor comprises the following components: the device comprises a base, a top cover and a signal processing circuit for a quartz crystal microbalance, wherein the base and the top cover can be matched into a closed structure with a hollow core, the signal processing circuit for the quartz crystal microbalance is arranged in the hollow structure, a fixed position of a quartz crystal microbalance chip, an external power supply interface and a frequency meter interface are reserved on the signal processing circuit, a sensitive material capable of detecting triacetonene peroxide is spin-coated on the surface of the quartz crystal microbalance chip, and an air inlet and an air outlet and holes corresponding to the power supply interface and the frequency meter interface are reserved on the top cover. The sensor can realize the rapid detection of 0.5-50 ppm of tripropionone peroxide within 1min, and after the nitrogen is introduced and the sensor is cleared, the sensor can detect the tripropionone peroxide again, the test precision is not influenced, and the sensor is small in size and convenient to carry.
Description
Technical Field
The invention belongs to the field of sensors, and particularly relates to a triacetoneperoxide detection sensor and a preparation method thereof.
Background
Triacetone trioxide (TATP) is a peroxide having a cyclic structure consisting of nine atoms, and is not stable and is highly explosive when subjected to collision, friction or heat. During the explosion process, the tripropionone peroxide molecule releases acetone to disperse the oxygen atoms connected together to form oxygen and ozone, and the energy released in the process is enough to enable another molecule to generate chemical reaction to maintain the continuous generation of the reaction, so that the tripropionone peroxide explosive is a novel peroxide explosive.
The triacetalone peroxide is easy to prepare, the preparation process is simple, and the compound does not contain nitrogen, so that the detection of many existing explosive detectors can be easily avoided, and the triacetalone peroxide is used by terrorists. With the great uneasiness and panic of the public caused by terrorist attacks in the world, the explosive detection becomes a highly important problem for all countries, and the hidden explosive can be timely and effectively detected, which becomes an urgent task in the international society.
The existing technology for detecting trace tripropionone peroxide mainly comprises a solid-phase extraction chromatography-mass spectrometry technology, a high performance liquid chromatography fluorescence technology, an ion mobility spectrometry technology, a selective ion flow tube mass spectrometry technology based on an ion-molecule reaction principle and the like. However, the above detection method is generally suitable for laboratory detection due to the complexity of the instrument volume and the analysis method, but it cannot satisfy the requirements of simple, rapid and effective detection.
Disclosure of Invention
In view of the above, the invention aims to provide a triacetoneperoxide detection sensor which is suitable for the current situation that the conventional triacetoneperoxide does not contain nitrogen elements, can easily avoid a plurality of conventional explosive detectors, and is generally only suitable for laboratory detection due to the complex volume and analysis method of the conventional triacetoneperoxide detection method.
In order to achieve the purpose, the specific technical scheme of the invention is as follows:
1. a triacetoneperoxide detection sensor, the sensor comprising:
the device comprises a base, a top cover and a signal processing circuit for a quartz crystal microbalance, wherein the base and the top cover can be matched into a closed structure with a hollow core, the signal processing circuit for the quartz crystal microbalance is arranged in the hollow structure, a fixed position of a quartz crystal microbalance chip, an external power supply interface and a frequency meter interface are reserved on the signal processing circuit, a sensitive material capable of detecting triacetonene peroxide is spin-coated on the surface of the quartz crystal microbalance chip, and an air inlet and an air outlet and holes corresponding to the power supply interface and the frequency meter interface are reserved on the top cover.
Preferably, the frequency of the quartz crystal microbalance chip is 5-300 MHz, and the sensitive material is a dendritic polymer with a large number of benzene ring structures and microporous structures.
Preferably, the dendrimer is core-based on tetrakis (4-phenyl) methane, and is multiply substituted with 2, 3, 4, 5-tetraphenyl-phenyl at the 4-phenyl para-position of the tetrakis (4-phenyl) methane.
Preferably, the 2, 3, 4, 5-tetraphenyl-phenyl group may be substituted by 1-7 generations; when substituted multiply, the substitution position is in the para position of the phenyl substituent in the 3 and/or 4 position of the 2, 3, 4, 5-tetraphenyl-phenyl group.
Preferably, the closed structure is a square structure, and the hollow structure is a square structure.
Preferably, the closed structure is a cuboid structure, and the hollow structure is a cuboid structure.
2. A preparation method of a triacetoneperoxide detection sensor comprises the following steps:
(1) taking a cuboid aluminum block, grooving the aluminum block in the width direction, and forming 4-6 holes in the periphery of a sensor base;
(2) installing a signal processing circuit for the quartz crystal microbalance in the middle of the aluminum block slot in the step (1), wherein a fixed position of a quartz crystal microbalance chip, a power interface and a frequency meter interface are reserved on the signal processing circuit;
(3) spin-coating a sensitive material capable of detecting triacetoneperoxide on a quartz crystal microbalance chip and placing the chip in the fixed position in the step (1);
(4) processing an aluminum block into a sensor top cover, wherein 4-6 pillars are arranged on the periphery of the top cover and matched with a base, the top cover is just combined with the base into a closed box after matching, meanwhile, air inlets and air outlets with the diameter of 2-6 mm are reserved on two sides of the top cover, and 2 holes in front of the top cover correspond to the positions of a power supply interface and a frequency meter interface;
(5) and (4) buckling the top cover in the step (4) on a sensor base provided with the step (2) and the step (3), and switching on a power supply and a frequency meter to obtain the triacetonene peroxide sensor.
Preferably, in the step (1), the length of the cuboid is 6-12 cm, the width of the cuboid is 5-8 cm, the height of the cuboid is 3-6 cm, the groove is opened along the width direction of the base, the length of the groove is 3-5 cm, and the depth of the groove is 1-2 cm.
Preferably, the sensitive material is a dendritic polymer having a large number of benzene ring structures and a microporous structure.
Preferably, the amount of the sensitive material spin-coated on the quartz crystal microbalance chip in the step (3) is 20-200 μ g.
The invention has the beneficial effects that:
compared with the prior art, the invention provides a triacetoneperoxide detection sensor, dendritic polymers with a large number of benzene ring structures and microporous structures are used as sensitive materials of the triacetoneperoxide, and after a target molecule to be detected is selectively adsorbed by the sensitive materials in the sensor, the weight, resistance, frequency and other physical parameters which can be directly measured change, so that the corresponding relation between the content of the target molecule and the physical parameters such as the weight, the resistance, the frequency and the like is established, and the online rapid detection of the trace amount of the triacetoneperoxide is realized. The sensor can realize the rapid detection of 0.5-50 ppm of tripropionone peroxide within 1min, and after the nitrogen is introduced and the sensor is cleared, the sensor can detect the tripropionone peroxide again, the test precision is not influenced, and the sensor is small in size and convenient to carry.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a plan view of the lower portion of the sensor cap of the present invention;
FIG. 2 is a top view of a lower portion of a sensor cap according to the present invention;
FIG. 3 is a planer view of the sensor head of the present invention;
FIG. 4 is a front view of a sensor top cover of the present invention;
FIG. 5 is a bottom view of the sensor top cover of the present invention;
FIG. 6 is a schematic structural diagram of a sensor sensitive material of the present invention;
fig. 7 is a detector response curve.
Reference numerals: 1-base, 2-signal processing circuit, 3-chip, 4-sensitive material, 5-hole, 6-power interface, 7-frequency meter interface, 8-top cover column, 9-gas port (91-gas inlet, 92-gas outlet), 10-top cover.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and examples may be combined with each other without conflict.
Wherein the showings are for the purpose of illustrating the invention only and not for the purpose of limiting the same, and in which there is shown by way of illustration only and not in the drawings in which there is no intention to limit the invention thereto; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components, and the terms describing the positional relationship in the drawings are only for illustrative purposes and are not to be construed as limiting the present invention, and the specific meanings of the above terms will be understood by those skilled in the art according to the specific circumstances.
The invention discloses a triacetoneperoxide detection sensor. The sensor comprises a base, a top cover and a signal processing circuit for a quartz crystal microbalance, wherein the base and the top cover can be matched into a closed structure with a hollow structure, the signal processing circuit for the quartz crystal microbalance is arranged in the hollow structure, a fixed position of a quartz crystal microbalance chip, an external power supply interface and a frequency meter interface are reserved on the signal processing circuit, a sensitive material capable of detecting triacetonene peroxide is spin-coated on the surface of the quartz crystal microbalance chip, and an air inlet and an air outlet and holes corresponding to the power supply interface and the frequency meter interface are reserved on the top cover.
The frequency of the quartz crystal microbalance chip is 5-300 MHz, and the sensitive material is a dendritic polymer with a large number of benzene ring structures and micropore structures. The dendritic polymer takes tetra (4-phenyl) methane as a core, the 4-phenyl para position of the tetra (4-phenyl) methane is sequentially substituted by 2, 3, 4, 5-tetraphenyl-phenyl for multiple generations, the closed structure is of a cubic structure, and the hollow structure is of a cubic structure.
The method of making the sensor of the present invention is described below with reference to figures 1-6.
Example 1
(1) Processing an aluminum block into a length of 12cm, a width of 8cm and a height of 4cm, wherein a groove is formed in the middle of the aluminum block, the groove is opened in the width direction of the base, the length direction of the base is 4cm, the depth of the base is 2cm, 6 open holes are formed in the periphery of the sensor base, and a planing surface diagram and a top view of the sensor base are respectively shown in an attached drawing 1 and an attached drawing 2;
(2) installing a commercialized quartz crystal microbalance in the middle of the aluminum block slot in the step (1) by using a signal processing circuit, wherein a fixed position of a quartz crystal microbalance chip, a power supply interface and a frequency meter interface are reserved on the signal processing circuit, and a planing surface diagram and a top view of the quartz crystal microbalance chip are respectively shown in the attached drawings 1 and 2;
(3) coating 30 mu g of sensitive material on a quartz crystal microbalance chip by spin coating, and then mounting the quartz crystal microbalance chip on the signal processing circuit in the substep (2), wherein the frequency of the quartz crystal microbalance chip is 5MHz, and the sensitive material has a structure shown in figure 6, wherein n is 2;
(4) processing an aluminum block into a sensor top cover, wherein 6 pillars are arranged on the periphery of the top cover and matched with a base, the top cover is just combined with the base into a closed box after being matched, meanwhile, air inlets and air outlets with the diameter of 4mm are reserved on two sides of the top cover, 2 holes are formed in the front of the top cover and correspond to the positions of a power supply interface and a frequency meter interface, and the planing surface diagram, the front view and the bottom view of the top cover are respectively shown in the attached drawings 3, 4 and 5;
(5) and (4) buckling the top cover in the step (4) on a sensor base provided with the step (2) and the step (3), and switching on a power supply and a frequency meter to obtain the triacetonene peroxide sensor.
Example 2
(1) Processing an aluminum block into a length of 12cm, a width of 8cm and a height of 4cm, wherein a groove is formed in the middle of the aluminum block, the groove is opened in the width direction of the base, the length direction of the base is 4cm, the depth of the base is 2cm, 6 open holes are formed in the periphery of the sensor base, and a planing surface diagram and a top view of the sensor base are respectively shown in an attached drawing 1 and an attached drawing 2;
(2) installing a commercialized quartz crystal microbalance in the middle of the aluminum block slot in the step (1) by using a signal processing circuit, wherein a fixed position of a quartz crystal microbalance chip, a power supply interface and a frequency meter interface are reserved on the signal processing circuit, and a planing surface diagram and a top view of the quartz crystal microbalance chip are respectively shown in the attached drawings 1 and 2;
(3) coating 100 mu g of sensitive material on a quartz crystal microbalance chip by spin coating, and then mounting the quartz crystal microbalance chip on the signal processing circuit in the substep (2), wherein the frequency of the quartz crystal microbalance chip is 5MHz, and the sensitive material has a structure shown in figure 6, wherein n is 2;
(4) processing an aluminum block into a sensor top cover, wherein 6 pillars are arranged on the periphery of the top cover and matched with a base, the top cover is just combined with the base into a closed box after being matched, meanwhile, air inlets and air outlets with the diameter of 4mm are reserved on two sides of the top cover, 2 holes are formed in the front of the top cover and correspond to the positions of a power supply interface and a frequency meter interface, and the planing surface diagram, the front view and the bottom view of the top cover are respectively shown in the attached drawings 3, 4 and 5;
(5) and (4) buckling the top cover in the step (4) on a sensor base provided with the step (2) and the step (3), and switching on a power supply and a frequency meter to obtain the triacetonene peroxide sensor.
Example 3
(1) Processing an aluminum block into a length of 12cm, a width of 8cm and a height of 4cm, wherein a groove is formed in the middle of the aluminum block, the groove is opened in the width direction of the base, the length direction of the base is 4cm, the depth of the base is 2cm, 6 open holes are formed in the periphery of the sensor base, and a planing surface diagram and a top view of the sensor base are respectively shown in an attached drawing 1 and an attached drawing 2;
(2) installing a commercialized quartz crystal microbalance in the middle of the aluminum block slot in the step (1) by using a signal processing circuit, wherein a fixed position of a quartz crystal microbalance chip, a power supply interface and a frequency meter interface are reserved on the signal processing circuit, and a planing surface diagram and a top view of the quartz crystal microbalance chip are respectively shown in the attached drawings 1 and 2;
(3) coating 30 mu g of sensitive material on a quartz crystal microbalance chip by spin coating, and then mounting the quartz crystal microbalance chip on the signal processing circuit in the substep (2), wherein the frequency of the quartz crystal microbalance chip is 100MHz, and the sensitive material has a structure shown in figure 6, wherein n is 2;
(4) processing an aluminum block into a sensor top cover, wherein 6 pillars are arranged on the periphery of the top cover and matched with a base, the top cover is just combined with the base into a closed box after being matched, meanwhile, air inlets and air outlets with the diameter of 4mm are reserved on two sides of the top cover, 2 holes are formed in the front of the top cover and correspond to the positions of a power supply interface and a frequency meter interface, and the planing surface diagram, the front view and the bottom view of the top cover are respectively shown in the attached drawings 3, 4 and 5;
(5) and (4) buckling the top cover in the step (4) on a sensor base provided with the step (2) and the step (3), and switching on a power supply and a frequency meter to obtain the triacetonene peroxide sensor.
Example 4
(1) Processing an aluminum block into a length of 10cm, a width of 7cm and a height of 6cm, wherein a groove is formed in the middle of the aluminum block, the groove is opened in the width direction of the base, the length direction of the base is 6cm, the depth of the base is 4cm, and 4 holes are formed in the periphery of the base of the sensor;
(2) installing a commercialized quartz crystal microbalance in the middle of the aluminum block slot in the step (1) by using a signal processing circuit, wherein a fixed position of a quartz crystal microbalance chip, a power supply interface and a frequency meter interface are reserved on the signal processing circuit, and a planing surface diagram and a top view of the quartz crystal microbalance chip are respectively shown in the attached drawings 1 and 2;
(3) coating 30 mu g of sensitive material on a quartz crystal microbalance chip by spin coating, and then mounting the quartz crystal microbalance chip on the signal processing circuit in the substep (2), wherein the frequency of the quartz crystal microbalance chip is 5MHz, and the sensitive material has a structure shown in figure 6, wherein n is 2;
(4) processing an aluminum block into a sensor top cover, wherein 4 pillars are arranged on the periphery of the top cover and matched with a base, the top cover is just combined with the base into a closed box after being matched, meanwhile, air inlets and air outlets with the diameter of 4mm are reserved on two sides of the top cover, 2 holes are formed in the front of the top cover and correspond to the positions of a power supply interface and a frequency meter interface, and the planing surface diagram, the front view and the bottom view of the top cover are respectively shown in the attached drawings 3, 4 and 5;
(5) and (4) buckling the top cover in the step (4) on a sensor base provided with the step (2) and the step (3), and switching on a power supply and a frequency meter to obtain the triacetonene peroxide sensor.
Example 5
(1) Processing an aluminum block into a length of 12cm, a width of 8cm and a height of 4cm, wherein a groove is formed in the middle of the aluminum block, the groove is opened in the width direction of the base, the length direction of the base is 4cm, the depth of the base is 2cm, 6 open holes are formed in the periphery of the sensor base, and a planing surface diagram and a top view of the sensor base are respectively shown in an attached drawing 1 and an attached drawing 2;
(2) installing a commercialized quartz crystal microbalance in the middle of the aluminum block slot in the step (1) by using a signal processing circuit, wherein a fixed position of a quartz crystal microbalance chip, a power supply interface and a frequency meter interface are reserved on the signal processing circuit, and a planing surface diagram and a top view of the quartz crystal microbalance chip are respectively shown in the attached drawings 1 and 2;
(3) coating 30 mu g of sensitive material on a quartz crystal microbalance chip by spin coating, and then mounting the quartz crystal microbalance chip on the signal processing circuit in the substep (2), wherein the frequency of the quartz crystal microbalance chip is 5MHz, and the sensitive material has a structure shown in figure 6, wherein n is 5;
(4) processing an aluminum block into a sensor top cover, wherein 6 pillars are arranged on the periphery of the top cover and matched with a base, the top cover is just combined with the base into a closed box after being matched, meanwhile, air inlets and air outlets with the diameter of 4mm are reserved on two sides of the top cover, 2 holes are formed in the front of the top cover and correspond to the positions of a power supply interface and a frequency meter interface, and the planing surface diagram, the front view and the bottom view of the top cover are respectively shown in the attached drawings 3, 4 and 5;
(5) and (4) buckling the top cover in the step (4) on a sensor base provided with the step (2) and the step (3), and switching on a power supply and a frequency meter to obtain the triacetonene peroxide sensor.
In order to verify the detection performance of the detector, the test is carried out according to the following steps:
the quartz crystal microbalance chip developed in example 1 was placed in a sample cell, the sample lid was closed, and the resonant frequency of the chip was first tested. The response curves when 8ppm of TATP gas was fed and saturated, nitrogen was fed again, and then 0.5, 2, and 8ppm of TATP gas was fed again after saturation, as shown in FIG. 7. It can be seen that whether the TATP gas is introduced or the nitrogen gas is introduced again, the QCM sensor can reach saturation within 1min, the sensor can desorb after the nitrogen gas is introduced, and the QCM sensor can detect 0.5ppm of TATP gas newly after the TATP gas is introduced again, so that the sensor prepared by the technical scheme can detect 0.5ppm of TATP gas within 1 min. Further, the same detection effect can be achieved by performing the detection in the above manner in examples 2 to 5.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (10)
1. A triacetoneperoxide detection sensor, comprising:
the device comprises a base, a top cover and a signal processing circuit for a quartz crystal microbalance, wherein the base and the top cover can be matched into a closed structure with a hollow core, the signal processing circuit for the quartz crystal microbalance is arranged in the hollow structure, a fixed position of a quartz crystal microbalance chip, an external power supply interface and a frequency meter interface are reserved on the signal processing circuit, a sensitive material capable of detecting triacetonene peroxide is spin-coated on the surface of the quartz crystal microbalance chip, and an air inlet and an air outlet and holes corresponding to the power supply interface and the frequency meter interface are reserved on the top cover.
2. The triacetoneperoxide detection sensor according to claim 1, wherein the quartz crystal microbalance chip has a frequency of 5-300 MHz, and the sensitive material is a dendritic polymer having a large number of benzene ring structures and a microporous structure.
3. The triacetoneperoxide detection sensor according to claim 2, wherein the dendrimer is core-tetrakis (4-phenyl) methane, and is substituted with 2, 3, 4, 5-tetraphenyl-phenyl at the 4-phenyl para-position of tetrakis (4-phenyl) methane in order of generations.
4. The triacetoneperoxide detection sensor according to claim 3, wherein the 2, 3, 4, 5-tetraphenyl-phenyl group can be substituted by 1 to 7; when substituted multiply, the substitution position is in the para position of the phenyl substituent in the 3 and/or 4 position of the 2, 3, 4, 5-tetraphenyl-phenyl group.
5. The triacetoneperoxide detection sensor according to claim 1, wherein the sealing structure has a cubic structure, and the hollow structure has a cubic structure.
6. The triacetoneperoxide detection sensor according to claim 1, wherein the closed structure has a rectangular parallelepiped structure, and the hollow structure has a rectangular parallelepiped structure.
7. A preparation method of a triacetoneperoxide detection sensor is characterized by comprising the following steps:
(1) taking a cuboid aluminum block, grooving the aluminum block in the width direction, and forming 4-6 holes in the periphery of a sensor base;
(2) installing a signal processing circuit for the quartz crystal microbalance in the middle of the aluminum block slot in the step (1), wherein a fixed position of a quartz crystal microbalance chip, a power interface and a frequency meter interface are reserved on the signal processing circuit;
(3) spin-coating a sensitive material capable of detecting triacetoneperoxide on a quartz crystal microbalance chip and placing the chip in the fixed position in the step (1);
(4) processing an aluminum block into a sensor top cover, wherein 4-6 pillars are arranged on the periphery of the top cover and matched with a base, the top cover is just combined with the base into a closed box after matching, meanwhile, air inlets and air outlets with the diameter of 2-6 mm are reserved on two sides of the top cover, and 2 holes in front of the top cover correspond to the positions of a power supply interface and a frequency meter interface;
(5) and (4) buckling the top cover in the step (4) on a sensor base provided with the step (2) and the step (3), and switching on a power supply and a frequency meter to obtain the triacetonene peroxide sensor.
8. The method for preparing the triacetoneperoxide detection sensor according to claim 7, characterized in that in the step (1), the rectangular body has a length of 6-12 cm, a width of 5-8 cm and a height of 3-6 cm, and the open groove is perforated along the width direction of the base, and has a length of 3-5 cm and a depth of 1-2 cm.
9. The method for preparing a triacetoneperoxide detection sensor according to claim 7, wherein the sensitive material is a dendrimer having a large number of benzene ring structures and pore structures.
10. The method for preparing a triacetoneperoxide detection sensor according to claim 7, wherein the amount of the sensitive material spin-coated on the quartz crystal microbalance chip in the step (3) is 20-200 μ g.
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| CN101105476A (en) * | 2006-07-14 | 2008-01-16 | 中国科学院声学研究所 | Difference frequency type film acoustic wave resonator based micro-mass sensor |
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