CN110627130B - Composite oxide gas-sensitive material sensitive to trimethylamine - Google Patents
Composite oxide gas-sensitive material sensitive to trimethylamine Download PDFInfo
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- CN110627130B CN110627130B CN201910835344.7A CN201910835344A CN110627130B CN 110627130 B CN110627130 B CN 110627130B CN 201910835344 A CN201910835344 A CN 201910835344A CN 110627130 B CN110627130 B CN 110627130B
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- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 63
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 39
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 35
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000035945 sensitivity Effects 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 239000012065 filter cake Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 21
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 19
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 19
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 16
- 239000002105 nanoparticle Substances 0.000 claims description 14
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 11
- 229940010552 ammonium molybdate Drugs 0.000 claims description 11
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 11
- 239000011609 ammonium molybdate Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 150000002505 iron Chemical class 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 150000008064 anhydrides Chemical class 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000012467 final product Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 206010006784 Burning sensation Diseases 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 235000013332 fish product Nutrition 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 230000000622 irritating effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0003—Composite materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
- Food Science & Technology (AREA)
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Abstract
The invention discloses a trimethylamine-sensitive composite oxide gas-sensitive material, which is prepared from MoO3、Fe2O3And SnO2The sensor can be used as a sensitive material of trimethylamine for a trimethylamine detector. The composite oxide gas-sensitive material has higher sensitivity to trimethylamine, high accuracy and shorter response time. Meanwhile, the preparation method of the composite oxide gas-sensitive material is simple in process, low in dosage price and suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the field of industrial sensor materials, and particularly relates to a trimethylamine-sensitive composite oxide gas-sensitive material which is composed of MoO3、Fe2O3And SnO2The sensor can be used as a sensitive material of trimethylamine for a trimethylamine detector.
Background
Trimethylamine is one of the most common major gaseous pollutants, and is flammable and explosive, and its vapor can form an explosive mixture with air. It is easy to cause combustion and explosion when exposed to fire and high heat. Toxic smoke is generated by thermal decomposition. Contact with the oxidizing agent will react violently. Its vapor is heavier than air and can diffuse to a considerable distance at a lower position, causing a flashback in the case of an open flame. The main harm to the human body is the irritating effect on the eyes, nose, throat and respiratory tract. Concentrated aqueous trimethylamine solution can cause severe burning sensation and flushing of the skin, and spot bleeding can still remain on the skin after the solution is washed away. The eyes, the nose and the throat feel dry and uncomfortable after long-term contact. The fishy smell of the fish product mainly comes from trimethylamine, so that the gas sensor for detecting the freshness of the fish is realized by detecting the trimethylamine. Therefore, the method has important significance for accurately detecting the concentration of the trimethylamine. Currently, various methods for detecting trimethylamine are available, such as ion chromatography, high performance chromatography, and the like. However, these methods cannot be applied to gas sensitive materials highly sensitive to trimethylamine. In order to further improve the detection accuracy and precision. There is a need to develop gas sensitive materials with higher sensitivity to trimethylamine.
Disclosure of Invention
In order to solve the problems in the prior art, according to one aspect of the invention, a composite oxide gas-sensitive material with high sensitivity to trimethylamine is provided, and the gas-sensitive material can be used for preparing a trimethylamine detector, can realize the rapid, high-precision and high-accuracy determination of the concentration of trace trimethylamine in air, and is not interfered by other coexisting substances.
The composite oxide gas-sensitive material consists of MoO3、Fe2O3And SnO2The weight ratio of the three substances is 3-6:3-9:1, preferably 3-4:3-5:1, more preferably 3:5:1, and the composite oxide gas-sensitive material is prepared by the following method:
1) dissolving ammonium molybdate and ferric salt in deionized water, dropwise adding ammonia water under stirring to adjust the pH value of the solution to 6.7-8.3, continuously stirring for 6-12 hours, standing for settling, filtering, washing a filter cake for 3 times by using the deionized water, then placing the filter cake in an oven, raising the temperature to 700 ℃ at the speed of raising the temperature by 6 ℃ per minute, then preserving the temperature for 2-4 hours, cooling to room temperature, and fully grinding to obtain MoO3And Fe2O3Composite nanoparticles;
2) SnCl4Dissolving in deionized water to form a solution, and then adding the MoO obtained in the step 1)3And Fe2O3Composite nano particles are added into the SnCl4And (3) dropwise adding ammonia water into the solution under the stirring condition to adjust the pH value of the solution to 7.5-9.4, continuously stirring for 4-6 hours, standing for settling, filtering, washing a filter cake for 3 times by using deionized water, then placing the filter cake in an oven, heating to 450 ℃ at the speed of heating to 6 ℃ per minute, then preserving heat for 2-4 hours, cooling to room temperature, and fully grinding to obtain the MoO-based nano-particles3、Fe2O3And SnO2The composite oxide gas-sensitive material is formed.
Preferably according to MoO3And Fe2O3The weight ratio of the added ammonium molybdate to the added iron salt in the step 1) is 1:0.5 to 1: 3.
Preferably, the iron salt in step 1) is selected from the group consisting of an anhydride of ferric chloride or ferric nitrate or a hydrate containing water of crystallization.
Preferably, according to SnO in step 2)2With MoO3And Fe2O3Total weight of both, SnCl4In such an amount that MoO is added3、Fe2O3And SnO2The weight ratio of the three substances is 3-6:3-9: 1.
Preferably, the dropping speed of the aqueous ammonia in the step 2) is controlled to be 0.5 to 1.5 drops/second.
Preferably, the particle size of the composite oxide gas-sensitive material obtained in the step 2) is between 20nm and 35 nm.
According to another aspect of the present invention, there is provided a trimethylamine detector using the composite oxide gas-sensitive material prepared according to the present invention.
Advantageous effects
The composite oxide gas-sensitive material prepared by the method has higher sensitivity to trimethylamine, high accuracy and shorter response time. Meanwhile, the preparation method of the composite oxide gas-sensitive material is simple in process, low in dosage price and suitable for large-scale industrial production.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The composite oxide gas-sensitive material consists of MoO3、Fe2O3And SnO2The weight ratio of the three substances is 3-6:3-9:1, preferably 3-4:3-5:1, more preferably 3:5:1, and when the ratio of the respective substances is within this range, the gas-sensitive material as trimethylamine has excellent sensitivity and selectivity.
The preparation method of the composite oxide gas-sensitive material comprises the following steps:
1) dissolving ammonium molybdate and ferric salt in deionized water, dropwise adding ammonia water under stirring to adjust the pH value of the solution to 6.7-8.3, continuously stirring for 6-12 hours, standing for settling, filtering, washing a filter cake for 3 times by using the deionized water, then placing the filter cake in an oven, raising the temperature to 700 ℃ at the speed of raising the temperature by 6 ℃ per minute, then preserving the temperature for 2-4 hours, cooling to room temperature, and fully grinding to obtain MoO3And Fe2O3Composite nanoparticles;
2) SnCl4Dissolving in deionized water to form a solution, and then adding the MoO obtained in the step 1)3And Fe2O3Composite nano particles are added into the SnCl4Adding ammonia water dropwise into the solution under stirring to adjust the pH value of the solution to 7.5-9.4, continuously stirring for 4-6 hours, standing for settling, filtering, washing the filter cake with deionized water for 3 times, placing the filter cake in an oven, raising the temperature to 450 ℃ at the speed of raising the temperature to 6 ℃ per minute, preserving the temperature for 2-4 hours, cooling to room temperature, and fully grinding to obtain the MoO-based catalyst3、Fe2O3And SnO2The composite oxide gas-sensitive material is formed.
Preferably according to MoO3And Fe2O3The weight ratio of the added ammonium molybdate to the added iron salt in the step 1) is 1:05 to 1: 3. When the proportion of ammonium molybdate and ferric salt is controlled within the range, the properties of the composite oxide gas-sensitive material, such as sensitivity, response time, accuracy and the like, can be effectively improved.
Preferably, according to SnO in step 2)2With MoO3And Fe2O3Total weight of both, SnCl4In such an amount that MoO is added3、Fe2O3And SnO2The weight ratio of the three substances is 3-6:3-9:1, preferably 3-4:3-5:1, and more preferably 3:5: 1. When the weight ratio of the above three substances is controlled within this range, the properties of the composite oxide gas-sensitive material can be optimized.
In addition, the inventors found that the dropping speed of the ammonia water in the step 2) has a certain influence on the performance of the final product, for example, controlling the dropping speed of the ammonia water to 0.5 to 1.5 drops/second can optimize the performance of the composite oxide gas-sensitive material, and if too slow or too fast, the performance of the final product is not good, which may be due to SnCl4The flocculation speed is different under the action of ammonia water, which results in MoO3And Fe2O3The adhesion on the composite nanoparticles is not sufficiently uniform or causes SnO during subsequent calcination2Overgrowth of (a).
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
1) About 15.11g of ammonium molybdate and about 37.46g of FeCl3Dissolving in 150ml of deionized water, dropwise adding ammonia water under the stirring condition to adjust the pH value of the solution to 7.5, continuously stirring for 6 hours, standing for settling, filtering, washing a filter cake for 3 times by using the deionized water, then placing the filter cake in an oven, raising the temperature to 700 ℃ at the speed of raising the temperature by 6 ℃ per minute, then preserving the temperature for 3 hours, cooling to room temperature, and fully grinding to obtain MoO3And Fe2O3Composite nanoparticles;
2) about 6.40g of SnCl4Dissolving the mixture in 200ml of deionized water to form a solution, and then adding the MoO obtained in the step 1)3And Fe2O3Composite nano particles are added into the SnCl4In the solution, ammonia water is dripped at the speed of 1 drop/second under the stirring condition to adjust the pH value of the solution to 8.7, the solution is continuously stirred for 6 hours, then the solution is kept stand and settled and filtered, a filter cake is washed by deionized water for 3 times, then the filter cake is placed in an oven, the temperature is raised to 450 ℃ at the speed of raising the temperature by 6 ℃ per minute, then the temperature is maintained for 2 to 4 hours, the filter cake is cooled to the room temperature and then fully ground, and MoO is obtained3、Fe2O3And SnO2Composed composite oxide gas-sensitive material in which MoO3、Fe2O3And SnO2The weight ratio of the three components is 3:5: 1.
And (4) analyzing by transmission electron microscope test, wherein the particle size of the obtained composite oxide gas-sensitive material is about 20nm to 35 nm.
The obtained composite oxide gas-sensitive material is used in a trimethylamine detector after being tabletted in a tablet press, and the linear detection range is 0.8-180 mg/m3The detection limit of trimethylamine is 0.05mg/m3There is no co-occurrence interference. It can be seen that the composite oxide gas-sensitive material prepared according to this example has high sensitivity.
Example 2
1) About 15.11g of ammonium molybdate and about 23.51g of FeCl3Dissolving in 150ml of deionized water, dropwise adding ammonia water under the stirring condition to adjust the pH value of the solution to 7.5, continuously stirring for 6 hours, standing for settling, filtering, washing a filter cake for 3 times by using the deionized water, then placing the filter cake in an oven, raising the temperature to 700 ℃ at the speed of raising the temperature by 6 ℃ per minute, then preserving the temperature for 3 hours, cooling to room temperature, and fully grinding to obtain MoO3And Fe2O3Composite nanoparticles;
2) about 6.40g of SnCl4Dissolving the mixture in 200ml of deionized water to form a solution, and then adding the MoO obtained in the step 1)3And Fe2O3Composite nano particles are added into the SnCl4In the solution, ammonia water is dripped at the speed of 1 drop/second under the stirring condition to adjust the pH value of the solutionStirring for 6 hours, standing for settling, filtering, washing the filter cake for 3 times by deionized water, placing the filter cake in an oven, heating to 450 ℃ at the speed of heating to 6 ℃ per minute, keeping the temperature for 2-4 hours, cooling to room temperature, and fully grinding to obtain the MoO-based active carbon nano-particles3、Fe2O3And SnO2Composed composite oxide gas-sensitive material in which MoO3、Fe2O3And SnO2The weight ratio of the three components is 3:3: 1.
And (4) analyzing by transmission electron microscope test, wherein the particle size of the obtained composite oxide gas-sensitive material is about 20nm to 35 nm.
The obtained composite oxide gas-sensitive material is used in a trimethylamine detector after being tabletted in a tablet press, and the linear detection range is 1.0 to 165mg/m3The detection limit of trimethylamine is 0.05mg/m3There is no co-occurrence interference. It can be seen that the composite oxide gas-sensitive material prepared according to this example has high sensitivity.
Example 3
1) About 15.11g of ammonium molybdate and about 67.42g of FeCl3Dissolving in 150ml of deionized water, dropwise adding ammonia water under the stirring condition to adjust the pH value of the solution to 7.5, continuously stirring for 6 hours, standing for settling, filtering, washing a filter cake for 3 times by using the deionized water, then placing the filter cake in an oven, raising the temperature to 700 ℃ at the speed of raising the temperature by 6 ℃ per minute, then preserving the temperature for 3 hours, cooling to room temperature, and fully grinding to obtain MoO3And Fe2O3Composite nanoparticles;
2) about 6.40g of SnCl4Dissolving the mixture in 200ml of deionized water to form a solution, and then adding the MoO obtained in the step 1)3And Fe2O3Composite nano particles are added into the SnCl4In the solution, ammonia water is dripped at the speed of 1 drop/second under the stirring condition to adjust the pH value of the solution to 8.7, the solution is continuously stirred for 6 hours, then the solution is kept stand and settled and filtered, a filter cake is washed by deionized water for 3 times, then the filter cake is placed in an oven, the temperature is raised to 450 ℃ at the speed of raising the temperature by 6 ℃ per minute, then the temperature is maintained for 2 to 4 hours, the filter cake is cooled to the room temperature and then fully ground, and MoO is obtained3、Fe2O3And SnO2Form a complexGas-sensitive materials of oxides, in which MoO3、Fe2O3And SnO2The weight ratio of the three components is 3:9: 1.
And (4) analyzing by transmission electron microscope test, wherein the particle size of the obtained composite oxide gas-sensitive material is about 40nm to 68 nm.
The obtained composite oxide gas-sensitive material is used in a trimethylamine detector after being tabletted in a tablet press, and the linear detection range is 1.2 to 154mg/m3The detection limit of trimethylamine is 0.8mg/m3There is no co-occurrence interference. It can be seen that the composite oxide gas-sensitive material prepared according to this example has high sensitivity.
Comparative example 1
A composite oxide gas-sensitive material was prepared in the manner of example 1, except that no iron salt was added. The obtained composite oxide gas-sensitive material is used in a trimethylamine detector after being tabletted in a tablet press, and the linear detection range is 2.7 to 136mg/m3The detection limit of trimethylamine is 1.2mg/m3There is no co-occurrence interference.
Comparative example 2
A composite oxide gas-sensitive material was prepared in the same manner as in example 1, except that ammonium molybdate was not added. The obtained composite oxide gas-sensitive material is used in a trimethylamine detector after being tabletted in a tabletting machine, is not sensitive to trimethylamine and cannot be detected.
Comparative example 3
Except that MoO3、Fe2O3And SnO2A composite oxide gas-sensitive material was prepared in the same manner as in example 1 except that the weight ratio of the three was adjusted to 3:5: 10. The obtained composite oxide gas-sensitive material is used in a trimethylamine detector after being tabletted in a tablet press, and the linear detection range is 1.0 to 164mg/m3The detection limit of trimethylamine is 0.9mg/m3However, there are cases where the coexisting materials interfere.
Comparative example 4
Except that SnO is not present2In addition, a composite oxide gas-sensitive material was prepared in the manner of example 1. The obtained composite oxide gas-sensitive material is used after being tabletted in a tablet pressIn the trimethylamine detector, the linear detection range is 5.46 to 102mg/m3The limit of trimethylamine detection is 3.4mg/m3There are cases of coexistence interference.
Comparative example 5
A composite oxide gas-sensitive material was prepared in the manner of example 1, except that the dropping speed of the aqueous ammonia in step 2) was controlled to 5 drops/sec. And (5) analyzing by transmission electron microscope test, wherein the particle size of the obtained composite oxide gas-sensitive material is about 80nm to 132 nm. The obtained composite oxide gas-sensitive material is used in a trimethylamine detector after being tabletted in a tablet press, and the linear detection range is 1.0 to 153mg/m3The detection limit of trimethylamine is 0.8mg/m3However, there are cases where the coexisting materials interfere.
As can be seen from comparison of the data of examples 1 to 3 and comparative examples 1 to 5, the composite oxide gas-sensitive material obtained by the preparation method of the present invention has a high sensitivity in detection of trimethylamine. Meanwhile, the preparation method also has important influence on the performance of the final product, for example, the adjustment of the dropping speed of the ammonia water in the comparative example 5 also has influence on the performance of the product.
Claims (8)
1. A composite oxide gas-sensitive material with high sensitivity to trimethylamine is prepared from MoO3、Fe2O3And SnO2The weight ratio of the three substances is 3-6:3-9:1, and the composite oxide gas-sensitive material is prepared by the following method:
1) dissolving ammonium molybdate and ferric salt in deionized water, dropwise adding ammonia water under stirring to adjust the pH value of the solution to 6.7-8.3, continuously stirring for 6-12 hours, standing for settling, filtering, washing a filter cake for 3 times by using the deionized water, then placing the filter cake in an oven, raising the temperature to 700 ℃ at the speed of raising the temperature by 6 ℃ per minute, then preserving the temperature for 2-4 hours, cooling to room temperature, and fully grinding to obtain MoO3And Fe2O3Composite nanoparticles;
2) SnCl4Dissolving in deionized water to form a solution, and then adding the MoO obtained in the step 1)3And Fe2O3Composite nano particles are added into the SnCl4Adding ammonia water dropwise into the solution under stirring to adjust the pH value of the solution to 7.5-9.4, continuously stirring for 4-6 hours, standing for settling, filtering, washing the filter cake with deionized water for 3 times, placing the filter cake in an oven, raising the temperature to 450 ℃ at the speed of raising the temperature to 6 ℃ per minute, preserving the temperature for 2-4 hours, cooling to room temperature, and fully grinding to obtain the MoO-based catalyst3、Fe2O3And SnO2The dropping speed of the ammonia water is controlled to be 0.5 drops/second to 1.5 drops/second.
2. The composite oxide gas-sensitive material of claim 1, wherein the MoO3、Fe2O3And SnO2The weight ratio of the three substances is 3-4:3-5: 1.
3. The composite oxide gas-sensitive material of claim 1, wherein the MoO3、Fe2O3And SnO2The weight ratio of the three substances is 3:5: 1.
4. The composite oxide gas-sensitive material according to any one of claims 1 to 3, characterized in that it is in terms of MoO3And Fe2O3The weight ratio of the added ammonium molybdate to the added iron salt in the step 1) is 1:0.5 to 1: 3.
5. The composite oxide gas-sensitive material according to any one of claims 1 to 3, wherein the iron salt in step 1) is selected from an anhydride of ferric chloride or ferric nitrate or a hydrate containing water of crystallization.
6. The composite oxide gas-sensitive material according to any one of claims 1 to 3, wherein in step 2) it is made according to SnO2With MoO3And Fe2O3Total weight of both, SnCl4In such an amount that MoO is added3、Fe2O3And SnO2The weight ratio of the three substances is 3-6:3-9: 1.
7. The composite oxide gas-sensitive material according to any one of claims 1 to 3, wherein the particle size of the composite oxide gas-sensitive material obtained in step 2) is between 20nm and 35 nm.
8. A trimethylamine detector, which is obtained by using the preparation of the composite oxide gas-sensitive material according to any one of claims 1 to 7.
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