CN103482705A - Method for preparing iron molybdate micro-nano materials with sensitive feature for low-concentration H2S - Google Patents

Method for preparing iron molybdate micro-nano materials with sensitive feature for low-concentration H2S Download PDF

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CN103482705A
CN103482705A CN201310421242.3A CN201310421242A CN103482705A CN 103482705 A CN103482705 A CN 103482705A CN 201310421242 A CN201310421242 A CN 201310421242A CN 103482705 A CN103482705 A CN 103482705A
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CN103482705B (en
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陈玉金
刘照虹
吴红雨
徐铮
朱春玲
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Nanhai Innovation And Development Base Of Sanya Harbin Engineering University
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Harbin Engineering University
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Abstract

The invention provides a method for preparing iron molybdate micro-nano materials with the sensitive feature for low-concentration H2S. The method comprises the steps of calcinating ammonium molybdate powder for four hours at the temperature of 500 DEG C, dissolving 30-35mg of MoO3 powder, 0.5-0.6g of urea and 30-35mg of thioacetamide in a mixed solution containing 15ml of deionized water and 25ml of ethyl alcohol, conducting heating for 24 hours at the temperature of 200 DEG C to obtain flower-shaped MoS2 powder, calcinating the MoS2 powder in the air for 2-5 hours at the temperature of 400-600 DEG C, dissolving the obtained product in a Fe(NO3)3 solution, conducting stirring for 1-3 hours in a 50-60 DEG C water bath, conducting suction filtration, adding the product obtained in the last step in the Fe(NO3)3 solution, then conducting stirring for 1-3 hours in the 50-60 DEG C water bath, conducting vacuum drying, conducting calcination for 3-5 hours in the air at the 5 DEG C/min heating rate at the temperature of 400-600 DEG C, conducting natural cooling, and obtaining the iron molybdate micro-nano materials with the sensitive feature for the low-concentration H2S. The method for preparing the iron molybdate micro-nano materials is simple, the obtained iron molybdate micro-nano materials are high in sensitivity for the low-concentration H2S, good in selection performance and short in response-recovery time, and at the temperature of 270 DEG C, the 0.5ppm H2S gas can be detected.

Description

A kind of have lower concentration H 2the preparation method of S sensitivity characteristics iron molybdate micro Nano material
Technical field
That the present invention relates to is a kind of nanostructure conductor oxidate gas sensor material preparation method, specifically a kind of H 2the preparation method of S gas sensitive can.
Background technology
Hydrogen sulfide is a kind of acute hypertoxic gas, and the people sucks a small amount of high-concentration hydrogen sulfide can be fatal within the short period of time.The hydrogen sulfide of lower concentration is all influential to eye, respiratory system and nervus centralis.Simultaneously, H 2s or a kind of inflammable gas, can form explosive mixture with air mixed, and chance naked light, high heat energy cause combustion explosion.Itself and concentrated nitric acid, oleum or other strong oxidizer vigorous reaction, blast.H 2s gas is heavier than air, and can be diffused in lower place quite far away, meets naked light and can cause and strile-back.
In the processes such as Chemical Manufacture, atmospheric environment detection, power system security detection, oil and gas and mineral deposit exploration, due to H 2the existence of S gas, can have a strong impact on production safety, so people urgently develop and can detect micro-H 2the gas sensor of S gas.Nearly ten years, both at home and abroad at H 2the aspects such as the research of S gas sensitive, exploitation and application have all obtained larger progress, simultaneously also exist some that problem to be solved is arranged, for example gas sensitive in highly sensitive (especially to lower concentration H 2s), the aspect such as quick-speed response-recovery fails to meet simultaneously; The stability of sensor is inadequate; Complicated process of preparation.
Summary of the invention
The purpose of this invention is to provide a kind of technique simple, prepared material highly sensitive, response-time of recovery is short has lower concentration H 2the preparation method of S sensitivity characteristics iron molybdate micro Nano material.
The object of the present invention is achieved like this:
(1) by ammonium molybdate powder 4 hours preparation MoO of 500 ℃ of temperature lower calcinations in air 3powder; MoO by 30-35mg 3powder, 0.5-0.6g urea and 30-35mg thioacetamide are dissolved in 15ml deionized water and 25ml alcohol mixed solution, and at 200 ℃ of temperature, heating is 24 hours, and cooling rear cleaning, drying, obtain flowers shape MoS 2powder raw material;
(2) by MoS 2powder, in air, is calcined 2-5 hour under 400 ℃ of-600 ℃ of conditions;
(3) the 0.01-0.075g products therefrom is dissolved in to the Fe (NO of 0.01-0.02mol/L 3) 3in solution, 50-60 ℃ of stirring in water bath 1-3 hour, suction filtration;
(4) upper step product is joined to the Fe (NO of 0.01-0.02mol/L 3) 350-60 ℃ of stirring in water bath 1-3 hour in solution;
(5) by products therefrom vacuum-drying;
(6) products therefrom is with the temperature rise rate 400-600 ℃ of calcining 3-5 hour in air of 5 ℃/min, and naturally cooling, obtain having lower concentration H 2s sensitivity characteristics iron molybdate micro Nano material.
Preparation method of the present invention is simple, and prepared iron molybdate micro Nano material is to lower concentration H 2s is highly sensitive, selectivity good, response-time of recovery is short, the H of 0.5ppm can be detected under 270 ℃ 2s gas.
The accompanying drawing explanation
Fig. 1 of the present inventionly has lower concentration H 2the electron scanning micrograph of S sensitivity characteristics iron molybdate micro Nano material;
Fig. 2 of the present inventionly has lower concentration H 2s sensitivity characteristics iron molybdate micro Nano material X ray diffracting data;
Fig. 3 of the present inventionly has lower concentration H 2the H of S sensitivity characteristics iron molybdate micro Nano material to different concns 2the response of S gas-recovery characteristics curve;
Fig. 4 of the present inventionly has lower concentration H 2s sensitivity characteristics iron molybdate micro Nano material is to the response of the alcohol gas of different concns-recovery characteristics curve;
Fig. 5 of the present inventionly has lower concentration H 2s sensitivity characteristics iron molybdate micro Nano material is to the response of the acetone gas of different concns-recovery characteristics curve.
Embodiment
Below for example the present invention is described in more detail.
Embodiment 1:
(1) starting material preparation: ammonium molybdate powder is calcined in air to 500 ℃ of 4 hours preparation MoO 3powder; MoO by 35mg 3powder, 0.6g urea and 35mg thioacetamide are dissolved in 15ml deionized water and 25ml alcohol mixed solution, be placed in autoclave, in baking oven 200 ℃, heat 24 hours, cooling rear cleaning, drying, obtain flowers shape MoS 2starting material.
(2) by 1g MoS 2powder in air 500 ℃ annealing 4 hours.
(3) the products therefrom 0.075g that will anneal is dissolved in the Fe (NO of the 0.014mol/L of 300mL 3) 3in solution, 50 ℃ of stirring in water bath 2 hours, suction filtration.
(4) the previous step product is all joined to the Fe (NO of the 0.014mol/L of 300mL 3) 3in solution, 50 ℃ of stirring in water bath are 2 hours.
(5) by products therefrom vacuum-drying in 40 ℃.
(6) products therefrom was with 500 ℃ of heating of the temperature rise rate of 5 ℃/min 4 hours.
Embodiment 2:
(1) starting material preparation: ammonium molybdate powder is calcined in air to 500 ℃ of 4 hours preparation MoO 3powder; MoO by 35mg 3powder, 0.6g urea and 35mg thioacetamide are dissolved in 15ml deionized water and 25ml alcohol mixed solution, be placed in autoclave, in baking oven 200 ℃, heat 24 hours, cooling rear cleaning, drying, obtain flowers shape MoS 2starting material.
(2) by 1g MoS 2powder in air 500 ℃ annealing 4 hours.
(3) the products therefrom 0.01g that will anneal is dissolved in the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 50 ℃ of stirring in water bath 2 hours, suction filtration.
(4) the previous step product is all joined to the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 50 ℃ of stirring in water bath are 2 hours.
(5) by products therefrom vacuum-drying in 40 ℃.
(6) products therefrom was with 500 ℃ of heating of the temperature rise rate of 5 ℃/min 4 hours.
Embodiment 3:
(1) starting material preparation: ammonium molybdate powder is calcined in air to 500 ℃ of 4 hours preparation MoO 3powder; MoO by 35mg 3powder, 0.6g urea and 35mg thioacetamide are dissolved in 15ml deionized water and 25ml alcohol mixed solution, be placed in autoclave, in baking oven 200 ℃, heat 24 hours, cooling rear cleaning, drying, obtain flowers shape MoS 2starting material.
(2) by 1g MoS 2powder in air 500 ℃ annealing 4 hours.
(3) the products therefrom 0.01g that will anneal is dissolved in the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 60 ℃ of stirring in water bath 2 hours, suction filtration.
(4) the previous step product is all joined to the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 60 ℃ of stirring in water bath are 2 hours.
(5) by products therefrom vacuum-drying in 40 ℃.
(6) products therefrom adds 3 hours with 500 ℃ of the temperature rise rates of 5 ℃/min.
Embodiment 4:
(1) starting material preparation: ammonium molybdate powder is calcined in air to 500 ℃ of 4 hours preparation MoO 3powder; MoO by 35mg 3powder, 0.6g urea and 35mg thioacetamide are dissolved in 15ml deionized water and 25ml alcohol mixed solution, be placed in autoclave, in baking oven 200 ℃, heat 24 hours, cooling rear cleaning, drying, obtain flowers shape MoS 2starting material.
(2) by 1g MoS 2powder in air 500 ℃ annealing 4 hours.
(3) the products therefrom 0.01g that will anneal is dissolved in the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 50 ℃ of stirring in water bath 3 hours, suction filtration.
(4) the previous step product is all joined to the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 50 ℃ of stirring in water bath are 3 hours.
(5) by products therefrom vacuum-drying in 40 ℃.
(6) products therefrom adds 3 hours with 500 ℃ of the temperature rise rates of 5 ℃/min.
Embodiment 5:
(1) starting material preparation: ammonium molybdate powder is calcined in air to 500 ℃ of 4 hours preparation MoO 3powder; MoO by 35mg 3powder, 0.6g urea and 35mg thioacetamide are dissolved in 15ml deionized water and 25ml alcohol mixed solution, be placed in autoclave, in baking oven 200 ℃, heat 24 hours, cooling rear cleaning, drying, obtain flowers shape MoS 2starting material.
(2) by 1g MoS 2powder in air 500 ℃ annealing 4 hours.
(3) the products therefrom 0.01g that will anneal is dissolved in the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 60 ℃ of stirring in water bath 3 hours, suction filtration.
(4) the previous step product is all joined to the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 60 ℃ of stirring in water bath are 3 hours.
(5) by products therefrom vacuum-drying in 40 ℃.
(6) products therefrom adds 3 hours with 600 ℃ of the temperature rise rates of 5 ℃/min.
Embodiment 6:
(1) starting material preparation: ammonium molybdate powder is calcined in air to 500 ℃ of 4 hours preparation MoO 3powder; MoO by 35mg 3powder, 0.6g urea and 35mg thioacetamide are dissolved in 15ml deionized water and 25ml alcohol mixed solution, be placed in autoclave, in baking oven 200 ℃, heat 24 hours, cooling rear cleaning, drying, obtain flowers shape MoS 2starting material.
(2) by 1g MoS 2powder in air 500 ℃ annealing 4 hours.
(3) the products therefrom 0.01g that will anneal is dissolved in the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 60 ℃ of stirring in water bath 3 hours, suction filtration.
(4) the previous step product is all joined to the Fe (NO of the 0.02mol/L of 300mL 3) 3in solution, 60 ℃ of stirring in water bath are 3 hours.
(5) by products therefrom vacuum-drying in 40 ℃.
(6) products therefrom adds 5 hours with 600 ℃ of the temperature rise rates of 5 ℃/min.
The gas sensitive device making method:
Gas sensor is made heater-type sintered type element by traditional method.Concrete making step is: sample thief a little, splash into appropriate ethanol, the furnishing pasty state, evenly be applied to the vitrified pipe outside with the Pt lead-in wire, after oven dry, vitrified pipe is welded on base and with RTD and connects.The device aging quick test of laggard promoting the circulation of qi in a day.
Air-sensitive test: under 270 ℃, carry out H 2the test of S gas sensitivity, add concentration to be respectively 0.5ppm, 1ppm, 5ppm, 10ppm, 30ppm, 50ppm.Under 270 ℃, carry out ethanol, acetone gas sensitivity test, add concentration to be respectively 100ppm, 200ppm, 300ppm, 500ppm.Referring to accompanying drawing 3, Fig. 4, Fig. 5 is respectively in the embodiment of the present invention 1 gained iron molybdate micro nano structure to gas with various (H 2s, ethanol, acetone) the test result of air-sensitive performance.Therefrom known, adopt the synthetic iron molybdate micro Nano material of the method, at identical temperature, to H 2s has good selectivity and higher sensitivity, and response-time of recovery is shorter simultaneously.

Claims (1)

1. one kind has lower concentration H 2the preparation method of S sensitivity characteristics iron molybdate micro Nano material is characterized in that:
(1) by ammonium molybdate powder 4 hours preparation MoO of 500 ℃ of temperature lower calcinations in air 3powder; MoO by 30-35mg 3powder, 0.5-0.6g urea and 30-35mg thioacetamide are dissolved in 15ml deionized water and 25ml alcohol mixed solution, and at 200 ℃ of temperature, heating is 24 hours, and cooling rear cleaning, drying, obtain flowers shape MoS 2powder raw material;
(2) by MoS 2powder, in air, is calcined 2-5 hour under 400 ℃ of-600 ℃ of conditions;
(3) the 0.01-0.075g products therefrom is dissolved in to the Fe (NO of 0.01-0.02mol/L 3) 3in solution, 50-60 ℃ of stirring in water bath 1-3 hour, suction filtration;
(4) upper step product is joined to the Fe (NO of 0.01-0.02mol/L 3) 350-60 ℃ of stirring in water bath 1-3 hour in solution;
(5) by products therefrom vacuum-drying;
(6) products therefrom is with the temperature rise rate 400-600 ℃ of calcining 3-5 hour in air of 5 ℃/min, and naturally cooling, obtain having lower concentration H 2s sensitivity characteristics iron molybdate micro Nano material.
CN201310421242.3A 2013-09-16 2013-09-16 Method for preparing iron molybdate micro-nano materials with sensitive feature for low-concentration H2S Expired - Fee Related CN103482705B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105259213A (en) * 2015-10-31 2016-01-20 武汉工程大学 Hydrogen-sulfide gas-sensitive material, preparation method thereof and preparation method for hydrogen-sulfide gas-sensitive device
CN105548263A (en) * 2016-01-29 2016-05-04 武汉工程大学 Hydrogen sulfide gas-sensitive material, preparation thereof and manufacturing method of hydrogen sulfide gas-sensitive device
CN106198647A (en) * 2016-07-22 2016-12-07 武汉工程大学 A kind of dimethylbenzene gas sensitive, dimethylbenzene gas sensitive device and preparation method thereof
CN106596452A (en) * 2016-12-30 2017-04-26 重庆理工大学 Hydrogen sulfide gas sensor and manufacturing method thereof and hydrogen sulfide concentration detection method
CN107459064A (en) * 2016-06-03 2017-12-12 中国科学院大连化学物理研究所 A kind of nanocube accumulates layered mesoporous FeMoO4The preparation method of solid material
CN109574082A (en) * 2018-11-28 2019-04-05 武汉科技大学 A kind of original position core-shell structure molybdic acid iron powder body and preparation method thereof
CN109610024A (en) * 2018-11-20 2019-04-12 华南理工大学 A kind of cellulose-molybdenum disulfide aeroge composite fibre and its preparation method and application
CN110124678A (en) * 2019-05-29 2019-08-16 中国矿业大学 The Fe prepared using waste silicon molybdenum rod2(MoO4)3/MoO3Catalysis material, method and its application
CN114609197A (en) * 2022-03-25 2022-06-10 电子科技大学 Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YU-JIN CHEN, ET AL.: ""Porous Iron Molybdate Nanorods: In situ Diffusion Synthesis and Low-Temperature H2S Gas Sensing"", 《ACS APPL. MATER. INTERFACES》 *

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105259213A (en) * 2015-10-31 2016-01-20 武汉工程大学 Hydrogen-sulfide gas-sensitive material, preparation method thereof and preparation method for hydrogen-sulfide gas-sensitive device
CN105259213B (en) * 2015-10-31 2018-11-06 武汉工程大学 The preparation method of hydrogen sulfide gas sensitive and its preparation and stink damp sensing device
CN105548263A (en) * 2016-01-29 2016-05-04 武汉工程大学 Hydrogen sulfide gas-sensitive material, preparation thereof and manufacturing method of hydrogen sulfide gas-sensitive device
CN107459064B (en) * 2016-06-03 2019-10-11 中国科学院大连化学物理研究所 A kind of layered mesoporous FeMoO of nanocube accumulation4The preparation method of solid material
CN107459064A (en) * 2016-06-03 2017-12-12 中国科学院大连化学物理研究所 A kind of nanocube accumulates layered mesoporous FeMoO4The preparation method of solid material
CN106198647A (en) * 2016-07-22 2016-12-07 武汉工程大学 A kind of dimethylbenzene gas sensitive, dimethylbenzene gas sensitive device and preparation method thereof
CN106596452B (en) * 2016-12-30 2019-03-22 重庆理工大学 The detection method of these hydrogen sulfide gas sensor and preparation method thereof and concentration of hydrogen sulfide
CN106596452A (en) * 2016-12-30 2017-04-26 重庆理工大学 Hydrogen sulfide gas sensor and manufacturing method thereof and hydrogen sulfide concentration detection method
CN109610024A (en) * 2018-11-20 2019-04-12 华南理工大学 A kind of cellulose-molybdenum disulfide aeroge composite fibre and its preparation method and application
CN109574082A (en) * 2018-11-28 2019-04-05 武汉科技大学 A kind of original position core-shell structure molybdic acid iron powder body and preparation method thereof
CN109574082B (en) * 2018-11-28 2021-05-04 武汉科技大学 In-situ core-shell structure iron molybdate powder and preparation method thereof
CN110124678A (en) * 2019-05-29 2019-08-16 中国矿业大学 The Fe prepared using waste silicon molybdenum rod2(MoO4)3/MoO3Catalysis material, method and its application
CN114609197A (en) * 2022-03-25 2022-06-10 电子科技大学 Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor
CN114609197B (en) * 2022-03-25 2023-11-21 电子科技大学 Gas-sensitive material, preparation method and NH (NH) thereof 3 Application in gas sensor

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