CN106018507B - A kind of preparation method of the mesoporous nickel oxide with ammonia air-sensitive performance - Google Patents
A kind of preparation method of the mesoporous nickel oxide with ammonia air-sensitive performance Download PDFInfo
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- CN106018507B CN106018507B CN201610321095.6A CN201610321095A CN106018507B CN 106018507 B CN106018507 B CN 106018507B CN 201610321095 A CN201610321095 A CN 201610321095A CN 106018507 B CN106018507 B CN 106018507B
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- nickel oxide
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Abstract
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, step are as follows：Neopelex and nickel nitrate are added in distilled water at room temperature and stirred evenly, ammonium carbonate is added, stirs to solution and be creamy white, above-mentioned pH value in solution is 9 10, continue to stand 3h after stirring 6h, filtered afterwards, filter cake is dried 6h in 120 DEG C obtains white powder；Mesoporous nickel oxide precursor is prepared in 550 DEG C of calcining 4h by above-mentioned, is cooled to room temperature, mesoporous nickel oxide is made.The application of the prepared mesoporous nickel oxide with excellent ammonia air-sensitive performance, monitors for online ammonia.It is an advantage of the invention that：Synthesis step is simple, of low cost, and the size of mesoporous nickel oxide is homogeneous controllable；High sensitivity, response time are short, it is possible to achieve rapid detection low concentration trace ammonia；Mesoporous nickel oxide has excellent stability, can recycle, further reduce its cost.
Description
Technical field
The invention belongs to gas sensitive preparation field, particularly a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance
Preparation method.
Background technology
Ammonia (NH3) have a wide range of applications in the fields such as industry, agricultural, it is a kind of colourless and has intense stimulus
The gas of property stink, it is lighter than air, it is a kind of alkaline matter.Ammonia has serious harm to environment, can to water body, soil and air
Pollute.Meanwhile the solubility of ammonia is high, there are stimulation and corrosiveness to the upper respiratory tract of animal or human body, often inhaled
It is attached in mucocutaneous and eye conjunctiva, is denatured tissue protein and destroys cell membrane, so as to produce stimulation and inflammation, it is possible to
It can cause respiratory disease and weaken human body to the resistance of disease, when ammonia concentration is excessive in addition to corrosiveness, can also may be used also
Cardiac arrest and breathing is caused to stop (asphyxia) by the reflex of trigeminal neuralgia tip.In addition, ammonia collects in space
There is potential explosive threat when gathering a certain concentration.Ammonia as defined in occupation health safety management board of Department of Labor (OSHA)
Gas acceptable concentration is 50ppm, and the upper limit as defined in professional safety and health research institute of the U.S. (NIOSH) is 25ppm.Therefore, it is right
The detection of ammonia especially low concentration trace ammonia detection is very necessary to protection health.
The method that predominantly detects of ammonia has：Quick electrode method of colorimetric method, photometry, chromatography, ammonia etc., there are work for these methods
Make temperature, poor selectivity, easily disturbed by aldehydes and sulfide, poor sensitivity, expensive, on-line checking poor performance, operated
The deficiencies of complexity, time-consuming analysis.Ammonia gas sensor method can realize online ammonia detection, in addition, ammonia gas sensor is with sensitive
The features such as degree is high, stability is good, easy to use, cheap, the response time is short, detectable limit is low, with carrying for people's living standard
High, environmental consciousness enhancing and the raising to living environment requirement, the real-time detection tool of ammonia are of great significance, especially
It is low concentration trace, as ammonia concentration is less than 1ppm.
The content of the invention
The purpose of the present invention is there are problem for above-mentioned, there is provided a kind of mesoporous oxidation with excellent ammonia air-sensitive performance
The preparation method of nickel, can be developed using mesoporous nickel oxide and carry out online ammonia monitoring, ammonia of low cost, accuracy in detection is high
Gas sensor realizes the efficient detection to low concentration trace ammonia.
Technical scheme：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, step are as follows：
1) synthesis of mesoporous nickel oxide precursor
Neopelex and nickel nitrate are added in distilled water at room temperature and stirred evenly, adds ammonium carbonate,
Stirring is creamy white to solution, and above-mentioned pH value in solution is 9-10, continues to stand 3h after stirring 6h, is filtered, will filtered afterwards
Cake dries 6h in 120 DEG C and obtains white powder, and neopelex, nickel nitrate, the mass ratio of distilled water and ammonium carbonate are
0.8-1.2：4.7-5.3：100：0.9-1.1；
2) synthesis of mesoporous nickel oxide
Mesoporous nickel oxide precursor is prepared in 550 DEG C of calcining 4h by above-mentioned at room temperature, is cooled to room temperature, mesoporous oxidation is made
Nickel.
A kind of application of the prepared mesoporous nickel oxide with excellent ammonia air-sensitive performance, monitors for online ammonia,
The air-sensitive performance test of mesoporous nickel oxide comprises the following steps that：
1) ammonia of various concentrations is each led into, it is the ammonia of 0.1-0.4ppm for concentration to test mesoporous nickel oxide
Sensitivity；
2) ammonia that concentration is 0.1-0.4ppm is passed through, tests the response time of mesoporous nickel oxide；
3) reuse mesoporous nickel oxide within 30 days, investigate the long-time stability of mesoporous nickel oxide.
The advantage of the invention is that：
1) synthesis step is simple, of low cost, and the size of mesoporous nickel oxide is homogeneous controllable；
2) high sensitivity, response time are short, it is possible to achieve rapid detection low concentration trace ammonia (below 0.5ppm)；
3) mesoporous nickel oxide has excellent stability, can recycle, further reduce its cost.
Embodiment
Embodiment 1：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, step are as follows：
1) synthesis of mesoporous nickel oxide precursor
1g neopelexes and 5g nickel nitrates are added in 100g distilled water at room temperature and stirred evenly, is added
1g ammonium carbonates, stir to solution and are creamy white, and above-mentioned pH value in solution is 9-10, continue to stand 3h after stirring 6h, carry out afterwards
Filter, filter cake is dried 6h in 120 DEG C obtains white powder；
2) synthesis of mesoporous nickel oxide
Mesoporous nickel oxide precursor is prepared in 550 DEG C of calcining 4h by above-mentioned at room temperature, is cooled to room temperature, mesoporous oxidation is made
Nickel A.
A kind of application of the prepared mesoporous nickel oxide with excellent ammonia air-sensitive performance, monitors for online ammonia,
The air-sensitive performance test of mesoporous nickel oxide comprises the following steps that：
1) ammonia that concentration is 0.1ppm is passed through, mesoporous nickel oxide A sensitivity is 21.1；
2) ammonia that concentration is 0.1ppm is passed through, the response time of mesoporous nickel oxide A is 14s；
3) mesoporous nickel oxide A is reused 30 days in the ammonia environment that concentration is 0.1ppm, its air-sensitive performance does not wane
Subtract.
Embodiment 2：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Neopelex dosage is changed to 1.2g, and mesoporous nickel oxide B is made.Mesoporous nickel oxide B sensitivity is
21.0, response time 15s, are reused 30 days, its air-sensitive performance is unattenuated.
Embodiment 3：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Nickel nitrate dosage is changed to 4.7g, and mesoporous nickel oxide C is made.Mesoporous nickel oxide C sensitivity is 20.9, response
Time 14s, is reused 30 days, its air-sensitive performance is unattenuated.
Embodiment 4：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Ammonium carbonate dosage is changed to 0.9g, and mesoporous nickel oxide D is made.Mesoporous nickel oxide D sensitivity is 21.2, response
Time 15s, is reused 30 days, its air-sensitive performance is unattenuated.
Embodiment 5：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Nickel nitrate dosage is changed to 5.3g, and mesoporous nickel oxide E is made.Mesoporous nickel oxide E sensitivity is 20.9, response
Time 14s, is reused 30 days, its air-sensitive performance is unattenuated.
Embodiment 6：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Neopelex dosage is changed to 0.8g, and mesoporous nickel oxide F is made.Mesoporous nickel oxide F sensitivity is
20.9, response time 14s, are reused 30 days, its air-sensitive performance is unattenuated.
Embodiment 7：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Ammonium carbonate dosage is changed to 1.1g, and mesoporous nickel oxide G is made.Mesoporous nickel oxide G sensitivity is 20.8, response
Time 14s, is reused 30 days, its air-sensitive performance is unattenuated.
Embodiment 8：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is identical more than step, is made
Mesoporous nickel oxide A.Difference is：In the air-sensitive performance test of mesoporous nickel oxide, ammonia concentration is changed to 0.25ppm, is situated between
Hole nickel oxide A sensitivity is 56.9, response time 38s, is reused 30 days, its air-sensitive performance is unattenuated.
Embodiment 9：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Neopelex dosage is changed to 1.2g, and mesoporous nickel oxide B is made.The gas sensing property of mesoporous nickel oxide
In testing, ammonia concentration is changed to 0.25ppm, and mesoporous nickel oxide B sensitivity is 57.1, response time 38s, reuses 30
My god, its air-sensitive performance is unattenuated.
Embodiment 10：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Nickel nitrate dosage is changed to 4.7g, and mesoporous nickel oxide C is made.In the air-sensitive performance test of mesoporous nickel oxide, ammonia
Gas concentration is changed to 0.25ppm, and mesoporous nickel oxide C sensitivity is 56.8, response time 39s, reuses 30 days, its gas sensing property
Can be unattenuated.
Embodiment 11：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Ammonium carbonate dosage is changed to 0.9g, and mesoporous nickel oxide D is made.In the air-sensitive performance test of mesoporous nickel oxide, ammonia
Gas concentration is changed to 0.25ppm, and mesoporous nickel oxide D sensitivity is 56.7, response time 39s, reuses 30 days, its gas sensing property
Can be unattenuated.
Embodiment 12：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Nickel nitrate dosage is changed to 5.3g, and mesoporous nickel oxide E is made.In the air-sensitive performance test of mesoporous nickel oxide, ammonia
Gas concentration is changed to 0.25ppm, and mesoporous nickel oxide E sensitivity is 56.8, response time 38s, reuses 30 days, its gas sensing property
Can be unattenuated.
Embodiment 13：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Neopelex dosage is changed to 0.8g, and mesoporous nickel oxide F is made.The gas sensing property of mesoporous nickel oxide
In testing, ammonia concentration is changed to 0.25ppm, and mesoporous nickel oxide F sensitivity is 56.8, response time 37s, reuses 30
My god, its air-sensitive performance is unattenuated.
Embodiment 14：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Ammonium carbonate dosage is changed to 1.1g, and mesoporous nickel oxide G is made.In the air-sensitive performance test of mesoporous nickel oxide, ammonia
Gas concentration is changed to 0.25ppm, and mesoporous nickel oxide G sensitivity is 57.0, response time 39s, reuses 30 days, its gas sensing property
Can be unattenuated.
Embodiment 15：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is identical more than step, is made
Mesoporous nickel oxide A.Difference is：In the air-sensitive performance test of mesoporous nickel oxide, ammonia concentration is changed to 0.4ppm, it is mesoporous
Nickel oxide A sensitivity is 91.9, response time 60s, is reused 30 days, its air-sensitive performance is unattenuated.
Embodiment 16：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Neopelex dosage is changed to 1.2g, and mesoporous nickel oxide B is made.The gas sensing property of mesoporous nickel oxide
In testing, ammonia concentration is changed to 0.4ppm, and mesoporous nickel oxide B sensitivity is 91.8, response time 60s, reuses 30
My god, its air-sensitive performance is unattenuated.
Embodiment 17：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Nickel nitrate dosage is changed to 4.7g, and mesoporous nickel oxide C is made.In the air-sensitive performance test of mesoporous nickel oxide, ammonia
Gas concentration is changed to 0.4ppm, and mesoporous nickel oxide C sensitivity is 91.6, response time 61s, reuses 30 days, its gas sensing property
Can be unattenuated.
Embodiment 18：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Ammonium carbonate dosage is changed to 0.9g, and mesoporous nickel oxide D is made.In the air-sensitive performance test of mesoporous nickel oxide, ammonia
Gas concentration is changed to 0.4ppm, and mesoporous nickel oxide D sensitivity is 91.7, response time 60s, reuses 30 days, its gas sensing property
Can be unattenuated.
Embodiment 19：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Nickel nitrate dosage is changed to 5.3g, and mesoporous nickel oxide E is made.In the air-sensitive performance test of mesoporous nickel oxide, ammonia
Gas concentration is changed to 0.4ppm, and mesoporous nickel oxide E sensitivity is 92.1, response time 61s, reuses 30 days, its gas sensing property
Can be unattenuated.
Embodiment 20：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Neopelex dosage is changed to 0.8g, and mesoporous nickel oxide F is made.The gas sensing property of mesoporous nickel oxide
In testing, ammonia concentration is changed to 0.4ppm, and mesoporous nickel oxide F sensitivity is 92.0, response time 60s, reuses 30
My god, its air-sensitive performance is unattenuated.
Embodiment 21：
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is essentially identical more than step,
Difference is：Ammonium carbonate dosage is changed to 1.1g, and mesoporous nickel oxide G is made.In the air-sensitive performance test of mesoporous nickel oxide, ammonia
Gas concentration is changed to 0.4ppm, and mesoporous nickel oxide G sensitivity is 91.6, response time 61s, reuses 30 days, its gas sensing property
Can be unattenuated.
Claims (2)
1. a kind of preparation method of the mesoporous nickel oxide with ammonia air-sensitive performance, it is characterised in that step is as follows：
1) synthesis of mesoporous nickel oxide precursor
Neopelex and nickel nitrate are added in distilled water at room temperature and stirred evenly, adds ammonium carbonate, is stirred
Be creamy white to solution, above-mentioned pH value in solution is 9-10, continue stir 6h after stand 3h, filtered afterwards, by filter cake in
120 DEG C of drying 6h obtain white powder, and neopelex, nickel nitrate, the mass ratio of distilled water and ammonium carbonate are 0.8-
1.2：4.7-5.3：100：0.9-1.1；
2) synthesis of mesoporous nickel oxide
Mesoporous nickel oxide precursor is calcined into 4h in 550 DEG C at room temperature, is cooled to room temperature, mesoporous nickel oxide is made.
2. the application of the mesoporous nickel oxide with ammonia air-sensitive performance prepared by a kind of claim 1, it is characterised in that be used for
Online ammonia monitoring, the air-sensitive performance test of mesoporous nickel oxide comprise the following steps that：
1) ammonia of various concentrations is each led into, it is the sensitive of the ammonia of 0.1-0.4ppm for concentration to test mesoporous nickel oxide
Degree；
2) ammonia that concentration is 0.1-0.4ppm is passed through, tests the response time of mesoporous nickel oxide；
3) reuse mesoporous nickel oxide within 30 days, investigate the long-time stability of mesoporous nickel oxide.
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Citations (7)
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| JP2009236693A (en) * | 2008-03-27 | 2009-10-15 | Kyushu Univ | Ammonia concentration measuring sensor element, ammonia concentration measuring instrument, and ammonia concentration measuring method |
| JP2010048596A (en) * | 2008-08-20 | 2010-03-04 | Nippon Soken Inc | Ammonia detecting element and ammonia sensor equipped with the same |
| CN101928979A (en) * | 2010-08-06 | 2010-12-29 | 厦门大学 | Surface structure regulation, control and preparation method of metallic nanocatalyst |
| CN102267729A (en) * | 2011-06-30 | 2011-12-07 | 合肥工业大学 | Preparation method of spherical nickel hydroxide used as battery cathode material |
| CN102385998A (en) * | 2011-12-08 | 2012-03-21 | 南开大学 | NiO electrode material with high specific capacitance and preparation method thereof |
| CN102603016A (en) * | 2012-03-08 | 2012-07-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing nanometer nickel oxide and application of method |
| CN103943379A (en) * | 2014-03-24 | 2014-07-23 | 上海大学 | Preparation method for graphene load flower-shaped porous nickel oxide composite materials |
-
2016
- 2016-05-16 CN CN201610321095.6A patent/CN106018507B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009236693A (en) * | 2008-03-27 | 2009-10-15 | Kyushu Univ | Ammonia concentration measuring sensor element, ammonia concentration measuring instrument, and ammonia concentration measuring method |
| JP2010048596A (en) * | 2008-08-20 | 2010-03-04 | Nippon Soken Inc | Ammonia detecting element and ammonia sensor equipped with the same |
| CN101928979A (en) * | 2010-08-06 | 2010-12-29 | 厦门大学 | Surface structure regulation, control and preparation method of metallic nanocatalyst |
| CN102267729A (en) * | 2011-06-30 | 2011-12-07 | 合肥工业大学 | Preparation method of spherical nickel hydroxide used as battery cathode material |
| CN102385998A (en) * | 2011-12-08 | 2012-03-21 | 南开大学 | NiO electrode material with high specific capacitance and preparation method thereof |
| CN102603016A (en) * | 2012-03-08 | 2012-07-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing nanometer nickel oxide and application of method |
| CN103943379A (en) * | 2014-03-24 | 2014-07-23 | 上海大学 | Preparation method for graphene load flower-shaped porous nickel oxide composite materials |
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