CN106018507A - Preparation method of mesoporous nickel oxide having excellent ammonia gas sensitive properties - Google Patents
Preparation method of mesoporous nickel oxide having excellent ammonia gas sensitive properties Download PDFInfo
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- CN106018507A CN106018507A CN201610321095.6A CN201610321095A CN106018507A CN 106018507 A CN106018507 A CN 106018507A CN 201610321095 A CN201610321095 A CN 201610321095A CN 106018507 A CN106018507 A CN 106018507A
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Abstract
A preparation method of mesoporous nickel oxide having excellent ammonia gas sensitive properties comprises the following steps that dodecyl benzene sodium sulfonate and nickel nitrate are added to distilled water at room temperature to be stirred evenly, then ammonium carbonate is added, stirring is performed till the solution is opalescent, a pH value of he solution is 9-10, stirring continues for 6 hours, then standing is performed for 3 hours, suction filtration is performed, a filter cake is dried at the temperature of 120 DEG C for 6 hours to obtain white powder; the prepared mesoporous nickel oxide precursor is calcinated at the temperature of 550 DEG C for 4 hours, cooling is performed to reach room temperature, and the mesoporous nickel oxide is prepared. The prepared mesoporous nickel oxide having the excellent ammonia gas sensitive properties is applied to online ammonia gas monitoring. The preparation method has the advantages that the synthetic steps are simple, the costs are low, and the mesoporous nickel oxide is uniform and controllable in size, high in sensitivity, short in response time and capable of rapidly detecting a trace amount of low-concentration ammonia gas. The mesoporous nickel oxide has excellent stability and can be recycled, and further the costs are reduced.
Description
Technical field
The invention belongs to gas sensitive preparation field, a kind of mesoporous oxygen with excellent ammonia air-sensitive performance
Change the preparation method of nickel.
Background technology
Ammonia (NH3) have a wide range of applications in the field such as industrial, agriculture, it is a kind of colourless and have strong
The gas of strong pungent odour, lta, is a kind of alkaline matter.Ammonia has serious harm to environment, right
Water body, soil and air can pollute.Meanwhile, the dissolubility of ammonia is high, exhales on animal or human body
Inhale road and have stimulation and corrosiveness, be often attracted to mucocutaneous with on eye conjunctiva, make tissue protein degeneration also
Destroy cell membrane, thus produce stimulation and inflammation, it is possible to respiratory disease can be caused and weaken human body to disease
Resistance, when ammonia concentration is too high in addition to corrosiveness, also can also by nervi trigeminus tip reflection make
With and cause asystole and respiratory arrest (suffocating).During additionally, ammonia gathers finite concentration in space
There is potential explosive threat.The ammonia that occupation health safety management board of Department of Labor (OSHA) specifies is allowed
Concentration is 50ppm, and the upper limit that U.S. professional safety and health institute (NIOSH) specifies is 25ppm.Therefore,
The detection especially low concentration trace ammonia of ammonia is detected protection health the most necessary.
The method that predominantly detects of ammonia has: colorimetry, photometry, chromatography, ammonia quick electrode method etc., these sides
Method exist operating temperature, poor selectivity, easily disturbed by aldehydes and sulfide, poor sensitivity, expensive,
On-line checking poor performance, operation is complicated, analyze the deficiencies such as time-consuming.Ammonia gas sensor method can be implemented in line ammonia
Detection, additionally, ammonia gas sensor has highly sensitive, good stability, easy to use, cheap, response time
The features such as short, detectable limit is low, along with the raising of people's living standard, the enhancing of environmental consciousness and to inhabitation ring
The raising that border requires, the in real time detection tool of ammonia is of great significance, especially low concentration trace, as
Ammonia concentration is less than 1ppm.
Summary of the invention
It is an object of the invention to for above-mentioned existing problems, it is provided that a kind of have the mesoporous of excellent ammonia air-sensitive performance
The preparation method of nickel oxide, utilizes mesoporous nickel oxide to develop and carries out online ammonia monitoring, with low cost, inspection
The ammonia gas sensor surveying accuracy high 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 is as follows:
1) synthesis of mesoporous nickel oxide precursor
At room temperature dodecylbenzene sodium sulfonate and nickel nitrate are added in distilled water and stir, add carbonic acid
Ammonium, stirring is creamy white to solution, and above-mentioned pH value in solution is 9-10, stands 3h after continuing stirring 6h,
Carry out sucking filtration afterwards, filter cake is dried 6h in 120 DEG C and obtains white powder, dodecylbenzene sodium sulfonate, nitre
Acid nickel, distilled water are 0.8-1.2:4.7-5.3:100:0.9-1.1 with the mass ratio of ammonium carbonate；
2) synthesis of mesoporous nickel oxide
Under room temperature by above-mentioned prepare mesoporous nickel oxide precursor in 550 DEG C calcine 4h, be cooled to room temperature, prepare
Mesoporous nickel oxide.
The application of a kind of prepared mesoporous nickel oxide with excellent ammonia air-sensitive performance, supervises for online ammonia
Survey, specifically comprising the following steps that of the air-sensitive performance test of mesoporous nickel oxide
1) each leading into the ammonia of variable concentrations, testing mesoporous nickel oxide for concentration is 0.1-0.4ppm
The sensitivity of ammonia；
2) it is passed through the ammonia that concentration is 0.1-0.4ppm, tests the response time of mesoporous nickel oxide；
3) within 30 days, reuse mesoporous nickel oxide, investigate the long-time stability of mesoporous nickel oxide.
It is an advantage of the current invention that:
1) synthesis step is simple, and with low cost, the size of mesoporous nickel oxide is homogeneous controlled；
2) highly sensitive, response time is short, it is possible to achieve rapidly detection low concentration trace ammonia (0.5ppm with
Under)；
3) mesoporous nickel oxide has the stability of excellence, can recycle, and reduces its cost further.
Detailed description of the invention
Embodiment 1:
A kind of preparation method of the mesoporous nickel oxide with excellent ammonia air-sensitive performance, step is as follows:
1) synthesis of mesoporous nickel oxide precursor
At room temperature 1g dodecylbenzene sodium sulfonate and 5g nickel nitrate are added in 100g distilled water and stir,
Adding 1g ammonium carbonate, stirring is creamy white to solution, and above-mentioned pH value in solution is 9-10, continues stirring 6h
Rear standing 3h, carries out sucking filtration afterwards, in 120 DEG C, filter cake is dried 6h and obtains white powder；
2) synthesis of mesoporous nickel oxide
Under room temperature by above-mentioned prepare mesoporous nickel oxide precursor in 550 DEG C calcine 4h, be cooled to room temperature, prepare
Mesoporous nickel oxide A.
The application of a kind of prepared mesoporous nickel oxide with excellent ammonia air-sensitive performance, supervises for online ammonia
Survey, specifically comprising the following steps that of the air-sensitive performance test of mesoporous nickel oxide
1) being passed through the ammonia that concentration is 0.1ppm, mesoporous nickel oxide A sensitivity is 21.1；
2) being passed through the ammonia that concentration is 0.1ppm, the response time of mesoporous nickel oxide A is 14s；
3) mesoporous nickel oxide A reuses 30 days in the ammonia environment that concentration is 0.1ppm, its air-sensitive
Performance is unattenuated.
Embodiment 2:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: dodecylbenzene sodium sulfonate consumption changes 1.2g into, prepares mesoporous nickel oxide B.It is situated between
Hole nickel oxide B sensitivity is 21.0, response time 15s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 3:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: nickel nitrate consumption changes 4.7g into, prepares mesoporous nickel oxide C.Mesoporous nickel oxide C
Sensitivity is 20.9, response time 14s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 4:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: ammonium carbonate consumption changes 0.9g into, prepares mesoporous nickel oxide D.Mesoporous nickel oxide D
Sensitivity is 21.2, response time 15s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 5:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: nickel nitrate consumption changes 5.3g into, prepares mesoporous nickel oxide E.Mesoporous nickel oxide E
Sensitivity is 20.9, response time 14s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 6:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: dodecylbenzene sodium sulfonate consumption changes 0.8g into, prepares mesoporous nickel oxide F.It is situated between
Hole nickel oxide F sensitivity is 20.9, response time 14s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 7:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: ammonium carbonate consumption changes 1.1g into, prepares mesoporous nickel oxide G.Mesoporous nickel oxide G
Sensitivity is 20.8, response time 14s, reuses 30 days, and 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,
Prepare mesoporous nickel oxide A.Difference is: in the air-sensitive performance test of mesoporous nickel oxide, by ammonia concentration
Changing 0.25ppm into, mesoporous nickel oxide A sensitivity is 56.9, and response time 38s reuses 30 days,
Its air-sensitive performance is unattenuated.
Embodiment 9:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: dodecylbenzene sodium sulfonate consumption changes 1.2g into, prepares mesoporous nickel oxide B.It is situated between
In the air-sensitive performance test of hole nickel oxide, ammonia concentration changes 0.25ppm into, and mesoporous nickel oxide B sensitivity is 57.1,
Response time 38s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 10:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: nickel nitrate consumption changes 4.7g into, prepares mesoporous nickel oxide C.Mesoporous nickel oxide
In air-sensitive performance test, ammonia concentration changes 0.25ppm into, and mesoporous nickel oxide C sensitivity is 56.8, during response
Between 39s, reuse 30 days, its air-sensitive performance is unattenuated.
Embodiment 11:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: ammonium carbonate consumption changes 0.9g into, prepares mesoporous nickel oxide D.Mesoporous nickel oxide
In air-sensitive performance test, ammonia concentration changes 0.25ppm into, and mesoporous nickel oxide D sensitivity is 56.7, during response
Between 39s, reuse 30 days, its air-sensitive performance is unattenuated.
Embodiment 12:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: nickel nitrate consumption changes 5.3g into, prepares mesoporous nickel oxide E.Mesoporous nickel oxide
In air-sensitive performance test, ammonia concentration changes 0.25ppm into, and mesoporous nickel oxide E sensitivity is 56.8, during response
Between 38s, reuse 30 days, its air-sensitive performance is unattenuated.
Embodiment 13:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: dodecylbenzene sodium sulfonate consumption changes 0.8g into, prepares mesoporous nickel oxide F.It is situated between
In the air-sensitive performance test of hole nickel oxide, ammonia concentration changes 0.25ppm into, and mesoporous nickel oxide F sensitivity is 56.8,
Response time 37s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 14:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: ammonium carbonate consumption changes 1.1g into, prepares mesoporous nickel oxide G.Mesoporous nickel oxide
In air-sensitive performance test, ammonia concentration changes 0.25ppm into, and mesoporous nickel oxide G sensitivity is 57.0, during response
Between 39s, reuse 30 days, its air-sensitive performance is 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,
Prepare mesoporous nickel oxide A.Difference is: in the air-sensitive performance test of mesoporous nickel oxide, by ammonia concentration
Changing 0.4ppm into, mesoporous nickel oxide A sensitivity is 91.9, and response time 60s reuses 30 days, its
Air-sensitive performance is unattenuated.
Embodiment 16:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: dodecylbenzene sodium sulfonate consumption changes 1.2g into, prepares mesoporous nickel oxide B.It is situated between
In the air-sensitive performance test of hole nickel oxide, ammonia concentration changes 0.4ppm into, and mesoporous nickel oxide B sensitivity is 91.8,
Response time 60s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 17:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: nickel nitrate consumption changes 4.7g into, prepares mesoporous nickel oxide C.Mesoporous nickel oxide
In air-sensitive performance test, ammonia concentration changes 0.4ppm into, and mesoporous nickel oxide C sensitivity is 91.6, response time
61s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 18:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: ammonium carbonate consumption changes 0.9g into, prepares mesoporous nickel oxide D.Mesoporous nickel oxide
In air-sensitive performance test, ammonia concentration changes 0.4ppm into, and mesoporous nickel oxide D sensitivity is 91.7, response time
60s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 19:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: nickel nitrate consumption changes 5.3g into, prepares mesoporous nickel oxide E.Mesoporous nickel oxide
In air-sensitive performance test, ammonia concentration changes 0.4ppm into, and mesoporous nickel oxide E sensitivity is 92.1, response time
61s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 20:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: dodecylbenzene sodium sulfonate consumption changes 0.8g into, prepares mesoporous nickel oxide F.It is situated between
In the air-sensitive performance test of hole nickel oxide, ammonia concentration changes 0.4ppm into, and mesoporous nickel oxide F sensitivity is 92.0,
Response time 60s, reuses 30 days, and its air-sensitive performance is unattenuated.
Embodiment 21:
The preparation method of a kind of mesoporous nickel oxide with excellent ammonia air-sensitive performance, embodiment 1 is basic more than step
Identical, difference is: ammonium carbonate consumption changes 1.1g into, prepares mesoporous nickel oxide G.Mesoporous nickel oxide
In air-sensitive performance test, ammonia concentration changes 0.4ppm into, and mesoporous nickel oxide G sensitivity is 91.6, response time
61s, reuses 30 days, and its air-sensitive performance is unattenuated.
Claims (2)
1. the preparation method of a mesoporous nickel oxide with excellent ammonia air-sensitive performance, it is characterised in that step is such as
Under:
1) synthesis of mesoporous nickel oxide precursor
At room temperature dodecylbenzene sodium sulfonate and nickel nitrate are added in distilled water and stir, add carbonic acid
Ammonium, stirring is creamy white to solution, and above-mentioned pH value in solution is 9-10, stands 3h after continuing stirring 6h,
Carry out sucking filtration afterwards, filter cake is dried 6h in 120 DEG C and obtains white powder, dodecylbenzene sodium sulfonate, nitre
Acid nickel, distilled water are 0.8-1.2:4.7-5.3:100:0.9-1.1 with the mass ratio of ammonium carbonate；
2) synthesis of mesoporous nickel oxide
Under room temperature by above-mentioned prepare mesoporous nickel oxide precursor in 550 DEG C calcine 4h, be cooled to room temperature, prepare
Mesoporous nickel oxide.
2. an application for the mesoporous nickel oxide with excellent ammonia air-sensitive performance prepared by claim 1, its
It is characterised by monitoring for online ammonia, specifically comprising the following steps that of the air-sensitive performance test of mesoporous nickel oxide
1) each leading into the ammonia of variable concentrations, testing mesoporous nickel oxide for concentration is 0.1-0.4ppm
The sensitivity of ammonia；
2) it is passed through the ammonia that concentration is 0.1-0.4ppm, tests the response time of mesoporous nickel oxide；
3) within 30 days, reuse mesoporous nickel oxide, 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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