CN105181768B - Formaldehyde sensor based on Pt chromium carbides/nanocarbon catalyst and preparation method thereof - Google Patents
Formaldehyde sensor based on Pt chromium carbides/nanocarbon catalyst and preparation method thereof Download PDFInfo
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- CN105181768B CN105181768B CN201510528511.5A CN201510528511A CN105181768B CN 105181768 B CN105181768 B CN 105181768B CN 201510528511 A CN201510528511 A CN 201510528511A CN 105181768 B CN105181768 B CN 105181768B
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Abstract
The invention discloses a kind of formaldehyde sensor based on Pt chromium carbides/nanocarbon catalyst and preparation method thereof.Described preparation method comprises the following steps：(1) preparation of chromium carbide/nano-carbon material；(2) preparation of Pt chromium carbides/nanocarbon catalyst；(3) preparation of formaldehyde sensor.Product prepared by the present invention is used to detect formaldehyde, has the advantages of cost-effective, simple to operate, the degree of accuracy is high, high sensitivity, may be adapted to mass produce.The present invention is applied to the detection of formaldehyde.The present invention solves the problems, such as that existing formaldehyde sensor price is high, portability is poor, poor operability, poor accuracy, sensitivity is low and leads to not apply in public places and in family.
Description
Technical field
The invention belongs to the technical field of formaldehyde sensor, and in particular to one kind is based on Pt- chromium carbides/nanocarbon catalyst
Formaldehyde sensor and preparation method thereof.
Background technology
With modern society's high speed development, science and technology is maked rapid progress, and caused result is greatly to meet people's lives
Various aspects, quality of life level is significantly increased.Wherein using chemical article, chemical synthesis articles for use etc., full society
The usage amount of meeting is also in cumulative year after year.Although these chemical synthesis articles for use have serviced the mankind, facilitate daily life,
Improve the quality of life of people.But everything all has dual character, while being beneficial to, the drawbacks of it should not be forgotten.Change
Learn synthesis articles for use transition use and waste, gradually start to have influence on people's health and living environment, among these
One of raw material of most important chemical synthesis articles for use are exactly formaldehyde, and it is had changed into as a shadow killer, there is suitable one
Crowd is divided to deeply hurt.For formaldehyde typically except being present in the factory of production formaldehyde, what is be most commonly encountered is exactly daily all with people
Closely bound up place --- it is indoor.In being detected to indoor noxious material, formaldehyde as a highly important index,
The personnel of being detected are monitored.The global World Health Organization (WTO) and environmental protection department of various countries are using formaldehyde as serious danger
One of evil human environment and the pollutant of health.
Formaldehyde, it is no color the characteristics of formaldehyde gas, but there is stronger irritating smell.Formaldehyde can be with molten
Solution is in ether, alcohol and water.Gaseous state is its state at room temperature.In daily life, the existence form of formaldehyde is typically all with water
The form of solution is present.Formalin is the aqueous solution of formaldehyde, the scientific name when concentration is 35~40%.In medical science and scientific research etc.
Relevant departments, formalin are commonly used for storing sample, it is therefore an objective to for preventing rotting for sample.It is big in room temperature and a standard
Under conditions of air pressure, the boiling point of formalin is about subzero 19.5 DEG C.Because boiling point is so low, indoor temperature is in so working as
Under the conditions of, the aqueous solution of formaldehyde, i.e. formalin can is evaporate into air.The evaporation rate and temperature of formalin simultaneously
Height have close relationship, when temperature raises, the speed of formalin volatilization can also be accelerated.In the relevant rule in China
In fixed, formaldehyde is number two position in the list of toxic chemical priority acccess control, it can be seen that, weight of the country for formaldehyde keeping
Visual range degree.Equally, one of carcinogenic or deforming arch-criminal is appointed as formaldehyde in the whole world, the international World Health Organization.By
Originally it is magma poisonous substance in formaldehyde, its molecular forms is extremely easily combined with protein, so as to destroy protein.When the body of human body
After the formaldehyde gas of interior suction higher concentration, the body of people can in the short period of time, and the malaise symptoms of appearance have：Respiratory tract
Serious stimulation and the different degrees of oedema of whole body, while can be with eyes stung, headache, serious may also be with bronchus
Asthma etc..If by skin and formalin, i.e. formalin directly contacts, and can cause dermatitis, even color spot, cutaneous necrosis.
If be exposed in long-time in the air containing formaldehyde gas, body can trigger the phenomenon of slow poisoning, respiratory tract occur
The uncomfortable symptom such as mucous hyperemia, allergic dermatitis, nail angling.Although the method for measure formaldehyde is many at present, light is such as divided
Method, chromatography, fluorescence method, chemical method, electrochemical process etc., it is most of in these methods must be first with air sampler by air
Formaldehyde be extracted into absorbing liquid, then take back laboratory and analyzed.Like this, experimental period is grown, and is not suitable for public place
Quick detection.With the continuous improvement of detection technique means, the detection means mainly used in China's industry at present is divided into electrification
Method and chemical analysis, used detecting instrument are mainly the external portable detector of import or entered in laboratory
The large-scale detection device of row analysis.Due to these detection means in price, convenience, operability it is defective, therefore set
A kind of Indoor Air Formaldehyde detector cost-effective, simple to operate, the degree of accuracy is high is counted, daily life can be risen great
Effect.And only electrochemical process can accomplish fast and accurately formaldehyde examination.
The content of the invention
To solve, existing formaldehyde sensor price is high, portability is poor, poor operability, poor accuracy, sensitivity is low leads
Cause the problem of can not being applied in public places and in family, primary and foremost purpose of the invention be to provide it is a kind of based on Pt- chromium carbides/
The preparation method of the formaldehyde sensor of nanocarbon catalyst.The preparation method technique is simple, may be adapted to mass produce.
Another object of the present invention is to provide that above-mentioned preparation method obtains based on Pt- chromium carbides/nanocarbon catalyst
Formaldehyde sensor, the formaldehyde sensor is cost-effective, simple to operate, the degree of accuracy is high, high sensitivity.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of the formaldehyde sensor based on Pt- chromium carbides/nanocarbon catalyst, comprises the following steps：
(1) preparation of chromium carbide/nanometer carbon matrix precursor：A certain amount of chromic salts is dissolved into water, then added into solution
A certain amount of nano-sized carbon, after ultrasonic disperse is uniform, 1~12h is stirred, is evaporated, obtains presoma；
(2) preparation of chromium carbide/nano-sized carbon：By the presoma of step (1) under certain atmosphere, with 2~10 DEG C/min's
Heating rate is warming up to 600~1200 DEG C, and is incubated 1~8h and carries out carbonization treatment, is prepared for chromium carbide/nano-carbon material；
(3) preparation of Pt- chromium carbides/nanocarbon catalyst：Platinum salt is dissolved in water, add certain mass the step of
(2) chromium carbide/nano-carbon material prepared by, after ultrasonic disperse is uniform, formic acid solution is added, after stirring 6~24h, washing,
Drying, has obtained Pt- chromium carbides/nanocarbon catalyst；
(4) preparation of formaldehyde sensor：Pt- chromium carbides/nanocarbon catalyst prepared by step (3) is coated on carbon paper,
PEM is placed as positive and negative two electrode, two electrodes centre after drying, then hot pressing under certain condition, is obtained
The formaldehyde sensor based on Pt- chromium carbides/nanocarbon catalyst.
Chromic salts described in step (1) is CrCl3、Cr(ClO4)3、Cr(NO3)3、K2Cr2O7、Na2CrO4And K2CrO4In
The mass ratio of one kind, wherein chromic salts and water is 1:100~1:20.
Nano-sized carbon described in step (1) is one kind in carbon black, activated carbon, mesoporous carbon and CNT, wherein nanometer
The mass ratio of carbon and chromic salts is 1:1~1:0.2.
Evaporated temperature described in step (1) is 85~120 DEG C.
Heat-treating atmosphere described in step (2) is one or two kinds of mixed in nitrogen, carbon monoxide and carbon dioxide
Close, gas flow is 90~200mL/min.
Platinum salt described in step (3) is one kind in platinic sodium chloride, chloroplatinic acid and potassium chloroplatinate.
The power of ultrasonic disperse processing described in step (3) is 60~120W, and ultrasonic time is 10~30min.
The mass ratio of platinum salt and chromium carbide/nano-sized carbon described in step (3) is 0.2:1~0.4:1, the matter of platinum salt and water
Amount is than being 0.003:1~0.007:1, the mass ratio of formic acid and platinum salt in formic acid solution is 5:1~35:1.
Pt- chromium carbides/load capacity of the nanocarbon catalyst on carbon paper described in step (4) is 1.5~5mg/cm2。
Hot pressing condition described in step (4) is：120~150 DEG C, pressure be 2~6MPa under conditions of hot pressing 2~
5min。
Present invention also offers a kind of first based on Pt- chromium carbides/nanocarbon catalyst obtained by above-mentioned preparation method
Aldehyde sensor.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) the formaldehyde sensor cost for preparing of the present invention is low, cost-effective, simple to operate, the degree of accuracy be up to 99.99% with
On, sensitivity 2ppm.
(2) preparation technology of the invention is simple, may be adapted to mass produce.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of Pt- chromium carbides/Nano Carbon body prepared by embodiment 24.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
A kind of formaldehyde sensor preparation method based on Pt- chromium carbides/nanocarbon catalyst of the present embodiment is by following steps
Suddenly complete：
(1) preparation of chromium carbide/nanometer carbon matrix precursor：By CrCl3It is dissolved into water, wherein CrCl3Mass ratio with water is
1:30；Carbon black, carbon black and CrCl are added into solution again3Mass ratio be 1:0.5, ultrasonic disperse is uniform under 100W power
Afterwards, 2h is stirred, is evaporated at 90 DEG C, obtains presoma；
(2) preparation of chromium carbide/nano-sized carbon：By the presoma of step (1) in a nitrogen atmosphere, gas flow 130mL/
Min, 800 DEG C are warming up to 5 DEG C/min heating rate, and are incubated 3h and carry out carbonization treatment, be prepared for chromium carbide/nano carbon material
Material；
(3) preparation of Pt- chromium carbides/nanocarbon catalyst：Potassium chloroplatinate is dissolved in water, the matter of potassium chloroplatinate and water
Amount is than being 0.004:1；Add chromium carbide/nano-carbon material prepared by step (2), potassium chloroplatinate and chromium carbide/nano-sized carbon
Mass ratio is 0.25:1, the ultrasonic 10min under the conditions of power is 80W, add formic acid solution (refer to the aqueous solution of formic acid, one
As buy is aqueous formic acid that concentration is 88%), wherein the mass ratio of the formic acid in formic acid solution and potassium chloroplatinate is 10:
1, after stirring 12h, washing, drying, obtain Pt- chromium carbides/nanocarbon catalyst；
(4) preparation of formaldehyde sensor：Pt- chromium carbides/nanocarbon catalyst prepared by step (3) is coated on carbon paper,
Wherein Pt- chromium carbides/load capacity of the nanocarbon catalyst on carbon paper is 2mg/cm2, two small pieces are therefrom taken after carbon paper is dried
As positive and negative the two poles of the earth, PEM is put among two electrodes, hot pressing under conditions of being then 3MPa in 130 DEG C, pressure
2min, it is prepared for formaldehyde sensor.
Embodiment 2：The present embodiment is as different from Example 1：Chromic salts described in step (1) is Cr (ClO4)3, remaining
Step is identical.
Embodiment 3：The present embodiment is as different from Example 2：Chromic salts described in step (1) is Cr (NO3)3, remaining step
It is rapid identical.
Embodiment 4：The present embodiment is as different from Example 3：Chromic salts described in step (1) is K2Cr2O7, remaining step
It is rapid identical.
Embodiment 5：The present embodiment is as different from Example 4：Chromic salts described in step (1) is Na2CrO4, remaining step
It is rapid identical.
Embodiment 6：The present embodiment is as different from Example 5：Chromic salts described in step (1) is K2CrO4, remaining step
It is identical.
Embodiment 7, remaining step are identical：The present embodiment is as different from Example 6：Chromic salts described in step (1) with
The mass ratio of water is 1:50.
Embodiment 8：The present embodiment is as different from Example 7：The mass ratio of chromic salts and water described in step (1) is 1:
80, remaining step is identical.
Embodiment 9：The present embodiment is as different from Example 8：Nano-sized carbon described in step (1) is activated carbon, remaining
Step is identical.
Embodiment 10：The present embodiment is as different from Example 9：Nano-sized carbon described in step (1) is mesoporous carbon, remaining
Step is identical.
Embodiment 11：The present embodiment is as different from Example 10：Nano-sized carbon described in step (1) is CNT,
Remaining step is identical.
Embodiment 12：The present embodiment is as different from Example 11：The quality of nano-sized carbon and chromic salts described in step (1)
Than for 1:0.7, remaining step is identical.
Embodiment 13：The present embodiment is as different from Example 12：Evaporated temperature described in step (1) is 105 DEG C, its
Remaining step is identical.
Embodiment 14：The present embodiment is as different from Example 13：Heat-treating atmosphere described in step (2) for nitrogen and
The mixed gas of carbon monoxide, remaining step are identical.
Embodiment 15：The present embodiment is as different from Example 14：Heat-treating atmosphere described in step (2) for nitrogen and
The mixed gas of carbon dioxide, remaining step are identical.
Embodiment 16：The present embodiment is as different from Example 15：Gas flow described in step (2) is 150mL/
Min, remaining step are identical.
Embodiment 17：The present embodiment is as different from Example 16：Platinum salt described in step (3) is platinic sodium chloride, its
Remaining step is identical.
Embodiment 18：The present embodiment is as different from Example 17：Platinum salt described in step (3) is chloroplatinic acid, remaining
Step is identical.
Embodiment 19：The present embodiment is as different from Example 18：The power of supersound process described in step (3) is
70W, ultrasonic time 30min, remaining step are identical.
Embodiment 20：The present embodiment is as different from Example 19：The power of supersound process described in step (3) is
110W, ultrasonic time 15min, remaining step are identical.
Embodiment 21：The present embodiment is as different from Example 20：Platinum salt and chromium carbide/nanometer described in step (3)
The mass ratio of carbon is 0.3:1, the mass ratio of platinum salt and water is 0.0035:1, remaining step is identical.
Embodiment 22：The present embodiment is as different from Example 21：Pt- chromium carbides/nano-sized carbon described in step (4) is urged
Load capacity of the agent on carbon paper is 2.5mg/cm2, remaining step is identical.
Embodiment 23：The present embodiment is as different from Example 22：Hot pressing condition described in step (4) is：135
DEG C, pressure be hot pressing 3min under conditions of 2MPa, remaining step is identical.
Embodiment 24
A kind of formaldehyde sensor preparation method based on Pt- chromium carbides/nanocarbon catalyst of the present embodiment is by following steps
Suddenly complete：
(1) preparation of chromium carbide/nanometer carbon matrix precursor：By CrCl3It is dissolved into water, wherein CrCl3Mass ratio with water is
1:40；Carbon black, nano carbon black and CrCl are added into solution again3Mass ratio be 1:0.4, ultrasonic disperse is equal under 90W power
After even, 2h is stirred, is evaporated at 105 DEG C, obtains presoma；
(2) preparation of chromium carbide/nano-sized carbon：By the presoma of step (1) in a nitrogen atmosphere, gas flow 110mL/
Min, 1000 DEG C are warming up to 2 DEG C/min heating rate, and are incubated 2h and carry out carbonization treatment, be prepared for chromium carbide/nano-sized carbon
Material；
(3) preparation of Pt- chromium carbides/nanocarbon catalyst：Chloroplatinic acid is dissolved in water, the mass ratio of chloroplatinic acid and water
For 0.005:1；Add chromium carbide/nano-carbon material prepared by step (2), chloroplatinic acid and the mass ratio of chromium carbide/nano-sized carbon
For 0.35:1, the ultrasonic 20min under the conditions of power is 100W, add formic acid solution, formic acid and chlorine wherein in formic acid solution
The mass ratio of platinic acid is 15:1, after stirring 8h, washing, drying, obtain Pt- chromium carbides/nanocarbon catalyst；
(4) preparation of formaldehyde sensor：Catalyst prepared by step (3) is coated on carbon paper, wherein catalyst is in carbon paper
On load capacity be 1.5mg/cm2, as positive and negative the two poles of the earth after drying, two electrodes centre is with PEM is put, then
Hot pressing 3min under conditions of being 2MPa in 140 DEG C, pressure, is prepared for formaldehyde sensor.
Fig. 1 is the X-ray diffraction spectrogram of Pt- chromium carbides/nanocarbon catalyst prepared by embodiment 24.By can be with figure
Find out obvious chromium carbide (Cr2C3) characteristic diffraction peak, illustrate that the crystallinity of chromium carbide is higher.Further, it can be seen that Pt spy
Levy diffraction maximum, it was demonstrated that be successfully prepared Pt- chromium carbides/nanocarbon catalyst., can after assembling membrane electrode as electrode material
For formaldehyde sensor, this formaldehyde sensor has the advantages that cost-effective, security is good, high sensitivity, accuracy are high,
It can be used in public place and family.
Formaldehyde sensor made from above-described embodiment 1~24 is used to detect formaldehyde, and the degree of accuracy is up to more than 99.99%, spirit
Sensitivity is 2ppm.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
- A kind of 1. preparation method of the formaldehyde sensor based on Pt- chromium carbides/nanocarbon catalyst, it is characterised in that including with Lower step：（1）Chromic salts is dissolved into water, then nano-sized carbon is added into solution, after ultrasonic disperse is uniform, 1 ~ 12 h is stirred, is evaporated, Obtain presoma；（2）By step（1）Obtained presoma is warming up to 600 under certain atmosphere, with 2 ~ 10 DEG C/min heating rate ~ 1200 DEG C, and be incubated 1 ~ 8 h and carry out carbonization treatment, chromium carbide/nano-carbon material is made；（3）Platinum salt is dissolved in water, adds step（2）Chromium carbide/nano-carbon material of preparation, after ultrasonic disperse is uniform, then Formic acid solution is added, after stirring 6 ~ 24 h, washing, drying, obtains Pt- chromium carbides/nanocarbon catalyst；（4）By step（3）Pt- chromium carbides/nanocarbon catalyst of preparation is coated on carbon paper, as positive and negative two after drying Electrode, two electrodes centre place PEM, then hot pressing, obtain the first based on Pt- chromium carbides/nanocarbon catalyst Aldehyde sensor；Step（1）Described in nano-sized carbon be carbon black, activated carbon, mesoporous carbon and CNT in one kind, wherein nano-sized carbon with The mass ratio of chromic salts is 1:1~1:0.2；Step（3）Described in platinum salt be platinic sodium chloride, chloroplatinic acid and potassium chloroplatinate in one kind；Described platinum salt and carbonization The mass ratio of chromium/nano-sized carbon is 0.2:1~0.4:1, the mass ratio of platinum salt and water is 0.003:1~0.007:1, in formic acid solution Formic acid and the mass ratio of platinum salt are 5:1~35:1.
- 2. the preparation method of the formaldehyde sensor according to claim 1 based on Pt- chromium carbides/nanocarbon catalyst, its It is characterised by, step（1）Described in chromic salts be CrCl3、Cr(ClO4)3、Cr(NO3)3、K2Cr2O7、Na2CrO4And K2CrO4In One kind, wherein the mass ratio of chromic salts and water be 1:100~1:20.
- 3. the preparation method of the formaldehyde sensor according to claim 1 based on Pt- chromium carbides/nanocarbon catalyst, its It is characterised by, step（1）Described in evaporated temperature be 85 ~ 120 DEG C.
- 4. the preparation method of the formaldehyde sensor according to claim 1 based on Pt- chromium carbides/nanocarbon catalyst, its It is characterised by, step（2）Described in carbonization treatment atmosphere be nitrogen, carbon monoxide and carbon dioxide in it is one or two kinds of Mixing, gas flow is 90 ~ 200 mL/min.
- 5. the preparation method of the formaldehyde sensor according to claim 1 based on Pt- chromium carbides/nanocarbon catalyst, its It is characterised by, step（3）Described in the power of ultrasonic disperse be 60 ~ 120 W, ultrasonic time is 10 ~ 30 min.
- 6. the preparation method of the formaldehyde sensor according to claim 1 based on Pt- chromium carbides/nanocarbon catalyst, its It is characterised by, step（4）Described in Pt- chromium carbides/load capacity of the nanocarbon catalyst on carbon paper be 1.5 ~ 5 mg/cm2。
- 7. the preparation method of the formaldehyde sensor according to claim 1 based on Pt- chromium carbides/nanocarbon catalyst, its It is characterised by, step（4）Described in hot pressing refer to：Hot pressing 2 ~ 5 under conditions of being 2 ~ 6 MPa in 120 ~ 150 DEG C, pressure min。
- 8. a kind of formaldehyde sensor based on Pt- chromium carbides/nanocarbon catalyst as described in any one of claim 1 to 7 The formaldehyde sensor based on Pt- chromium carbides/nanocarbon catalyst that preparation method obtains.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830463A (en) * | 2010-05-31 | 2010-09-15 | 河南工业大学 | Method for preparing nano chromium carbide powder |
| CN103736484A (en) * | 2014-01-13 | 2014-04-23 | 中山大学 | Supported integrated catalyst for formaldehyde purification and preparation method thereof |
| CN104181219A (en) * | 2014-08-29 | 2014-12-03 | 武汉理工大学 | Formaldehyde gas sensor |
| CN104549235A (en) * | 2014-12-19 | 2015-04-29 | 上海交通大学 | Preparation method of carbon supported nano platinum catalyst |
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| KR101035003B1 (en) * | 2008-07-16 | 2011-05-20 | 한국과학기술연구원 | A gas sensor of metaloxide including catalyst and a fbrication method thereof |
| US11371951B2 (en) * | 2012-09-27 | 2022-06-28 | Sensirion Ag | Gas sensor comprising a set of one or more sensor cells |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830463A (en) * | 2010-05-31 | 2010-09-15 | 河南工业大学 | Method for preparing nano chromium carbide powder |
| CN103736484A (en) * | 2014-01-13 | 2014-04-23 | 中山大学 | Supported integrated catalyst for formaldehyde purification and preparation method thereof |
| CN104181219A (en) * | 2014-08-29 | 2014-12-03 | 武汉理工大学 | Formaldehyde gas sensor |
| CN104549235A (en) * | 2014-12-19 | 2015-04-29 | 上海交通大学 | Preparation method of carbon supported nano platinum catalyst |
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