CN108218298A - A kind of rare earth doped gas sensitive and preparation method thereof - Google Patents
A kind of rare earth doped gas sensitive and preparation method thereof Download PDFInfo
- Publication number
- CN108218298A CN108218298A CN201810055887.2A CN201810055887A CN108218298A CN 108218298 A CN108218298 A CN 108218298A CN 201810055887 A CN201810055887 A CN 201810055887A CN 108218298 A CN108218298 A CN 108218298A
- Authority
- CN
- China
- Prior art keywords
- parts
- rare earth
- product
- earth doped
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/28—Polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00991—Uses not provided for elsewhere in C04B2111/00 for testing
Abstract
The present invention provides a kind of rare earth doped gas sensitives and preparation method thereof.Preparation method is as follows：Nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed and flowed back, cools down to obtain product A；Citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water are mixed and reacted；Cooling adds in tungstic acid, nano lanthanum oxide, nano tin dioxide, polypyrrole, polyvinylpyrrolidone and acetic acid, is stirred to react；Washing to upper liquid is clarified after centrifugation；Dry to obtain product B；By product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N' and the mixing of N, N dimethylformamide disperse to obtain dispersion liquid；Product A and N, N dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；Ultrasound, it is still aging；It centrifuges, washing and drying；It is put into Muffle furnace and calcines, be cooled to room temperature to obtain the final product.The material of the present invention increases the susceptibility of hydrogen sulfide gas with the increase of its concentration, and gas sensing property is strong, while repeatable usability is good.
Description
Technical field
The present invention relates to gas sensing property Material Fields, and in particular to a kind of rare earth doped gas sensitive and preparation method thereof.
Background technology
With the rapid development of economy, people’s lives level is also greatly improved, and at the same time, our life
Environment living is also constantly discharged by serious destruction, especially our atmospheric environment, toxic and harmful gas, hydrogen sulfide
It is exactly wherein more serious one kind.It is a kind of acute severe toxicity, suck a small amount of high-concentration hydrogen sulfide can in fatal in the short time,
The hydrogen sulfide of low concentration all has an impact eye, respiratory system and nervous centralis.Therefore, it lives in order to which we are effectively detected
Gaseous environment, need to research and develop a kind of gas sensor that can effectively detect nitrogen oxides in time.Gas sensor
Refer to tested gas concentration and ingredient can be converted into according to certain rule the device or device of usable output signal.By grinding
Study carefully has become numerous enterprises and researcher studies jointly come the performance for the gas sensitive for providing effective detection hydrogen sulfide gas
Target.
Invention content
Technical problems to be solved：The object of the present invention is to provide a kind of rare earth doped gas sensitive, to stink damp
The susceptibility of body increases with the increase of its concentration, and gas sensing property is strong, while repeatable usability is good.
Technical solution：A kind of rare earth doped gas sensitive is prepared by following component with parts by weight：Citric acid 0.1-
0.3 part, 10-20 parts of nine water ferric nitrate, 5-10 parts of zinc acetate dihydrate, 0.2-0.3 parts of tungstic acid, nano lanthanum oxide 0.5-0.8
Part, 0.1-0.2 parts of dehydroactic acid sodium, 0.3-0.5 parts of N, N'- bis- oleoyl ethylenediamine diethyl sodium sulfonates, N, N- dimethyl formyls
80-100 parts of amine, 0.2-0.5 parts of nano tin dioxide, 5-10 parts of mucopolysaccharide, 0.1-0.3 parts of polypyrrole, polyvinylpyrrolidone
0.05-0.1 parts, 0.5-1 parts of acetic acid, 4-6 parts of ethylene glycol, 80-100 parts of distilled water.
It is further preferred that a kind of rare earth doped gas sensitive, is prepared by following component with parts by weight：Lemon
0.2 part of acid, 15 parts of nine water ferric nitrate, 8 parts of zinc acetate dihydrate, 0.25 part of tungstic acid, 0.7 part of nano lanthanum oxide, dehydroactic acid
0.15 part of sodium, 0.4 part of the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N, N'-, 90 parts of N,N-dimethylformamide, nano tin dioxide
0.4 part, 8 parts of mucopolysaccharide, 0.2 part of polypyrrole, 0.08 part of polyvinylpyrrolidone, 0.8 part of acetic acid, 5 parts of ethylene glycol, distilled water 90
Part.
The preparation method of above-mentioned rare earth doped gas sensitive includes the following steps：
(1) nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed, flow back 15-20min at 150-160 DEG C, slowly cools to
Room temperature obtains product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2-3h at 150-170 DEG C of temperature；
(4) 100-120 DEG C is cooled to, adds in tungstic acid, nano lanthanum oxide, nano tin dioxide, polypyrrole, polyvinylpyrrolidine
Ketone and acetic acid, are stirred to react 2-3h；
(5) it is washed after being washed with distilled water 2-4 times after being centrifuged under rotating speed 6000-7000rpm with centrifuge with absolute ethyl alcohol
It is clarified to upper liquid；
(6) it is put into baking oven, dries 11-12h at 80-90 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 60-80 parts of n,N-Dimethylformamide, are surpassed
Sound dispersion 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 1-2h, still aging 23-24h；
(10) it is centrifuged under rotating speed 6000-7000rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 11-12h at 80-90 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 2-3h at 400-500 DEG C of temperature, be cooled to room temperature to obtain the final product.
It is further preferred that reflux temperature is 155 DEG C in step (1), return time 19min.
It is further preferred that reaction temperature is 160 DEG C in step (3), reaction time 2.5h.
It is further preferred that 110 DEG C are cooled in step (4), reaction time 2.5h.
It is further preferred that ultrasonic time is 1.5h, digestion time 23.5h in step (9).
It is further preferred that temperature is 450 DEG C in step (12), the calcination time is 2.5h.
Advantageous effect：The present invention rare earth doped gas sensitive to the susceptibility of hydrogen sulfide gas with the increase of its concentration and
Increase, 6.9 are reached as high as to hydrogen sulfide gas susceptibility under 100ppm concentration, when concentration reaches 2000ppm, susceptibility
Highest can rise to 16.0, and gas sensing property is strong, while repeatable usability is good.
Specific embodiment
Embodiment 1
A kind of rare earth doped gas sensitive is prepared by following component with parts by weight：0.1 part of citric acid, nine water ferric nitrates
10 parts, 5 parts of zinc acetate dihydrate, 0.2 part of tungstic acid, 0.5 part of nano lanthanum oxide, 0.1 part of dehydroactic acid sodium, the bis- oleoyls of N, N'-
0.3 part of base ethylenediamine diethyl sodium sulfonate, 80 parts of N,N-dimethylformamide, 0.2 part of nano tin dioxide, 5 parts of mucopolysaccharide, polypyrrole
0.1 part, 0.05 part of polyvinylpyrrolidone, 0.5 part of acetic acid, 4 parts of ethylene glycol, 80 parts of distilled water.
The preparation method of above-mentioned rare earth doped gas sensitive is：
(1) nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed, flow back 15min at 150 DEG C, is slowly cooled to room temperature, obtains
Product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2h at 150 DEG C of temperature；
(4) be cooled to 100 DEG C, add in tungstic acid, nano lanthanum oxide, nano tin dioxide, polypyrrole, polyvinylpyrrolidone and
Acetic acid is stirred to react 2h；
(5) after being washed with distilled water 2 times after being centrifuged under rotating speed 6000rpm with centrifuge upper liquid is washed till with absolute ethyl alcohol
Clarification；
(6) it is put into baking oven, dries 11h at 80 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 60 parts of n,N-Dimethylformamide, ultrasound point
Scattered 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 1h, still aging 23h；
(10) it is centrifuged under rotating speed 6000rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 11h at 80 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 2h at 400 DEG C of temperature, be cooled to room temperature to obtain the final product.
Embodiment 2
A kind of rare earth doped gas sensitive is prepared by following component with parts by weight：0.2 part of citric acid, nine water ferric nitrates
12 parts, 7 parts of zinc acetate dihydrate, 0.25 part of tungstic acid, 0.6 part of nano lanthanum oxide, the bis- oil of 0.15 part of dehydroactic acid sodium, N, N'-
0.4 part of Ethylene Diamine diethyl sodium sulfonate, 85 parts of N,N-dimethylformamide, 0.3 part of nano tin dioxide, 6 parts of mucopolysaccharide, poly- pyrrole
Cough up 0.15 part, 0.07 part of polyvinylpyrrolidone, 0.7 part of acetic acid, 5 parts of ethylene glycol, 85 parts of distilled water.
The preparation method of above-mentioned rare earth doped gas sensitive is：
(1) nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed, flow back 17min at 155 DEG C, is slowly cooled to room temperature, obtains
Product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2.5h at 160 DEG C of temperature；
(4) be cooled to 110 DEG C, add in tungstic acid, nano lanthanum oxide, nano tin dioxide, polypyrrole, polyvinylpyrrolidone and
Acetic acid is stirred to react 2.5h；
(5) after being washed with distilled water 3 times after being centrifuged under rotating speed 6500rpm with centrifuge upper liquid is washed till with absolute ethyl alcohol
Clarification；
(6) it is put into baking oven, dries 11.5h at 85 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 70 parts of n,N-Dimethylformamide, ultrasound point
Scattered 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 1.5h, still aging 23.5h；
(10) it is centrifuged under rotating speed 6000rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 11h at 80 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 2h at 450 DEG C of temperature, be cooled to room temperature to obtain the final product.
Embodiment 3
A kind of rare earth doped gas sensitive is prepared by following component with parts by weight：0.2 part of citric acid, nine water ferric nitrates
15 parts, 8 parts of zinc acetate dihydrate, 0.25 part of tungstic acid, 0.7 part of nano lanthanum oxide, the bis- oil of 0.15 part of dehydroactic acid sodium, N, N'-
0.4 part of Ethylene Diamine diethyl sodium sulfonate, 90 parts of N,N-dimethylformamide, 0.4 part of nano tin dioxide, 8 parts of mucopolysaccharide, poly- pyrrole
Cough up 0.2 part, 0.08 part of polyvinylpyrrolidone, 0.8 part of acetic acid, 5 parts of ethylene glycol, 90 parts of distilled water.
The preparation method of above-mentioned rare earth doped gas sensitive is：
(1) nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed, flow back 18min at 155 DEG C, is slowly cooled to room temperature, obtains
Product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2.5h at 160 DEG C of temperature；
(4) be cooled to 110 DEG C, add in tungstic acid, nano lanthanum oxide, nano tin dioxide, polypyrrole, polyvinylpyrrolidone and
Acetic acid is stirred to react 2.5h；
(5) after being washed with distilled water 3 times after being centrifuged under rotating speed 6500rpm with centrifuge upper liquid is washed till with absolute ethyl alcohol
Clarification；
(6) it is put into baking oven, dries 11.5h at 85 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 70 parts of n,N-Dimethylformamide, ultrasound point
Scattered 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 1.5h, still aging 23.5h；
(10) it is centrifuged under rotating speed 6500rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 11.5h at 85 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 2.5h at 450 DEG C of temperature, be cooled to room temperature to obtain the final product.
Embodiment 4
A kind of rare earth doped gas sensitive is prepared by following component with parts by weight：0.3 part of citric acid, nine water ferric nitrates
20 parts, 10 parts of zinc acetate dihydrate, 0.3 part of tungstic acid, 0.8 part of nano lanthanum oxide, 0.2 part of dehydroactic acid sodium, the bis- oleoyls of N, N'-
0.5 part of base ethylenediamine diethyl sodium sulfonate, 100 parts of N,N-dimethylformamide, 0.5 part of nano tin dioxide, 10 parts of mucopolysaccharide, poly- pyrrole
Cough up 0.3 part, 0.1 part of polyvinylpyrrolidone, 1 part of acetic acid, 6 parts of ethylene glycol, 100 parts of distilled water.
The preparation method of above-mentioned rare earth doped gas sensitive is：
(1) nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed, flow back 20min at 160 DEG C, is slowly cooled to room temperature, obtains
Product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2-3h at 170 DEG C of temperature；
(4) be cooled to 120 DEG C, add in tungstic acid, nano lanthanum oxide, nano tin dioxide, polypyrrole, polyvinylpyrrolidone and
Acetic acid is stirred to react 3h；
(5) after being washed with distilled water 4 times after being centrifuged under rotating speed 7000rpm with centrifuge upper liquid is washed till with absolute ethyl alcohol
Clarification；
(6) it is put into baking oven, dries 12h at 90 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 80 parts of n,N-Dimethylformamide, ultrasound point
Scattered 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 2h, it is still aging for 24 hours；
(10) it is centrifuged under rotating speed 7000rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 12h at 90 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 3h at 500 DEG C of temperature, be cooled to room temperature to obtain the final product.
Comparative example 1
Difference lies in replace zinc acetate dihydrate with nine water ferric nitrates with embodiment 1 for the present embodiment.Specifically：
A kind of rare earth doped gas sensitive is prepared by following component with parts by weight：0.1 part of citric acid, nine water ferric nitrates
15 parts, 0.2 part of tungstic acid, 0.5 part of nano lanthanum oxide, 0.1 part of dehydroactic acid sodium, the bis- oleoyl ethylenediamine diethyl sulphurs of N, N'-
Sour 0.3 part of sodium, 80 parts of N,N-dimethylformamide, 0.2 part of nano tin dioxide, 5 parts of mucopolysaccharide, 0.1 part of polypyrrole, polyethylene pyrrole
0.05 part of pyrrolidone, 0.5 part of acetic acid, 4 parts of ethylene glycol, 80 parts of distilled water.
The preparation method of above-mentioned rare earth doped gas sensitive is：
(1) nine water ferric nitrates and ethylene glycol are mixed, flow back 15min at 150 DEG C, is slowly cooled to room temperature, obtains product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2h at 150 DEG C of temperature；
(4) be cooled to 100 DEG C, add in tungstic acid, nano lanthanum oxide, nano tin dioxide, polypyrrole, polyvinylpyrrolidone and
Acetic acid is stirred to react 2h；
(5) after being washed with distilled water 2 times after being centrifuged under rotating speed 6000rpm with centrifuge upper liquid is washed till with absolute ethyl alcohol
Clarification；
(6) it is put into baking oven, dries 11h at 80 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 60 parts of n,N-Dimethylformamide, ultrasound point
Scattered 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 1h, still aging 23h；
(10) it is centrifuged under rotating speed 6000rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 11h at 80 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 2h at 400 DEG C of temperature, be cooled to room temperature to obtain the final product.
Comparative example 2
Difference lies in do not contain nano lanthanum oxide with embodiment 1 for the present embodiment.Specifically：
A kind of gas sensitive is prepared by following component with parts by weight：0.1 part of citric acid, 10 parts of nine water ferric nitrate, two water vinegar
Sour 5 parts of zinc, 0.2 part of tungstic acid, 0.1 part of dehydroactic acid sodium, 0.3 part of the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N, N'-, N, N-
80 parts of dimethylformamide, 0.2 part of nano tin dioxide, 5 parts of mucopolysaccharide, 0.1 part of polypyrrole, 0.05 part of polyvinylpyrrolidone,
0.5 part of acetic acid, 4 parts of ethylene glycol, 80 parts of distilled water.
The preparation method of above-mentioned rare earth doped gas sensitive is：
(1) nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed, flow back 15min at 150 DEG C, is slowly cooled to room temperature, obtains
Product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2h at 150 DEG C of temperature；
(4) 100 DEG C are cooled to, adds in tungstic acid, nano tin dioxide, polypyrrole, polyvinylpyrrolidone and acetic acid, stirring is anti-
Answer 2h；
(5) after being washed with distilled water 2 times after being centrifuged under rotating speed 6000rpm with centrifuge upper liquid is washed till with absolute ethyl alcohol
Clarification；
(6) it is put into baking oven, dries 11h at 80 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 60 parts of n,N-Dimethylformamide, ultrasound point
Scattered 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 1h, still aging 23h；
(10) it is centrifuged under rotating speed 6000rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 11h at 80 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 2h at 400 DEG C of temperature, be cooled to room temperature to obtain the final product.
Comparative example 3
Difference lies in do not contain tungstic acid and nano tin dioxide with embodiment 1 for the present embodiment.Specifically：
A kind of rare earth doped gas sensitive is prepared by following component with parts by weight：0.1 part of citric acid, nine water ferric nitrates
10 parts, 5 parts of zinc acetate dihydrate, 0.5 part of nano lanthanum oxide, 0.1 part of dehydroactic acid sodium, the bis- oleoyl ethylenediamine diethyl sulphurs of N, N'-
Sour 0.3 part of sodium, 80 parts of N,N-dimethylformamide, 5 parts of mucopolysaccharide, 0.1 part of polypyrrole, 0.05 part of polyvinylpyrrolidone, second
0.5 part of acid, 4 parts of ethylene glycol, 80 parts of distilled water.
The preparation method of above-mentioned rare earth doped gas sensitive is：
(1) nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed, flow back 15min at 150 DEG C, is slowly cooled to room temperature, obtains
Product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2h at 150 DEG C of temperature；
(4) 100 DEG C are cooled to, nano lanthanum oxide, polypyrrole, polyvinylpyrrolidone and acetic acid is added in, is stirred to react 2h；
(5) after being washed with distilled water 2 times after being centrifuged under rotating speed 6000rpm with centrifuge upper liquid is washed till with absolute ethyl alcohol
Clarification；
(6) it is put into baking oven, dries 11h at 80 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 60 parts of n,N-Dimethylformamide, ultrasound point
Scattered 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 1h, still aging 23h；
(10) it is centrifuged under rotating speed 6000rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 11h at 80 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 2h at 400 DEG C of temperature, be cooled to room temperature to obtain the final product.
The rare earth doped gas sensitive of table 1 is to the sensibility of hydrogen sulfide gas
Note：The determination sensor operating temperature of gas sensing property is 250 DEG C
Material of the present invention sees the above table the sensibility of hydrogen sulfide gas, to the susceptibility of hydrogen sulfide gas with the increase of its concentration
And increase, 6.9 are reached as high as to hydrogen sulfide gas susceptibility under 100ppm concentration, it is sensitive when concentration reaches 2000ppm
Degree highest can rise to 16.0, and gas sensing property is strong, while repeatable usability is good.
Claims (8)
1. a kind of rare earth doped gas sensitive, it is characterised in that：It is prepared by following component with parts by weight：Citric acid 0.1-
0.3 part, 10-20 parts of nine water ferric nitrate, 5-10 parts of zinc acetate dihydrate, 0.2-0.3 parts of tungstic acid, nano lanthanum oxide 0.5-0.8
Part, 0.1-0.2 parts of dehydroactic acid sodium, 0.3-0.5 parts of N, N'- bis- oleoyl ethylenediamine diethyl sodium sulfonates, N, N- dimethyl formyls
80-100 parts of amine, 0.2-0.5 parts of nano tin dioxide, 5-10 parts of mucopolysaccharide, 0.1-0.3 parts of polypyrrole, polyvinylpyrrolidone
0.05-0.1 parts, 0.5-1 parts of acetic acid, 4-6 parts of ethylene glycol, 80-100 parts of distilled water.
2. a kind of rare earth doped gas sensitive according to claim 1, it is characterised in that：By following component with parts by weight
It is prepared：0.2 part of citric acid, 15 parts of nine water ferric nitrate, 8 parts of zinc acetate dihydrate, 0.25 part of tungstic acid, nano lanthanum oxide
0.7 part, 0.15 part of dehydroactic acid sodium, 0.4 part of the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N, N'-, N,N-dimethylformamide 90
Part, 0.4 part of nano tin dioxide, 8 parts of mucopolysaccharide, 0.2 part of polypyrrole, 0.08 part of polyvinylpyrrolidone, 0.8 part of acetic acid, second two
5 parts of alcohol, 90 parts of distilled water.
3. a kind of preparation method of rare earth doped gas sensitive of claim 1 to 2 any one of them, it is characterised in that：Packet
Include following steps：
(1) nine water ferric nitrates, zinc acetate dihydrate and ethylene glycol are mixed, flow back 15-20min at 150-160 DEG C, slowly cools to
Room temperature obtains product A；
(2) 20min is mixed in citric acid, dehydroactic acid sodium, mucopolysaccharide and distilled water；
(3) it is put into reaction kettle, reacts 2-3h at 150-170 DEG C of temperature；
(4) 100-120 DEG C is cooled to, adds in tungstic acid, nano lanthanum oxide, nano tin dioxide, polypyrrole, polyvinylpyrrolidine
Ketone and acetic acid, are stirred to react 2-3h；
(5) it is washed after being washed with distilled water 2-4 times after being centrifuged under rotating speed 6000-7000rpm with centrifuge with absolute ethyl alcohol
It is clarified to upper liquid；
(6) it is put into baking oven, dries 11-12h at 80-90 DEG C of temperature, obtain product B；
(7) by product B, N, the bis- oleoyl ethylenediamine diethyl sodium sulfonates of N'- are mixed with 60-80 parts of n,N-Dimethylformamide, are surpassed
Sound dispersion 2h obtains dispersion liquid；
(8) product A and remaining n,N-Dimethylformamide are mixed, are slowly added drop-wise in above-mentioned dispersion liquid；
(9) with Ultrasound Instrument ultrasound 1-2h, still aging 23-24h；
(10) it is centrifuged under rotating speed 6000-7000rpm with centrifuge, is washed after being washed with water with absolute ethyl alcohol；
(11) it is put into baking oven, dries 11-12h at 80-90 DEG C of temperature；
(12) it is put into Muffle furnace, calcines 2-3h at 400-500 DEG C of temperature, be cooled to room temperature to obtain the final product.
4. a kind of preparation method of rare earth doped gas sensitive according to claim 3, it is characterised in that：The step
(1) reflux temperature is 155 DEG C in, return time 19min.
5. a kind of preparation method of rare earth doped gas sensitive according to claim 3, it is characterised in that：The step
(3) reaction temperature is 160 DEG C in, reaction time 2.5h.
6. a kind of preparation method of rare earth doped gas sensitive according to claim 3, it is characterised in that：The step
(4) 110 DEG C are cooled in, reaction time 2.5h.
7. a kind of preparation method of rare earth doped gas sensitive according to claim 3, it is characterised in that：The step
(9) ultrasonic time is 1.5h, digestion time 23.5h in.
8. a kind of preparation method of rare earth doped gas sensitive according to claim 3, it is characterised in that：The step
(12) temperature is 450 DEG C in, and the calcination time is 2.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810055887.2A CN108218298A (en) | 2018-01-18 | 2018-01-18 | A kind of rare earth doped gas sensitive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810055887.2A CN108218298A (en) | 2018-01-18 | 2018-01-18 | A kind of rare earth doped gas sensitive and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108218298A true CN108218298A (en) | 2018-06-29 |
Family
ID=62668202
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810055887.2A Withdrawn CN108218298A (en) | 2018-01-18 | 2018-01-18 | A kind of rare earth doped gas sensitive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108218298A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111613820A (en) * | 2020-05-08 | 2020-09-01 | 深圳氢时代新能源科技有限公司 | Composite proton exchange membrane, preparation method thereof and fuel cell |
| CN114813880A (en) * | 2022-04-28 | 2022-07-29 | 安徽大学 | Integrated electrochemical gas sensor and preparation process thereof |
-
2018
- 2018-01-18 CN CN201810055887.2A patent/CN108218298A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111613820A (en) * | 2020-05-08 | 2020-09-01 | 深圳氢时代新能源科技有限公司 | Composite proton exchange membrane, preparation method thereof and fuel cell |
| CN111613820B (en) * | 2020-05-08 | 2021-03-12 | 深圳氢时代新能源科技有限公司 | Composite proton exchange membrane, preparation method thereof and fuel cell |
| CN114813880A (en) * | 2022-04-28 | 2022-07-29 | 安徽大学 | Integrated electrochemical gas sensor and preparation process thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108218298A (en) | A kind of rare earth doped gas sensitive and preparation method thereof | |
| Li et al. | Reaction-based highly selective and sensitive monomer/polymer probes with Schiff base groups for the detection of Hg2+ and Fe3+ ions | |
| CN104926981A (en) | Preparation method for fluorescence sensing material based on molecular imprinting and carbon dots | |
| CN107383037A (en) | A kind of long wave elongated H2S fluorescence probes and its synthetic method and application | |
| CN107699234A (en) | A kind of Schiff bases Multifunction fluorescent probe and its preparation method and application | |
| CN106916822A (en) | A kind of method of utilization adaptor molecules switch detection AFB1 | |
| CN109867611A (en) | A kind of for red wine and in vivo water-soluble two-photon hydrogen sulfide fluorescence probe and its preparation method and application of sulfurated hydrogen detection | |
| Căta et al. | Evaluation of antioxidant activities of some small fruits containing anthocyanins using electrochemical and chemical methods | |
| Panhwar et al. | Synthesis and properties of zirconium (IV) and molybdate (II) morin complexes | |
| CN111795964A (en) | Method for quantitatively detecting caprylyl hydroximic acid in cosmetics based on spectrophotometry | |
| CN104561307B (en) | Primer for detecting trichothecene group B-class toxin of fusaria through PCR and application of primer | |
| CN107325083B (en) | Coumarin fluorophore ratio fluorescent molecular probe for iron ion detection and synthesis and use methods thereof | |
| CN108622944B (en) | Preparation and application of copper ferrite nickel material with soft magnetism and acetone gas sensitivity regulated and controlled by pH value and adhesive | |
| CN106153768B (en) | Amanita hemolysin molecular engram material is used for the solid phase extraction method of α-amanitin and β-amanitin | |
| CN107760298A (en) | A kind of fluorescence probe for detecting bisulfite and preparation method and application | |
| CN109211985A (en) | A kind of flexibility alkaline gas sensing chip and preparation method thereof | |
| CN103196851A (en) | Measuring method of arsenic content of glyceryl triacetate | |
| CN112067674A (en) | Molecular imprinting electrochemical sensor and method for detecting folic acid content by using same | |
| CN106198826B (en) | With the method for tocopherol and tocotrienols content in the positive chemical source mass Spectrometry for Determination edible vegetable oil of gas-chromatography | |
| Yoe et al. | Reactivity of substituted thioureas with inorganic ions | |
| CN110501402A (en) | A kind of electrochemical sensor and its detection method of super sensitivity detection sulphathiazole | |
| CN104655604B (en) | It is a kind of to be used to detect fluorescent optical sensor of fluorine ion and preparation method thereof | |
| CN110627530A (en) | Gas sensor for detecting trimethylamine | |
| CN103819693B (en) | A kind of preparation method of formaldehyde responsive type nano-particle solution | |
| Singh et al. | Synthesis, characterization and ion-exchanging properties of a novel ion-exchange resin, part II |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180629 |