CN108732213A - A kind of preparation method of room temperature high-performance ethanol-sensing material - Google Patents
A kind of preparation method of room temperature high-performance ethanol-sensing material Download PDFInfo
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- CN108732213A CN108732213A CN201810591520.2A CN201810591520A CN108732213A CN 108732213 A CN108732213 A CN 108732213A CN 201810591520 A CN201810591520 A CN 201810591520A CN 108732213 A CN108732213 A CN 108732213A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The present invention provides a kind of preparation methods of room temperature high-performance ethanol-sensing material, include the following steps：Take willow wood wood powder that nano-cellulose is made brilliant；It takes graphene oxide water solution, nano-cellulose crystalline substance aqueous dispersions and vitamin C to be uniformly mixed, pours into heated sealed in mold and react, it is cooling；It is poured out after being impregnated with water and ethyl alcohol, it is dry；It pulverizes and sieves, obtains hybrid aerogel powder；By hydrochloric acid and the molten mixing of absolute ethyl alcohol, add stannous chloride, add doping titanium tetrachloride, continues to stir；Hybrid aerogel powder is added to be stirred to react；Washing centrifuges, dry；It is put into Muffle furnace, heat up to obtain hybrid powder；Pyrroles is added drop-wise in the water dissolved with polyvinyl alcohol and is stirred；Add hybrid powder to stir, adjusts pH, be exposed to after stirring60It is irradiated under Co- gamma-rays；It centrifuges, collects precipitation, washing is freeze-dried to obtain the final product.Room temperature high-performance ethanol-sensing material prepared by this law has the quick effect of good wine at normal temperatures, while having long-time stability.
Description
Technical field
The present invention relates to a kind of preparation methods of room temperature high-performance ethanol-sensing material.
Background technology
In today that modern industrial or agricultural and information technology develop rapidly, gas sensor is applied to environmental protection, food
The fields such as safety, communications and transportation and daily life, for poisonous and harmful, flammable explosive gas detection and forecast.Environment is dirty
Dye is 21
One of the project of century sternness the most, whether water pollution or air pollution all carry out the health care belt of the mankind huge
It threatens.In various organic pollutions, alcohol is most common organic matter, it brings convenience same to people's life
When, environmental pollution is also brought, therefore it is an important Task to the detection of alcohol to realize.The quick sensing technology of wine is met the tendency of
And give birth to, alcohol sensor becomes the research hotspot of sensory field, this just needs a large amount of fast response times, high sensitivity, using temperature
Spend low alcohol sensor.As the improvement of people's living standards, the quantity of motor vehicle is more and more, driving when intoxicated, there have to be huge
Security risk, the especially new appearance for handing over rule, increases the dynamics of punishing driven when intoxicated, therefore become more next to the detection of alcohol
It is more important.But the temperature in use or relatively-high temperature of current many alcohol sensors, it is not very convenient, therefore, research and development
A kind of high sensitivity, temperature in use is low, and the ethanol-sensing material that the response time is short and stability is high just plays a very important role.
Invention content
Technical problems to be solved：It for current most of ethanol-sensing material needs that just there is ethyl alcohol at high temperature good
Sensitivity, provides a kind of preparation method of room temperature high-performance ethanol-sensing material, and prepared ethanol-sensing material just has very at normal temperatures
The good quick effect of wine, the response time is short, while having long-time stability.
Technical solution：A kind of preparation method of room temperature high-performance ethanol-sensing material, ingredient by weight, including following step
Suddenly：
（1）2-4 parts of willow wood wood powders are taken, it is 2 that 30-40 parts of volume ratios, which are added,:1 benzyl carbinol solution carries out soxhlet type, removing
Extract handles 5-6h with sodium chlorite at pH4-5,75 DEG C, then handles 2-3h at 90 DEG C with 2wt% oxygen potassium oxide；
（2）1h is handled at pH4-5 with sodium chlorite, then handles 2-3h at 90 DEG C with 5wt% oxygen potassium oxide；
（3）5-10ml distilled water is added, is placed in ultrasonic wave plant cell pulverizer and is ultrasonically treated, ultrasonic power 1200W surpasses
The sound time is 30min, obtains nano-cellulose crystalline substance；
（4）Take the graphene oxide water solution of 2 parts of 5mg/mL, the nano-cellulose crystalline substance aqueous dispersions and 40-50 of 2 parts of 1-2mg/mL
Part vitamin C is uniformly mixed, and pours into salable mold, mold is sealed, be placed into 95 DEG C of baking oven and heat 4-5h
After take out, cooled to room temperature；
（5）By in mold there are liquid pour out, deionized water is added thereto, pours out deionized water after 10min, then add
Enter after ethyl alcohol impregnates 2h and pour out, adds ethyl alcohol and impregnated and poured out afterwards for 24 hours, be put into 65 DEG C of air dry oven and be dried
For 24 hours, it crushes, crosses 60 mesh sieve, obtain hybrid aerogel powder；
（6）By 1-1.5 parts of hydrochloric acid and 40-50 parts of absolute ethyl alcohols 20 min of molten mixing, 0.25-0.3 parts of stannous chloride are added,
1-2 parts of titanium tetrachlorides are added dropwise again, continue magnetic agitation 50-60 min；
（7）Hybrid aerogel powder is added, stirs 3-4 h, moves in reaction kettle, be put into drying box and react 24 at 180 DEG C
H, cooled to room temperature；
（8）Obtained sediment is washed with deionized water and absolute ethyl alcohol respectively, centrifuges, is put into air dry oven
It is dry at 50-60 DEG C；
（9）It is put into Muffle furnace, is warming up to 600 DEG C, heat preservation 2-3h obtains hybrid powder, wherein heating rate is 5 DEG C/min；
（10）0.5-1 parts of pyrroles are added drop-wise in the 50-80 parts of distilled water dissolved with 1-2 parts of polyvinyl alcohol under magnetic stirring and are stirred
5-10min；
（11）Hybrid powder stirring is added, it is 0.8-1 to adjust pH with the concentrated sulfuric acid, continues to be exposed to after stirring 5-10min60Co-γ
Under ray radioactive activity be 1.3 × 1015Bq-1.5×1015It is irradiated under Bq, dosage rate 37.8-38.0Gy/mi, the time
For 22-24h；
（12）It is centrifuged in the case where rotating speed is 15000-16000rpm, collects precipitation, be washed with deionized 3 times, be freeze-dried
Up to room temperature high-performance ethanol-sensing material.
It uses ethyl alcohol as adhesive, room temperature high-performance ethanol-sensing material of the present invention is uniformly coated on the ceramic tube with gold electrode
Outside, it places and dries in the cool at room temperature, be placed in baking oven, 5h is dried at 60 DEG C, in air 24 h of aging, then by Pt
Lead is welded to component mount and ethanol-sensing component is made on gold electrode.The second of various concentration is injected into gas chamber with miniature injector
Alcohol gas then passes to air and excludes gas, and the change with resistance in desorption process is being adsorbed with online inspection software record gas
Change.The sensitivity definition of element is S=Ra/Rg in experiment, element aerial resistance value when wherein Ra unimplanted gases,
Rg is the stationary value of the resistance of element after injecting a certain concentration under test gas after a period of time.Response time is element one
Determine the 80% required time for reaching peak response in concentration under test gas.
Advantageous effect：
Ethanol-sensing material of the present invention has good gas sensing property at normal temperatures, to ethyl alcohol, when ethanol gas concentration is 50 ppm,
Sensitivity is 1.57, when ethanol gas concentration is 200 ppm, sensitivity 3.48, when ethanol gas concentration is 400 ppm
When, sensitivity 4.98, the response time all in 9s or so, meanwhile, to the sensitivity of ethyl alcohol with the time variation undulating value very
It is small, there are good long-time stability.
Specific implementation mode
Embodiment 1
A kind of preparation method of room temperature high-performance ethanol-sensing material, ingredient by weight, include the following steps：
（1）2 parts of willow wood wood powders are taken, it is 2 that 30 parts of volume ratios, which are added,:1 benzyl carbinol solution carries out soxhlet type, removing extracting
Object handles 5h with sodium chlorite at pH4,75 DEG C, then handles 2h at 90 DEG C with 2wt% oxygen potassium oxide；
（2）1h is handled at pH4 with sodium chlorite, then handles 2h at 90 DEG C with 5wt% oxygen potassium oxide；
（3）5ml distilled water is added, is placed in ultrasonic wave plant cell pulverizer and is ultrasonically treated, ultrasonic power 1200W, ultrasound
Time is 30min, obtains nano-cellulose crystalline substance；
（4）Take the graphene oxide water solution of 2 parts of 5mg/mL, the nano-cellulose crystalline substance aqueous dispersions and 40 parts of dimensions of 2 parts of 1mg/mL
Raw element C is uniformly mixed, and pours into salable mold, mold is sealed, and is placed into after heating 4h in 95 DEG C of baking oven and is taken out,
Cooled to room temperature；
（5）By in mold there are liquid pour out, deionized water is added thereto, pours out deionized water after 10min, then add
Enter after ethyl alcohol impregnates 2h and pour out, adds ethyl alcohol and impregnated and poured out afterwards for 24 hours, be put into 65 DEG C of air dry oven and be dried
For 24 hours, it crushes, crosses 60 mesh sieve, obtain hybrid aerogel powder；
（6）By 1 part of hydrochloric acid and 40 parts of absolute ethyl alcohols 20 min of molten mixing, 0.25 part of stannous chloride is added, then be added dropwise 1
Part titanium tetrachloride, continues magnetic agitation 50min；
（7）Hybrid aerogel powder is added, stirs 3 h, moves in reaction kettle, be put into drying box at 180 DEG C and react 24 h,
Cooled to room temperature；
（8）Obtained sediment is washed with deionized water and absolute ethyl alcohol respectively, centrifuges, is put into air dry oven
It is dry at 50 DEG C；
（9）It is put into Muffle furnace, is warming up to 600 DEG C, heat preservation 2h obtains hybrid powder, wherein heating rate is 5 DEG C/min；
（10）0.5 part of pyrroles is added drop-wise in 50 parts of distilled water dissolved with 1 part of polyvinyl alcohol under magnetic stirring and stirs 5min；
（11）Hybrid powder stirring is added, it is 0.8 to adjust pH with the concentrated sulfuric acid, continues to be exposed to after stirring 5min60Co- gamma-rays
Under radioactive activity be 1.3 × 1015It is irradiated under Bq, dosage rate 37.8Gy/mi, time 22h；
（12）It is centrifuged in the case where rotating speed is 15000rpm, collects precipitation, be washed with deionized 3 times, be freeze-dried up to often
Temperature high-performance ethanol-sensing material.
Embodiment 2
A kind of preparation method of room temperature high-performance ethanol-sensing material, ingredient by weight, include the following steps：
（1）3 parts of willow wood wood powders are taken, it is 2 that 35 parts of volume ratios, which are added,:1 benzyl carbinol solution carries out soxhlet type, removing extracting
Object handles 5.5h with sodium chlorite at pH4.5,75 DEG C, then handles 2.5h at 90 DEG C with 2wt% oxygen potassium oxide；
（2）1h is handled at pH4.5 with sodium chlorite, then handles 2.5h at 90 DEG C with 5wt% oxygen potassium oxide；
（3）8ml distilled water is added, is placed in ultrasonic wave plant cell pulverizer and is ultrasonically treated, ultrasonic power 1200W, ultrasound
Time is 30min, obtains nano-cellulose crystalline substance；
（4）Take the graphene oxide water solution of 2 parts of 5mg/mL, the nano-cellulose crystalline substance aqueous dispersions of 2 parts of 1.5mg/mL and 45 parts
Vitamin C is uniformly mixed, and pours into salable mold, mold is sealed, and is placed into after heating 4.5h in 95 DEG C of baking oven
It takes out, cooled to room temperature；
（5）By in mold there are liquid pour out, deionized water is added thereto, pours out deionized water after 10min, then add
Enter after ethyl alcohol impregnates 2h and pour out, adds ethyl alcohol and impregnated and poured out afterwards for 24 hours, be put into 65 DEG C of air dry oven and be dried
For 24 hours, it crushes, crosses 60 mesh sieve, obtain hybrid aerogel powder；；
（6）By 1.3 parts of hydrochloric acid and 45 parts of absolute ethyl alcohols 20 min of molten mixing, 0.28 part of stannous chloride is added, then add dropwise
Enter 1.5 parts of titanium tetrachlorides, continues magnetic agitation 55min；
（7）Hybrid aerogel powder is added, stirs 3.5 h, moves in reaction kettle, be put into drying box and react 24 at 180 DEG C
H, cooled to room temperature；
（8）Obtained sediment is washed with deionized water and absolute ethyl alcohol respectively, centrifuges, is put into air dry oven
It is dry at 55 DEG C；
（9）It is put into Muffle furnace, is warming up to 600 DEG C, heat preservation 2.5h obtains hybrid powder, wherein heating rate is 5 DEG C/min；
（10）0.8 part of pyrroles is added drop-wise in 65 parts of distilled water dissolved with 1.5 parts of polyvinyl alcohol under magnetic stirring and stirs 8min；
（11）Hybrid powder stirring is added, it is 0.9 to adjust pH with the concentrated sulfuric acid, continues to be exposed to after stirring 8min60Co- gamma-rays
Under radioactive activity be 1.4 × 1015It is irradiated under Bq, dosage rate 37.9Gy/mi, time 23h；
（12）It is centrifuged in the case where rotating speed is 15500rpm, collects precipitation, be washed with deionized 3 times, be freeze-dried up to often
Temperature high-performance ethanol-sensing material.
Embodiment 3
A kind of preparation method of room temperature high-performance ethanol-sensing material, ingredient by weight, include the following steps：
（1）4 parts of willow wood wood powders are taken, it is 2 that 40 parts of volume ratios, which are added,:1 benzyl carbinol solution carries out soxhlet type, removing extracting
Object handles 6h with sodium chlorite at pH5,75 DEG C, then handles 3h at 90 DEG C with 2wt% oxygen potassium oxide；
（2）1h is handled at pH5 with sodium chlorite, then handles 3h at 90 DEG C with 5wt% oxygen potassium oxide；
（3）10ml distilled water is added, is placed in ultrasonic wave plant cell pulverizer and is ultrasonically treated, ultrasonic power 1200W, ultrasound
Time is 30min, obtains nano-cellulose crystalline substance；
（4）Take the graphene oxide water solution of 2 parts of 5mg/mL, the nano-cellulose crystalline substance aqueous dispersions and 50 parts of dimensions of 2 parts of 2mg/mL
Raw element C is uniformly mixed, and pours into salable mold, mold is sealed, and is placed into after heating 5h in 95 DEG C of baking oven and is taken out,
Cooled to room temperature；
（5）By in mold there are liquid pour out, deionized water is added thereto, pours out deionized water after 10min, then add
Enter after ethyl alcohol impregnates 2h and pour out, adds ethyl alcohol and impregnated and poured out afterwards for 24 hours, be put into 65 DEG C of air dry oven and be dried
For 24 hours, it crushes, crosses 60 mesh sieve, obtain hybrid aerogel powder；
（6）By 1.5 parts of hydrochloric acid and 50 parts of absolute ethyl alcohols 20 min of molten mixing, 0.3 part of stannous chloride is added, then be added dropwise
2 parts of titanium tetrachlorides continue 60 min of magnetic agitation；
（7）Hybrid aerogel powder is added, stirs 4 h, moves in reaction kettle, be put into drying box at 180 DEG C and react 24 h,
Cooled to room temperature；
（8）Obtained sediment is washed with deionized water and absolute ethyl alcohol respectively, centrifuges, is put into air dry oven
It is dry at 60 DEG C；
（9）It is put into Muffle furnace, is warming up to 600 DEG C, heat preservation 3h obtains hybrid powder, wherein heating rate is 5 DEG C/min；
（10）1 part of pyrroles is added drop-wise in 80 parts of distilled water dissolved with 2 parts of polyvinyl alcohol under magnetic stirring and stirs 10min；
（11）Hybrid powder stirring is added, it is 1 to adjust pH with the concentrated sulfuric acid, continues to be exposed to after stirring 10min60Under Co- gamma-rays
It is 1.5 × 10 in radioactive activity15It is irradiated under Bq, dosage rate 38.0Gy/mi, the time is for 24 hours；
（12）It is centrifuged in the case where rotating speed is 16000rpm, collects precipitation, be washed with deionized 3 times, be freeze-dried up to often
Temperature high-performance ethanol-sensing material.
The sensitivity of 1 room temperature high-performance ethanol-sensing material of table
2 change of sensitivity in 0-30 of embodiment 3 of table
From table 1 it will be seen that the sensitivity of room temperature high-performance ethanol-sensing material of the present invention at normal temperatures, has very ethyl alcohol
Good gas sensing property, when ethanol gas concentration is 50 ppm, sensitivity 1.57, when ethanol gas concentration is 200 ppm,
Sensitivity is 3.48, and when ethanol gas concentration is 400 ppm, sensitivity 4.98, the response time is all in 9s or so, response
Between it is short, meanwhile, as known from Table 2, embodiment 3 finds sensitivity at any time to the sensitivity of ethyl alcohol with the variation of time in 30 days
Between undulating value very little, illustrate ethanol-sensing material of the present invention have good long-time stability.
Claims (1)
1. a kind of preparation method of room temperature high-performance ethanol-sensing material, it is characterised in that：Ingredient by weight, including following step
Suddenly：
（1）2-4 parts of willow wood wood powders are taken, it is 2 that 30-40 parts of volume ratios, which are added,:1 benzyl carbinol solution carries out soxhlet type, removing
Extract handles 5-6h with sodium chlorite at pH4-5,75 DEG C, then handles 2-3h at 90 DEG C with 2wt% oxygen potassium oxide；
（2）1h is handled at pH4-5 with sodium chlorite, then handles 2-3h at 90 DEG C with 5wt% oxygen potassium oxide；
（3）5-10ml distilled water is added, is placed in ultrasonic wave plant cell pulverizer and is ultrasonically treated, ultrasonic power 1200W surpasses
The sound time is 30min, obtains nano-cellulose crystalline substance；
（4）Take the graphene oxide water solution of 2 parts of 5mg/mL, the nano-cellulose crystalline substance aqueous dispersions and 40-50 of 2 parts of 1-2mg/mL
Part vitamin C is uniformly mixed, and pours into salable mold, mold is sealed, be placed into 95 DEG C of baking oven and heat 4-5h
After take out, cooled to room temperature；
（5）By in mold there are liquid pour out, deionized water is added thereto, pours out deionized water after 10min, then add
Enter after ethyl alcohol impregnates 2h and pour out, adds ethyl alcohol and impregnated and poured out afterwards for 24 hours, be put into 65 DEG C of air dry oven and be dried
For 24 hours, it crushes, crosses 60 mesh sieve, obtain hybrid aerogel powder；
（6）By 1-1.5 parts of hydrochloric acid and 40-50 parts of absolute ethyl alcohols 20 min of molten mixing, 0.25-0.3 parts of stannous chloride are added,
1-2 parts of titanium tetrachlorides are added dropwise again, continue magnetic agitation 50-60 min；
（7）Hybrid aerogel powder is added, stirs 3-4 h, moves in reaction kettle, be put into drying box and react 24 at 180 DEG C
H, cooled to room temperature；
（8）Obtained sediment is washed with deionized water and absolute ethyl alcohol respectively, centrifuges, is put into air dry oven
It is dry at 50-60 DEG C；
（9）It is put into Muffle furnace, is warming up to 600 DEG C, heat preservation 2-3h obtains hybrid powder, wherein heating rate is 5 DEG C/min；
（10）0.5-1 parts of pyrroles are added drop-wise in the 50-80 parts of distilled water dissolved with 1-2 parts of polyvinyl alcohol under magnetic stirring and are stirred
5-10min；
（11）Hybrid powder stirring is added, it is 0.8-1 to adjust pH with the concentrated sulfuric acid, continues to be exposed to after stirring 5-10min60Co-γ
Under ray radioactive activity be 1.3 × 1015Bq-1.5×1015It is irradiated under Bq, dosage rate 37.8-38.0Gy/mi, the time
For 22-24h；
（12）It is centrifuged in the case where rotating speed is 15000-16000rpm, collects precipitation, be washed with deionized 3 times, be freeze-dried
Up to room temperature high-performance ethanol-sensing material.
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