CN108802117A - A kind of method and application preparing alcohol gas-sensitive material based on tin mud modification - Google Patents
A kind of method and application preparing alcohol gas-sensitive material based on tin mud modification Download PDFInfo
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Abstract
The invention belongs to comprehensive reutilization, gas sensing material and the field of environment protection of the by-product tin mud in tin secondary resource-electrotinning production, relate to a kind of method and application preparing alcohol gas-sensitive material based on tin mud modification.The ethanol-sensing material of the present invention be deposited in being produced by electrotinning plating trench bottom trade waste tin mud it is acidified, washing is dry, precious metal doping and subsequent heat treatment process obtain.Manufactured gas sensor has higher sensitivity, the quickly excellent air-sensitive performance such as response regeneration rate to ethyl alcohol.It is applied to gas sensitive field while reducing tin resource waste, reducing economic cost, reduction environmental pollution, is a kind of research method of environmentally friendly sustainable development.
Description
Technical field
The invention belongs to tin secondary resource comprehensive reutilization, gas sensing materials and environmentally friendly development field are special
Be not to electrotinning produce in by-product-tin mud modification and its applied to the preparation of alcohol gas sensor.
Background technology
Tin belongs to rare precious metal, and China's tin metal industry is larger for requirement, and market total requirement continues to increase, and tin in a short time
Resource is not in be significantly increased, therefore to the reasonable efficient utilization of tin secondary resource, can not only successfully manage tin resource shortage
And waste problem, be greatly facilitated economic development, while being conducive to environmental protection.Tin mud is as a kind of important secondary money of high yield tin
Source, is the waste that plating trench bottom generates in electrotinning production, its presence can promote tin plate to generate surface defect, increase simultaneously
Add the consumption of tin anode, and its exclusion processing more aggravates the deterioration of environment, such as rationally cannot effectively utilize, even more tin resource
Serious waste, it is meant that the increase of economic cost.On the basis of environmental protection, the effective recycling of tin resource and exploitation are improved
Applied to the more worth research of other research fields and concern.
The main component of tin mud is stannic oxide (SnO2), as a kind of important metal oxide semiconductor, due to changing
Learn that stability is good, the advantages that haveing excellent performance, is of low cost is widely used to gas sensor domain.Made of stannic oxide
Gas sensor, to many combustible gases, environmental pollution gas and toxic and harmful gas have very high sensitivity.Ethyl alcohol is made
It is a kind of volatile inflammable colourless transparent liquid for the main component of wine.In recent years, drunk driving has become threat public transport
The principal element of safety, great hidden danger is brought to personal safety.Therefore, particularly important is become to the strict inspection of drunk driving, it is right
Cause the extensive concern of researcher with the research of excellent alcohol sensible performance materials.Such as Wang et al. using hydro-thermal method and
Simple infusion path prepares the 3D SnO of Pt doping2Nano flower gas sensitive shows alcohol at being 100 DEG C in operating temperature
Go out excellent air-sensitive performance (L.W.Wang, et al.A novel low temperature gas sensor based on
Pt-decoratedhierarchical 3D SnO2nanocomposites,Sens.Actuator B-Chem.232(2016)
91-101)；Chen et al. synthesizes the SnO of a diameter of 3nm using hydro-thermal method2Nanometer rods are used for the detection of alcohol gas, work as exposure
When 300ppm alcohol gas, the high sensitivity of sensor is up to 83.8, and the material is to the response and gas of alcohol gas
Concentration (Y.J.Chen, et al.Linear ethanol sensing of SnO in a linear relationship2nanorods with
extremely high sensitivity,Appl.Phys.Lett.88(2006)083105).These prepare alcohol sensor
Method it is mostly complicated and be not easy to realize in large-scale industrial production material morphology is accurately controlled, and electrotinning is given birth to
The reasonable recycle of by-product tin mud in production is rarely reported so far in the preparation of alcohol gas sensor.
Invention content
The present invention uses following scheme to solve above-mentioned technical problem,
A method of alcohol gas-sensitive material is prepared based on tin mud modification, is included the following steps：
A. tin mud is dissolved in diluted acid, carries out acidification, washing to neutrality, centrifugation is placed in baking oven dry；
B. it by the obtained solid high-energy ball millings of step a at uniform powder, is dissolved in solvent A under magnetic agitation, it is described
Solvent A is the mixed liquor of deionized water and absolute ethyl alcohol；CTAB conducts are added into solution at being 40 DEG C -70 DEG C in bath temperature
Then protective agent is 0.5%-3% according to the ratio between amount of substance of noble metal and powder；Precious metal solution and vitamin C is added
Solution is in above-mentioned mixed solution, the reaction was continued 0.5h-2h；
C. the product after being reacted in step b is washed to neutrality and is placed on drying in baking oven；
D. obtained product in step c is ground into uniform powder, then carries out 300~600 DEG C of heat treatment 1-4h,
Alcohol gas-sensitive material is made.
It is further preferred that the sintering temperature in above-mentioned steps d is 450 DEG C~600 DEG C, time 2h.
Further, precious metal solution described in above-mentioned steps b is platinum acid chloride solution or chlorine palladium acid solution.
It is further preferred that precious metal solution described in above-mentioned steps b is platinum acid chloride solution, the amount of the substance of platinum and powder
The ratio between be 1%-2%.
Further, in above-mentioned steps a diluted acid be a concentration of 1M~4M hydrochloric acid.
Further, in above-mentioned steps b vitamin C and noble metal molar ratio 1.5:1.
Further, acidification is to carry out magnetic agitation at 30 DEG C -60 DEG C of bath temperature in above-mentioned steps a.
Further, solvent A described in above-mentioned steps b is deionized water and absolute ethyl alcohol by volume 1:1 mixed liquor.
Further, it is to pass through deionized water and anhydrous second to be washed to neutral concrete operations in above-mentioned steps a and step c
Alcohol is alternately washed till neutrality.Preferably, specially alternately washing and alcohol three times are washed three times.
Further, drying temperature is 60~80 DEG C in above-mentioned steps a and step c.
The application of alcohol gas-sensitive material made from above method, specially：
Obtained alcohol gas-sensitive material is ground into uniformed powder, solvent is then added, powder is made after slurry and continue to grind
Mill, slurry coating is in the Al with gold electrode2O3Ceramic tube outer surface；Muffle furnace is gone to after its natural air drying 300~500
DEG C heat treatment 0.5-2h, cools to the furnace after room temperature Ni-Cr heater strips passing through ceramic tube, by heater strip and Al2O3Ceramic tube
Four leads are welded on pedestal, are placed on agingtable and are carried out burin-in process, and alcohol gas sensor is made.
Further, the solvent described in is the mixed liquor of deionized water and absolute ethyl alcohol.
Beneficial effects of the present invention are：
(1) the by-product tin mud in electrotinning production passes through the acidification of diluted acid as important tin secondary resource, washes
It washs after the modes such as dry and oxidizing roasting handle, alcohol gas sensor is made as basis material to detect alcohol gas,
Air-sensitive performance is excellent, has good response to ethyl alcohol；
(2) since noble metal nano particles have extremely strong catalytic activity, promote oxygen molecule and the ethyl alcohol of reproducibility point
Son is adsorbed on material surface.The response and response regeneration rate improved to alcohol gas is modified by precious metal doping；
(3) by the recycling to tin secondary resource-tin mud and applied to gas sensitive material field, tin money is not only reduced
The waste in source reduces economic cost, mitigates the problems such as environmental pollution, while providing new application side for reluctant tin mud
To providing new Research Thinking for gas sensitive field.With multiple benefits such as resource, economy, environmental protection.
Description of the drawings
Fig. 1 is the SEM figures of tin mud after acidified activation process in the embodiment of the present invention 1；
Fig. 2 is the 1%Pt-SnO after doping vario-property in the embodiment of the present invention 12It is right at 200 DEG C of operating temperature
The response recovery curve figure of 100ppm alcohol gas.
Specific embodiment
Embodiment 1:
The tin mud that molten tin bath bottom is accumulated in taking 5g electrotinnings to produce is dissolved in the hydrochloric acid of 30ml2M, is 50 DEG C in bath temperature
Lower magnetic agitation 60min carries out acidification, is then filtered to liquid, to filter residue alternately washing and three times alcohol three times
It washes, by dry 12h in the product placement baking oven after washing 60 DEG C.By the sample high energy milling after drying at uniform powder,
It is dissolved in 40mlV under magnetic agitationWater:VAbsolute ethyl alcohol=1:In 1 mixed liquor, 0.5g is added into above-mentioned solution under 50 DEG C of bath temperatures
Then CTAB adds according to the ratio between the amount of the substance of the solute of precious metal solution and the amount of substance of powder for 1% as protective agent
Enter platinum acid chloride solution and 0.15g vitamin Cs in above-mentioned solution, magnetic agitation 1h.
Product after above-mentioned reaction is alternately washed to wash to go to alcohol three times three times and dries 12h in baking oven at 60 DEG C, is set
Sample is ground into uniform powder in mortar, is then sintered 2h at 550 DEG C in Muffle furnace, is waited for after completion of the reaction with furnace cooling
But to room temperature.The electron microscope of sample is as shown in Figure 1.
Sample made from 0.5g is weighed to be placed in agate mortar after grinding 10min by VWater:VAbsolute ethyl alcohol=1:1 sample is made
Slurry continues to grind 20min, and slurry coating is in the Al with gold electrode2O3Ceramic tube outer surface；Horse is gone to after its natural air drying
Not be heat-treated 1h at 400 DEG C in stove, cool to the furnace after room temperature and Ni-Cr heater strips are passed through into ceramic tube, then by heater strip and
Al2O3Four leads of ceramic tube are welded on pedestal, are placed on agingtable and are carried out burin-in process, are placed on agingtable at aging
It manages 7 days in case detection.
Gas sensor after aging carries out air-sensitive performance test to 100ppm alcohol gas, and the results are shown in Figure 2 shows
When operating temperature is 260 DEG C, the gas sensitive to the high sensitivity of 100ppm alcohol gas up to 45.8, when response time/recovery
Between be respectively less than 5s.
This research is deposited in plating trench bottom trade waste tin mud in being produced with electrotinning is acidified, washing is dry,
Precious metal doping and subsequent heat treatment process have obtained alcohol gas-sensitive material, have the sensitivity of superelevation to alcohol gas, ring
It answers and resume speed is fast, can achieve the purpose that monitor in real time, correlative study method is rarely reported.Realize having for tin secondary resource
While effect rationally utilizes, it is reduced to the pollution of environment and is applied to gas sensitive field.
Embodiment 2：
The tin mud that molten tin bath bottom is accumulated in taking 5g electrotinnings to produce is dissolved in the hydrochloric acid of 30ml1M, is 30 DEG C in bath temperature
Lower magnetic agitation 60min carries out acidification, is then filtered to liquid, to filter residue alternately washing and three times alcohol three times
It washes, by dry 12h in the product placement baking oven after washing 60 DEG C.By the sample high energy milling after drying at uniform powder,
It is dissolved in 40mlV under magnetic agitationWater:VAbsolute ethyl alcohol=1:In 1 mixed liquor, 0.5g is added into above-mentioned solution under 40 DEG C of bath temperatures
CTAB is then 0.5% according to the ratio between the amount of the substance of the solute of precious metal solution and the amount of substance of powder as protective agent
Chlorine palladium acid solution and 0.1g vitamin Cs is added in above-mentioned solution, magnetic agitation 1h.
Product after above-mentioned reaction is alternately washed to wash to go to alcohol three times three times and dries 12h in baking oven at 60 DEG C, is set
Sample is ground into uniform powder in mortar, is then sintered 1h at 300 DEG C in Muffle furnace, is waited for after completion of the reaction with furnace cooling
But to room temperature.
Sample made from 0.5g is weighed to be placed in agate mortar after grinding 10min by VWater:VAbsolute ethyl alcohol=1:1 sample is made
Slurry continues to grind 20min, and slurry coating is in the Al with gold electrode2O3Ceramic tube outer surface；Horse is gone to after its natural air drying
Not be heat-treated 1h at 300 DEG C in stove, cool to the furnace after room temperature and Ni-Cr heater strips are passed through into ceramic tube, then by heater strip and
Al2O3Four leads of ceramic tube are welded on pedestal, are placed on agingtable and are carried out burin-in process, are placed on agingtable at aging
It manages 7 days in case detection.
Embodiment 3：
The tin mud that molten tin bath bottom is accumulated in taking 5g electrotinnings to produce is dissolved in the hydrochloric acid of 30ml 2M, is 50 in bath temperature
At DEG C magnetic agitation 60min carry out acidification, then liquid is filtered, to filter residue alternately three times washing and three times
Alcohol is washed, by dry 12h in the product placement baking oven after washing 60 DEG C.By the sample high energy milling after drying at uniform powder
Body is dissolved in 40mlV under magnetic agitationWater:VAbsolute ethyl alcohol=1:In 1 mixed liquor, it is added into above-mentioned solution under 50 DEG C of bath temperatures
Then 0.5g CTAB are according to the amount of the substance of the solute of precious metal solution and the ratio between the amount of substance of powder as protective agent
1% is added platinum acid chloride solution and 0.15g vitamin Cs in above-mentioned solution, magnetic agitation 1h.
Product after above-mentioned reaction is alternately washed to wash to go to alcohol three times three times and dries 12h in baking oven at 60 DEG C, is set
Sample is ground into uniform powder in mortar, is then sintered 2h at 550 DEG C in Muffle furnace, is waited for after completion of the reaction with furnace cooling
But to room temperature.Sample made from 0.5g is weighed to be placed in agate mortar after grinding 10min by VWater:VAbsolute ethyl alcohol=1:1 sample is made
Slurry continues to grind 20min, and slurry coating is in the Al with gold electrode2O3Ceramic tube outer surface；Horse is gone to after its natural air drying
Not be heat-treated 1h at 400 DEG C in stove, cool to the furnace after room temperature and Ni-Cr heater strips are passed through into ceramic tube, then by heater strip and
Al2O3Four leads of ceramic tube are welded on pedestal, are placed on agingtable and are carried out burin-in process, are placed on agingtable at aging
It manages 7 days in case detection.
Embodiment 4：
The tin mud that molten tin bath bottom is accumulated in taking 5g electrotinnings to produce is dissolved in the hydrochloric acid of 30ml4M, is 60 DEG C in bath temperature
Lower magnetic agitation 60min carries out acidification, is then filtered to liquid, to filter residue alternately washing and three times alcohol three times
It washes, by dry 12h in the product placement baking oven after washing 60 DEG C.By the sample high energy milling after drying at uniform powder,
It is dissolved in 40mlV under magnetic agitationWater:VAbsolute ethyl alcohol=1:In 1 mixed liquor, 0.5g is added into above-mentioned solution under 70 DEG C of bath temperatures
Then CTAB adds according to the ratio between the amount of the substance of the solute of precious metal solution and the amount of substance of powder for 3% as protective agent
Enter chlorine palladium acid solution and 0.3g vitamin Cs in above-mentioned solution, magnetic agitation 2h.
Product after above-mentioned reaction is alternately washed to wash to go to alcohol three times three times and dries 12h in baking oven at 60 DEG C, is set
Sample is ground into uniform powder in mortar, is then sintered 4h at 600 DEG C in Muffle furnace, is waited for after completion of the reaction with furnace cooling
But to room temperature.Sample made from 0.5g is weighed to be placed in agate mortar after grinding 10min by VWater:VAbsolute ethyl alcohol=1:1 sample is made
Slurry continues to grind 20min, and slurry coating is in the Al with gold electrode2O3Ceramic tube outer surface；Horse is gone to after its natural air drying
Not be heat-treated 2h at 500 DEG C in stove, cool to the furnace after room temperature and Ni-Cr heater strips are passed through into ceramic tube, then by heater strip and
Al2O3Four leads of ceramic tube are welded on pedestal, are placed on agingtable and are carried out burin-in process, are placed on agingtable at aging
It manages 7 days in case detection.
Embodiment 5：
The tin mud that molten tin bath bottom is accumulated in taking 5g electrotinnings to produce is dissolved in the hydrochloric acid of 30ml3M, is 50 DEG C in bath temperature
Lower magnetic agitation 60min carries out acidification, is then filtered to liquid, to filter residue alternately washing and three times alcohol three times
It washes, by dry 12h in the product placement baking oven after washing 70 DEG C.By the sample high energy milling after drying at uniform powder,
It is dissolved in 40mlV under magnetic agitationWater:VAbsolute ethyl alcohol=1:In 1 mixed liquor, 0.5g is added into above-mentioned solution under 60 DEG C of bath temperatures
Then CTAB adds according to the ratio between the amount of the substance of the solute of precious metal solution and the amount of substance of powder for 2% as protective agent
Enter platinum acid chloride solution and 0.2g vitamin Cs in above-mentioned solution, magnetic agitation 1.5h.
Product after above-mentioned reaction is alternately washed to wash to go to alcohol three times three times and dries 12h in baking oven at 60 DEG C, is set
Sample is ground into uniform powder in mortar, is then sintered 2h at 500 DEG C in Muffle furnace, is waited for after completion of the reaction with furnace cooling
But to room temperature.
Sample made from 0.5g is weighed to be placed in agate mortar after grinding 10min by VWater:VAbsolute ethyl alcohol=1:1 sample is made
Slurry continues to grind 20min, and slurry coating is in the Al with gold electrode2O3Ceramic tube outer surface；Horse is gone to after its natural air drying
It not is heat-treated 1.5h at 450 DEG C in stove, cools to the furnace after room temperature and Ni-Cr heater strips is passed through into ceramic tube, then by heater strip
And Al2O3Four leads of ceramic tube are welded on pedestal, are placed on agingtable and are carried out burin-in process, are placed in aging on agingtable
It handles 7 days in case detection.
Embodiment 6：
The tin mud that molten tin bath bottom is accumulated in taking 5g electrotinnings to produce is dissolved in the hydrochloric acid of 30ml 2M, is 60 in bath temperature
At DEG C magnetic agitation 60min carry out acidification, then liquid is filtered, to filter residue alternately three times washing and three times
Alcohol is washed, by dry 12h in the product placement baking oven after washing 80 DEG C.By the sample high energy milling after drying at uniform powder
Body is dissolved in 40mlV under magnetic agitationWater:VAbsolute ethyl alcohol=1:In 1 mixed liquor, it is added into above-mentioned solution under 70 DEG C of bath temperatures
Then 0.5g CTAB are according to the amount of the substance of the solute of precious metal solution and the ratio between the amount of substance of powder as protective agent
3% is added platinum acid chloride solution and 0.3g vitamin Cs in above-mentioned solution, magnetic agitation 2h.
Product after above-mentioned reaction is alternately washed to wash to go to alcohol three times three times and dries 12h in baking oven at 60 DEG C, is set
Sample is ground into uniform powder in mortar, is then sintered 3h at 450 DEG C in Muffle furnace, is waited for after completion of the reaction with furnace cooling
But to room temperature.
Sample made from 0.5g is weighed to be placed in agate mortar after grinding 10min by VWater:VAbsolute ethyl alcohol=1:1 sample is made
Slurry continues to grind 20min, and slurry coating is in the Al with gold electrode2O3Ceramic tube outer surface；Horse is gone to after its natural air drying
Not be heat-treated 2h at 500 DEG C in stove, cool to the furnace after room temperature and Ni-Cr heater strips are passed through into ceramic tube, then by heater strip and
Al2O3Four leads of ceramic tube are welded on pedestal, are placed on agingtable and are carried out burin-in process, are placed on agingtable at aging
It manages 7 days in case detection.
Claims (10)
1. a kind of method preparing alcohol gas-sensitive material based on tin mud modification, which is characterized in that include the following steps：
A. tin mud is dissolved in diluted acid, carries out acidification, washing to neutrality, centrifugation is placed in baking oven dry；
B. it by the obtained solid high-energy ball millings of step a at uniform powder, is dissolved in solvent A under magnetic agitation, the solvent A
For the mixed liquor of deionized water and absolute ethyl alcohol；CTAB is added as protection into solution at being 40 DEG C -70 DEG C in bath temperature
Then agent is 0.5%-3% according to the ratio between amount of substance of noble metal and powder；Precious metal solution and vitamin c solution is added
In above-mentioned mixed solution, the reaction was continued 0.5h-2h；
C. the product after being reacted in step b is washed to neutrality and is placed on drying in baking oven；
D. obtained product in step c is ground into uniform powder, then carries out 300~600 DEG C of heat treatment 1-4h, is made
Alcohol gas-sensitive material.
2. the method according to claim 1 for preparing alcohol gas-sensitive material based on tin mud modification, which is characterized in that step d
In heat treatment temperature be 450 DEG C~600 DEG C, time 2h.
3. the method according to claim 1 or 2 for preparing alcohol gas-sensitive material based on tin mud modification, which is characterized in that step
Precious metal solution described in rapid b is platinum acid chloride solution or chlorine palladium acid solution.
4. the method according to claim 3 for preparing alcohol gas-sensitive material based on tin mud modification, which is characterized in that step b
Described in precious metal solution be platinum acid chloride solution, the ratio between amount of substance of platinum and powder is 1%-2%.
5. the method for preparing alcohol gas-sensitive material based on tin mud modification according to claim 1 or 2 or 4, which is characterized in that
Diluted acid is the hydrochloric acid of a concentration of 1M~4M in step a.
6. the method according to claim 3 for preparing alcohol gas-sensitive material based on tin mud modification, which is characterized in that step a
Middle diluted acid is the hydrochloric acid of a concentration of 1M~4M.
7. the method for preparing alcohol gas-sensitive material based on tin mud modification according to claims 1 or 2 or 4 or 6, feature exist
In the molar ratio 1.5 of vitamin C and noble metal in step b:1.
8. the method for preparing alcohol gas-sensitive material based on tin mud modification according to claims 1 or 2 or 4 or 6, feature exist
In acidification is to carry out magnetic agitation at 30 DEG C -60 DEG C of bath temperature in step a.
9. the method for preparing alcohol gas-sensitive material based on tin mud modification according to claims 1 or 2 or 4 or 6, feature exist
In, solvent A described in step b be deionized water and absolute ethyl alcohol by volume 1:1 mixed liquor.
10. the application of alcohol gas-sensitive material made from claim 1-9 either method, it is characterised in that：
Obtained alcohol gas-sensitive material is ground into uniformed powder, solvent is then added, powder is made after slurry and continue to grind,
The solvent is the mixed liquor of deionized water and absolute ethyl alcohol；Slurry coating is in the Al with gold electrode2O3Ceramic tube outer surface；
Muffle furnace is gone to after its natural air drying and is heat-treated 0.5-2h at 300~500 DEG C, heats Ni-Cr after cooling to room temperature with the furnace
Silk passes through ceramic tube, by heater strip and Al2O3Four leads of ceramic tube are welded on pedestal, are placed on agingtable and are carried out aging
Alcohol gas sensor is made in processing.
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| CN111017988A (en) * | 2019-12-31 | 2020-04-17 | 深圳爱多科传感技术有限公司 | Formaldehyde gas-sensitive material based on recovery treatment of tin mud and preparation method thereof |
| CN112142098A (en) * | 2019-06-28 | 2020-12-29 | 东北大学 | Ag coated SnO2Preparation of SO2Method for sensing material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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