CN108802117B - Method for preparing alcohol gas-sensitive material based on tin mud modification and application - Google Patents
Method for preparing alcohol gas-sensitive material based on tin mud modification and application Download PDFInfo
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Abstract
The invention belongs to the fields of comprehensive recycling of tin secondary resources, namely byproduct tin mud in electrotinning production, gas sensing materials and environmental protection, and relates to a method for preparing an alcohol gas-sensitive material based on tin mud modification and application. The alcohol sensitive material is prepared from industrial waste tin mud accumulated at the bottom of a plating tank in electrotinning production through acidification, washing and drying, noble metal doping and subsequent heat treatment. The prepared gas sensor has high sensitivity to ethanol, high response recovery rate and other excellent gas-sensitive properties. The method is applied to the field of gas sensitive materials while reducing tin resource waste, economic cost and environmental pollution, and is an environment-friendly sustainable development research method.
Description
Technical Field
The invention belongs to the fields of comprehensive recycling of tin secondary resources, gas-sensitive sensing materials and environment-friendly development, and particularly relates to modification treatment of tin mud which is a byproduct in electrotinning production and application of the tin mud to preparation of an alcohol gas-sensitive sensor.
Background
The tin belongs to rare and precious metals, the supply demand of the tin metal industry in China is large, the total market demand is continuously increased, and the tin resource is not greatly increased in a short period, so that the secondary tin resource is reasonably and efficiently utilized, the problems of tin resource shortage and waste can be effectively solved, the economic development is greatly promoted, and the environmental protection is facilitated. The tin mud is used as an important high-yield tin secondary resource, is waste generated at the bottom of a plating tank in the production of electrolytic tinning, can promote a tinning plate to generate surface defects, increases the consumption of a tin anode, and aggravates the environmental deterioration by removing treatment, if the tin mud cannot be reasonably and effectively utilized, the tin mud is seriously wasted, and the economic cost is increased. On the basis of environmental protection, the effective recycling of tin resources is improved, and the tin resources are developed and applied to other research fields, so that the method is worthy of research and attention.
The main component of the tin mud is tin dioxide (SnO)2) As an important semiconductor metal oxide, it has been widely used in the field of gas sensors due to its advantages of good chemical stability, excellent performance, low cost, etc. The gas sensor made of tin dioxide has high sensitivity to various combustible gases, environmental pollution gases and toxic and harmful gases. The ethanol is used as main component of wine, and is a volatile, inflammable, colorless and transparent liquid. In recent years, drunk driving has become a main factor threatening public transportation safety, and great hidden danger is brought to personal safety. Therefore, strict detection of drunk driving becomes more important, and research on materials with excellent ethanol sensitivity has attracted extensive attention of researchers. For example, Wang et al prepared Pt-doped 3D SnO by hydrothermal method and simple impregnation route2The nano flower gas-sensitive material shows excellent gas-sensitive performance to alcohol (L.W.Wang, et al.A novel low temperature sensor based on Pt-porous 3D SnO)2nanocomposites, sens. acutator B-chem.232(2016) 91-101); synthesis of SnO having a diameter of 3nm by Chen et al by hydrothermal method2The nano-rod is used for detecting alcohol gas, when the nano-rod is exposed to 300ppm of alcohol gas, the sensitivity of the sensor is as high as 83.8, and the response value of the material to the alcohol gas is in a linear relation with the gas concentration (Y.J.Chen, et al.Linear ethanol sensing of SnO)2nanorods with the xtensile high sensitivity, appl. phys. lett.88(2006) 083105). Most of the methods for preparing the alcohol sensor are complicated and are difficult to realize the precise control of the material morphology in large-scale industrial production, and the reasonable recycling of the byproduct tin mud in the electrotinning production and the application of the byproduct tin mud in the preparation of the alcohol gas sensor are reported so far.
Disclosure of Invention
The invention adopts the following scheme to solve the technical problems,
a method for preparing an alcohol gas-sensitive material based on tin mud modification comprises the following steps:
a. dissolving the tin mud in dilute acid, carrying out acidification treatment, washing to be neutral, centrifugally separating, and then placing in an oven for drying;
b. b, performing high-energy ball milling on the solid obtained in the step a to obtain uniform powder, and dissolving the powder in a solvent A under magnetic stirring, wherein the solvent A is a mixed solution of deionized water and absolute ethyl alcohol; CTAB is added into the solution as a protective agent at the water bath temperature of 40-70 ℃, and then the mass ratio of the noble metal to the powder is 0.5-3%; adding noble metal solution and vitamin C solution into the mixed solution, and continuously reacting for 0.5-2 h;
c. c, washing the product reacted in the step b to be neutral, and then placing the product in an oven for drying;
d. and c, grinding the product obtained in the step c into uniform powder, and then carrying out heat treatment at 300-600 ℃ for 1-4h to obtain the alcohol gas-sensitive material.
Further preferably, the sintering temperature in the step d is 450-600 ℃ and the time is 2 h.
Further, in the step b, the noble metal solution is chloroplatinic acid solution or chloropalladic acid solution.
Further preferably, in the step b, the precious metal solution is a chloroplatinic acid solution, and the ratio of the platinum to the powder is 1% -2%.
Further, the diluted acid in the step a is hydrochloric acid with the concentration of 1M-4M.
Further, the molar ratio of the vitamin C to the noble metal in the step b is 1.5: 1.
Further, the acidification treatment in the step a is to carry out magnetic stirring at the water bath temperature of 30-60 ℃.
Further, the solvent A in the step b is a mixed solution of deionized water and absolute ethyl alcohol according to a volume ratio of 1: 1.
Further, the washing to neutrality in the above steps a and c is specifically performed by alternately washing to neutrality with deionized water and absolute ethyl alcohol. Preferably, three water washes and three alcohol washes are performed alternately.
Further, the drying temperature in the step a and the step c is 60-80 ℃.
The application of the alcohol gas-sensitive material prepared by the method comprises the following specific steps:
grinding the obtained alcohol gas-sensitive material into uniform powder, adding a solvent to prepare slurry, continuously grinding, and coating the slurry on Al with a gold electrode2O3An outer surface of the ceramic tube; transferring the dried powder to a muffle furnace for heat treatment at 300-500 ℃ for 0.5-2h after the dried powder is naturally air-dried, cooling the powder to room temperature along with the furnace, penetrating a Ni-Cr heating wire through a ceramic tube, and passing the heating wire and Al2O3And welding four lead wires of the ceramic tube on the base, and placing the ceramic tube on an aging table for aging treatment to obtain the alcohol gas sensor.
Further, in the application, the solvent is a mixed solution of deionized water and absolute ethyl alcohol.
The invention has the beneficial effects that:
(1) the byproduct tin mud in electrotinning production is taken as an important tin secondary resource, is treated by the modes of acidification treatment of dilute acid, washing, drying, oxidizing roasting and the like, and is taken as a base material to prepare an alcohol gas sensor for detecting alcohol gas, so that the gas-sensitive property of the alcohol gas sensor is excellent, and the alcohol gas sensor has good response to alcohol;
(2) because the noble metal nano particles have extremely strong catalytic activity, oxygen molecules and reductive ethanol molecules are promoted to be adsorbed on the surface of the material. The response value and the response recovery rate to the ethanol gas are improved through doping modification of the noble metal;
(3) by recycling the tin secondary resource, namely tin mud, and applying the tin secondary resource to the field of gas sensitive materials, the problems of tin resource waste, economic cost reduction, environmental pollution reduction and the like are solved, a new application direction is provided for the tin mud which is difficult to treat, and a new research idea is provided for the field of gas sensitive materials. Has multiple benefits of resource, economy, environmental protection and the like.
Drawings
FIG. 1 is an SEM image of tin sludge after being subjected to acid activation treatment in example 1 of the present invention;
FIG. 2 shows the doping-modified 1% Pt-SnO in example 1 of the present invention2In the workerA graph showing the recovery of the response to 100ppm of ethanol gas at a temperature of 200 ℃ was prepared.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1:
dissolving 5g of tin mud accumulated at the bottom of a tin bath in electrolytic tinning production in 30ml of 2M hydrochloric acid, carrying out magnetic stirring for 60min at the water bath temperature of 50 ℃ for acidification treatment, then carrying out suction filtration on the liquid, alternately carrying out three times of water washing and three times of alcohol washing on filter residues, and drying the washed product in an oven at the temperature of 60 ℃ for 12 hours. Grinding the dried sample into uniform powder with high energy, and dissolving in 40mlV under magnetic stirringWater (W):VAnhydrous ethanolTo the mixed solution 1:1, 0.5g of CTAB as a protective agent was added to the solution at a water bath temperature of 50 ℃, and then a chloroplatinic acid solution and 0.15g of vitamin C were added to the solution at a ratio of 1% of the amount of the solute in the noble metal solution to the amount of the powder, and the mixture was magnetically stirred for 1 hour.
And alternately carrying out three times of water washing and three times of alcohol washing on the reaction product, transferring the reaction product into an oven, drying the reaction product for 12 hours at the temperature of 60 ℃, putting the reaction product into a mortar, grinding the sample into uniform powder, sintering the powder in a muffle furnace at the temperature of 550 ℃ for 2 hours, and cooling the powder to the room temperature along with the furnace after the reaction is finished. An electron micrograph of the sample is shown in FIG. 1.
0.5g of the prepared sample is weighed and put in an agate mortar for grinding for 10min and then is ground according to VWater (W):VAnhydrous ethanolThe sample was slurried for 20min at 1:1 and the slurry was applied to Al with gold electrodes2O3An outer surface of the ceramic tube; transferring to a muffle furnace for heat treatment at 400 ℃ for 1h after natural air drying, cooling to room temperature along with the furnace, penetrating a Ni-Cr heating wire through a ceramic tube, and then, passing the heating wire and Al2O3Four lead wires of the ceramic tube are welded on the base, placed on an aging table for aging treatment, and placed on the aging table for aging treatment for 7 days for detection.
The gas-sensitive performance of the aged gas-sensitive element on 100ppm ethanol gas is tested, and the result is shown in fig. 2, which shows that when the working temperature is 260 ℃, the sensitivity of the gas-sensitive material on 100ppm ethanol gas is as high as 45.8, and the response time/recovery time is less than 5 s.
According to the research, the alcohol gas-sensitive material is obtained by carrying out acidification, washing and drying, noble metal doping and subsequent heat treatment on industrial waste tin mud accumulated at the bottom of a plating tank in electrotinning production, the alcohol gas-sensitive material has ultrahigh sensitivity to ethanol gas, is high in response and recovery speed, can achieve the purpose of real-time monitoring, and relevant research methods are reported. The method realizes effective and reasonable utilization of the secondary tin resource, reduces the pollution of the secondary tin resource to the environment and is applied to the field of gas sensitive materials.
Example 2:
dissolving 5g of tin mud accumulated at the bottom of a tin bath in electrolytic tinning production in 30ml of 1M hydrochloric acid, carrying out magnetic stirring for 60min at the water bath temperature of 30 ℃ for acidification treatment, then carrying out suction filtration on the liquid, alternately carrying out three times of water washing and three times of alcohol washing on filter residues, and drying the washed product in an oven at the temperature of 60 ℃ for 12 h. Grinding the dried sample into uniform powder with high energy, and dissolving in 40mlV under magnetic stirringWater (W):VAnhydrous ethanolTo the mixed solution 1:1, 0.5g of CTAB as a protective agent was added to the solution at a water bath temperature of 40 ℃, and then a chloropalladate solution and 0.1g of vitamin C were added to the solution in such an amount that the ratio of the amount of the solute in the noble metal solution to the amount of the powder was 0.5%, followed by magnetic stirring for 1 hour.
And alternately carrying out three times of water washing and three times of alcohol washing on the reaction product, transferring the reaction product into an oven, drying for 12 hours at the temperature of 60 ℃, placing the reaction product into a mortar, grinding the sample into uniform powder, sintering the powder in a muffle furnace at the temperature of 300 ℃ for 1 hour, and cooling the powder to the room temperature along with the furnace after the reaction is finished.
0.5g of the prepared sample is weighed and put in an agate mortar for grinding for 10min and then is ground according to VWater (W):VAnhydrous ethanolThe sample was slurried for 20min at 1:1 and the slurry was applied to Al with gold electrodes2O3An outer surface of the ceramic tube; transferring to a muffle furnace for heat treatment at 300 ℃ for 1h after natural air drying, cooling to room temperature along with the furnace, penetrating a Ni-Cr heating wire through a ceramic tube, and then, passing the heating wire and Al2O3Four lead wires of the ceramic tube are welded on the base, placed on an aging table for aging treatment, and placed on the aging table for aging treatment for 7 days for detection.
Example 3:
dissolving 5g of tin mud accumulated at the bottom of a tin bath in 30ml of 2M hydrochloric acid in electrotinning production, carrying out magnetic stirring for 60min at the water bath temperature of 50 ℃ for acidification treatment, then carrying out suction filtration on the liquid, alternately carrying out three times of water washing and three times of alcohol washing on filter residues, and drying the washed product in an oven at the temperature of 60 ℃ for 12 h. Grinding the dried sample into uniform powder with high energy, and dissolving in 40mlV under magnetic stirringWater (W):VAnhydrous ethanolTo the mixed solution 1:1, 0.5g of CTAB as a protective agent was added to the solution at a water bath temperature of 50 ℃, and then a chloroplatinic acid solution and 0.15g of vitamin C were added to the solution at a ratio of 1% of the amount of the solute in the noble metal solution to the amount of the powder, and the mixture was magnetically stirred for 1 hour.
And alternately carrying out three times of water washing and three times of alcohol washing on the reaction product, transferring the reaction product into an oven, drying the reaction product for 12 hours at the temperature of 60 ℃, putting the reaction product into a mortar, grinding the sample into uniform powder, sintering the powder in a muffle furnace at the temperature of 550 ℃ for 2 hours, and cooling the powder to the room temperature along with the furnace after the reaction is finished. 0.5g of the prepared sample is weighed and put in an agate mortar for grinding for 10min and then is ground according to VWater (W):VAnhydrous ethanolThe sample was slurried for 20min at 1:1 and the slurry was applied to Al with gold electrodes2O3An outer surface of the ceramic tube; transferring to a muffle furnace for heat treatment at 400 ℃ for 1h after natural air drying, cooling to room temperature along with the furnace, penetrating a Ni-Cr heating wire through a ceramic tube, and then, passing the heating wire and Al2O3Four lead wires of the ceramic tube are welded on the base, placed on an aging table for aging treatment, and placed on the aging table for aging treatment for 7 days for detection.
Example 4:
dissolving 5g of tin mud accumulated at the bottom of a tin bath in 30ml of 4M hydrochloric acid, carrying out magnetic stirring for 60min at the water bath temperature of 60 ℃ for acidification treatment, carrying out suction filtration on liquid, alternately carrying out three times of water washing and three times of alcohol washing on filter residues, and drying the washed product in an oven at the temperature of 60 ℃ for 12 h. Grinding the dried sample into uniform powder with high energy, and dissolving in 40mlV under magnetic stirringWater (W):VAnhydrous ethanolAdding 0.5g CTAB as a protective agent into the mixed solution at 70 ℃ in a water bath, and addingAdding chloropalladate solution and 0.3g of vitamin C into the noble metal solution according to the ratio of the amount of solute to the amount of powder of the noble metal solution being 3%, and magnetically stirring for 2 h.
And alternately carrying out three times of water washing and three times of alcohol washing on the reaction product, transferring the reaction product into an oven, drying for 12 hours at the temperature of 60 ℃, placing the reaction product into a mortar, grinding the sample into uniform powder, sintering for 4 hours in a muffle furnace at the temperature of 600 ℃, and cooling to room temperature along with the furnace after the reaction is finished. 0.5g of the prepared sample is weighed and put in an agate mortar for grinding for 10min and then is ground according to VWater (W):VAnhydrous ethanolThe sample was slurried for 20min at 1:1 and the slurry was applied to Al with gold electrodes2O3An outer surface of the ceramic tube; transferring to a muffle furnace for heat treatment at 500 ℃ for 2h after natural air drying, cooling to room temperature along with the furnace, penetrating a Ni-Cr heating wire through a ceramic tube, and then, passing the heating wire and Al2O3Four lead wires of the ceramic tube are welded on the base, placed on an aging table for aging treatment, and placed on the aging table for aging treatment for 7 days for detection.
Example 5:
dissolving 5g of tin mud accumulated at the bottom of a tin bath in 30ml of 3M hydrochloric acid in electrolytic tinning production, carrying out magnetic stirring for 60min at the water bath temperature of 50 ℃ to carry out acidification treatment, then carrying out suction filtration on liquid, alternately carrying out three times of water washing and three times of alcohol washing on filter residues, and drying the washed product in an oven at 70 ℃ for 12 h. Grinding the dried sample into uniform powder with high energy, and dissolving in 40mlV under magnetic stirringWater (W):VAnhydrous ethanolTo the mixed solution 1:1, 0.5g of CTAB as a protective agent was added to the solution at a water bath temperature of 60 ℃, and then a chloroplatinic acid solution and 0.2g of vitamin C were added to the solution at a ratio of 2% of the amount of the solute in the noble metal solution to the amount of the powder, and the mixture was magnetically stirred for 1.5 hours.
And alternately carrying out three times of water washing and three times of alcohol washing on the reaction product, transferring the reaction product into an oven, drying for 12 hours at the temperature of 60 ℃, placing the reaction product into a mortar, grinding the sample into uniform powder, sintering for 2 hours in a muffle furnace at the temperature of 500 ℃, and cooling to room temperature along with the furnace after the reaction is finished.
0.5g of the prepared sample was weighed and ground in an agate mortar 10After min, press VWater (W):VAnhydrous ethanolThe sample was slurried for 20min at 1:1 and the slurry was applied to Al with gold electrodes2O3An outer surface of the ceramic tube; transferring to a muffle furnace for heat treatment at 450 ℃ for 1.5h after the alloy is naturally air-dried, cooling to room temperature along with the furnace, passing a Ni-Cr heating wire through a ceramic tube, and then passing the heating wire and Al2O3Four lead wires of the ceramic tube are welded on the base, placed on an aging table for aging treatment, and placed on the aging table for aging treatment for 7 days for detection.
Example 6:
dissolving 5g of tin mud accumulated at the bottom of a tin bath in 30ml of 2M hydrochloric acid, carrying out magnetic stirring for 60min at the water bath temperature of 60 ℃ for carrying out acidification treatment, then carrying out suction filtration on the liquid, alternately carrying out three times of water washing and three times of alcohol washing on filter residues, and drying the washed product in an oven at the temperature of 80 ℃ for 12 h. Grinding the dried sample into uniform powder with high energy, and dissolving in 40mlV under magnetic stirringWater (W):VAnhydrous ethanolTo the mixed solution 1:1, 0.5g of CTAB as a protective agent was added to the solution at a water bath temperature of 70 ℃, and then a chloroplatinic acid solution and 0.3g of vitamin C were added to the solution in such an amount that the ratio of the amount of the solute in the noble metal solution to the amount of the powder was 3%, followed by magnetic stirring for 2 hours.
And alternately carrying out three times of water washing and three times of alcohol washing on the reaction product, transferring the reaction product into an oven, drying for 12 hours at the temperature of 60 ℃, putting the reaction product into a mortar, grinding the sample into uniform powder, sintering for 3 hours in a muffle furnace at the temperature of 450 ℃, and cooling to room temperature along with the furnace after the reaction is finished.
0.5g of the prepared sample is weighed and put in an agate mortar for grinding for 10min and then is ground according to VWater (W):VAnhydrous ethanolThe sample was slurried for 20min at 1:1 and the slurry was applied to Al with gold electrodes2O3An outer surface of the ceramic tube; transferring to a muffle furnace for heat treatment at 500 ℃ for 2h after natural air drying, cooling to room temperature along with the furnace, penetrating a Ni-Cr heating wire through a ceramic tube, and then, passing the heating wire and Al2O3Welding four lead wires of the ceramic tube on the base, placing on an aging table for aging treatment, and placing on the aging table for aging treatment for 7 days for inspectionAnd (6) measuring.
Claims (4)
1. A method for preparing an alcohol gas-sensitive material based on tin mud modification is characterized by comprising the following steps:
a. dissolving tin mud in dilute acid, and carrying out acidification treatment, wherein the acidification treatment is to carry out magnetic stirring at the water bath temperature of 30-60 ℃; the dilute acid is hydrochloric acid with the concentration of 1-4M, is washed to be neutral, and is dried in an oven after centrifugal separation;
b. b, performing high-energy ball milling on the solid obtained in the step a to obtain uniform powder, and dissolving the powder in a solvent A under magnetic stirring, wherein the solvent A is a mixed solution of deionized water and absolute ethyl alcohol; CTAB is added into the solution as a protective agent at the water bath temperature of 40-70 ℃, and then the mass ratio of the noble metal to the powder is 0.5-3%; adding a noble metal solution and a vitamin C solution into the mixed solution, wherein the molar ratio of the vitamin C to the noble metal is 1.5: 1; the noble metal solution is a chloroplatinic acid solution, and the mass ratio of platinum to powder is 1-2%; continuously reacting for 0.5-2 h;
c. c, washing the product reacted in the step b to be neutral, and then placing the product in an oven for drying;
d. and c, grinding the product obtained in the step c into uniform powder, and then carrying out heat treatment at 300-600 ℃ for 1-4h to obtain the alcohol gas-sensitive material.
2. The method for preparing the alcohol gas-sensitive material based on tin sludge modification as claimed in claim 1, wherein the heat treatment temperature in the step d is 450 ℃ to 600 ℃, and the time is 2 hours.
3. The method for preparing the alcohol gas-sensitive material based on tin mud modification according to claim 1 or 2, wherein the solvent A in the step b is a mixed solution of deionized water and absolute ethyl alcohol in a volume ratio of 1: 1.
4. Use of an alcoholic gas-sensitive material prepared by the method of any one of claims 1 to 3, characterized in that:
grinding the obtained alcohol gas-sensitive material into uniform powder, and addingAdding a solvent to prepare powder into slurry, and then continuously grinding, wherein the solvent is a mixed solution of deionized water and absolute ethyl alcohol; the paste is coated on Al with gold electrode2O3An outer surface of the ceramic tube; transferring the dried powder to a muffle furnace for heat treatment at 300-500 ℃ for 0.5-2h after the dried powder is naturally air-dried, cooling the powder to room temperature along with the furnace, penetrating a Ni-Cr heating wire through a ceramic tube, and passing the heating wire and Al2O3And welding four lead wires of the ceramic tube on the base, and placing the ceramic tube on an aging table for aging treatment to obtain the alcohol gas sensor.
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| CN104131177A (en) * | 2014-07-31 | 2014-11-05 | 河北钢铁股份有限公司 | Method for recovering refined stannum for tinning from electroplate tin mud |
| CN107561133A (en) * | 2017-08-28 | 2018-01-09 | 东北大学 | A kind of preparation method and application of precious metal doping WO3 base formaldehyde gas sensitive materials |
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| CN105628748B (en) * | 2015-12-24 | 2018-10-30 | 东北师范大学 | A kind of the tin dioxide nano fiber gas sensitive and its gas sensor of Supported Pt Nanoparticles |
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| CN104131177A (en) * | 2014-07-31 | 2014-11-05 | 河北钢铁股份有限公司 | Method for recovering refined stannum for tinning from electroplate tin mud |
| CN107561133A (en) * | 2017-08-28 | 2018-01-09 | 东北大学 | A kind of preparation method and application of precious metal doping WO3 base formaldehyde gas sensitive materials |
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| 《The effect of noble metal (Au, Pd and Pt) nanoparticles on the gas sensing performance of SnO2-based sensors: a case study on the {221} high-index faceted SnO2 octahedra》;Chang Liu et al.;《CrystEngComm》;20150907;第17卷;第6309页第2.1-2.2节 * |
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