CN116282387A - Method for preparing straw carbon-hydroxypropyl membrane electrode by melting pyrolysis with cadmium removal - Google Patents
Method for preparing straw carbon-hydroxypropyl membrane electrode by melting pyrolysis with cadmium removal Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 37
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- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 27
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002844 melting Methods 0.000 title claims abstract description 24
- 230000008018 melting Effects 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 10
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 16
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- 238000001035 drying Methods 0.000 claims description 12
- 238000011282 treatment Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000007790 scraping Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
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- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 235000005822 corn Nutrition 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
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- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 240000007594 Oryza sativa Species 0.000 claims 2
- 235000007164 Oryza sativa Nutrition 0.000 claims 2
- 240000008042 Zea mays Species 0.000 claims 2
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- 238000001132 ultrasonic dispersion Methods 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 229910052786 argon Inorganic materials 0.000 claims 1
- 238000002386 leaching Methods 0.000 claims 1
- 239000002296 pyrolytic carbon Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 229910021642 ultra pure water Inorganic materials 0.000 claims 1
- 239000012498 ultrapure water Substances 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 25
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 239000002351 wastewater Substances 0.000 abstract description 12
- 238000004070 electrodeposition Methods 0.000 abstract description 8
- 239000007772 electrode material Substances 0.000 abstract description 7
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
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- 239000012495 reaction gas Substances 0.000 description 2
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- 239000007787 solid Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
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- 231100000693 bioaccumulation Toxicity 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46152—Electrodes characterised by the shape or form
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a method for preparing a straw carbon-hydroxypropyl membrane electrode by melting pyrolysis for removing cadmium, which takes straw carbon obtained by high-temperature melting pyrolysis as a raw material, has a stable structure, higher specific surface area and reasonable pore distribution based on the straw carbon, and then loads the straw carbon-hydroxypropyl membrane electrode on a graphite electrode, so that the removal performance of heavy metal ions is remarkably enhanced; can be applied to Cd-containing 2+ And the waste water of the equivalent heavy metal ions is purified and removed, and the recycling rate of the electrode after the reaction is finished is high. The invention has simple preparation process, low cost, low requirements on equipment and environmental conditions, high purification and removal rate of some heavy metal cadmium, and can realize clean recovery of heavy metal elements, thereby providing a new insight and scheme for solving the problems of high cost of electrode materials, complex process, low effective utilization rate of heavy metal and the like in the traditional electrodeposition method for removing heavy metal. Is an effective heavy metalThe removal technology has good application prospect in the electrochemical field.
Description
Technical Field
The invention belongs to the technical field of innovative electrode material preparation, and particularly relates to a method for preparing a straw carbon-hydroxypropyl membrane electrode by melting pyrolysis for removing cadmium.
Background
In recent years, the industrialization process of China is increasingly accelerated, and the problem of environmental pollution caused by the exceeding of the weight metal content of water in industrial wastewater is more obvious. Cadmium-containing wastewater is most representative in heavy metal-containing wastewater and is often characterized by high stability,Difficult degradation, high toxicity hazard, strong bioaccumulation and the like, and causes serious damage to daily life of animals, plants and human bodies. Has become one of the important sources of environmental pollution. At present, the purification treatment method for the cadmium-containing wastewater is commonly chemical conversion treatment, heavy metal ion exchange, resin method and the like. These treatments tend to result in too high treatment inputs, susceptibility to secondary contaminants, and the adsorbed species and Cd employed 2+ Difficult separation and desorption, resulting in Cd 2+ The secondary use cannot be performed, and the adsorbent itself cannot be recycled. Based on these problems, the advantages of the electrochemical deposition method are becoming more pronounced because it is easy to handle, clean and efficient, and is relatively environmentally friendly. The ion removal efficiency of the heavy metal wastewater treated by the electrodeposition method is very high, no secondary pollution is generated, and the method is an ideal and efficient heavy metal wastewater treatment method. This approach is mainly to use high energy electron beams as reducing agents, and no or less chemical agents are typically added to enhance electrophoresis. However, the existing electrode manufacturing method by the electrodeposition method has the disadvantages of complicated process, incapability of independently forming materials, high cost and low recycling rate, and greatly limits the application of the method in the aspect of heavy metal wastewater treatment.
China is one of the largest straw producing countries in the world, for example, 2021 the national corn yield accounts for 22% of the global corn yield. In the process of crop production and consumption, the straw used as the byproduct waste has a single utilization mode and low conversion efficiency, the straw in China is one of main agricultural waste, about 6 hundred million tons of straw is used as incineration direct combustion treatment each year, the degree of environmental pollution is aggravated, and the straw also has an important threat to the healthy living environment of human beings. Therefore, the method has great significance in searching for a more efficient straw recycling conversion mode. According to the invention, the straw biochar-hydroxypropyl cellulose membrane electrode capable of being independently formed is manufactured by taking the agricultural waste straw as a raw material, the prepared material is applied to the treatment of the waste water containing heavy metal cadmium ions by an electrodeposition method, and experimental results show that the treatment efficiency of the simulated waste water reaches 80% under lower power consumption, the cost is greatly reduced while the treatment efficiency is ensured, the heavy metal hazardous waste production is obviously reduced, the recycling efficiency is higher, and ideal economic and environmental benefits are generated. Provides new insight and effective way for the application of the electrodeposition method in the aspect of heavy metal wastewater treatment, and has very important practical significance.
Biomass pyrolysis charcoal making technology is one of the important modes of biomass heat utilization. The biochar is a byproduct obtained by biomass pyrolysis, and the preparation of the biochar has the advantages of simple process, low cost, enrichment of the biochar carbon and the like. Among them, biochar has a wide variety of applications and uses, and the utilization of waste biomass pyrolysis for producing charcoal to be recycled contributes to the reduction of non-renewable resource consumption. The biomass can fix most of C in the biochar through thermal conversion, and then the biomass is prepared and modified through functionalization, so that the renewable electrochemical energy storage material with high benefit, negative carbon and environment friendliness with minimum process loss is easily obtained, after the fibrous biomass is subjected to high-temperature melting pyrolysis to obtain the biochar, the graphitization degree of the biomass charcoal is high, the biomass charcoal has a high specific surface area and a stable pore structure, and the mechanical strength of the biochar is also greatly improved. Meanwhile, the electrode material prepared from the biochar has excellent electrochemical characteristics of good thermal stability and chemical stability, compatibility with rapid electron transfer capability, higher storage capacity and the like. The method makes the biochar possible to prepare the membrane electrode material with high heavy metal removal rate, high thermal stability and high chemical stability and easy adjustment.
Disclosure of Invention
The invention aims to provide a method for preparing a straw carbon-hydroxypropyl membrane electrode by melting pyrolysis for removing cadmium. The method adopts a high-temperature melting pyrolysis process and adopts a graphite electrode and a film forming agent to prepare a membrane electrode material to solve the problems of high cost and low material recycling rate of the traditional electrodeposition method, and provides a simple and low-cost preparation method for preparing the straw biochar-hydroxypropyl cellulose membrane electrode material for removing heavy metal cadmium in the environment.
The invention adopts the following technical scheme to solve the technical problems:
a method for preparing straw carbon-hydroxypropyl membrane electrode by melting pyrolysis for removing cadmium comprises a substrate electrode and a membrane electrode layer; the membrane electrode layer is a high-temperature melting biochar-hydroxypropyl cellulose composite material membrane layer, and the substrate electrode is a graphite electrode.
In a preferred embodiment of the present invention, the overall material thickness of the membrane electrode layer is about 100. Mu.m.
The invention provides a method for preparing a straw carbon-hydroxypropyl membrane electrode by melting pyrolysis for removing cadmium, which comprises the following steps:
1. preparation of high-temperature melting pyrolysis straw charcoal
Drying in-situ biomass straws, crushing and granulating, taking the mixing proportion (a hierarchical pore structure or a communicating pore structure can be constructed according to the known granularity relation) of crushed straw raw materials at different positions into consideration, and putting the mixture into a granulator to obtain a formed granule raw material; feeding the formed particles into a horizontal tube furnace, and continuously introducing N 2 Ar is used as heating medium gas, and the high-temperature melting pyrolysis is carried out by controlling the heating rate to 25 ℃/min, the reaction temperature to 1400 ℃, the reaction time to 30 min and the gas flow to 5L/min. However, it is noted that Ar is preferable as a reaction gas when chemical change of high-temperature nitrogen doping exists, and the solid obtained after pyrolysis is biomass high-temperature molten biochar, and the sample is taken out by taking care of cooling in a protective atmosphere. Placing the extracted biochar in an analytically pure HCl and HF solution with the mass ratio of 1:1, placing the solution in a shaking table for pickling and oscillating 12 h, washing the solution to the pH=7.0 of supernatant by deionized water, pouring out the washing solution, placing the solution in a drying box with the temperature of 105+/-5 ℃, drying 2 h, and taking out for later use.
2. Preparation of straw carbon-hydroxypropyl membrane electrode
Adding absolute ethyl alcohol and 1.5 g high-temperature melting pyrolysis straw carbon into a 50 ml beaker, sending the straw carbon into an ultrasonic dispersing instrument to be ultrasonically dispersed until the particle size is less than or equal to 1 mu m, taking out the straw carbon, putting the dispersed straw carbon into the beaker, adding 15 mL absolute ethyl alcohol and 0.5 g hydroxypropyl cellulose, transferring the straw carbon onto a magnetic stirrer, controlling the constant temperature to be 60-65 ℃, and magnetically stirring the straw carbon for 10 min by using a rotor magnetic stirrer to set parameters of 1200 r/min until the hydroxypropyl cellulose is completely dissolved, so that the ratio of the three is 30:3:1. And then stirring for 10 min continuously with the stirring speed unchanged until the three substances are uniformly mixed to obtain the membrane liquid. And (3) placing the obtained membrane liquid in a membrane scraping device to control the thickness to be 100 mu m for membrane scraping treatment, placing the obtained membrane in a drying oven, and drying at 105+/-5 ℃ for 1h to obtain the material, namely the straw carbon-hydroxypropyl cellulose membrane electrode.
3. Membrane electrode cadmium removal test
Pressing the prepared straw carbon-hydroxypropyl membrane electrode on a graphite carbon electrode, placing the graphite carbon electrode in cadmium ion-containing heavy metal wastewater, setting the working voltage to be 36V, ensuring that the reaction current intensity changes linearly or periodically along with time, and then respectively extracting the solution 10 ml as a sample in the 10 th, 20 th, 30 th, 60 th, 120 th, 240 th and 480 th min in the water purification reaction process, and testing the cadmium concentration to determine the cadmium removal efficiency.
Advantageous effects
The graphitized carbon obtained by high-temperature melting pyrolysis is used as a substrate, and has the advantages of stable structure, higher specific surface area, reasonable pore distribution, and remarkable performance of enhancing heavy metal ion removal by loading the graphitized carbon onto the biochar electrode through the straw carbon film electrode. Preparing the straw biochar-hydroxypropyl cellulose film-forming electrode. The prepared electrode is used for removing cadmium-containing wastewater, the cadmium removal efficiency can be approximately 80% within 480 min, the electrode has a good cadmium removal effect, the electrode can be applied to purification and removal of heavy metal wastewater containing cadmium and the like, and the recycling rate of the electrode is high after the reaction is finished. The preparation method has the advantages of simple process, low cost, low requirements on equipment and environmental conditions, high purification removal rate of some heavy metals (such as cadmium and the like), realization of clean recovery of heavy metal elements, and provision of a new insight and scheme for solving the problems of high cost, complex process, low effective utilization rate of heavy metals and the like of the electrode material in the traditional electrodeposition method for removing the heavy metals, and is an effective preparation technology of the functionalized membrane electrode applied to heavy metal removal.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention. In more detail, the preferred embodiments of the technical scheme of the invention are as follows:
preparing high-temperature melting pyrolysis straw carbon: drying in-situ biomass straws, crushing and granulating, taking the mixing proportion (a hierarchical pore structure or a communicating pore structure can be constructed according to the known granularity relation) of crushed straw raw materials at different positions into consideration, and putting the mixture into a granulator to obtain a formed granule raw material; feeding the formed particles into a horizontal tube furnace, and continuously introducing N 2 Ar is used as heating medium gas, and the high-temperature melting pyrolysis is carried out by controlling the heating rate to 25 ℃/min, the reaction temperature to 1400 ℃, the reaction time to 30 min and the gas flow to 5L/min. However, it is noted that Ar is preferably used as a reaction gas when the possibility of chemical change of high-temperature nitrogen doping exists, the solid obtained after pyrolysis is high-temperature molten straw carbon, and the sample is taken out after taking care of cooling in a protective atmosphere. Placing the extracted biochar in an analytically pure HCl and HF solution with the mass ratio of 1:1, placing the solution in a shaking table for pickling and oscillating 12 h, washing the solution to the pH=7.0 of supernatant by deionized water, pouring out the washing solution, placing the solution in a drying box with the temperature of 105+/-5 ℃, drying 2 h, and taking out for later use.
Preparation of a straw biochar-hydroxypropyl cellulose film forming electrode: adding absolute ethyl alcohol and 1.5 g high-temperature melting pyrolysis biochar into a 50 ml beaker, sending the obtained product into an ultrasonic dispersing instrument to be ultrasonically dispersed until the particle size is less than or equal to 1 mu m, taking out the obtained product, putting the dispersed biochar into the beaker, adding 15 mL absolute ethyl alcohol and 0.5 g hydroxypropyl cellulose, transferring the obtained product onto a magnetic stirrer, controlling the constant temperature to be 60-65 ℃, and magnetically stirring the obtained product for 10 minutes by using a rotor magnetic stirrer to set parameters of 1200 r/min until the hydroxypropyl cellulose is completely dissolved, so that the ratio of the three components is 30:3:1. And then stirring for 10 min continuously with the stirring speed unchanged until the three substances are uniformly mixed to obtain the membrane liquid. And (3) placing the obtained membrane solution in a membrane scraping device to control the thickness to be 100 mu m for membrane scraping treatment, placing the obtained membrane in a drying oven, and drying at 105+/-5 ℃ for 1h to obtain the material, namely the biochar-hydroxypropyl cellulose membrane electrode.
And (3) removing and testing heavy metal cadmium of the membrane electrode: taking a certain amount of cadmium-containing wastewater with the concentration of 100 mg/L in a beaker, extracting 10 ml of the wastewater as a control group sample, setting three groups of parallel experiments, placing a straw biochar-hydroxypropyl cellulose film-forming electrode and a substrate biochar graphite electrode in the beaker, switching on the anode and the cathode of a direct current stabilized power supply, under the condition that the voltage is 36V and the reaction current intensity is ensured to linearly or periodically change along with time, then respectively extracting 10 ml of solution as a sample in 10 th, 20 th, 30 th, 60 th, 120 th, 240 th and 480 th min in the water purification reaction process, and testing the cadmium concentration to determine the cadmium removal efficiency.
Claims (4)
1. A method for preparing a straw carbon-hydroxypropyl membrane electrode by melting pyrolysis for removing cadmium is characterized by comprising the following steps of: preferably, the corn stalk/rice straw is used for obtaining high-temperature melting pyrolytic carbon: the method specifically comprises the steps of collecting biomass such as corn straws/rice straws and the like, drying, crushing to a granularity of more than 120 meshes, taking a proper amount of the biomass, putting the biomass into a high-temperature tubular pyrolysis furnace, continuously introducing argon, exhausting and isolating air in the furnace, heating a hearth to a temperature above a target temperature of 1400 ℃ at a heating rate of 25 ℃/min, controlling the gas flow to be 5L/min, reacting for 30 min, cooling crude carbon to room temperature, taking out the crude carbon, oscillating the crude carbon by a solution acid leaching table configured by HCl and HF according to a mass ratio of 1:1 for 12 h, washing the crude carbon to a supernatant pH value of 7.0 by deionized water/ultrapure water, and drying to obtain molten pyrolytic biochar; preparation of a membrane electrode: adding a proper amount of absolute ethyl alcohol and high-temperature melting pyrolysis straw carbon into a container, performing ultrasonic dispersion, taking out, heating to a certain temperature, adding film forming agent hydroxypropyl cellulose, using a magnetic stirrer, adding a stirrer, fully stirring, pouring the obtained film liquid into a film scraping device for film scraping treatment after the hydroxypropyl cellulose is fully dissolved, and taking out after the obtained film is fully dried in an oven, thus obtaining the film electrode.
2. The method for preparing the straw charcoal-hydroxypropyl membrane electrode by melting pyrolysis with cadmium removal according to claim 1, which is characterized in that: the temperature of the pyrolysis furnace is set to be more than 1400 ℃ in the preparation process of the biochar.
3. The method for preparing the straw charcoal-hydroxypropyl membrane electrode by removing cadmium through melt pyrolysis according to claim 1, which is characterized in that: the added solvent is absolute ethyl alcohol, and the film forming agent is hydroxypropyl cellulose powder.
4. The method for preparing the straw charcoal-hydroxypropyl membrane electrode by removing cadmium through melt pyrolysis according to claim 1, which is characterized in that: firstly, adding absolute ethyl alcohol and melting pyrolysis straw carbon into a container, then performing ultrasonic dispersion until the particle size is less than or equal to 1 mu m, adding film forming agent hydroxypropyl cellulose when the temperature is raised to about 60-65 ℃ in the film forming process, so that the mass ratio of the absolute ethyl alcohol to the melting pyrolysis straw carbon is 30:3:1, the ratio is the optimal preparation condition for manufacturing a film electrode, and finally controlling the thickness of a scraping film of the film electrode to be 100 mu m.
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| CN102602913A (en) * | 2012-03-23 | 2012-07-25 | 上海大学 | Preparation method of biochar |
| CN104785207A (en) * | 2015-03-27 | 2015-07-22 | 四川农业大学 | High-adsorption performance biochar for heavy metal ions and preparation method for high-adsorption-performance biochar |
| CN108315016A (en) * | 2018-03-10 | 2018-07-24 | 湖南科技大学 | A kind of porous magnetic humic acid/charcoal particle and preparation method thereof for heavy metal reparation |
| CN114890509A (en) * | 2022-06-27 | 2022-08-12 | 谭中欣 | Preparation technology of straw biochar-ethyl cellulose film-forming electrode for removing heavy metals in environment |
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