CN113321212A - Preparation method and application of novel modified rubber seed shell biochar material - Google Patents
Preparation method and application of novel modified rubber seed shell biochar material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 21
- 239000010949 copper Substances 0.000 claims abstract description 19
- 239000010420 shell particle Substances 0.000 claims abstract description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 238000010000 carbonizing Methods 0.000 claims abstract description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 5
- 238000009656 pre-carbonization Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 11
- 238000003763 carbonization Methods 0.000 claims description 10
- 239000011363 dried mixture Substances 0.000 claims description 8
- 239000002351 wastewater Substances 0.000 claims description 5
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- 239000000356 contaminant Substances 0.000 claims 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000008367 deionised water Substances 0.000 abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 7
- 239000002028 Biomass Substances 0.000 abstract description 5
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- 238000004140 cleaning Methods 0.000 description 6
- 229910001431 copper ion Inorganic materials 0.000 description 6
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
Abstract
The invention relates to a preparation method and application of a novel modified rubber seed shell biochar material, belonging to the field of biomass carbon materials, wherein the preparation method comprises the following steps: crushing, sieving and drying the rubber seed shells to obtain rubber seed shell particles; pre-carbonizing rubber seed shell particles in a tubular furnace; adding rubber seed shell biochar after pre-carbonization into KMnO4In the solution, carrying out ultrasonic treatment for 1 h; drying the mixture after the ultrasonic treatment; calcining the dried material in nitrogen atmosphere again, washing the carbonized biochar with deionized water, and drying to obtain the final productA capsule shell biochar material. The novel modified rubber seed shell biochar material is applied to removing heavy metal copper in sewage, and the removal rate of copper reaches 94%.
Description
Technical Field
The invention belongs to the field of biomass carbon materials, and particularly relates to a preparation method and application of a novel modified rubber seed shell biochar material.
Background
Today, one of the most serious environmental pollution problems is water pollution. With the rapid development of industrial activities, water pollution caused by toxic metals in industrial wastewater discharge has become a serious environmental and public health problem. Wherein, the metal copper is a common pollutant in industrial wastewater, and the industrial activities such as metal plating, smelting, mining and the like can discharge the wastewater containing copper pollutants with different concentrations into the environment. Copper can cause harm to the ecological environment and human body, and excessive intake of copper can cause liver and kidney injury, chronic copper poisoning, brain injury and the like in the human body. Therefore, it is important to remove high concentration Cu (II) in water.
At present, the main methods for removing Cu (II) in wastewater include ion exchange method, coagulation method, chemical precipitation method, biological treatment method, adsorption method, membrane separation method and the like. These methods have their own advantages and disadvantages. For example, chemical precipitation methods, while relatively simple and cost effective to operate, are susceptible to secondary contamination. Although the removal rate is high, methods such as ion exchange and membrane separation are expensive and costly. Among them, the adsorption method is considered as an economical and effective option for removing heavy metals in wastewater, and has been paid attention by researchers because of its advantages of low cost, high efficiency, convenient operation, environmental friendliness, etc. However, the use of low cost adsorbents is also an important economic consideration.
The agricultural and forestry wastes can be used as fertilizer, feed, biogas, biomass energy, fuel and raw materials of petroleum products, and can also be used for preparing adsorbing materials for sewage treatment, and the like, so that the agricultural and forestry wastes have wide market prospects for recycling. Biomass has great advantages in sewage treatment due to its abundant functional groups and huge specific surface area. The biochar is a carbon material with high chemical stability obtained by pyrolyzing biomass under the condition of limited oxygen or no oxygen, the surface of the biochar is rich in various oxygen-containing functional groups, and the biochar has a porous structure and has strong adsorption affinity for heavy metals. The concept of 'treating waste with waste' is undoubtedly a direction worth researching, and the rubber seed shell is used as agricultural and forestry waste and is used as a raw material of biochar in a preparation method and used for removing heavy metals.
Disclosure of Invention
In order to overcome the problems in the background art, the invention provides a preparation method and application of a novel modified rubber seed shell biochar material, which utilizes KMnO4Modified preparation method adsorbent and KMnO prepared by modified preparation method adsorbent4The modified biochar has larger specific surface area, abundant pore channel structures and abundant oxygen-containing functional groups, and the series of advantages can enable the biochar modified by KMnO4 to become a good adsorbent material.
In order to realize the purpose, the invention is realized by the following technical scheme:
the preparation method of the novel modified rubber seed shell biochar material comprises the following steps:
(1) crushing, sieving and drying the rubber seed shells to obtain rubber seed shell particles;
(2) pre-carbonizing and calcining the rubber seed shell particles in the step (1) in a nitrogen atmosphere;
(3) adding the material pre-carbonized in the step (2) into KMnO4In the solution, carrying out ultrasonic treatment in an ultrasonic instrument, and drying the mixture after the ultrasonic treatment is finished;
(4) and (4) putting the dried mixture in the step (3) into nitrogen atmosphere again for calcination and carbonization, filtering and washing the carbonized biochar, and drying to obtain the rubber seed shell biochar material.
Further, in the step (1), the sieving mesh number of the rubber seed shells is 40-60 meshes, and the drying temperature is 60-80 ℃.
Further, in the step (2), the pre-carbonization temperature is 300-.
Further, in the step (3), KMnO4The mass ratio of the rubber seed shell carbon to the rubber seed shell carbon is 1: 1-3.
Further, in the step (4), the carbonization temperature is 500-.
Further, in the step (4), the drying temperature is 60-80 ℃.
Furthermore, the novel modified rubber seed shell biochar material is applied to removal of metal copper pollutants in wastewater.
The invention has the beneficial effects that:
according to the invention, the rubber seed shell activated carbon is modified by adopting KMnO4, not only is the KMnO4 strong in oxidizing property, so that oxygen-containing functional groups on the surface of the biochar can be increased, but also the pores of the biochar can be improved; MnOx generated by the reaction of KMnO4 and organic functional groups with reducibility on the surface of the biochar is loaded on the surface of the biochar, and heavy metals can be removed by complexing with the MnOx. The complex, the cation-pi bond, the electrostatic attraction, the ion exchange and the like are formed, so that the interaction between the biochar and the heavy metal is promoted, the complex reaction between the heavy metal copper and the biochar is promoted, the excellent removal efficiency is finally achieved, and the removal rate is high.
Drawings
FIG. 1 is KMnO of example 24 A 2-micron SEM image of the modified rubber seed shell biochar;
FIG. 2 is KMnO of example 24 5 μm SEM image of modified rubber seed shell biochar;
FIG. 3 is a graph showing the effect of different amounts of adsorbent on Cu (II) removal.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, preferred embodiments of the present invention will be described in detail below to facilitate understanding of the skilled person.
Example 1
Preparation method and application of novel modified rubber seed shell biochar material
(1) Crushing the rubber seed shells, sieving the crushed rubber seed shells with a 40-mesh sieve to obtain rubber seed shell particles, and drying at the temperature of 60 ℃ for 12 hours.
(2) And (2) pre-carbonizing the dried rubber seed shell particles in the step (1) in a tubular furnace, uniformly heating to the calcining temperature of 300 ℃ at a heating rate of 5 ℃/min, and calcining for 1h at constant temperature.
(3) Adding the material pre-carbonized in the step (2) into 100mLKMno4In a solution beaker, here KMnO4The mass ratio of the rubber seed shell carbon to the rubber seed shell carbon is 1:1, the beaker is subjected to ultrasonic treatment for 1 hour in an ultrasonic instrument, and after the ultrasonic treatment is finished, the mixture is dried in an oven at 60 ℃.
(4) And (4) placing the dried mixture obtained in the step (3) in a tubular furnace again, heating to the calcination temperature of 500 ℃ at a constant speed at a heating rate of 5 ℃/min, calcining for 1h at a constant temperature for carbonization, cleaning the carbonized charcoal with deionized water, and placing in a vacuum drying oven at 60 ℃ for drying overnight to obtain the modified rubber seed shell charcoal material.
0.01g of the modified rubber seed shell biochar material prepared in the example is weighed and added into a 150mL conical flask containing 50mL of 50mg/L copper ion solution, and then the mixture is oscillated for 24 hours in a constant temperature oscillation box at 25 ℃ and 150rpm, the Cu (II) removal rate is 90%, and the adsorption capacity is 181.53 mg/g.
Example 2: preparation method and application of novel modified rubber seed shell biochar material
(1) Crushing the rubber seed shells, sieving the crushed rubber seed shells with a 60-mesh sieve to obtain rubber seed shell particles, and drying at the temperature of 80 ℃ for 12 hours.
(2) And (2) pre-carbonizing the dried rubber seed shell particles in the step (1) in a tubular furnace, uniformly heating to the calcining temperature of 500 ℃ at the heating rate of 5 ℃/min, and calcining for 1h at constant temperature.
(3) Adding the material pre-carbonized in the step (2) into a container containing 100mL of KMnO4In a beaker of solution, here KMnO4The mass ratio of the rubber seed shell carbon to the rubber seed shell carbon is 1:2, the beaker is subjected to ultrasonic treatment for 1 hour in an ultrasonic instrument, and after the ultrasonic treatment is finished, the mixture is dried in an oven at 80 ℃.
(4) And (4) placing the dried mixture obtained in the step (3) in a tubular furnace again, uniformly heating to the calcination temperature of 800 ℃ at the heating rate of 5 ℃/min, calcining at constant temperature for 2h for carbonization, cleaning the carbonized charcoal with deionized water, and placing in a vacuum drying oven at 80 ℃ for drying overnight to obtain the modified rubber seed shell charcoal material.
0.025g of the modified rubber seed shell biochar material prepared in the example was weighed into a 150mL conical flask containing 50mL of 50mg/L copper ion solution, and then shaken in a constant temperature shaking oven at 150rpm and 25 ℃ for 24h, with a Cu (II) removal rate of 94% and an adsorption capacity of 94.40 mg/g.
Example 3: preparation method and application of novel modified rubber seed shell biochar material
(1) Crushing the rubber seed shells, sieving the crushed rubber seed shells with a 40-mesh sieve to obtain rubber seed shell particles, and drying at the temperature of 70 ℃ for 12 hours.
(2) And (2) pre-carbonizing the dried rubber seed shell particles in the step (1) in a tubular furnace, uniformly heating to the calcining temperature of 400 ℃ at a heating rate of 5 ℃/min, and calcining for 1h at constant temperature.
(3) Adding the material pre-carbonized in the step (2) into a container containing 100mL of KMnO4In a beaker of solution, here KMnO4The mass ratio of the rubber seed shell carbon to the rubber seed shell carbon is 1:3, the beaker is subjected to ultrasonic treatment for 1 hour in an ultrasonic instrument, and after the ultrasonic treatment is finished, the mixture is dried in an oven at 70 ℃.
(4) And (4) placing the dried mixture obtained in the step (3) in a tubular furnace again, uniformly heating to the calcination temperature of 600 ℃ at the heating rate of 5 ℃/min, calcining at constant temperature for 2h for carbonization, cleaning the carbonized charcoal with deionized water, and placing in a vacuum drying oven at 70 ℃ for drying overnight to obtain the modified rubber seed shell charcoal material.
0.05g of the modified rubber seed shell biochar material prepared in the embodiment is weighed and added into a 150mL conical flask containing 50mL and 50mg/L of copper ion solution, and then the mixture is oscillated for 24 hours in a constant temperature oscillation box with the temperature of 25 ℃ and the rpm of 150, the Cu (II) removal rate is 96 percent, and the adsorption capacity is 48.01 mg/g.
Example 4: preparation method and application of novel modified rubber seed shell biochar material
(1) Crushing the rubber seed shells, sieving the crushed rubber seed shells with a 60-mesh sieve to obtain rubber seed shell particles, and drying at the temperature of 60 ℃ for 12 hours.
(2) And (2) pre-carbonizing the dried rubber seed shell particles in the step (1) in a tubular furnace, uniformly heating to the calcining temperature of 300 ℃ at a heating rate of 5 ℃/min, and calcining for 1h at constant temperature.
(3) Adding the material pre-carbonized in the step (2) into a container containing 100mL of KMnO4In a beaker of solution, here KMnO4The mass ratio of the rubber seed shell carbon to the rubber seed shell carbon is 1:1, the beaker is subjected to ultrasonic treatment for 1 hour in an ultrasonic instrument, and after the ultrasonic treatment is finished, the mixture is dried in an oven at 60 ℃.
(4) And (4) placing the dried mixture obtained in the step (3) in a tubular furnace again, uniformly heating to the calcination temperature of 700 ℃ at the heating rate of 5 ℃/min, calcining at the constant temperature for 2h for carbonization, cleaning the carbonized charcoal with deionized water, and placing the charcoal in a vacuum drying oven at 60 ℃ for drying overnight to obtain the modified rubber seed shell charcoal material.
0.075g of the modified rubber seed shell biochar material prepared in the example is weighed and added into a 150mL conical flask containing 50mL and 50mg/L of copper ion solution, and then the conical flask is shaken for 24 hours in a constant temperature shaking box at 25 ℃ and 150rpm, the Cu (II) removal rate is 96%, and the adsorption capacity is 32.09 mg/g.
Example 5: preparation method and application of novel modified rubber seed shell biochar material
(1) Crushing the rubber seed shells, sieving the crushed rubber seed shells with a 40-mesh sieve to obtain rubber seed shell particles, and drying at the temperature of 70 ℃ for 12 hours.
(2) And (2) pre-carbonizing the dried rubber seed shell particles in the step (1) in a tubular furnace, uniformly heating to the calcining temperature of 400 ℃ at a heating rate of 5 ℃/min, and calcining for 1h at constant temperature.
(3) Adding the material pre-carbonized in the step (2) into a container containing 100mL of KMnO4In a beaker of solution, here KMnO4The mass ratio of the rubber seed shell carbon to the rubber seed shell carbon is 1:2, the beaker is subjected to ultrasonic treatment for 1 hour in an ultrasonic instrument, and after the ultrasonic treatment is finished, the mixture is dried in an oven at 70 ℃.
(4) And (4) placing the dried mixture obtained in the step (3) in a tubular furnace again, uniformly heating to the calcination temperature of 600 ℃ at the heating rate of 5 ℃/min, calcining at constant temperature for 2h for carbonization, cleaning the carbonized charcoal with deionized water, and placing in a vacuum drying oven at 70 ℃ for drying overnight to obtain the modified rubber seed shell charcoal material.
0.1g of the modified rubber seed shell biochar material prepared in the embodiment is weighed and added into a 150mL conical flask containing 50mL and 50mg/L of copper ion solution, and then the mixture is oscillated for 24 hours in a constant temperature oscillation box at 25 ℃ and 150rpm, the Cu (II) removal rate is 95 percent, and the adsorption capacity is 23.80 mg/g.
Example 6: preparation method and application of novel modified rubber seed shell biochar material
(1) Crushing the rubber seed shells, sieving the crushed rubber seed shells with a 40-mesh sieve to obtain rubber seed shell particles, and drying at the temperature of 80 ℃ for 12 hours.
(2) And (2) pre-carbonizing the dried rubber seed shell particles in the step (1) in a tubular furnace, uniformly heating to the calcining temperature of 500 ℃ at the heating rate of 5 ℃/min, and calcining for 1h at constant temperature.
(3) Adding the material pre-carbonized in the step (2) into a container containing 100mL of KMnO4In a beaker of solution, here KMnO4The mass ratio of the rubber seed shell carbon to the rubber seed shell carbon is 1:3, the beaker is subjected to ultrasonic treatment for 1 hour in an ultrasonic instrument, and after the ultrasonic treatment is finished, the mixture is dried in an oven at 80 ℃.
(4) And (4) placing the dried mixture obtained in the step (3) in a tubular furnace again, uniformly heating to the calcination temperature of 800 ℃ at the heating rate of 5 ℃/min, calcining at constant temperature for 2h for carbonization, cleaning the carbonized charcoal with deionized water, and placing in a vacuum drying oven at 80 ℃ for drying overnight to obtain the modified rubber seed shell charcoal material.
0.15g of the modified rubber seed shell biochar material prepared in the embodiment is weighed and added into a 150mL conical flask containing 50mL and 50mg/L of copper ion solution, and then the mixture is oscillated for 24 hours in a constant temperature oscillation box at 25 ℃ and 150rpm, the Cu (II) removal rate is 93 percent, and the adsorption capacity is 15.59 mg/g.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of a novel modified rubber seed shell biochar material is characterized by comprising the following steps: the method comprises the following steps:
(1) crushing, sieving and drying the rubber seed shells to obtain rubber seed shell particles;
(2) pre-carbonizing and calcining the rubber seed shell particles in the step (1) in a nitrogen atmosphere;
(3) adding the material pre-carbonized in the step (2) into KMnO4Carrying out ultrasonic treatment in the solution, and drying the mixture after the ultrasonic treatment is finished;
(4) and (4) putting the dried mixture in the step (3) into nitrogen atmosphere again for calcination and carbonization, filtering and washing the carbonized biochar, and drying to obtain the rubber seed shell biochar material.
2. The preparation method of the novel modified rubber seed shell biochar material as claimed in claim 1, characterized in that: in the step (1), the rubber seed shells are sieved by a 40-60 mesh sieve, and the drying temperature is 60-80 ℃.
3. The preparation method of the novel modified rubber seed shell biochar material as claimed in claim 1, characterized in that: in the step (2), the pre-carbonization temperature is 300-.
4. The preparation method of the novel modified rubber seed shell biochar material as claimed in claim 1, characterized in that: in step (3), KMnO4The mass ratio of the rubber seed shell carbon to the rubber seed shell carbon is 1: 1-3.
5. The preparation method of the novel modified rubber seed shell biochar material as claimed in claim 1, characterized in that: in the step (4), the carbonization temperature is 500-.
6. The preparation method of the novel modified rubber seed shell biochar material as claimed in claim 1, characterized in that: in the step (4), the drying temperature is 60-80 ℃.
7. Use of the novel modified rubber seed husk biochar material of any one of claims 1-6 in the removal of metallic copper contaminants from wastewater.
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