CN113457658A - Surface modification method of biomass carbon material - Google Patents

Surface modification method of biomass carbon material Download PDF

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CN113457658A
CN113457658A CN202110899314.XA CN202110899314A CN113457658A CN 113457658 A CN113457658 A CN 113457658A CN 202110899314 A CN202110899314 A CN 202110899314A CN 113457658 A CN113457658 A CN 113457658A
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carbon material
biomass carbon
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CN113457658B (en
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陈德志
权红英
曹秀坤
张芮
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Nanchang Hangkong University
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    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/725Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/34Organic compounds containing oxygen
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    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

本发明一种生物质碳材料的表面改性方法以生物质为原料,通过粉碎、裂解、球磨和低温等离子体放电处理,制得表面改性的生物质碳材料。其中裂解以5~15℃/min的升温速率,从室温升温至800~1200℃的裂解温度,其后保温2~4h;以200~600rpm的球磨转速,将生物质碳材料球磨3~6h;在30‑60Pa时通入惰性气体,进行低温等离子体放电表面处理生物质碳材料15~60min。本发明制备方法简单,条件温和,绿色环保,易于规模化生产,有利于推广应用;制备的生物质碳材料作为催化剂,在水体中能有效激活过硫酸根用于有机污染物的降解,具有很好的催化降解效果。

Figure 202110899314

The method for surface modification of biomass carbon material of the present invention uses biomass as raw material, and obtains surface modified biomass carbon material through pulverization, cracking, ball milling and low temperature plasma discharge treatment. The pyrolysis is carried out at a heating rate of 5~15°C/min, from room temperature to a pyrolysis temperature of 800~1200°C, and then kept for 2~4h; the biomass carbon material is ball-milled for 3~6h at a ball milling speed of 200~600rpm; Inert gas was introduced at 30-60Pa, and the biomass carbon material was surface-treated by low-temperature plasma discharge for 15-60min. The preparation method has the advantages of simple preparation method, mild conditions, green and environmental protection, easy large-scale production, and favorable promotion and application; the prepared biomass carbon material, as a catalyst, can effectively activate persulfate in water body for the degradation of organic pollutants, and has the advantages of high efficiency. good catalytic degradation effect.

Figure 202110899314

Description

Surface modification method of biomass carbon material
Technical Field
The invention relates to a surface modification method of a biomass carbon material, and particularly belongs to the technical field of catalytic materials.
Background
The biomass carbon material has abundant raw materials, is widely concerned in the catalysis fields of electrocatalytic oxygen reduction, persulfate activation and the like after surface modification, and has become a hotspot for the research of the technical field of catalytic materials.
The surface modification of the carbon material is mainly realized by a chemical oxidation method, and is usually realized by mixing concentrated sulfuric acid and concentrated nitric acid with strong oxidizing property with the carbon material, and then carrying out oxidation reaction on carbon atoms on the surface of the carbon material by means of the strong oxidizing property of the concentrated sulfuric acid or the concentrated nitric acid and destroying the original carbon atom skeleton structure of the carbon material. However, in the treatment process, the method is easy to cause the release of toxic gas containing nitrogen, and pollutes the production site and the surrounding environment, and the waste liquid of concentrated sulfuric acid and concentrated nitric acid left after the surface treatment of the carbon material belongs to dangerous waste, and the post-treatment cost is high. Based on the above problems, there is a need to develop a safe, convenient and environment-friendly method for surface modification of biomass carbon material.
Disclosure of Invention
In order to achieve the above purpose, the present invention provides a surface modification method of biomass carbon material, which aims to solve the defects of the prior art.
The invention discloses a surface modification method of a biomass carbon material, which is characterized in that biomass is used as a raw material, the biomass carbon material is treated by low-temperature plasma discharge, and the surface modified biomass carbon material is prepared, and the method specifically comprises the following steps:
step 1: drying, crushing and sieving biomass to obtain biomass powder;
step 2: isolating the biomass powder from air, and performing pyrolysis to obtain a biomass carbon material; controlling cracking parameters: heating from room temperature to a cracking temperature of 800-1200 ℃ at a heating rate of 5-15 ℃/min, and then preserving heat for 2-4 h;
and step 3: ball milling the biomass carbon material for 3-6 h at a ball milling rotating speed of 200-600 rpm;
and 4, step 4: and placing the ball-milled biomass carbon material in a reaction cavity in low-temperature plasma, vacuumizing until the air pressure is stabilized at 30-60Pa, introducing inert gas, discharging the low-temperature plasma in the inert atmosphere, and performing surface treatment on the ball-milled biomass carbon material for 15-60 min to obtain the surface-modified biomass carbon material.
The power of the low-temperature plasma discharge is 50-300W.
The inert gas is nitrogen or argon.
The biomass carbon material is used as a catalyst to activate persulfate so as to degrade organic pollutants in a water body.
The invention has the beneficial effects that: the preparation method is simple, mild in condition, green and environment-friendly, is easy for large-scale production, and is beneficial to popularization and application. The prepared biomass carbon material is used as a catalyst, can effectively activate persulfate in a water body for degrading organic pollutants, and has a good catalytic degradation effect.
Drawings
FIG. 1 is a graph showing the comparison of the treatment effect of different biomass carbon materials on tetracycline-containing wastewater in example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Example 1
Drying, crushing and sieving the camellia oleifera shells to obtain biomass powder; carrying out anaerobic pyrolysis on the biomass powder at 800 ℃, heating the biomass powder from room temperature to a preset pyrolysis temperature at a heating rate of 5 ℃/min, and carrying out heat preservation for 2h after heating to the preset pyrolysis temperature to obtain a biomass carbon material; performing ball milling treatment on the biomass carbon material, wherein the ball milling rotation speed is 200rpm, and the ball milling time is 3 h; and placing the ball-milled biomass carbon material in a reaction cavity in low-temperature plasma, vacuumizing until the air pressure is stabilized at 30Pa, introducing nitrogen, and performing low-temperature plasma discharge treatment for 15min at the discharge power of 50w to obtain the surface-treated biomass carbon material.
The biomass carbon material after surface treatment is applied to the treatment of tetracycline-containing wastewater, and a comparison test is carried out:
100ml of tetracycline wastewater with the concentration of 20mg/L is respectively placed in three beakers, and the three beakers are placed in a bath kettle to be continuously stirred at room temperature, wherein the temperature is always kept at 30 ℃, and the stirring speed is 400 rmp.
0.1g of oxone was added to each of three beakers containing tetracycline wastewater, and then 40mg of untreated biomass carbon material, ball-milled biomass carbon material, and ball-milled and plasma-discharged biomass carbon material were added thereto.
2.5ml of the solution was sampled at a constant time interval under conditions of 30 ℃ and a stirring speed of 400rmp, the obtained sample was filtered, and the obtained clear solution was immediately added to a methanol solution to quench and terminate the reaction.
Experiments show that: after quenching and reaction termination after 75min, the degradation rates of tetracycline are respectively 52.2% (biomass carbon material without ball milling before treatment), 51.1% (biomass carbon material after ball milling treatment) and 73.5% (biomass carbon material after plasma discharge treatment), which indicates that the biomass carbon material after plasma discharge treatment has significant effect in treating wastewater containing tetracycline.
Example 2
Drying, crushing and screening passion fruit shells to obtain biomass powder; carrying out anaerobic pyrolysis on the biomass powder at 900 ℃, heating the biomass powder from room temperature to a preset pyrolysis temperature at a heating rate of 7 ℃/min, and carrying out heat preservation for 2.5h after heating to the preset pyrolysis temperature to obtain a biomass carbon material; performing ball milling treatment on the biomass carbon material, wherein the ball milling rotation speed is 300rpm, and the ball milling time is 3.5 h; placing the ball-milled biomass carbon material in a reaction cavity in low-temperature plasma, vacuumizing until the air pressure is stabilized at 35Pa, introducing nitrogen, and performing low-temperature plasma discharge treatment for 30min to obtain the biomass carbon material rich in surface defects; the power of the low-temperature plasma discharge was 100 w.
The biomass carbon material after surface treatment is applied to the treatment of tetracycline-containing wastewater, and a comparison test is carried out:
100ml of tetracycline wastewater with the concentration of 20mg/L is respectively placed in three beakers, and the three beakers are placed in a bath kettle to be continuously stirred at room temperature, wherein the temperature is always kept at 30 ℃, and the stirring speed is 400 rmp.
0.1g of oxone was added to each of three beakers containing tetracycline wastewater, and then 40mg of untreated biomass carbon material, ball-milled biomass carbon material, and ball-milled and plasma-discharged biomass carbon material were added thereto.
2.5ml of the solution was sampled at a constant time interval under conditions of 30 ℃ and a stirring speed of 400rmp, the obtained sample was filtered, and the obtained clear solution was immediately added to a methanol solution to quench and terminate the reaction.
Experiments show that: after quenching and reaction termination after 75min, the degradation rates of tetracycline are 67.4% (biomass carbon material without ball milling), 66.6% (biomass carbon material subjected to ball milling) and 87.2% (biomass carbon material subjected to plasma discharge treatment), respectively, which indicates that the effect of the biomass carbon material subjected to plasma discharge treatment on tetracycline-containing wastewater treatment is remarkable.
Example 3
Drying, crushing and sieving the peanut shells to obtain biomass powder; carrying out anaerobic pyrolysis on the biomass powder at 1000 ℃, heating the biomass powder from room temperature to a preset pyrolysis temperature at a heating rate of 10 ℃/min, and carrying out heat preservation for 3h after heating to the preset pyrolysis temperature to obtain a biomass carbon material; performing ball milling treatment on the biomass carbon material, wherein the ball milling rotation speed is 400rpm, and the ball milling time is 4 h; placing the ball-milled biomass carbon material in a reaction cavity in low-temperature plasma, vacuumizing until the air pressure is stabilized at 40Pa, introducing nitrogen, and performing low-temperature plasma discharge treatment for 40min to obtain the biomass carbon material rich in surface defects; the power of the low-temperature plasma discharge was 150 w.
The biomass carbon material after surface treatment is applied to the treatment of tetracycline-containing wastewater, and a comparison test is carried out:
100ml of tetracycline wastewater with the concentration of 20mg/L is respectively placed in three beakers, and the three beakers are placed in a bath kettle to be continuously stirred at room temperature, wherein the temperature is always kept at 30 ℃, and the stirring speed is 400 rmp.
0.1g of oxone was added to each of three beakers containing tetracycline wastewater, and then 40mg of untreated biomass carbon material, ball-milled biomass carbon material, and ball-milled and plasma-discharged biomass carbon material were added thereto.
2.5ml of the solution was sampled at a constant time interval under conditions of 30 ℃ and a stirring speed of 400rmp, the obtained sample was filtered, and the obtained clear solution was immediately added to a methanol solution to quench and terminate the reaction.
Experiments show that: after quenching and reaction termination after 75min, the degradation rates of tetracycline are respectively 75.9% (biomass carbon material without ball milling), 75.5% (biomass carbon material subjected to ball milling) and 95.1% (biomass carbon material subjected to plasma discharge treatment), which indicates that the biomass carbon material subjected to plasma discharge treatment has a remarkable effect in treating wastewater containing tetracycline.
Example 4
Drying, crushing and sieving the camellia oleifera shells to obtain biomass powder; carrying out anaerobic pyrolysis on the biomass powder at 1100 ℃, heating the biomass powder from room temperature to a preset pyrolysis temperature at a heating rate of 12 ℃/min, heating the biomass powder to the preset pyrolysis temperature, and then preserving heat for 3.5h to obtain a biomass carbon material; performing ball milling treatment on the biomass carbon material, wherein the ball milling rotation speed is 500rpm, and the ball milling time is 5 h; placing the ball-milled biomass carbon material in a reaction cavity in low-temperature plasma, vacuumizing until the air pressure is stabilized at 50Pa, introducing nitrogen, and performing low-temperature plasma discharge treatment for 50min to obtain the biomass carbon material rich in surface defects; the power of the low-temperature plasma discharge was 200 w.
The biomass carbon material after surface treatment is applied to the treatment of tetracycline-containing wastewater, and a comparison test is carried out:
100ml of tetracycline wastewater with the concentration of 20mg/L is respectively placed in three beakers, and the three beakers are placed in a bath kettle to be continuously stirred at room temperature, wherein the temperature is always kept at 30 ℃, and the stirring speed is 400 rmp.
0.1g of oxone was added to each of three beakers containing tetracycline wastewater, and then 40mg of untreated biomass carbon material, ball-milled biomass carbon material, and ball-milled and plasma-discharged biomass carbon material were added thereto.
2.5ml of the solution was sampled at a constant time interval under conditions of 30 ℃ and a stirring speed of 400rmp, the obtained sample was filtered, and the obtained clear solution was immediately added to a methanol solution to quench and terminate the reaction.
Experiments show that: after quenching and reaction termination after 75min, the degradation rates of tetracycline are respectively 68.7% (biomass carbon material without ball milling), 70.1% (biomass carbon material subjected to ball milling) and 90.2% (biomass carbon material subjected to plasma discharge treatment), which indicates that the effect of the biomass carbon material subjected to plasma discharge treatment on tetracycline-containing wastewater treatment is remarkable.
Example 5
Drying, crushing and screening passion fruit shells to obtain biomass powder; carrying out anaerobic pyrolysis on the biomass powder at 1200 ℃, heating the biomass powder from room temperature to a preset pyrolysis temperature at a heating rate of 15 ℃/min, and keeping the temperature for 4h after heating to the preset pyrolysis temperature to obtain a biomass carbon material; performing ball milling treatment on the biomass carbon material, wherein the ball milling rotation speed is 600rpm, and the ball milling time is 6 hours; placing the ball-milled biomass carbon material in a reaction cavity in low-temperature plasma, vacuumizing until the air pressure is stabilized at 60Pa, introducing nitrogen, and performing low-temperature plasma discharge treatment for 60min to obtain the biomass carbon material rich in surface defects; the power of the low-temperature plasma discharge was 300 w.
The biomass carbon material after surface treatment is applied to the treatment of tetracycline-containing wastewater, and a comparison test is carried out:
100ml of tetracycline wastewater with the concentration of 20mg/L is respectively placed in three beakers, and the three beakers are placed in a bath kettle to be continuously stirred at room temperature, wherein the temperature is always kept at 30 ℃, and the stirring speed is 400 rmp.
0.1g of oxone was added to each of three beakers containing tetracycline wastewater, and then 40mg of untreated biomass carbon material, ball-milled biomass carbon material, and ball-milled and plasma-discharged biomass carbon material were added thereto.
2.5ml of the solution was sampled at a constant time interval under conditions of 30 ℃ and a stirring speed of 400rmp, the obtained sample was filtered, and the obtained clear solution was immediately added to a methanol solution to quench and terminate the reaction.
Experiments show that: after quenching and reaction termination after 75min, the degradation rates of tetracycline are 72.1% (biomass carbon material without ball milling), 70.9% (biomass carbon material subjected to ball milling) and 92.2% (biomass carbon material subjected to plasma discharge treatment), respectively, which indicates that the effect of the biomass carbon material subjected to plasma discharge treatment on tetracycline-containing wastewater treatment is remarkable.

Claims (4)

1.一种生物质碳材料的表面改性方法,其特征在于:所述的表面改性方法以生物质为原料,通过低温等离子体放电处理生物质碳材料,制得表面改性的生物质碳材料,具体包括以下步骤:1. a surface modification method of biomass carbon material, it is characterized in that: described surface modification method takes biomass as raw material, treats biomass carbon material by low temperature plasma discharge, makes the biomass of surface modification Carbon material, including the following steps: 步骤1:将生物质干燥、粉碎和过筛,得到生物质粉末;Step 1: drying, pulverizing and sieving the biomass to obtain biomass powder; 步骤2:将生物质粉末隔绝空气,进行高温裂解,得到生物质碳材料;裂解参数控制:以5~15℃/min的升温速率,从室温升温至800~1200℃的裂解温度,其后保温2~4h;Step 2: The biomass powder is isolated from the air, and pyrolyzed at high temperature to obtain biomass carbon material; pyrolysis parameter control: at a heating rate of 5~15°C/min, the temperature is raised from room temperature to a pyrolysis temperature of 800~1200°C, and then kept warm 2~4h; 步骤3:以200~600rpm的球磨转速,将生物质碳材料球磨3~6h;Step 3: Ball milling the biomass carbon material for 3 to 6 hours at a ball milling speed of 200 to 600 rpm; 步骤4:将球磨后的生物质碳材料置于低温等离子体内的反应腔中,抽真空至气压稳定在30-60Pa,通入惰性气体,在惰性气氛下低温等离子体放电,对球磨后的生物质碳材料进行表面处理15~60min,制得表面改性的生物质碳材料。Step 4: Place the ball-milled biomass carbon material in a reaction chamber in a low-temperature plasma, evacuate until the air pressure is stable at 30-60Pa, pass in an inert gas, and discharge the low-temperature plasma in an inert atmosphere, and the ball-milled biomass is discharged. The biomass carbon material is subjected to surface treatment for 15-60 minutes to obtain a surface-modified biomass carbon material. 2.根据权利要求1所述的一种生物质碳材料的表面改性方法,其特征在于:所述的低温等离子体放电的功率为50~300W。2 . The method for surface modification of a biomass carbon material according to claim 1 , wherein the power of the low-temperature plasma discharge is 50-300W. 3 . 3.根据权利要求1所述的一种生物质碳材料的表面改性方法,其特征在于:所述的惰性气体为氮气或氩气。3. The method for surface modification of a biomass carbon material according to claim 1, wherein the inert gas is nitrogen or argon. 4.根据权利要求1所述的一种生物质碳材料的表面改性方法,其特征在于:所述的生物质碳材料作为催化剂激活过硫酸根用于降解水体中的有机污染物。4 . The method for surface modification of biomass carbon material according to claim 1 , wherein the biomass carbon material is used as a catalyst to activate persulfate for degrading organic pollutants in water bodies. 5 .
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