阅读说明：本技术 具有吸附甲苯作用的高比表面积生物质炭材料的制备方法 (Preparation method of biomass charcoal material with high specific surface area and toluene adsorption effect ) 是由 袁明 周会平 安昭辉 陈东辉 于 2019-09-29 设计创作，主要内容包括：本发明涉及具有吸附甲苯作用的高比表面积生物质炭材料的制备方法,洗净高山竹表面并干燥切割得到竹块；将得到的竹块放入坩埚中送入管式炉中,通入保护气体煅烧得到碳化后的竹块；取碳化后的竹块,用破碎机打磨破碎,随后筛分得到竹炭；取筛分后的竹炭与KOH混合,加乙醇溶解,然后干燥；通入保护气体,对干燥后的产物进行活化护理；将活化处理得到的产物经浸泡、洗涤、干燥处理得到多孔生物质碳。本发明制备得到高表面以及它分级多孔特性,提高了多孔生物质炭的应用性能及吸附性能；本工艺具有易于控制,成本低,方法简便的优点,适合工业化生产,在吸附、电极材料、分离、传感、气体储存及催化剂载体等领域均有着潜在的应用价值。(The invention relates to a preparation method of a biomass charcoal material with high specific surface area and toluene adsorption effect, which comprises the steps of cleaning the surface of alpine bamboo, drying and cutting to obtain bamboo blocks; putting the obtained bamboo blocks into a crucible, feeding the crucible into a tubular furnace, and introducing protective gas to calcine the bamboo blocks to obtain carbonized bamboo blocks; taking the carbonized bamboo blocks, grinding and crushing the bamboo blocks by using a crusher, and then screening to obtain bamboo charcoal; mixing the screened bamboo charcoal with KOH, adding ethanol for dissolving, and then drying; introducing protective gas, and activating and nursing the dried product; and soaking, washing and drying the product obtained by the activation treatment to obtain the porous biomass carbon. The high surface and the graded porous characteristic of the high surface are obtained by the preparation method, so that the application performance and the adsorption performance of the porous biomass carbon are improved; the process has the advantages of easy control, low cost and simple and convenient method, is suitable for industrial production, and has potential application value in the fields of adsorption, electrode materials, separation, sensing, gas storage, catalyst carriers and the like.)

1. The preparation method of the biomass charcoal material with high specific surface area and toluene adsorption function is characterized by comprising the following steps:

(1) Cleaning the surface of the alpine bamboo, drying and cutting to obtain bamboo blocks;

(2) Putting the obtained bamboo blocks into a crucible, feeding the crucible into a tubular furnace, and introducing protective gas to calcine the bamboo blocks to obtain carbonized bamboo blocks;

(3) Taking the carbonized bamboo blocks, grinding and crushing the bamboo blocks by using a crusher, and then screening to obtain bamboo charcoal;

(4) mixing the screened bamboo charcoal with KOH, adding ethanol for dissolving, and then drying;

(5) introducing protective gas, and activating and nursing the dried product;

(6) and soaking, washing and drying the product obtained by the activation treatment to obtain the porous biomass carbon.

2. the preparation method of the biomass charcoal material with the high specific surface area and the toluene adsorbing effect according to claim 1, wherein the drying temperature in the step (1) is 80-105 ℃.

3. The method for preparing biomass charcoal material with high specific surface area and toluene adsorbing effect according to claim 1, wherein the protective gas introduced in step (2) is one or more of nitrogen, helium, neon, argon, krypton or xenon.

4. The preparation method of biomass charcoal material with high specific surface area and toluene adsorbing effect according to claim 1, wherein the calcining is started after introducing protective gas for 15-20min in step (2).

5. The preparation method of the biomass charcoal material with the high specific surface area and the toluene adsorbing effect according to claim 4, wherein the temperature rise speed is 2-10 ℃/min, the calcination temperature is 350-600 ℃, and the heat preservation time is 1-3 h.

6. The preparation method of the biomass charcoal material with the high specific surface area and the toluene adsorbing function according to claim 1, wherein the bamboo charcoal with the size of 40-60 meshes is selected by screening in the step (3).

7. The preparation method of the biomass charcoal material with the toluene adsorbing effect according to claim 1, wherein in the step (4), the bamboo charcoal and KOH are dissolved in 50 wt% of ethanol at a mass ratio of 1: 1-1: 5, and the drying temperature is 80-105 ℃.

8. The method for preparing biomass charcoal material with high specific surface area and toluene adsorbing effect according to claim 1, wherein the protective gas introduced in step (5) is one or more of nitrogen, helium, neon, argon, krypton or xenon.

9. the preparation method of the biomass charcoal material with the toluene adsorbing effect and the high specific surface area according to claim 1, wherein the activating and calcining temperature in the step (5) is 750-850 ℃, the temperature rising speed is 1-5 ℃/min, and the heat preservation time is 2-4 h.

10. the preparation method of the biomass charcoal material with the high specific surface area and the toluene adsorbing effect according to claim 1, wherein the biomass charcoal material with the high specific surface area and the toluene adsorbing effect is soaked in 1M HCl in the step (6), washed to be neutral, and dried at a temperature of 80-105 ℃. The prepared biomass charcoal material has a hierarchical porous network microstructure.

Technical Field

The invention belongs to the technical field of biomass charcoal materials, and particularly relates to a preparation method of a biomass charcoal material with a high specific surface area and a toluene adsorption effect.

Background

The biomass is various organisms generated by utilizing the photosynthesis of air, water, land and the like, mainly refers to the matters such as lignocellulose of straws, trees and the like except grains and fruits, leftovers of agricultural product processing industry, agricultural and forestry wastes and the like in the production process of agriculture and forestry, and has the main characteristics of wide sources, low cost and regeneration, and the porous carbon material prepared by taking the biomass as the raw material has higher specific surface area and good adsorbability and wettability and is considered as an ideal choice of the adsorption material. However, the carbon materials obtained from different biomass raw materials have large morphology difference and greatly different performances, so that the carbon material obtained by selecting a proper biomass raw material has high specific surface area, high adsorption capacity, large specific capacitance and good cycling stability, and the preparation method is simple, low in cost and high in yield.

the emission of Volatile Organic Compounds (VOCs) has become one of the most serious environmental threats in many industrial processes. Large amounts of volatile organic compounds can be emitted in domestic or industrial processes, such as paints, printing, cleaning with organic solvents, the use of perfumes and industrial solvents. The presence of volatile organic compounds in the atmosphere is one of the major contributors to photochemical ozone and secondary organic aerosols, which can lead to health hazards and serious environmental problems. The most common concentration levels of released volatile organic compounds are at low ppm levels, where dynamic adsorption is a proven effective method of reducing volatile organic compounds. Microporous adsorbents are ideal adsorbents for the reduction of volatile organic compounds due to their low concentration. The most commonly used microporous materials are carbon materials (including biomass carbon materials, activated carbon, etc.).

However, the preparation of the porous carbon material is complicated at present, and most of the selected carbon source is organic, so that the cost is increased, and the preparation process causes harm to human bodies and secondary pollution to the environment. The biomass charcoal material has simple process, greatly reduces the production cost, does not cause physical damage to producers in the preparation process and does not cause secondary pollution, thereby being an ideal charcoal material. However, how to prepare a specific biomass charcoal material so as to be applied to the field of toluene adsorption is a technical problem to be solved urgently.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a preparation method of a biomass carbon material with high specific surface area and toluene adsorption effect, and the carbon material with rich micropores, large specific surface area and good adsorption performance is obtained by regulating a specific preparation method and process parameters.

The purpose of the invention can be realized by the following technical scheme:

the preparation method of the biomass charcoal material with high specific surface area and toluene adsorption function comprises the following steps:

(1) Cleaning the surface of the alpine bamboo, drying and cutting to obtain bamboo blocks;

(2) Putting the obtained bamboo blocks into a crucible, feeding the crucible into a tubular furnace, and introducing protective gas to calcine the bamboo blocks to obtain carbonized bamboo blocks;

(3) taking the carbonized bamboo blocks, grinding and crushing the bamboo blocks by using a crusher, and then screening to obtain bamboo charcoal;

(4) Mixing the screened bamboo charcoal with KOH, adding ethanol for dissolving, and then drying;

(5) introducing protective gas, and activating and nursing the dried product;

(6) And soaking, washing and drying the product obtained by the activation treatment to obtain the porous biomass carbon.

In the step (1), the drying temperature is 80-105 ℃.

And (3) introducing a protective gas in the step (2) which is one or more of nitrogen, helium, neon, argon, krypton or xenon.

and (3) introducing protective gas in the step (2) for 15-20min, and then starting to heat up for calcination.

The temperature rising speed is 2-10 ℃/min, the calcining temperature is 350-600 ℃, and the heat preservation time is 1-3 h.

And (3) screening and selecting bamboo charcoal with 40-60 meshes.

in the step (4), the bamboo charcoal and KOH are added in a mass ratio of 1: 1-1: 5, 50 wt% of ethanol is added for dissolution, and the drying temperature is 80-105 ℃.

And (3) introducing a protective gas in the step (5), wherein the protective gas is one or more of nitrogen, helium, neon, argon, krypton or xenon.

in the step (5), the activation and calcination temperature is 750-850 ℃, the temperature rise speed is 1-5 ℃/min, and the heat preservation time is 2-4 h.

And (6) soaking the biomass charcoal material in 1M HCl, washing the biomass charcoal material until the biomass charcoal material is neutral, and drying the biomass charcoal material at 80-105 ℃ to obtain the biomass charcoal material with a hierarchical porous network microstructure.

compared with the prior art, the invention has the following advantages:

1. The invention takes the biochar material as the carbon source, greatly reduces the preparation cost of the adsorbing material, does not cause secondary pollution at the same time, and plays a role in environmental protection.

2. According to the invention, bamboo charcoal is used as a carbon source to prepare the porous carbon with high specific surface area and hierarchical porous characteristic, and the specific activation temperature and the heat preservation time are controlled to greatly influence the surface area and the pore structure of the bamboo charcoal, so that the adsorbing material for VOCs is prepared, and the application range of the biomass charcoal material is expanded.

3. according to the invention, KOH is used as an activating agent to prepare the microporous carbon material, and the material can generate abundant micropores and increase the surface area under the specific temperature range, the ratio of KOH to the carbon material and the heat preservation time, so that the obtained material has a very great beneficial effect on the adsorption of toluene.

4. the biomass material prepared by the invention has potential application value in the fields of adsorption, electrode material, separation, sensing, gas storage, catalyst carrier and the like

Drawings

FIG. 1 is an electron micrograph of a product prepared in example 1.

FIG. 2 is an electron micrograph of a product prepared in example 2.

FIG. 3 is an electron micrograph of a product prepared in example 3.

FIG. 4 is an electron micrograph of a product prepared in example 4.

Detailed Description

The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.

the preparation method of the biomass charcoal material with high specific surface area and toluene adsorption function comprises the following steps:

(1) Washing the surface of the alpine bamboo by using deionized water, drying at 80-105 ℃, and then cutting the alpine bamboo into bamboo blocks with the size of about 20mm multiplied by 80 mm;

(2) Putting the obtained bamboo blocks into a crucible, feeding the bamboo blocks into a tube furnace, introducing nitrogen, helium, neon, argon, krypton or xenon and the like as protective gas, calcining the bamboo blocks to obtain carbonized bamboo blocks, specifically, heating the bamboo blocks for calcining after introducing the protective gas for 15-20min at the heating speed of 2-10 ℃/min at the calcining temperature of 350-600 ℃ for 1-3 h;

(3) Taking the carbonized bamboo blocks, grinding and crushing the bamboo blocks by using a crusher, and screening and selecting bamboo charcoal with 40-60 meshes;

(4) Mixing the screened bamboo charcoal with KOH according to the mass ratio of 1: 1-1: 5, adding 50 wt% of ethanol for dissolving, and then drying at the temperature of 80-105 ℃;

(5) introducing nitrogen, helium, neon, argon, krypton or xenon and the like as protective gases, and performing activation nursing on the dried product, wherein the activation and calcination temperature is 750-850 ℃, the heating rate is 1-5 ℃/min, and the heat preservation time is 2-4 h;

(6) and soaking and washing the product obtained by activation treatment by 1M HCl until the product is neutral, and drying the product at the temperature of 80-105 ℃ to obtain the porous biomass carbon. The prepared biomass charcoal material has a hierarchical porous network microstructure.

The following are more detailed embodiments, and the technical solutions and the technical effects obtained by the present invention will be further described by the following embodiments.