CN102381703B - Method for preparing activated carbon by using flax straws - Google Patents

Method for preparing activated carbon by using flax straws Download PDF

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CN102381703B
CN102381703B CN 201110210898 CN201110210898A CN102381703B CN 102381703 B CN102381703 B CN 102381703B CN 201110210898 CN201110210898 CN 201110210898 CN 201110210898 A CN201110210898 A CN 201110210898A CN 102381703 B CN102381703 B CN 102381703B
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activated carbon
flax
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active carbon
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CN102381703A (en
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陈燕丹
陈卫群
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Fujian Agriculture and Forestry University
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Abstract

The invention discloses a method for preparing activated carbon by using flax straws. The method comprises the following technological processes of: performing treatments of peeling, crushing, sieving through a 40-mesh screen, drying for 12-24h at 105-120 DEG C and the like on the flax straws to obtain absolute dry pretreated materials, uniformly mixing the absolute dry pretreated materials with an activator solution, impregnating for 4-12h at room temperature, then drying for 12-24h at 105-120 DEG C, placing in a muffle furnace, heating to 700-900 DEG C, preserving the heat for 1-3h, naturally cooling to room temperature, and then performing acid cleaning, water washing, drying, grinding, and sieving through a 200-mesh screen to obtain a finished product of powdery activated carbon. In the method, the flax straws are used as raw materials, a novel activator with low impregnation ratio is adopted to prepare the activated carbon with special performance. In addition, the activated carbon with favorable performance is prepared by means of multiple activation functions induced by an activator high-temperature pyrolysis effect in the method, so that the dose of the activator and the production cost are reduced, and the obvious economic and social benefits are achieved.

Description

一种用麻杆制备活性炭的方法A kind of method of preparing activated carbon with hemp stalk

技术领域 technical field

 本发明涉及一种用麻杆制备活性炭的方法,特别涉及一种钾盐为活化剂制备活性炭的方法,属于粉末活性炭的制备技术领域。 The invention relates to a method for preparing activated carbon with hemp stalks, in particular to a method for preparing activated carbon with potassium salt as an activator, which belongs to the technical field of powdered activated carbon preparation.

背景技术 Background technique

活性炭作为一种具有特殊微晶结构、发达孔隙结构、高比表面积和较强吸附能力的含碳材料。其化学稳定性好,具有耐酸、耐碱、耐高温等特点,人们对活性炭的研究及应用开发越来越多。要满足制得的活性炭性能稳定、成本低廉等要求,原材料必须质量稳定、容易获取,同时要求生产工艺简单、经济、环保。开发低级活性炭的用途及利用特殊的废弃物以发现特殊的机能等就成了重要研究课题。目前活性炭的研究有几种趋势:一是制备应用量大、使用面广、性能一般且价格低廉的活性炭;二是制备性能优良、具有特殊用途的高性能活性炭;三是开发节能高效且环保的活性炭。合理地利用丰富的农林废弃物不仅可以达到保护环境的目的,还可以带来较高的附加价值,对于发展可持续经济、实现资源再生也有着重要意义。 Activated carbon is a carbonaceous material with special microcrystalline structure, developed pore structure, high specific surface area and strong adsorption capacity. It has good chemical stability and has the characteristics of acid resistance, alkali resistance and high temperature resistance. There are more and more researches and application developments on activated carbon. To meet the requirements of stable performance and low cost of the prepared activated carbon, the raw materials must be of stable quality and easy to obtain, and the production process must be simple, economical and environmentally friendly. The development of the use of low-grade activated carbon and the use of special waste to discover special functions have become important research topics. At present, there are several trends in the research of activated carbon: one is to prepare activated carbon with large application, wide range of use, general performance and low price; the other is to prepare high-performance activated carbon with excellent performance and special purpose; Activated carbon. Rational use of abundant agricultural and forestry wastes can not only achieve the purpose of protecting the environment, but also bring higher added value, which is also of great significance to the development of sustainable economy and the realization of resource regeneration.

利用农林废弃物麻杆制备活性炭有很多研究报道,Soheil Aber等采用K2HPO4为活化剂制备红麻基活性炭纤维,研究其对苯酚和硝基苯酚的吸附,结果表明Langmuir吸附等温线能更好的和实验数据相吻合。Michio Inagaki等采用水蒸气活化法制备出高比表面积的红麻基活性炭。Eduardo M.Cuerda-Correa 等以红麻为原料制备出孔隙结构发达的红麻活性炭纤维。公开号为CN 101181993B的发明专利公开了一种麻杆活性炭及其制备方法,该方法以麻杆为原料制备出具有优异吸附性能的颗粒活性炭,比表面积达4800m2/g,苯吸附值达120mg/g。采用低浓度高锰酸钾作为活化剂,在极低活化剂和原料浸渍比条件下制备活性炭的相关研究尚未见报道。寻求新型高效的功能活化剂,不仅可降低活性炭生产成本,减少污染,还能同步赋予活性炭更加突出的功能,对活性炭的制备具有重要意义。 There are many research reports on the preparation of activated carbon from agricultural and forestry waste hemp stalks. Soheil Aber et al. used K 2 HPO 4 as the activator to prepare kenaf-based activated carbon fibers, and studied the adsorption of phenol and nitrophenol. The results showed that the Langmuir adsorption isotherm can be more accurate. It is in good agreement with the experimental data. Michio Inagaki et al prepared kenaf-based activated carbon with high specific surface area by steam activation method. Eduardo M. Cuerda-Correa et al. used kenaf as raw material to prepare kenaf activated carbon fibers with developed pore structure. The invention patent with the publication number CN 101181993B discloses a hemp stalk activated carbon and its preparation method. The method uses hemp stalks as raw materials to prepare granular activated carbon with excellent adsorption performance, with a specific surface area of 4800m 2 /g and a benzene adsorption value of 120mg /g. Using low concentration of potassium permanganate as the activator, the research on the preparation of activated carbon under the condition of extremely low activator and raw material impregnation ratio has not been reported yet. The search for new and efficient functional activators can not only reduce the production cost of activated carbon and reduce pollution, but also give activated carbon more prominent functions at the same time, which is of great significance to the preparation of activated carbon.

发明内容 Contents of the invention

本发明的目的在于提供一种用麻杆制备活性炭的方法,它是一种用麻杆作为原料,采用低浸渍比的新型活化剂制备专用性能的活性炭的方法。该方法是利用活化剂热分解作用引起多重活化功能来制备优良性能的活性炭,减少活化剂的用量,降低生产成本,具有显著的经济和社会效益。 The object of the present invention is to provide a kind of method for preparing gac with hemp stalk, it is a kind of method with hemp stalk as raw material, adopts the novel activator of low impregnation ratio to prepare the gac of special performance. The method utilizes thermal decomposition of the activator to cause multiple activation functions to prepare activated carbon with excellent performance, reduces the consumption of the activator, lowers the production cost, and has significant economic and social benefits.

为实现上述目的,本发明采用如下技术方案: To achieve the above object, the present invention adopts the following technical solutions:

(1)预处理:将红麻或黄麻通过剥皮、粉碎、过40目数筛网、105~120℃干燥12-24h等处理得到预处理绝干料,与质量浓度为0.2~1.0%的高锰酸钾溶液按质量比为1~6:100混合均匀,室温浸渍4~12h后105~120℃烘干12-24h得混合料。 (1) Pretreatment: Peel kenaf or jute, pass through a 40-mesh sieve, and dry at 105~120°C for 12-24 hours to obtain pretreated absolute dry material, with a mass concentration of 0.2~1.0% high Potassium manganate solution is mixed evenly according to the mass ratio of 1~6:100, impregnated at room temperature for 4~12h, and then dried at 105~120°C for 12-24h to obtain the mixture.

(2)炭化活化处理:将步骤(1)所述的混合料置于马弗炉中,以5~10℃/min的速度升温至700~900℃,保温1~3h,保温期间温差小于±15℃,自然冷却至室温得炭化活化样。 (2) Carbonization activation treatment: put the mixture described in step (1) in a muffle furnace, raise the temperature to 700-900°C at a rate of 5-10°C/min, keep it warm for 1-3h, and the temperature difference during the hold is less than ± 15°C, naturally cooled to room temperature to obtain carbonized activated samples.

(3)后处理:将步骤(2)所述的炭化活化样用质量分数为5~10%的HCl溶液在70~90℃蒸煮30~60min,然后用去离子水反复洗至pH为6~7、105~120℃干燥12-24h,最后研磨、过200目数筛网得粉末活性炭成品。 (3) Post-treatment: Cook the carbonized activated sample described in step (2) with HCl solution with a mass fraction of 5-10% at 70-90°C for 30-60 min, and then wash repeatedly with deionized water until the pH is 6-6 7. Dry at 105-120°C for 12-24 hours, finally grind and pass through a 200-mesh sieve to obtain the finished powder activated carbon.

按照国家标准GB/T 12496.10-1999和GB/T 12496.8-1999规定活性炭试验方法检测,本发明制备的麻杆芯活性炭碘吸附值800~950mg/g,亚甲基蓝吸附值120~270mg/g。 According to the national standard GB/T 12496.10-1999 and GB/T 12496.8-1999 regulated activated carbon test method, the hemp core activated carbon prepared by the present invention has an iodine adsorption value of 800-950 mg/g, and a methylene blue adsorption value of 120-270 mg/g.

本方法的显著优点在于: The significant advantages of this method are:

(1)采用储量丰富的非木材纤维资源红麻为原料,合理的利用农林废弃物资源,节约了资源,保护了环境。 (1) Using kenaf, a non-wood fiber resource with abundant reserves, as raw material, rationally utilizing agricultural and forestry waste resources, saving resources and protecting the environment.

(2)采用高锰酸钾为活化剂制备了优良吸附性能的活性炭,碘吸附值800~950mg/g,亚甲基蓝吸附值120~270mg/g。 (2) Potassium permanganate was used as the activator to prepare activated carbon with excellent adsorption performance, with iodine adsorption value of 800-950 mg/g and methylene blue adsorption value of 120-270 mg/g.

(3)采用高锰酸钾为活化剂,活化剂用量很少,减少了污染物的产生,活化剂无需回收,节省了生产周期,提高生产效率,降低了生产成本。 (3) Potassium permanganate is used as the activator, the amount of activator is small, the generation of pollutants is reduced, the activator does not need to be recycled, the production cycle is saved, the production efficiency is improved, and the production cost is reduced.

附图说明 Description of drawings

图1为本发明所得的麻杆芯活性炭的场发射扫描电镜图(放大倍率×4000)。 Fig. 1 is the field emission scanning electron microscope image (magnification × 4000) of the hemp stalk core activated carbon obtained in the present invention.

图2为本发明所得的麻杆芯活性炭的场发射扫描电镜图(放大倍率×100000)。 Fig. 2 is a field emission scanning electron micrograph (magnification × 100000) of the hemp stalk core activated carbon obtained in the present invention.

具体实施方式 Detailed ways

实施例1Example 1

将红麻或黄麻通过剥皮、粉碎、过40目数筛网、105℃干燥12h等处理得到预处理绝干料称20g,与质量浓度为0.2%的高锰酸钾溶液按质量比为2:100混合均匀,室温浸渍12h后105℃烘干24h得混合料。然后将混合料置于马弗炉中,以5℃/min的速度升温至800℃,保温120min,保温期间温差小于±15℃,自然冷却至室温得炭化活化样。最后将炭化活化样用质量分数为5%的HCl溶液在70℃蒸煮30min,然后用去离子水反复洗至pH为6~7、105℃干燥24h,最后研磨、过200目数筛网得粉末活性炭成品。 The kenaf or jute is peeled, crushed, passed through a 40-mesh sieve, and dried at 105°C for 12 hours to obtain a pretreated dry material weighing 20g, and the mass ratio of the potassium permanganate solution with a mass concentration of 0.2% is 2: 100 and mix evenly, impregnate at room temperature for 12 hours, then dry at 105°C for 24 hours to obtain a mixture. Then put the mixture in a muffle furnace, raise the temperature to 800°C at a rate of 5°C/min, keep it warm for 120 minutes, the temperature difference during the heat preservation period is less than ±15°C, and cool naturally to room temperature to obtain a carbonized activated sample. Finally, the carbonized activated sample was cooked with 5% HCl solution at 70°C for 30 minutes, then repeatedly washed with deionized water until the pH was 6~7, dried at 105°C for 24 hours, finally ground, and passed through a 200-mesh sieve to obtain a powder Activated carbon finished product.

实施例2Example 2

将红麻或黄麻通过剥皮、粉碎、过40目数筛网、120℃干燥12h等处理得到预处理绝干料称20g,与质量浓度为0.6%的高锰酸钾溶液按质量比为1:100混合均匀,室温浸渍8h后120℃烘干12h得混合料。然后将混合料置于马弗炉中,以10℃/min的速度升温至900℃,保温60min,保温期间温差小于±15℃,自然冷却至室温得炭化活化样。最后将炭化活化样用质量分数为10%的HCl溶液在90℃蒸煮60min,然后用去离子水反复洗至pH为6~7、120℃干燥12h,最后研磨、过200目数筛网得粉末活性炭成品。 The kenaf or jute is peeled, crushed, passed through a 40-mesh sieve, and dried at 120°C for 12 hours to obtain a pretreated absolute dry material weighing 20g, and the mass ratio of the potassium permanganate solution with a mass concentration of 0.6% is 1: 100 and mix evenly, impregnate at room temperature for 8 hours, then dry at 120°C for 12 hours to obtain a mixture. Then put the mixture in a muffle furnace, raise the temperature to 900°C at a rate of 10°C/min, hold it for 60 minutes, and keep the temperature difference less than ±15°C during the hold, and cool it down to room temperature naturally to obtain a carbonized activated sample. Finally, the carbonized activated sample was digested with 10% HCl solution at 90°C for 60 minutes, then repeatedly washed with deionized water until the pH was 6~7, dried at 120°C for 12 hours, finally ground, and passed through a 200-mesh sieve to obtain a powder Activated carbon finished product.

实施例3Example 3

将红麻或黄麻通过剥皮、粉碎、过40目数筛网、110℃干燥12h等处理得到预处理绝干料称20g,与质量浓度为1.0%的高锰酸钾溶液按质量比为6:100混合均匀,室温浸渍4h后108℃烘干18h得混合料。然后将混合料置于马弗炉中,以8℃/min的速度升温至700℃,保温180min,保温期间温差小于±15℃,自然冷却至室温得炭化活化样。最后将炭化活化样用质量分数为8%的HCl溶液在80℃蒸煮45min,然后用去离子水反复洗至pH为6~7、108℃干燥20h,最后研磨、过200目数筛网得粉末活性炭成品。 The kenaf or jute is peeled, crushed, passed through a 40-mesh sieve, and dried at 110°C for 12 hours to obtain a pretreated dry material weighing 20g, and the mass ratio of the potassium permanganate solution with a mass concentration of 1.0% is 6: 100, mix evenly, soak at room temperature for 4 hours, then dry at 108°C for 18 hours to obtain a mixture. Then put the mixture in a muffle furnace, raise the temperature to 700°C at a rate of 8°C/min, hold it for 180 minutes, and keep the temperature difference less than ±15°C during the hold, and cool it down to room temperature naturally to obtain a carbonized activated sample. Finally, the carbonized activated sample was cooked with 8% HCl solution at 80°C for 45min, then repeatedly washed with deionized water until the pH was 6~7, dried at 108°C for 20h, finally ground, and passed through a 200-mesh sieve to obtain a powder Activated carbon finished product.

实施例4Example 4

按照国家标准GB/T 12496.10-1999和GB/T 12496.8-1999规定测定制备的麻杆芯活性炭。 According to the national standard GB/T 12496.10-1999 and GB/T 12496.8-1999, the activated carbon with hemp core was measured.

结果表明:本发明制备的麻杆芯活性炭碘吸附值800~950mg/g,亚甲基蓝吸附值120~270mg/g。 The results show that the iodine adsorption value of the hemp stalk core activated carbon prepared by the invention is 800-950 mg/g, and the methylene blue adsorption value is 120-270 mg/g.

实施例5Example 5

用高分辨场发射扫描电镜观测本发明制备的麻杆芯活性炭。 The hemp stalk core activated carbon prepared by the present invention was observed with a high-resolution field emission scanning electron microscope.

结果表明:本发明制备的麻杆芯活性炭为中孔较发达的活性炭。 The results show that the hemp stalk core activated carbon prepared by the present invention is an activated carbon with well-developed mesopores.

以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。 The above descriptions are only preferred embodiments of the present invention, and all equivalent changes and modifications made according to the scope of the patent application of the present invention shall fall within the scope of the present invention.

Claims (6)

1. one kind prepares process of active carbon with waste of flax, it is characterized in that concrete steps are following:
(1) pre-treatment: waste of flax is obtained pre-treatment over dry material through peeling, pulverizing, after crossing 40 order number sieve nets, 105 ~ 120 ℃ of dry 12-24h, mix with activator solution, 105 ~ 120 ℃ of oven dry 12-24h get compound behind room temperature dipping 4 ~ 12h;
(2) carbonization-activation is handled: the described compound of step (1) is placed retort furnace, be warming up to 700 ~ 900 ℃, naturally cool to room temperature behind insulation 1 ~ 3h and get carbonization-activation appearance;
(3) aftertreatment: the described carbonization-activation appearance of step (2) is got the Powdered Activated Carbon finished product through pickling, washing, oven dry, grinding, mistake 200 order number sieve nets;
The described acvator of step (1) is a potassium permanganate, and the mass concentration of potassium permanganate solution is 0.2 ~ 1.0%;
Step (1) described pre-treatment over dry material and activator solution are that 1 ~ 6:100 mixes by mass ratio.
2. according to claim 1ly prepare process of active carbon with waste of flax, it is characterized in that: the described waste of flax of step (1) is bluish dogbane or jute.
3. according to claim 1ly prepare process of active carbon with waste of flax, it is characterized in that: the described heat-up rate of step (2) is 5 ~ 10 ℃/min, and the temperature difference is less than ± 15 ℃ between soak.
4. according to claim 1ly prepare process of active carbon with waste of flax, it is characterized in that: the described pickling of step (3) is that carbonization-activation appearance is used massfraction is that 5 ~ 10% HCl solution is at 70 ~ 90 ℃ of boiling 30 ~ 60min.
5. according to claim 1ly prepare process of active carbon with waste of flax, it is characterized in that: the described washing of step (3) is that to use deionized water to be washed till pH repeatedly be 6 ~ 7.
6. according to claim 1ly prepare process of active carbon with waste of flax, it is characterized in that: 105 ~ 120 ℃ of the described drying temperatures of step (3), be 12-24h time of drying.
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红麻杆芯活性炭的制备及其孔结构;陈燕丹等;《河南科技大学学报: 自然科学版》;20100228;第31卷(第1期);第70-73页 *
陈燕丹等.红麻杆芯活性炭的制备及其孔结构.《河南科技大学学报: 自然科学版》.2010,第31卷(第1期),第70-73页.

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