CN102249228B - Method for preparing activated carbon from pinecone - Google Patents
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- CN102249228B CN102249228B CN2011101586952A CN201110158695A CN102249228B CN 102249228 B CN102249228 B CN 102249228B CN 2011101586952 A CN2011101586952 A CN 2011101586952A CN 201110158695 A CN201110158695 A CN 201110158695A CN 102249228 B CN102249228 B CN 102249228B
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Abstract
本发明公开了一种用松塔制备活性炭的方法,具有以下步骤:①将松塔在100℃~120℃的温度下烘干20h~30h;②将步骤①的烘干后的松塔破碎至粒径为1mm~3mm,得到松塔颗粒;③将步骤②的松塔颗粒与氢氧化钾按照1∶1~1∶4的重量比混合,并加水使之浸渍20h~30h,而得到混合物料;④将步骤③的混合物料置于微波炉中进行炭化和活化,微波辐照功率为200W~700W,微波辐照时间为5min~10min,得到活化后的混合物料;⑤将步骤④的活化后的混合物料依次进行酸洗、水洗、烘干、研磨得到活性炭。本发明的方法原料廉价易得,降低了活性炭的生产成本。而且变废为宝,使得资源循环,促进低碳经济的发展。The invention discloses a method for preparing activated carbon by using pine cones. The particle size is 1mm ~ 3mm, to obtain pine cone particles; ③ mix the pine cone particles and potassium hydroxide in step ② according to the weight ratio of 1:1 ~ 1:4, and add water to make it soak for 20h ~ 30h, and obtain the mixed material ; ④ put the mixed material in step ③ into a microwave oven for carbonization and activation, the microwave irradiation power is 200W to 700W, and the microwave irradiation time is 5min to 10min to obtain the activated mixed material; ⑤ the activated mixed material in step ④ The mixed materials are sequentially pickled, washed with water, dried and ground to obtain activated carbon. The raw materials of the method of the invention are cheap and easy to obtain, and the production cost of activated carbon is reduced. Moreover, turning waste into wealth makes resource recycling and promotes the development of a low-carbon economy.
Description
技术领域 technical field
本发明涉及一种活性炭的制备方法,特别是涉及一种用松塔制备活性炭的方法。 The invention relates to a method for preparing activated carbon, in particular to a method for preparing activated carbon with a pine cone.
背景技术 Background technique
活性炭是一种极其重要的吸附剂,其优良的性能使之广泛应用于食品加工、制药、化工、石油炼制、生物工程、能源和环保等领域。活性炭在环保领域的应用主要是用于饮用水的纯化、废水的处理和吸附有毒有害气体。近年来,环境污染日趋严重,世界各国高度重视饮用水深度净化、废水处理、空气净化。而在我国,随着国家水质标准的提高,长三角、珠三角等地区已将活性炭净水工艺全部覆盖到县级自来水厂。因此国内外活性炭的市场前景都非常广阔。但昂贵的原材料和生产成本却使之价格居高不下,因此寻求制备活性炭的新原料具有现实意义和商业化前景。 Activated carbon is an extremely important adsorbent, and its excellent properties make it widely used in food processing, pharmaceuticals, chemicals, petroleum refining, bioengineering, energy and environmental protection and other fields. The application of activated carbon in the field of environmental protection is mainly used for the purification of drinking water, the treatment of waste water and the adsorption of toxic and harmful gases. In recent years, environmental pollution has become increasingly serious, and countries all over the world have attached great importance to the deep purification of drinking water, wastewater treatment, and air purification. In my country, with the improvement of national water quality standards, the Yangtze River Delta, Pearl River Delta and other regions have fully covered the activated carbon water purification process to county-level water plants. Therefore, the market prospect of activated carbon at home and abroad is very broad. However, expensive raw materials and production costs keep the price high, so seeking new raw materials for preparing activated carbon has practical significance and commercial prospects.
中国是世界上最大的活性炭生产国,活性炭的产量占世界产量的三分之一,现有制备活性炭的原材料主要是不可再生的和昂贵的资源,如煤和木材等,煤基活性炭占总产量的60%,木质活性炭占总产量的35%,果壳活性炭仅占总产量的5%。 China is the largest activated carbon producer in the world. The output of activated carbon accounts for one-third of the world's output. The raw materials for preparing activated carbon are mainly non-renewable and expensive resources, such as coal and wood. Coal-based activated carbon accounts for the total output. 60% of the total output, wood activated carbon accounted for 35% of the total output, and shell activated carbon accounted for only 5% of the total output.
目前国内外尚未见有利用松塔制备活性炭的报道。 At present, there are no reports of using pine cones to prepare activated carbon at home and abroad.
发明内容 Contents of the invention
本发明的目的在于解决上述问题,提供一种生产成本低的用松塔制备活性炭的方法。 The purpose of the present invention is to solve the above problems, and a method for preparing gac with a pine cone with low production cost is provided.
实现本发明目的的技术方案是:一种用松塔制备活性炭的方法,具有以下步骤:①将松塔在100℃~120℃的温度下烘干20h~30h;②将步骤①的烘干后的松塔破碎至粒径为1mm~3mm,得到松塔颗粒;③将步骤②的松塔颗粒与氢氧化钾按照1∶1~1∶4的重量比混合,并加水使之浸渍20h~30h,而得到混合物料;④将步骤③的混合物料置于微波炉中进行炭化和活化,微波辐照功率为200W~700W,微波辐照时间为5min~10min,得到活化后的混合物料;⑤将步骤④的活化后的混合物料依次进行酸洗、水洗、烘干、研磨得到活性炭。 The technical solution for realizing the object of the present invention is: a method for preparing activated carbon with pine cones, which has the following steps: 1. drying the pine cones at a temperature of 100°C to 120°C for 20h to 30h; The pine cone is crushed to a particle size of 1 mm to 3 mm to obtain pine cone particles; ③ the pine cone particles in step ② are mixed with potassium hydroxide in a weight ratio of 1:1 to 1:4, and water is added to impregnate it for 20h to 30h , to obtain the mixed material; ④ place the mixed material in step ③ in a microwave oven for carbonization and activation, the microwave irradiation power is 200W to 700W, and the microwave irradiation time is 5min to 10min to obtain the activated mixed material; ⑤ put the step ④ The activated mixed material is sequentially pickled, washed, dried, and ground to obtain activated carbon.
上述步骤③中所述的松塔颗粒与氢氧化钾的重量比为1∶3~1∶4。 The weight ratio of the pine cone particles described in the above step 3. to potassium hydroxide is 1: 3~1: 4.
上述步骤④中所述的微波辐照功率为280W~600W,微波辐照时间为7min~9min。 The microwave irradiation power in the above step ④ is 280W-600W, and the microwave irradiation time is 7min-9min.
上述步骤⑤中所述的酸洗是用体积比为1∶10的盐酸在80℃~100℃下煮20min~40min。 The pickling described in the above step ⑤ is to use hydrochloric acid with a volume ratio of 1:10 at 80°C to 100°C for 20min to 40min.
上述步骤⑤中所述的水洗是用蒸馏水将酸洗后的物料漂洗至pH为6.5~7.5。 The water washing described in the above step ⑤ is to rinse the pickled material with distilled water until the pH is 6.5-7.5.
上述步骤①中的松塔优选取自东北地区的经自然风干的红松松塔。 The pine cone in the above-mentioned steps 1. is preferably taken from the naturally air-dried Korean pine cone in Northeast China.
本发明具有的积极效果:本发明首次利用了松塔来制备活性炭,不仅原料廉价易得,降低了活性炭的生产成本。由于在加工完松子后,松塔常常被扔掉,因此本发明还变废为宝,使得资源循环,促进低碳经济的发展。 The present invention has positive effects: the present invention uses pine cones to prepare activated carbon for the first time, not only the raw materials are cheap and easy to obtain, but also the production cost of activated carbon is reduced. Since the pine cones are often thrown away after the pine nuts are processed, the invention also turns wastes into treasures, recycles resources and promotes the development of low-carbon economy.
具体实施方式 Detailed ways
(实施例1) (Example 1)
实施例的活性炭的制备方法具有以下步骤: The preparation method of the gac of embodiment has the following steps:
①将取自东北地区的经自然风干的红松松塔在108℃的温度下烘干24h。 ①The naturally air-dried Korean pine cones from Northeast China were dried at 108°C for 24 hours.
②将步骤①的烘干后的松塔破碎至粒径为2mm左右,得到松塔颗粒。 ② crushing the dried pine cones in step ① to a particle size of about 2 mm to obtain pine cone particles.
③取8g步骤②的松塔颗粒与24g的KOH颗粒混合,加50ml水搅拌均匀,浸渍24h后得到混合物料。 ③Take 8g of pine cone granules from step ② and mix them with 24g of KOH granules, add 50ml of water and stir evenly, and soak for 24 hours to get the mixed material.
④将步骤③的混合物料置于微波炉中在300W的微波辐照功率下炭化、活化9min,得到活化后的混合物料。 ④ Put the mixed material in step ③ into a microwave oven for carbonization and activation for 9 minutes under the microwave irradiation power of 300W to obtain the activated mixed material.
⑤将步骤④的活化后的混合物料先用体积比为1∶10的盐酸(是指36wt%的浓盐酸的体积与水的体积之比)在90℃下煮30min,然后用蒸馏水漂洗至pH为7,再在120℃的温度下烘干,最后研磨至200目得到活性炭。该活性炭的碘吸附值为1253mg/g。 ⑤ Cook the activated mixed material in step ④ with hydrochloric acid with a volume ratio of 1:10 (referring to the volume ratio of 36wt% concentrated hydrochloric acid to water volume) at 90°C for 30 minutes, then rinse with distilled water to pH 7, then dried at 120°C, and finally ground to 200 mesh to obtain activated carbon. The iodine adsorption value of this activated carbon was 1253 mg/g.
(实施例2) (Example 2)
实施例的活性炭的制备方法具有以下步骤: The preparation method of the gac of embodiment has the following steps:
①将取自东北地区的经自然风干的红松松塔在108℃的温度下烘干24h。 ①The naturally air-dried Korean pine cones from Northeast China were dried at 108°C for 24 hours.
②将步骤①的烘干后的松塔破碎至粒径为2mm左右,得到松塔颗粒。 ② crushing the dried pine cones in step ① to a particle size of about 2 mm to obtain pine cone particles.
③取8g步骤②的松塔颗粒与24g的KOH颗粒混合,加50ml水搅拌均匀,浸渍24h后得到混合物料。 ③Take 8g of pine cone granules from step ② and mix them with 24g of KOH granules, add 50ml of water and stir evenly, and soak for 24 hours to get the mixed material.
④将步骤③的混合物料置于微波炉中在560W的微波辐照功率下炭化、活化9min,得到活化后的混合物料。 ④ Put the mixed material in step ③ into a microwave oven for carbonization and activation for 9 minutes under the microwave irradiation power of 560W to obtain the activated mixed material.
⑤将步骤④的活化后的混合物料先用体积比为1∶10的盐酸(是指36wt%的浓盐酸的体积与水的体积之比)在90℃下煮30min,然后用蒸馏水漂洗至pH为7,再在120℃的温度下烘干,最后研磨至200目得到活性炭。该活性炭的碘吸附值为1424mg/g。 ⑤ Cook the activated mixed material in step ④ with hydrochloric acid with a volume ratio of 1:10 (referring to the volume ratio of 36wt% concentrated hydrochloric acid to the volume of water) at 90°C for 30 minutes, then rinse with distilled water to pH 7, then dried at 120°C, and finally ground to 200 mesh to obtain activated carbon. The iodine adsorption value of this activated carbon was 1424 mg/g.
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