微波法玉米秸秆活性炭制备与应用研究
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摘要
我国是农业大国,农业资源废料和副产品产生量巨大。农业废料在生产过程中由于可利用品位不高,成分复杂,二次开发成本高、难度大,同时缺乏政策的引导和资金的投入,导致农业废料污染呈现出数量大、品质差、危害多的特点,目前这些废料大多被随意丢弃在农田,或是被直接燃烧掉了,不仅造成资源的大量浪费,还会产生严重的环境污染,特别是大气污染。因此农业废料已成为社会一大公害,开展农业废弃物的资源化综合利用具有重要的现实意义。
本研究是以农业废料中的玉米秸秆为原料,利用微波加热化学活化的方法将其转化为优质活性炭的方法。研究了主要操作条件(活化剂与原料的浸泡比例、活化剂浓度、活化剂浸渍时间、微波功率、辐照时间)对活性炭吸附能力的影响,以正交实验方法得出活性炭生产的最佳工艺条件,并将实验产品用于对二级生化处理出水的吸附。
通过制备与吸附实验,以氯化锌为活化剂,微波法玉米秸秆活性炭的制备条件中各因素对产品碘值的影响顺序从大到小为:固液比,活化剂浓度,浸渍时间,微波功率,辐照时间;对产品亚甲基蓝吸附值的影响顺序从大到小为:固液比,微波功率,活化剂浓度,微波辐照时间,浸渍时间;对玉米秸秆活性炭产率的影响从大到小依此是:微波功率,固液比,微波辐照时间,活化剂浓度,浸渍时间。最佳制备条件为微波功率595W,活化剂氯化锌浸渍浓度为40%,微波辐照时间为9min,浸渍时间为24h,固液比为1:3.0。以磷酸为活化剂时,各因素对玉米秸秆活性炭碘值的影响从大到小依此是:微波功率,活化剂浓度,辐照时间,浸渍时间;对玉米秸秆活性炭亚甲基蓝吸附值的影响从大到小依此是:微波功率,活化剂浓度,微波辐照时间,浸渍时间;对玉米各因素对玉米秸秆活性炭产率的影响从大到小依此是:微波功率,活化剂浓度,浸渍时间,微波辐照时间。最佳制备条件为微波功率595W,活化剂磷酸浓度为50%,微波辐照时间为8min,浸渍时间为36h。
通过对微波氯化锌法制备的活性炭对二级出水中的COD与P作静态吸附实验的研究,考察了活性炭投加量,吸附平衡时间,废水的pH值三种因素对吸附效果的影响,并以弗兰德利希模型作吸附等温线。结果表明对COD的吸附,最佳吸附条件是:活性炭投加量不少于14g/L,吸附平衡时间40min,pH控制为5至7之间,吸附容量为4.127mg/g。对污水厂二级出水中的P进行吸附,最佳的吸附条件是:活性炭投加量不小于3g/L,吸附平衡时间为90min,溶液pH值控制在3～7之间,吸附后P浓度为0.2728mg/g。
以农业废弃物为原料,采用微波加热化学活化法制备活性炭不仅可以解决农业废弃物的回收再利用问题,拓宽活性炭生产的原料来源,还为污水厂的污水深度处理提供了新的尝试与材料,具有较好的社会经济和环境效益。
Our country is the Great Power of agriculture, the agricultural waste material and by-product creation amounts are enormous, for the low grade of usage, complicated components, high redevelopment cost and degree of difficulty, while shorting of policy guidance and fund, the agriculture waste material have the characteristics such as big quantity, bad quality and more dangerous. At present, these waste material is abandoned at the farmland mostly, or burned away directly, not only bringing about large amount of dissipation of resource, but also may produce grave environmental pollution, especially air pollution, therefore, the agriculture waste material already becomes one big social effects of pollution, the resource comprehensive utilization carrying out agriculture waste's has important practical significancy.
This study takes corn stalk of agriculture waste material as raw material, by using microwave changes agriculture waste material into high grade activated carbon. Study at the main conditions, which affecting the adsorption ability of activated carbon such as (the dipping proportions of activating agent and raw material, the concentration of activating agent, activator dipping time, microwave power、microwave irradiation time). Reaches the best technological conditions through activated carbon produce with orthogonality experiment, and apply the product into the experiment for the adsorption of secondary effluent.
Through preparation and the adsorption experiment, with zinc chloride as activating agent, factors conclusions for iodine value is in proper order big by as follows: the dipping proportions of activating agent and raw material, the concentration of activating agent, activator dipping time, microwave power, and radiation time; The effect order to methylene adsorption value is max by: the dipping proportions of activating agent and raw material, microwave power, radiation time, activator dipping time; the effect to corn stalk activated carbon yield order big by: microwave power, the dipping proportions of activating agent and raw material, microwave irradiation time, the concentration of activating agent, activator dipping time. The best preparation condition is microwave power 595 W, concentration of activating agent chlorinating zinc is 40% , radiation time is 9 minutes, dipping time is 24 hours , the proportions of raw material and activating agent is 1: 3.0. While taking phosphoric acid as activating agent, the impact of every factor over corn stalk activated carbon iodine value is in proper order large by: Microwave power , concentration of activating agent, radiation time, dipping time; The effect for methtylene blue Decolourizing ability of corn stalk activated carbon value is in proper order by: Microwave power, concentration of activating agent, radiation time, dipping time; each factor over corn stalk activated carbon yield is in proper order by: Microwave power , concentration of activating agent, dipping time ,radiation time. The best preparation condition is microwave power 595 W, concentration of activating agent chlorinating zinc is 50%, radiation time is 8 minutes , steep time in water being 36 hours.
Using activated carbon that prepared by microwave radiating, with chlorinating zinc, do the research of adsorption experiment by COD and P in secondary effluent. Inspected the impact of activated carbon adding amounts, adsorbing balance time, the pH value of waste water over adsorption effect, under the adsorption isothermal line model of Freundich. Result indicates an best adsorbs condition to COD is as follows: Activated carbon adding amounts can not less than 14 g/L, adsorb balancing time is 40 minutes, pH value being controlled between 5 to 7, adsorption amounts are 4.127mg/g. The adsorption of P in secondary effluent, optimum adsorption condition is: Activated carbon adding amounts not being smaller than 3g/L, adsorption balance time is 90 minutes, pH value being controlled between 3 to 7, adsorption amounts are 0.2728 mg/g.
Using agricultural material as raw material, and by microwaving with activating agent, the produced activated carbon not only solve the problems of recycle and reuse agricultural byproducts and widen the resources of the raw material of activated carbon, but also provide the new materials for the polishing process. So the manufactures are god for social and environment.
本研究是以农业废料中的玉米秸秆为原料,利用微波加热化学活化的方法将其转化为优质活性炭的方法。研究了主要操作条件(活化剂与原料的浸泡比例、活化剂浓度、活化剂浸渍时间、微波功率、辐照时间)对活性炭吸附能力的影响,以正交实验方法得出活性炭生产的最佳工艺条件,并将实验产品用于对二级生化处理出水的吸附。
通过制备与吸附实验,以氯化锌为活化剂,微波法玉米秸秆活性炭的制备条件中各因素对产品碘值的影响顺序从大到小为:固液比,活化剂浓度,浸渍时间,微波功率,辐照时间;对产品亚甲基蓝吸附值的影响顺序从大到小为:固液比,微波功率,活化剂浓度,微波辐照时间,浸渍时间;对玉米秸秆活性炭产率的影响从大到小依此是:微波功率,固液比,微波辐照时间,活化剂浓度,浸渍时间。最佳制备条件为微波功率595W,活化剂氯化锌浸渍浓度为40%,微波辐照时间为9min,浸渍时间为24h,固液比为1:3.0。以磷酸为活化剂时,各因素对玉米秸秆活性炭碘值的影响从大到小依此是:微波功率,活化剂浓度,辐照时间,浸渍时间;对玉米秸秆活性炭亚甲基蓝吸附值的影响从大到小依此是:微波功率,活化剂浓度,微波辐照时间,浸渍时间;对玉米各因素对玉米秸秆活性炭产率的影响从大到小依此是:微波功率,活化剂浓度,浸渍时间,微波辐照时间。最佳制备条件为微波功率595W,活化剂磷酸浓度为50%,微波辐照时间为8min,浸渍时间为36h。
通过对微波氯化锌法制备的活性炭对二级出水中的COD与P作静态吸附实验的研究,考察了活性炭投加量,吸附平衡时间,废水的pH值三种因素对吸附效果的影响,并以弗兰德利希模型作吸附等温线。结果表明对COD的吸附,最佳吸附条件是:活性炭投加量不少于14g/L,吸附平衡时间40min,pH控制为5至7之间,吸附容量为4.127mg/g。对污水厂二级出水中的P进行吸附,最佳的吸附条件是:活性炭投加量不小于3g/L,吸附平衡时间为90min,溶液pH值控制在3～7之间,吸附后P浓度为0.2728mg/g。
以农业废弃物为原料,采用微波加热化学活化法制备活性炭不仅可以解决农业废弃物的回收再利用问题,拓宽活性炭生产的原料来源,还为污水厂的污水深度处理提供了新的尝试与材料,具有较好的社会经济和环境效益。
Our country is the Great Power of agriculture, the agricultural waste material and by-product creation amounts are enormous, for the low grade of usage, complicated components, high redevelopment cost and degree of difficulty, while shorting of policy guidance and fund, the agriculture waste material have the characteristics such as big quantity, bad quality and more dangerous. At present, these waste material is abandoned at the farmland mostly, or burned away directly, not only bringing about large amount of dissipation of resource, but also may produce grave environmental pollution, especially air pollution, therefore, the agriculture waste material already becomes one big social effects of pollution, the resource comprehensive utilization carrying out agriculture waste's has important practical significancy.
This study takes corn stalk of agriculture waste material as raw material, by using microwave changes agriculture waste material into high grade activated carbon. Study at the main conditions, which affecting the adsorption ability of activated carbon such as (the dipping proportions of activating agent and raw material, the concentration of activating agent, activator dipping time, microwave power、microwave irradiation time). Reaches the best technological conditions through activated carbon produce with orthogonality experiment, and apply the product into the experiment for the adsorption of secondary effluent.
Through preparation and the adsorption experiment, with zinc chloride as activating agent, factors conclusions for iodine value is in proper order big by as follows: the dipping proportions of activating agent and raw material, the concentration of activating agent, activator dipping time, microwave power, and radiation time; The effect order to methylene adsorption value is max by: the dipping proportions of activating agent and raw material, microwave power, radiation time, activator dipping time; the effect to corn stalk activated carbon yield order big by: microwave power, the dipping proportions of activating agent and raw material, microwave irradiation time, the concentration of activating agent, activator dipping time. The best preparation condition is microwave power 595 W, concentration of activating agent chlorinating zinc is 40% , radiation time is 9 minutes, dipping time is 24 hours , the proportions of raw material and activating agent is 1: 3.0. While taking phosphoric acid as activating agent, the impact of every factor over corn stalk activated carbon iodine value is in proper order large by: Microwave power , concentration of activating agent, radiation time, dipping time; The effect for methtylene blue Decolourizing ability of corn stalk activated carbon value is in proper order by: Microwave power, concentration of activating agent, radiation time, dipping time; each factor over corn stalk activated carbon yield is in proper order by: Microwave power , concentration of activating agent, dipping time ,radiation time. The best preparation condition is microwave power 595 W, concentration of activating agent chlorinating zinc is 50%, radiation time is 8 minutes , steep time in water being 36 hours.
Using activated carbon that prepared by microwave radiating, with chlorinating zinc, do the research of adsorption experiment by COD and P in secondary effluent. Inspected the impact of activated carbon adding amounts, adsorbing balance time, the pH value of waste water over adsorption effect, under the adsorption isothermal line model of Freundich. Result indicates an best adsorbs condition to COD is as follows: Activated carbon adding amounts can not less than 14 g/L, adsorb balancing time is 40 minutes, pH value being controlled between 5 to 7, adsorption amounts are 4.127mg/g. The adsorption of P in secondary effluent, optimum adsorption condition is: Activated carbon adding amounts not being smaller than 3g/L, adsorption balance time is 90 minutes, pH value being controlled between 3 to 7, adsorption amounts are 0.2728 mg/g.
Using agricultural material as raw material, and by microwaving with activating agent, the produced activated carbon not only solve the problems of recycle and reuse agricultural byproducts and widen the resources of the raw material of activated carbon, but also provide the new materials for the polishing process. So the manufactures are god for social and environment.
引文
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