煤基超细复合吸附剂的制备及吸附特性研究
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摘要
煤分子中含有多种含氧官能团，内部具有丰富的孔隙结构，既是一种天然吸附剂也是制造吸附剂的优质原料。煤在粉碎超细化的过程中，随着粒度的减小，煤粉的比表面积增大、表面活性增加、孔体积增大，吸附性能增加。超细煤粉成型过程中，煤粉颗粒之间的紧密堆积会构成新的孔隙，进一步提高吸附性能。以煤为原料制备煤基超细复合吸附剂，对探索煤炭利用的新途径，开发研制高性能煤基吸附剂有着重要的意义。本文以神府煤为原料，首次研究了煤粉特别是超细煤粉粒度与吸附性能关系和吸附机理，在此基础上分别采用机械力化学法和液相化学氧化法首次制备了煤基超细复合吸附剂，并对其对水溶液中苯酚、苯胺、硝基苯和Ni~(2+)的吸附性能和机理进行了研究，与市售煤基活性炭(CAC)进行比较。
不同粒度煤粉吸附苯酚的动力学研究表明，吸附符合二级吸附动力学模型。煤粉吸附苯酚的过程由膜扩散和孔隙内扩散联合控制。求出了颗粒内有效扩散系数和颗粒内扩散速率常数。试验范围内，煤粉的粒径(d)与苯酚吸附量(q)之间符合q=28.1378×exp|d／(-5.7328)|+24.1453。不同粒径煤粉对苯酚的吸附符合Freundlich或Langmuir吸附等温式。随着温度的增加，超细煤粉对苯酚的吸附量下降。吸附热力学参数△H为．11.18kJ·mol~(-1)、AS为．23.39J·mol~(-1)·K~(-1)、AG在不同温度时均为负值。
煤粉与KMnO_4共球磨可以增加煤粉对苯酚的吸附量。红外光谱表明，球磨过程中发生了机械力化学反应，主要产物为腐植酸盐。在质量比KMnO_4：煤=10∶100条件下，球磨6h后经过碱洗、酸洗、水洗干燥后在微波功率为540W的条件下处理15min得到煤基超细复合吸附剂MMCA。断面扫描电镜研究表明，MMCA由许多细小颗粒粘结在一起构成，内部具有丰富的孔隙。小颗粒粒径200nm左右，大颗粒粒径在500nm左右。
经过H_2O_2适度氧化，超细煤粉的苯酚吸附量增加。在浓度为2M、反应温度20℃、H_2O_2／煤=0.23(质量比)的条件下反应，混合液抽滤后分别经过碱洗、酸洗、
水洗抽滤至中性、干燥得到煤基吸附剂HCA。HCA用丙酮浸渍处理，制得煤基超
细复合吸附剂AHCA.断面扫描电镜表明，AHCA由许多细小颗粒粘结在一起构成。
其中小颗粒粒径约ZOOIun，大颗粒粒径约SOOnm。
煤基吸附剂MMCA、HCA、AHCA和CAC对水溶液中苯酚、苯胺、硝基苯和
Ni2+的吸附符合二级动力学模型。除了MMCA对硝基苯的吸附过程为颗粒内扩散控
制过程外，其余均为颗粒内扩散和膜扩散联合控制过程。求出了颗粒内有效扩散系
数和颗粒内扩散速率常数。四种吸附剂对水溶液中苯酚、苯胺和硝基苯的吸附量大
小次序为cAc>AHcA>HcA>MMcA，而对Ni2+的吸附量大小次序为MMcA>
AHcA)cAc>HcA。相同平衡浓度下MMcA对Ni2+的吸附量约为cAc的两倍。四
种煤基吸附剂对苯酚、苯胺、硝基苯和Ni2+的吸附符合Langmni:或Freundlich吸附
等温式。MMCA和AHCA对苯酚的吸附t随着温度的升高而下降。MMCA和AHCA
吸附苯酚的热力学参数八付分别为一9.15和·n .79kJ·mol一，绍为一19.37和一23.01
J.mol’’·K一’，△G均为负值.煤基超细复合吸附剂MMcA吸附苯酚、苯胺和硝基苯的
红外光谱研究表明，吸附主要以形成分子间氢键的形式结合，提出了吸附反应方程
式。
本文以传质理论为基础，建立了球形颗粒吸附剂的一级吸附动力学模型。四种
煤基吸附剂吸附苯酚、苯胺、硝基苯和N护十的动力学数据对该模型的拟合结果较好。
根据四种煤基吸附剂吸附四种污染物的动力学数据，建立了吸附量预测的BP神经
网络预测模型，达到非常高的拟合精度和较好的预测效果。
Coal is not only natural adsorbent but also good materials to prepare adsorbent owing to various oxygen-containing groups and pore structure. The specific surface area and pore volume increase with the size of coal particles decreasing during superfine pulverization. New pores will be formed and the adsorption capacities will be enhanced when coal particles accumulated together compactly. It is valuable to prepare coal based superfine composite adsorbent both in probing new ways of coal utilization and in preparing coal based adsorbents with high capacity. In this paper, based on the studies of mechanism and relationships of coal powders, especially superfine coal powders with adsorption capacity. Two methods both mechanochemistry and liquid phase chemical oxidization were used to prepare coal based superfine composite adsorbents. Adsorption capacity and mechanism of phenol, aniline, nitrobenzene and nickel ion (Ni2+) onto coal based superfine composite adsorbents were studied respectively compared with comm
ercial coal based activated carbon.
The kinetic studies showed that phenol adsorption onto various size coal powders accords with the second order model, the processes were controlled both by film and pore diffusion. The effective diffusion coefficient and rate constant of intraparticle transport were calculated. The relationship between diameter of coal powders and phenol
adsorption capacity conforms to equation: q = 28.1378 exp+ 24.1453.
The adsorption equilibrium of phenol onto various size coal powders can be described in terms of the Freundlich or Langmuir isotherm. Phenol adsorption capacity onto superfine coal powders decrease with increasing temperature. The adsorption parameters of thermodynamics H is -11.18kJ-mol-1. S is-23.39J mol-1-K-1,G are negative.
Phenol adsorption capacity increases when coal powder was milled together with KMnO4. Infrared spectra (FTIR) showed that mechanochemistry reaction occurred and the resultants mainly were humic acid salt during milling. When the mass ratio of KMnO4 to coal was 10:100, after 6h milled coal powder was washed with alkali solution, acid solution and distilled water, then treated with microwave radiation for 15 minutes under 540W after dried. Coal based superfine composite adsorbent was obtained standing for MMCA. Scanning electron microscope (SEM) analysis of section showed that MMCA was made up of a lot of small particles conglutination with each other, diameter of the smaller particles are 200nm,the bigger particles are 500nm.There are abundant pores in MMCA.
The phenol adsorption capacity increased when superfine coal powder was oxidized by H2O2 rnoderately. Coal powder was rinsed with alkali solution, acid solution and distilled water respectively after oxidized by H2O2 under conditions that mass ratio of H2O2 to coal was 0.23, concentration 2M and temperature 20 C.The mixture was filtrated and the residue was dried (sample standing for HCA). Coal based superfine composite adsorbent standing for AHCA obtained after impregnated in acetone and dried. SEM analysis of sections showed that AHCA is made up of a lot of small particles conglutination with each other, diameter of the smaller particles are 200nm,the bigger particles are about 500nm.There are abundant pores in AHCA.
The kinetics of phenol, aniline, nitrobenzene and Ni2+ adsorbed respectively onto coal based superfine composite adsorbents fit the second order kinetic model. The adsorption processes were controlled by both film and pore diffusion except nitrobenzene adsorption onto MMCA which was controlled by pore diffusion. The effective diffusion coefficient and rate constant of intraparticle transport were calculated. The order of adsorption capacities of phenol, aniline, nitrobenzene onto four kinds of adsorbents in turns was CAC>AHCA>HCA>MMCA, however Ni2+ was MMCA> AHCA>CAC>HCA. The adsorption equilibrium of phenol, aniline, nitrobenzene and Ni2+ onto four kinds of coal based adsorbents can be described in terms of the Langmuir or Freundlich isotherm.
Phenol adsorption c
不同粒度煤粉吸附苯酚的动力学研究表明，吸附符合二级吸附动力学模型。煤粉吸附苯酚的过程由膜扩散和孔隙内扩散联合控制。求出了颗粒内有效扩散系数和颗粒内扩散速率常数。试验范围内，煤粉的粒径(d)与苯酚吸附量(q)之间符合q=28.1378×exp|d／(-5.7328)|+24.1453。不同粒径煤粉对苯酚的吸附符合Freundlich或Langmuir吸附等温式。随着温度的增加，超细煤粉对苯酚的吸附量下降。吸附热力学参数△H为．11.18kJ·mol~(-1)、AS为．23.39J·mol~(-1)·K~(-1)、AG在不同温度时均为负值。
煤粉与KMnO_4共球磨可以增加煤粉对苯酚的吸附量。红外光谱表明，球磨过程中发生了机械力化学反应，主要产物为腐植酸盐。在质量比KMnO_4：煤=10∶100条件下，球磨6h后经过碱洗、酸洗、水洗干燥后在微波功率为540W的条件下处理15min得到煤基超细复合吸附剂MMCA。断面扫描电镜研究表明，MMCA由许多细小颗粒粘结在一起构成，内部具有丰富的孔隙。小颗粒粒径200nm左右，大颗粒粒径在500nm左右。
经过H_2O_2适度氧化，超细煤粉的苯酚吸附量增加。在浓度为2M、反应温度20℃、H_2O_2／煤=0.23(质量比)的条件下反应，混合液抽滤后分别经过碱洗、酸洗、
水洗抽滤至中性、干燥得到煤基吸附剂HCA。HCA用丙酮浸渍处理，制得煤基超
细复合吸附剂AHCA.断面扫描电镜表明，AHCA由许多细小颗粒粘结在一起构成。
其中小颗粒粒径约ZOOIun，大颗粒粒径约SOOnm。
煤基吸附剂MMCA、HCA、AHCA和CAC对水溶液中苯酚、苯胺、硝基苯和
Ni2+的吸附符合二级动力学模型。除了MMCA对硝基苯的吸附过程为颗粒内扩散控
制过程外，其余均为颗粒内扩散和膜扩散联合控制过程。求出了颗粒内有效扩散系
数和颗粒内扩散速率常数。四种吸附剂对水溶液中苯酚、苯胺和硝基苯的吸附量大
小次序为cAc>AHcA>HcA>MMcA，而对Ni2+的吸附量大小次序为MMcA>
AHcA)cAc>HcA。相同平衡浓度下MMcA对Ni2+的吸附量约为cAc的两倍。四
种煤基吸附剂对苯酚、苯胺、硝基苯和Ni2+的吸附符合Langmni:或Freundlich吸附
等温式。MMCA和AHCA对苯酚的吸附t随着温度的升高而下降。MMCA和AHCA
吸附苯酚的热力学参数八付分别为一9.15和·n .79kJ·mol一，绍为一19.37和一23.01
J.mol’’·K一’，△G均为负值.煤基超细复合吸附剂MMcA吸附苯酚、苯胺和硝基苯的
红外光谱研究表明，吸附主要以形成分子间氢键的形式结合，提出了吸附反应方程
式。
本文以传质理论为基础，建立了球形颗粒吸附剂的一级吸附动力学模型。四种
煤基吸附剂吸附苯酚、苯胺、硝基苯和N护十的动力学数据对该模型的拟合结果较好。
根据四种煤基吸附剂吸附四种污染物的动力学数据，建立了吸附量预测的BP神经
网络预测模型，达到非常高的拟合精度和较好的预测效果。
Coal is not only natural adsorbent but also good materials to prepare adsorbent owing to various oxygen-containing groups and pore structure. The specific surface area and pore volume increase with the size of coal particles decreasing during superfine pulverization. New pores will be formed and the adsorption capacities will be enhanced when coal particles accumulated together compactly. It is valuable to prepare coal based superfine composite adsorbent both in probing new ways of coal utilization and in preparing coal based adsorbents with high capacity. In this paper, based on the studies of mechanism and relationships of coal powders, especially superfine coal powders with adsorption capacity. Two methods both mechanochemistry and liquid phase chemical oxidization were used to prepare coal based superfine composite adsorbents. Adsorption capacity and mechanism of phenol, aniline, nitrobenzene and nickel ion (Ni2+) onto coal based superfine composite adsorbents were studied respectively compared with comm
ercial coal based activated carbon.
The kinetic studies showed that phenol adsorption onto various size coal powders accords with the second order model, the processes were controlled both by film and pore diffusion. The effective diffusion coefficient and rate constant of intraparticle transport were calculated. The relationship between diameter of coal powders and phenol
adsorption capacity conforms to equation: q = 28.1378 exp+ 24.1453.
The adsorption equilibrium of phenol onto various size coal powders can be described in terms of the Freundlich or Langmuir isotherm. Phenol adsorption capacity onto superfine coal powders decrease with increasing temperature. The adsorption parameters of thermodynamics H is -11.18kJ-mol-1. S is-23.39J mol-1-K-1,G are negative.
Phenol adsorption capacity increases when coal powder was milled together with KMnO4. Infrared spectra (FTIR) showed that mechanochemistry reaction occurred and the resultants mainly were humic acid salt during milling. When the mass ratio of KMnO4 to coal was 10:100, after 6h milled coal powder was washed with alkali solution, acid solution and distilled water, then treated with microwave radiation for 15 minutes under 540W after dried. Coal based superfine composite adsorbent was obtained standing for MMCA. Scanning electron microscope (SEM) analysis of section showed that MMCA was made up of a lot of small particles conglutination with each other, diameter of the smaller particles are 200nm,the bigger particles are 500nm.There are abundant pores in MMCA.
The phenol adsorption capacity increased when superfine coal powder was oxidized by H2O2 rnoderately. Coal powder was rinsed with alkali solution, acid solution and distilled water respectively after oxidized by H2O2 under conditions that mass ratio of H2O2 to coal was 0.23, concentration 2M and temperature 20 C.The mixture was filtrated and the residue was dried (sample standing for HCA). Coal based superfine composite adsorbent standing for AHCA obtained after impregnated in acetone and dried. SEM analysis of sections showed that AHCA is made up of a lot of small particles conglutination with each other, diameter of the smaller particles are 200nm,the bigger particles are about 500nm.There are abundant pores in AHCA.
The kinetics of phenol, aniline, nitrobenzene and Ni2+ adsorbed respectively onto coal based superfine composite adsorbents fit the second order kinetic model. The adsorption processes were controlled by both film and pore diffusion except nitrobenzene adsorption onto MMCA which was controlled by pore diffusion. The effective diffusion coefficient and rate constant of intraparticle transport were calculated. The order of adsorption capacities of phenol, aniline, nitrobenzene onto four kinds of adsorbents in turns was CAC>AHCA>HCA>MMCA, however Ni2+ was MMCA> AHCA>CAC>HCA. The adsorption equilibrium of phenol, aniline, nitrobenzene and Ni2+ onto four kinds of coal based adsorbents can be described in terms of the Langmuir or Freundlich isotherm.
Phenol adsorption c
引文
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