Loading strategy for the active components of monolithic catalyst and its influences on the microwave enhanced catalytic combustion of toluene
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摘要: 针对催化剂活性组分脱落问题，采用载体预处理和添加硅溶胶的策略来强化活性组分负载，微波单模腔中催化燃烧甲苯以考察催化剂活性，并对牢固负载的催化剂进行表征分析。研究表明，常温下采用10%盐酸溶液对蜂窝状堇青石（CH）载体预处理、硅溶胶添加量与载体吸水量比值为0.125条件下所制备的Cu-Mn-Ce（硅溶胶）/CH催化剂脱落率为0.0129%，明显低于Cu-Mn-Ce/CH催化剂的0.950%。Cu-Mn-Ce（硅溶胶）/CH催化剂具有更小的活性颗粒尺寸、更大的比表面积和更多样的活性晶体，在甲苯进气浓度1000 mg/m3、进气量0.12 m3/h、微波功率200 W和床层温度350℃条件下，催化剂对甲苯的催化燃烧效率和矿化率分别为98.5%和87.9%；连续实验43 h后，催化剂活性保持稳定且活性组分脱落率低（0.0328%）。硅溶胶的添加增强了活性组分与载体之间的相互作用力，生成的硅氧烷化学键提高了活性组分的结合牢固度。Abstract: Aiming at solving the shedding problem of active components, a loading strategy that includes carrier pretreatment and addition of silica sol was adopted to strengthen the combination of the active components with the carrier. Catalytic activity of the catalyst was investigated in toluene combustion by using microwave single-mode cavity, and high-firmness catalysts were characterized subsequently. The study showed that the shedding rate of Cu-Mn-Ce(silica sol)/cordierite honeycomb(CH) catalyst prepared under conditions of 10% hydrochloric acid pretreatment at room temperature and 0.125 of the mass ratio of silica sol to water absorption amount of CH carrier was 0.0129%, which was much lower than 0.950% of Cu-Mn-Ce/CH catalyst. Cu-Mn-Ce(silica sol)/CH catalyst had smaller active particles, larger specific surface area and more active crystals than Cu-Mn-Ce/CH catalyst. Under conditions of 1000 mg/m3 of initial concentration, 0.12 m3/h of air flow, 200 W of microwave power and 350 ℃ of bed temperature, the removal and mineralization rates of toluene by Cu-Mn-Ce(silica sol)/CH catalyst were 98.5% and 87.9%, respectively. The Cu-Mn-Ce(silica sol)/CH catalyst owned high catalytic activity and stability after 43 h run, and the shedding rate of active components was 0.0328%. The addition of silica sol could enhance the interaction forces between the active components and the catalyst carrier, and the formation of siloxane chemical bonds could greatly improve the connection of active components to prolong the service life of the catalyst.
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Key words:
- firmness /
- silica sol /
- microwave catalysis /
- toluene /
- mineralization /
- characterization
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图 1 实验装置流程示意图
Figure 1 Schematic of the experimental device flow
1: air compressor; 2: silica gel column; 3: activated carbon column; 4: flowmeter; 5: syringe pump; 6: evaporation flask; 7: explosion-proof zeolite; 8: electric furnace; 9: buffer bottle; 10: inlet sampling point; 11: gas chromatograph; 12: microwave device; 13: water-cooling system; 14: K-type thermocouple; 15: fixed bed reactor; 16: outlet sampling point; 17: organic solvent bottle; 18: alkaline solution bottle
图 2 预处理后催化剂活性组分负载量和脱落率
Figure 2 Load and shedding rates of the active components of catalysts after pretreatment
G1: control group; G2: ultrasonic vibration; G3: 5%HNO3; G4: 10% HNO3; G5: 15% HNO3; G6: 30% HNO3; G7: 20%H2C2O4; G8: 30% H2C2O4; G9: 40% H2C2O4; G10: 27%NH3·H2O; G11: 10%HCl; G12: 0.5 mol/L NaOH
图 3 添加硅溶胶后催化剂活性组分负载量和脱落率
Figure 3 Load and shedding rates of the active components of catalysts after adding silica sol
k1=0; k2=0.0500; k3=0.0750; k4=0.1000; k5=0.1063; k6=0.1125; k7=0.1188; k8=0.1250; k9=0.1500; msilica sol/mwater absorption refer to the mass ratio of silica sol to water absorption amount of the carrier
图 4 堇青石基催化剂的SEM照片(“New-、Old-”分别代表新制备、稳定性实验后的催化剂)
Figure 4 SEM images of the cordierite-based catalysts("New-, Old-" refers to the new catalysts and used catalysts after stabilitytest, respectively)
图 5 催化剂的XRD谱图
Figure 5 XRD patterns of the catalysts
a: New/Cu-Mn-Ce(silica sol)/CH catalyst; b: New/Cu-Mn-Ce/CH catalyst; c: CH carrier(acid etching); d: Old/Cu-Mn-Ce(silica sol)/CH catalyst; e: Old/Cu-Mn-Ce/CH catalyst
图 6 催化剂FT-IR谱图
Figure 6 FT-IR spectra of catalysts
a: New/Cu-Mn-Ce/CH catalyst; b: New/Cu-Mn-Ce(silica sol)/CH catalyst
图 7 催化剂吸波升温曲线
Figure 7 Temperature-rising curves of the catalysts under microwave irradiation
■: CH carrier (acid etching); ●: Cu-Mn-Ce(silica sol)/CH catalyst; ▲:Cu-Mn-Ce/CH catalyst reaction conditions:P=200 W, bed height 100 mm, catalyst volume 6.15×10-5 m3
图 8 床层温度300 ℃下两种催化剂对甲苯的催化降解
Figure 8 Catalytic degradation of toluene at 300 ℃ of bed temperature over two catalysts separately
■: Cu-Mn-Ce/CH catalyst; ●: Cu-Mn-Ce(silica sol)/CH catalyst reaction conditions: toluene initial concentration 1000 mg/m3, air flow rate 0.12 m3/h, catalyst volume 6.15×10-5 m3, bed height 100 mm, bed temperature 300 ℃, Cu-Mn-Ce/CH catalyst:Pheating=100 W, Pinsulation=75 W; Cu-Mn-Ce (silica sol)/CH catalyst: Pheating=250 W, Pinsulation=150 W
图 9 不同床层温度下Cu-Mn-Ce(硅溶胶)/CH催化剂对甲苯的催化降解
Figure 9 Catalytic degradation of toluene at different bed temperatures over Cu-Mn-Ce(silica sol)/CH catalyst
■: 150 ℃(Pheating=100 W, Pinsulation=75 W); □: 200 ℃(Pheating=100 W, Pinsulation=87 W); ▲: 250 ℃(Pheating=200 W, Pinsulation=105 W); △: 300 ℃(Pheating=250 W, Pinsulation=150 W); ●: 350 ℃(Pheating=250 W, Pinsulation=220 W); ○: 400 ℃(Pheating=300 W, Pinsulation=275 W)
图 10 两种催化剂对甲苯的矿化率
Figure 10 Mineralization rate of toluene over two different catalysts
■: mineralization rate of toluene over the Cu-Mn-Ce(silica sol)/CH catalyst; □: mineralization rate of toluene over the Cu-Mn-Ce/CH catalyst; ●: Cu-Mn-Ce(silica sol)/CH catalyst activity; ○: Cu-Mn-Ce/CH catalyst activity reaction conditions: toluene concentration 1000 mg/m3, air flow rate 0.12 m3/h, catalystvolume 6.15×10-5 m3, bed height 100 mm, bed temperature 350 ℃, Pheating=250 W, Pinsulation=220 W
图 11 催化剂的稳定性测试
Figure 11 Stability test of catalysts
■: toluene removal rate; ●: active components shedding rate reaction conditions: toluene concentration 1000 mg/m3, air flow rate 0.12 m3/h, catalyst volume 6.15×10-5 m3, bed height 100 mm, temperature 350 ℃, Cu-Mn-Ce/CH catalyst: Pheating=150 W, Pinsulation=123 W; Cu-Mn-Ce(silica sol)/CH catalyst: Pheating=250 W, Pinsulation=220 W
图 12 活性组分在催化剂表面的结合机理
Figure 12 Connection mechanism of the active components on the catalyst surface
表 1 预处理后堇青石载体的吸水率
Table 1 Water absorption of the cordierite carrier after pretreatment
Pretreatmentsolution Controlgroup Ultrasonic vibration 5%HNO3 10%HNO3 15%HNO3 30%HNO3 20%H2C2O4 30%H2C2O4 40%H2C2O4 27%NH3·H2O 10%HCl 0.5 mol/LNaOH Water absorption /% 38.26 44.62 44.16 56.63 60.07 43.04 67.91 59.66 51.00 50.53 53.18 52.19 note：5%, 10%, 40%, 27%, etc. are the mass percentages when the acid and alkali solutions are diluted 
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表 2 催化剂的比表面积和孔结构参数
Table 2 Specific surface area and pore structure parameters of different carriers and catalysts
Sample BET special surface area A/(m2·g-1) Micropore area A/(m2·g-1) Total pore volume v/ (cm3·g-1) Micropore volume v/(cm3·g-1) Average pore size d/nm CH carrier 0.98 0.47 0.00080 0.00050 9.56 CH carrier(acid etching) 2.80 0.37 0.0036 0.00024 20.18 New/Cu-Mn-Ce/CH catalyst 13.93 8.47 0.052 0.0065 32.90 New/Cu-Mn-Ce(silica sol)/CH catalyst 28.28 12.72 0.089 0.0098 22.99 Old/Cu-Mn-Ce/CH catalyst 9.04 3.27 0.016 0.0017 26.38 Old/Cu-Mn-Ce(silica sol)/CH catalyst 19.24 10.70 0.074 0.0035 18.23
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表 3 实验前后两种催化剂的活性组分牢固度分析
Table 3 Firmness analysis of the active components of two catalysts before and after stability test
Sample Quality of cordierite carrier after pretreatment m0/g Quality of supported catalyst m1/g Initial active components loading w1/% Quality of catalyst after firmness test m2/g Active components shedding rate △w/% Final active components loading w2/% New/Cu-Mn-Ce/CH catalyst 31.8772 34.8520 9.33 34.8105 0.119 9.20 New/Cu-Mn-Ce (silica sol)/CH catalyst 32.4818 35.8107 10.25 35.8048 0.0165 10.23 Old/Cu-Mn-Ce/CH catalyst 33.2763 36.3777 9.32 36.2455 0.363 8.92 Old/Cu-Mn-Ce (silica sol)/CH catalyst 32.3773 35.7025 10.27 35.6908 0.0328 10.23
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