Preparation and properties of supplementary cementing materials based on recycling of straw solid wastes
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摘要: 针对双碳目标下水泥及其复材降低碳排放问题，本研究以玉米秸秆固废 (Corn straw waste, CSW) 为原料，发展预处理-热解-研磨三步工艺，制备一种可作为水泥辅助胶凝材料的可持续生物质灰材料。重点研究了预处理方式(未处理，蒸馏水洗涤，盐酸洗涤)、热解温度(500 ℃、600 ℃、700 ℃)和热解时间(1 h、2 h、3 h)对CSA性能的影响，以及不同预处理类型和玉米秸秆灰(Corn straw ash, CSA)掺量对水泥砂浆性能的影响。实验结果表明，随着热解温度的升高和热解时间的增长，CSA中SiO2含量逐渐增加，且热解温度对SiO2结晶的影响远大于热解时间的影响。掺入量为5 wt%的CSA可使砂浆抗压强度提高11.7%。当CSA掺入量超过5 wt%时，过多的多孔结构导致抗压强度降低。未处理、水洗和酸洗CSA的复掺，依次引发水泥基体内C-S-H形貌从蜂窝状、纤维状转变为致密的凝胶状，CSW经酸洗预处理、600 ℃下热解2 h制备的CSA具有优异的火山灰活性，可作为良好的水泥辅助胶凝材料。Abstract: This paper is aimed at the problem of reducing carbon emissions of cement and its composites under the Carbon Peaking and Carbon Neutrality Goals. This study used corn straw waste (CSW) as raw material to develop a three-step process of pretreatment-pyrolysis-grinding to prepare a sustainable corn straw ash (CSA) material that can be used as supplementary cementing materials. The study focused on studying the effects of pretreatment methods (untreated, distilled water washing, hydrochloric acid washing), pyrolysis temperature (500℃, 600℃, 700℃) and pyrolysis durations (1 h, 2 h, 3 h) on CSA activity, as well as the effects of different pretreatment types and blending amounts of CSA on the performance of prepared mortars. The experimental results showed that the content of SiO2 of CSA increased with the enhancement of pyrolysis temperature and duration. And the effect of pyrolysis temperature on SiO2 crystallization was much greater than that of pyrolysis durations. The incorporation of 5 wt% CSA increased the compressive strength of mortar by 11.7%. The incorporation of over 5 wt% CSA decreased the compressive strength due to the porous structure of CSA. The incorporation of untreated, distilled water washing and hydrochloric acid washing CSA demonstrated caused the C-S-H morphology in the cement matrix to change from honeycomb and fibrous to dense gel. The CSA treated by acid washing and pyrolysis at 600℃ for 2 h showed excellent pozzolanic activity and can be used as good supplementary cementing materials.
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图 6 不同CSA水泥浆样品的等温量热
Figure 6. Isothermal calorimetry of cement pastes samples containing different CSA
图 9 混合水泥浆体的SEM图像(5000×)(a) OPM；(b) M5-A；(c) M10-A；(d) M5-U；(e) M5-W
Figure 9. SEM images of blended cement pastes (5000×) (a) OPM；(b) M5-A；(c) M10-A；(d) M5-U；(e) M5-W
表 1 水泥的化学成分
Table 1. Chemical composition of cement
wt% SiO2 CaO Al2O3 Fe2O3 MgO SO3 TiO2 K2O Na2O LOI Cement 20.25 62.30 6.04 3.41 2.01 3.65 0.39 0.84 0.17 3.24 
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表 2 玉米秸秆灰(CSA)样品的制备条件
Table 2. The preparation conditions of corn straw ash (CSA) samples
Sample code Washing method Pyrolysis temperature Heating rate Pyrolysis duration Grinding time A1 500℃ 2 h A2 500℃ 3 h A3 600℃ 1 h A4 -U, -W, -A 600℃ 10℃/min 2 h 30 min A5 600℃ 3 h A6 700℃ 1 h A7 700℃ 2 h Notes: -U means unwashed. -W means pure water washed. -A means acid-washed.
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表 3 砂浆的配合比
Table 3. Mix-proportion details of mortars
Series Cementing materials/wt. % water/binder ratio SP/wt. % Sand/binder ratio Cement CSA OPM 100 — — — 3 M3-A 97 3 0.5 0.15 3 M5-A 95 5 0.5 0.15 3 M10-A 90 10 0.5 0.15 3 M5-U 95 5 0.5 0.15 3 M5-W 95 5 0.5 0.15 3 Notes：OPM means Ordinary Portland mortar. SP means superplasticizer.
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表 4 不同洗涤方式下CSA的化学组成及烧失量(LOI，Loss on ignition)
Table 4. Chemical composition and loss on ignition of CSA under different washing methods
wt% A5-U A5-W A5-A A6-U A6-W A6-A SiO2 24.386 66.748 75.653 23.109 68.675 76.749 Al2O3 0.980 0.919 0.909 0.981 0.985 0.927 Fe2O3 0.954 1.868 1.251 0.713 1.435 0.977 CaO 7.440 20.479 13.914 9.130 19.152 13.235 K2O 36.794 0.962 0.934 35.747 1.172 1.097 MgO 7.337 4.805 2.863 8.593 4.652 2.678 Na2O 2.767 0.011 0.032 2.391 0.085 0.013 P2O5 6.959 1.202 1.712 6.439 1.236 1.548 ZnO 0.057 0.199 0.080 0.075 0.135 0.048 SO3 0.951 2.386 2.011 1.162 1.936 2.291 Cl 10.977 0.273 0.480 11.234 0.360 0.187 Others 0.398 0.148 0.161 0.426 0.177 0.250 LOI 4.65 2.94 2.39 4.39 2.93 2.24
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表 5 不同热解条件下CSA的氧化物组成及LOI
Table 5. Oxide composition and loss on ignition of CSA under different pyrolysis conditions
wt% A1-A A3-A A4-A A5-U A7-A SiO2 67.458 71.519 73.644 75.653 77.495 Al2O3 1.028 0.944 0.858 0.909 0.803 Fe2O3 0.889 1.713 1.674 1.251 1.272 CaO 15.380 15.676 14.302 13.914 12.385 K2O 2.805 1.756 1.178 0.934 1.091 MgO 6.708 3.516 3.967 2.863 2.699 Na2O 0.092 0.044 0.054 0.032 0.035 P2O5 1.781 1.222 1.409 1.712 1.532 ZnO 0.259 0.151 0.147 0.080 0.126 SO3 2.385 2.929 2.253 2.011 2.096 Cl 0.892 0.293 0.313 0.380 0.251 Others 0.323 0.237 0.201 0.261 0.215 LOI 2.82 2.79 2.66 2.39 2.21
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