Analysis of early microscopic pore structure of electrolytic manganese residue modified polymer magnesium phosphate cement composites
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摘要: 利用电解锰渣(Electrolytic Manganese Residue，EMR)可减缓聚合物磷酸镁水泥复合材料水化速率，延长凝结时间，改善微细观结构等特点，通过宏观物理力学性能、工作性能，结合微观手段X射线衍射(XRD)、扫描电子显微镜(SEM)、同步热分析(TG-DTG)及低场核磁共振技术(NMR)等测试手段研究EMR掺量对聚合物磷酸镁水泥早期宏观和微细观孔隙结构性能影响机制。结果表明：加入EMR后能够改善浆体的工作性能，提升后期强度并有效细化孔隙结构；掺加2% EMR的28 d抗压强度值达到49.5 MPa，3%、4%掺量强度明显降低；水化产物除了长细条树状鸟粪石(Struvite，MgKPO4·6H2O&Mg[NH4]PO4·6H2O)和原料中片块状MgO外，Mn元素参与反应形成含锰化合物，水化产物相互搭接形成致密微细观结构细化了孔隙；TG-DTG曲线中在100℃出现明显的吸热峰对应鸟粪石的吸热脱水现象，质量损失率为13.299%；掺加EMR的试件出现3个吸热峰，包括Mn(OH)2和Mn3(PO4)·6H2O失去结合水的过程；T2谱弛豫时间会滞后，孔径在过渡孔和毛细孔的分布范围较大，总孔隙度随掺量增大降低，渗透率先减小后增大，1%和2%掺量的复合材料主要以凝胶孔和过渡孔分布，大孔分布面积较少，内部结构较密实，渗透率低，束缚流体饱和度高，自由流体饱和度较低。Abstract: Electrolytic manganese residue (EMR) can slow down the hydration rate of polymer magnesium phosphate cement composite mortar, prolong the setting time and improve the microstructure. Through macroscopic physical and mechanical properties, working performance, combined with microscopic means such as X-ray diffraction (XRD), scanning electron microscopy (SEM) simultaneous thermal analysis (TG-DTG) and low field nuclear magnetic resonance (NMR) techniques were used to investigate the mechanism of the influence of EMR dosage on the early macroscopic and microscopic pore structure properties of magnesium phosphate cement. The results show that the addition of EMR can improve the working performance of the slurry, enhance the later strength and effectively refine the pore structure; The 28 d compressive strength value of adding 2% EMR reaches 49.5 MPa, and the strength of 3% and 4% additives is significantly reduced; In addition to the elongated tree like struvite (MgKPO4·6H2O) and block like MgO in the raw material, Mn elements participate in the reaction to form manganese containing compounds, and the hydration products overlap with each other to form a dense microstructure which refines the pores; TG-DTG curve at 100 ℃ appeared obvious heat-absorption peak corresponds to the heat-absorption dehydration phenomenon of guano stone, the mass loss rate is 13.299%; EMR-doped specimens appeared three heat-absorption peaks, including the process of the loss of bound water by Mn(OH)2 and Mn3(PO4)·6H2O; T2 spectra relaxation time will be lagging behind, the pore size in the range of the transition pores and the distribution of the capillary pores. The total porosity decreases with the increase of doping, and the permeability decreases first and then increases. The pores of composites with 1% and 2% doping are mainly distributed by gel pores and transition pores, the distribution area of macropores is less, the internal structure is more dense, and the permeability is low, the saturation of bound fluid is high, and the saturation of free fluid is low.
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图 1 EMR (Electrolytic Manganese Residue) 制备工艺
Figure 1. EMR (Electrolytic Manganese Residue) preparation proces
图 3 微观SEM、XRD、TG-DTG及NMR测试样品
Figure 3. Microscopic SEM, XRD, TG-DTG and NMR test specimens
图 4 不同EMR掺量复合材料EMR-PMPC早期工作和收缩性能
Figure 4. Early work shrinkage performance of EMR-PMPC specimens with different EMR dosage composites
图 5 不同EMR掺量的复合材料EMR-PMPC试件早期力学性能
Figure 5. Early mechanical properties of composite EMR-PMPC specimens with different EMR doping levels
图 6 复合材料EMR-PMPC试件7 d龄期水化产物的XRD图谱
Figure 6. XRD patterns of hydration products of composite EMR-PMPC specimens at 7 d of age
图 7 复合材料EMR-PMPC试样7 d龄期的SEM图谱
Figure 7. SEM mapping of composite EMR-PMPC specimens at 7 d of age
图 9 复合材料EMR-PMPC试件7 d龄期的TG-DTG曲线
Figure 9. TG-DTG curves of composite EMR-PMPC specimens at 7 d of age
图 10 不同EMR-PMPC试件7 d龄期下核磁共振T2谱分布曲线
Figure 10. Distribution curves of NMR T2 spectra of different EMR-PMPC specimens at 7 d age
图 13 EMR-PMPC试件孔径占比分布图
Figure 13. EMR-PMPC specimen pore size percentage distribution graph
图 14 不同EMR-PMPC试件7 d龄期下孔隙度、渗透率及饱和度参数
Figure 14. Porosity, permeability and saturation parameters of different EMR-PMPC specimens at 7 d age
表 1 原材料的化学成分(wt%)
Table 1. Chemical composition of raw materials (wt%)
Component SiO2 Fe2O3 Al2O3 CaO MgO Na2O SO3 K2O MnO P2O5 TiOi2 MgO 2.1 0.4 0.4 1.7 95 0.21 0.02 0.01 0.06 0.43 0.03 Fly Ash(FA) 49.07 4.15 32.48 3.89 1.02 0.56 0.92 1.41 0.05 EVA 5010 4.28 0.39 2.72 19.35 0.34 0.18 0.11 0.10 0.02 0.03 0.34 Electrolytic Manganese Residue (EMR) 31.74 6.67 8.94 11.32 0.98 0.92 20.18 2.29 1.97 Na2B4O7·10H2O 0.13 0.01 0.11 0.10 0.19 13.34 0.24 0.03 - 0.06 - KH2PO4 0.36 0.03 0.11 0.18 0.02 2.13 0.09 31.87 - 42.77 - Defoaming Agent 27.73 0.04 0.10 0.09 0.02 0.24 0.45 0.05 - 0.08 - 
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表 2 EVA 5010胶粉的基本性能
Table 2. Basic properties of EVA 5010 rubber powder
Performance Appearance Apparent density/
(g·L−1)Solid content/% Stabilized system Main particle size/μm Minimum film forming temperature/℃ Target White powder 540+50 99+1 Polyvinyl alcohol 0.5-0.8 4
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表 3 EMR-PMPC复合材料配合比(wt%)
Table 3. EMR-PMPC composite mortar mix ratio (wt%)
No. M/P FA/M BX/M W/B S/B EMR/B EVA/B DA/B Water reducer/% EMR0
2
0.1
0.4
0.2
10
4
0.10.50 EMR1 1 0.80 EMR2 2 1.20 EMR3 3 1.26 EMR4 4 1.30 Notes: B=M+P+FA，binder; M-MgO; P-KH2PO4; FA-Fly ash; BX-Na2B4O7·10H2O, borax; S-sand; W-mixing water; In order to be able to make the numbering well presented in the figure, the specimen numbers are abbreviated as composite material (EMR-PMPC), i.e., EMR0 is the abbreviation of EMR0-PMPC, EMR1 is the abbreviation of EMR1-PMPC, EMR2 is the abbreviation of EMR2-PMPC, EMR3 is the abbreviation of EMR3-PMPC, EMR4 is the abbreviation of EMR4-PMPC.
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表 4 EMR-PMPC试件不同龄期抗压抗折强度增长率(%)
Table 4. Growth rate of compressive and flexural strength of EMR-PMPC specimens at different ages (%)
No. Age Growth rate of compressive strength% Growth rate of flexural strength% 3 h 1 d 3 d 7 d 14 d 28 d 3 h 1 d 3 d 7 d 14 d 28 d EMR0 0 0 0 0 0 0 0 0 0 0 0 0 EMR1 −0.097 −0.11 −0.17 −0.13 −0.2 −0.25 −0.03 −0.136 −0.144 −0.29 −0.054 −0.11 EMR2 −0.118 −0.15 −0.18 −0.23 −0.2 −0.25 −0.05 −0.106 −0.118 −0.16 −0.175 −0.17 EMR3 −0.158 −0.18 −0.22 −0.25 −0.3 −0.32 −0.10 −0.166 −0.184 −0.24 −0.219 −0.24 EMR4 −0.165 −0.20 −0.28 −0.27 −0.37 −0.36 −0.16 −0.23 −0.24 −0.27 −0.25 −0.31
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表 5 不同EMR-PMPC试件7 d龄期T2谱特征峰面积比
Table 5. Characteristic peak area ratio of T2 spectrum of different EMR-PMPC specimens at 7 d age
No. Peak area First peak Second peak Third peak Fourth peak Fifth peak Peak area Proportion Peak area Proportion Peak area Proportion Peak area Proportion Peak area Proportion EMR0 2054.131 1006.616 49.004 639.529 31.134 271.979 13.241 134.077 6.527 1.93 0.094 EMR1 1275.019 407.78 31.982 769.561 60.357 94.764 7.432 2.914 0.229 - - EMR2 954.739 252.912 26.49 370.708 38.828 213.308 22.342 105.579 11.058 2.233 1.281 EMR3 1110.128 341.543 30.766 136.631 12.308 547.628 49.33 81.395 7.332 2.931 0.264 EMR4 875.831 240.718 27.485 152.935 17.462 426.216 48.664 52.779 6.026 3.183 0.363
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