Effect of stearic acid, zinc stearate coating on the properties of synthetic hydromagnesite

Synthetic hydromagnesite (SHM), used as flame retardant for polymers, may have similar or better flame retardancy effectiveness than aluminum tri-hydroxide (ATH) and magnesium di-hydroxide (MDH). Suitable surface modifiers are often employed to improve its dispersion and compatibility with polymer matrix. In this study, we chose stearic acid (SA) and zinc stearate (ZS) as the surface modifier, and investigated the properties of SHM modified with various surface modifier content using dry blending coating process. Scanning electron microscope (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetry (TG), particle size distribution, contact angle, oil absorption, bulk density, tapped density and Carr's index were employed to characterize the effect of surface modification. The results showed that the surface of SHM powders was changed from hydrophilic to lipophilic. The flowability of the surface modified powder was also improved. TG graphs showed that the surface modifier had no obvious influence on the degradation pathway of the SHM.     

DTA and FT-IR analysis of the rehydration of basic magnesium carbonate

The rehydration characteristics of a commercially produced hydromagnesite and two basic magnesium carbonates synthetically produced from Mg(OH)₂, are presented. The products were dehydrated and dehydroxylated at 325°C before rehydration was attempted. DTA and FT-IR were used to follow the structural changes that occurred during the rehydration processes. The results obtained for the commercially and synthetically produced hydromagnesite products indicated that the original symmetry of the groups was reclaimed during rehydration. This was not observed for the synthetically produced unidentified basic magnesium carbonate product. This investigation provides insight into the rehydration characteristics of a select group of basic magnesium carbonates. This revised version was published online in July 2006 with corrections to the Cover Date.     

高比表面积介孔网状氧化镁的制备、表征及对废水中Pb(Ⅱ)的吸附性能和机理

以天然水菱镁矿为原料，通过"煅烧-水化-煅烧"的简单方法制备了高比表面积介孔网状MgO，且实验过程中无须加入任何试剂。系统性研究了氧化镁用量、吸附时间、吸附温度及pH对氧化镁吸附模拟废水中铅离子吸附性能的影响，揭示了吸附机理，并考察了氧化镁对多种离子的吸附效果。结果表明：该氧化镁吸附剂具有188 m²·g^-1的高比表面积和0.85 cm³·g^-1的高孔体积，平均孔径为12.33 nm，其吸附动力学和等温线数据与伪二级模型和Langmuir模型高度吻合，表明重金属离子在氧化镁上为单层化学吸附。MgO介孔网状结构表现出对Pb（Ⅱ）的高吸附性能，最大吸附量为7 431.5 mg·g^-1，该数值远高于其他报道的基于MgO吸附剂的数值，铅去除率高达99.8%以上。介孔网状MgO的吸附机理主要是羟基官能团以及Mg（Ⅱ）与MgO表面重金属离子之间的离子交换所致。另外，该氧化镁可同时吸附多种离子，对Cd、Cr、Ni、As、Co、P、Se、Be、Bi、Cu、Fe、Mn、V、Zn、Al离子均具有优异的吸附性能。     

微波对碱式碳酸镁结晶过程的影响

在微波外场作用下,利用氯化镁和碳酸钠溶液反应结晶法直接合成碱式碳酸镁晶体。通过对比微波、水浴两种加热方式下镁离子变化曲线和产物的差异,XRD、FTIR,SEM等对相转移过程的物相分析表征,探索微波对反应的强化影响。结果表明,反应结晶直接合成碱式碳酸镁过程分为絮状物→出现晶体→完全转变为球状碱式碳酸镁3个阶段。微波对反应3个阶段中都有强化作用,促进絮状物的形成,加快相转变,提高反应转化率,微波加热条件下在粒径分布与组装方式与水浴加热方式均有不同,微波作用下较小颗粒是由纳米片层平行组装而成,而较大颗粒可能是无定形物在球状小颗粒表面继续转变,形成交错的表层纹理的大颗粒碱式碳酸镁。     

Raman spectroscopic study of the magnesium carbonate mineral hydromagnesite (Mg5[(CO3)4(OH)2]· 4H2O)

Magnesium minerals are important for understanding the concept of geosequestration. One method of studying the hydrated hydroxy magnesium carbonate minerals is through vibrational spectroscopy. A combination of Raman and infrared spectroscopy has been used to study the mineral hydromagnesite. An intense band is observed at 1121 cm⁻¹, attributed to the CO₃²⁻ν₁ symmetric stretching mode. A series of infrared bands at 1387, 1413 and 1474 cm⁻¹ are assigned to the CO₃²⁻ν₃ antisymmetric stretching modes. The CO₃²⁻ν₃ antisymmetric stretching vibrations are extremely weak in the Raman spectrum and are observed at 1404, 1451, 1490 and 1520 cm⁻¹. A series of Raman bands at 708, 716, 728 and 758 cm⁻¹ are assigned to the CO₃²⁻ν₂ in‐plane bending mode. The Raman spectrum in the OH stretching region is characterized by bands at 3416, 3516 and 3447 cm⁻¹. In the infrared spectrum, a broad band is found at 2940 cm⁻¹, which is assigned to water stretching vibrations. Infrared bands at 3430, 3446, 3511, 2648 and 3685 cm⁻¹ are attributed to MgOH stretching modes. Copyright © 2011 John Wiley & Sons, Ltd.     

玫瑰花状多孔碱式碳酸镁微球的合成

介绍了一种便利的玫瑰花状多孔碱式碳酸镁(4MgCO₃·Mg(OH)₂·4H₂O)微球的合成方法,该方法分为三水碳酸镁(MgCO₃·3H₂O)前驱物合成与其在水中的热解制备过程。采用搅拌诱导结晶辅助陈化的方法合成前驱物,得到长约115 μm,长径比约10.4的均一微棒,将微棒在353.2 K的水中热解,即可得到由弯曲的纳米片组成的具有“卡片箱”结构（house of cards）的玫瑰花状多孔碱式碳酸镁微球,微球直径为30~60 μm,平均约40 μm,具有良好分散性。研究了热解过程中的形貌转变和相转移过程,采用XRD,FTIR及SEM表征样品的结构和形貌。结果表明：MgCO₃·3H₂O在较高温度下因不稳定而溶解,形成局部过饱和,生成无定形颗粒,并在微棒上成核结晶为4MgCO₃·Mg(OH)₂·4H₂O纳米片。纳米片由与微棒附着部位向外生长,形成玫瑰花状微球,微球长大伴随微棒的消溶,生长在棒上不同部位的颗粒在微观结构上将留有不同痕迹。分析认为热解转变过程是(MgCO₃·3H₂O)溶解－无定形物生成-(4MgCO₃·Mg(OH)₂·4H₂O)结晶的过程。     

Thermo‐Raman spectroscopy of synthetic nesquehonite — implication for the geosequestration of greenhouse gases

Pure nesquehonite (MgCO₃·3H₂O)/Mg(HCO₃)(OH)·2H₂O was synthesised and characterised by a combination of thermo‐Raman spectroscopy and thermogravimetry with evolved gas analysis. Thermo‐Raman spectroscopy shows an intense band at 1098 cm⁻¹, which shifts to 1105 cm⁻¹ at 450 °C, assigned to the ν₁CO₃²⁻ symmetric stretching mode. Two bands at 1419 and 1509 cm⁻¹ assigned to the ν₃ antisymmetric stretching mode shift to 1434 and 1504 cm⁻¹ at 175 °C. Two new peaks at 1385 and 1405 cm⁻¹ observed at temperatures higher than 175 °C are assigned to the antisymmetric stretching modes of the (HCO₃)⁻ units. Throughout all the thermo‐Raman spectra, a band at 3550 cm⁻¹ is attributed to the stretching vibration of OH units. Raman bands at 3124, 3295 and 3423 cm⁻¹ are assigned to water stretching vibrations. The intensity of these bands is lost by 175 °C. The Raman spectra were in harmony with the thermal analysis data. This research has defined the thermal stability of one of the hydrous carbonates, namely nesquehonite. Thermo‐Raman spectroscopy enables the thermal stability of the mineral nesquehonite to be defined, and, further, the changes in the formula of nesquehonite with temperature change can be defined. Indeed, Raman spectroscopy enables the formula of nesquehonite to be better defined as Mg(OH)(HCO₃)·2H₂O. Copyright © 2008 John Wiley & Sons, Ltd.     

Forest fire retardancy evaluation of carbonate minerals using DTG and LOI

Two methods were employed for measuring fire retardancy of minerals hydromagnesite, huntite and natural hydromagnesite/huntite mixtures, on forest species. The first was based on DTG under N₂ atmosphere, to isolate pyrolysis of forest species and the second on LOI for combustion measurements. The selected forest species: Pinus halepensis Mill. and Cistus incanus L., were collected from a WUI zone and were treated with 5, 10, 15 and 20 mass/mass% of minerals. Regarding DTG analysis, the minerals decrease pyrolysis rate and increase mass residue of forest species. Regarding LOI tests, minerals increase pilot ignitability of forest fuels. Hydromagnesite exhibits the best overall performance.     

Effect of mechanical grinding on the reaction pathway and kinetics of the thermal decomposition of hydromagnesite

Effect of mechanical grinding of hydromagnesite on the reaction pathway and kinetic behaviors of the thermal decomposition process was investigated by means of thermoanalytical techniques, together with crystallographic and morphological measurements. A crystalline hydromagnesite, the as-received sample, was decomposed in two distinguished mass loss steps of overlapped dehydration-dehydroxylation and dehydroxylation-decarbonation via an amorphous intermediate of carbonate compound. Thermal decomposition of an amorphous hydromagnesite, obtained by mechanical grinding of the as-received sample, was characterized by three well-separated decomposition processes of dehydration, dehydroxylation and decarbonation. The kinetic behaviors of the respective decomposition steps were estimated separately using a mathematical deconvolution of the partially overlapped reaction steps. From the formal kinetic analyses of the respective reaction processes, it was revealed that the dehydration and dehydroxylation processes indicate the decelerate rate behaviors controlled by diffusion, while the rate behavior of nucleation limited type is predominant for the decarbonation process.     

十二烷基硫酸钠辅助下低温合成碱式碳酸镁微球

在SDS辅助下,利用氯化镁和碳酸钠溶液在较低温度下(<55℃)反应结晶直接合成碱式碳酸镁微球。利用XRD、FTIR,SEM等技术研究了SDS加入量,反应温度,反应物浓度以及NaCl浓度等合成条件对产物的影响。结果表明:在反应温度低于55℃时,控制反应物浓度小于0.20 mol.L-1,加入一定量的SDS,可以有效抑制无定形颗粒向MgCO3.3H2O生长,促使无定形纳米颗粒通过相转移与自组装直接向碱式碳酸镁4MgCO3.Mg(OH)2.4H2O转变。SDS加入量,反应温度,反应物浓度以及NaCl浓度对碱式碳酸镁微球尺寸和微观形貌均起到调节作用。