掺锑氧化锡纳米晶体的制备及性能研究

以SnCl4.5H2O和SbCl3乙醇溶液为原料,用离子交换除氯水解法制备得到无氯离子的前驱体掺锑氢氧化锡胶体沉淀。采用了乙酸异戊酯有机溶剂作脱水剂以消除掺锑氢氧化锡胶体干燥过程中硬团聚的形成,并和常用的正丁醇共沸溶剂进行了粉体性能的比较。用BET、XRD和TEM等方法对前驱体和掺锑氧化锡纳米粉体进行表征。结果表明,乙酸异戊酯溶剂比正丁醇溶剂更有效防止了粉体干燥过程中硬团聚的形成;将乙酸异戊酯干燥所得掺锑氢氧化锡干粉经热处理后得到了高比表面积的掺锑氧化锡纳米粉体,并对晶粒的生长过程进行了研究。     

纳米层状双金属氢氧化物的制备及结构表征

采用恒定pH 12±0.2,按n(Mg2+)∶n(Al3+)∶n(OH-)∶n(CO2-3)=6∶2∶16∶1配制溶液,采用一步反应液相法,制备纳米层状双金属氢氧化物(LDH)粉体.为了获得无团聚、分散均匀的纳米粉体,探讨了溶剂置换干燥、真空干燥、常压干燥对纳米LDH粉体形成团聚的影响;用X射线衍射仪、透射电镜、红外光谱仪和元素分析仪对样品的物相、形貌、粒径和组成进行了表征.结果表明,溶剂置换干燥能够有效防止纳米粉体形成硬团聚,样品分散性好,呈针状形态,长50 nm,宽5 nm.     

白炭黑结构对胎面胶性能的影响

从堆积状态和比表面积两方面研究不同结构白炭黑对胎面胶性能的影响。结果表明：对于相同堆积状态、不同比表面积的白炭黑,白炭黑的比表面积越大,其填充胶料的混炼温升越高,混炼功率越大,加工难度也越大;随着白炭黑的比表面积增大、初生粒径减小,白炭黑的团聚体增多,分散性变差;对于相同比表面积(200 m~2·g^-1)、不同堆积状态的白炭黑,气相法白炭黑A200在橡胶基体中的分散性最好,沉淀法白炭黑200MP的分散性次之,沉淀法白炭黑200GR的分散性最差;相比于沉淀法白炭黑200MP和200GR,气相法白炭黑A200可以同时增强和增韧硫化胶,并减小硫化胶的滚动阻力和磨耗量,但是硫化胶的抗湿滑性能较差。     

成核阶段对沉淀法白炭黑团聚程度的影响

白炭黑制备过程中发生的团聚会影响其分散性,研究影响白炭黑制备过程中团聚程度的主要因素有助于制备高分散的白炭黑。本文采用正交实验法研究了沉淀法白炭黑制备过程中成核阶段各个因素对白炭黑团聚程度的影响,采用透射电镜表征白炭黑一次粒子大小和团聚程度,采用激光粒度仪表征白炭黑的平均粒径。结果表明,反应温度、硅酸钠浓度及加酸速度是影响白炭黑二次粒子平均粒径及团聚程度的主要因素;高温下,白炭黑一次粒子约为50 nm,团聚程度较高,但二次粒子平均粒径较小;低温下,白炭黑一次粒子约为10 nm,团聚程度略小。随着低温反应时间的增长,白炭黑一次粒子团聚程度增加。     

超剪切在沉淀白炭黑分散细化中的研究

二氧化硅是高比表面积的粉体物料,在水中形成极易团聚的沉淀白炭黑。为全面提高其分散性,使其平均粒径达到2—5μm,利用最新的超剪切技术,对沉淀白炭黑进行分散细化处理,研究了基于超剪切过程的原理和方法,并通过响应面实验对沉淀白炭黑进行了分散细化实验研究,结果表明超剪切技术对易团聚、难分散的液固态物料的分散细化具有极佳的效果。     

干燥方法对化学沉淀法合成HA粉体团聚的影响

化学沉淀法合成羟基磷灰石粉体工艺简单,成本低廉,但这种方法得到的羟基磷灰石粉体极易团聚,限制了羟基磷灰石的广泛使用.本文研究了在羟基磷灰石粉体的合成过程中不同干燥方法对粉体团聚的影响.结果表明:在烘箱干燥得到的粉体团聚较严重,微波干燥使粉体的团聚程度有所减轻,冷冻干燥可有效地减弱粉体的团聚,所得到的粉体比表面积较高.同时,本文还讨论了粉体在干燥过程中团聚形成的机理.     

锑掺杂氧化锡纳米粉体的制备研究

以五水氯化锡和三氯化锑乙醇溶液为原料制备得到前驱体锑掺杂氢氧化锡胶体沉淀,采用乙酸异戊酯共沸干燥法对前驱体进行干燥;用XRD,TEM,IR,BET等方法对粉体的物相、形貌、分散性和比表面积进行表征.结果表明,乙酸异戊酯干燥所得的锑掺杂氢氧化锡微粉经热处理后得到了团聚少、分散性好、晶体颗粒小、粒度均匀的锑掺杂氧化锡纳米粉体.     

高分散性纳米碳酸钙的制备及表面改性研究

研究了利用共沸蒸馏来克服纳米碳酸钙粒子在干燥过程中形成硬团聚的可行性,采用直接在正丁醇中加入改性剂的新工艺进行了表面改性。确定了改性剂最佳用量为3％,利用TEM、DTA-TG、BET粒度分布等手段进行了表征,探讨了共沸蒸馏克服硬团聚的机理。结果表明,共沸蒸馏后可制得分散性好的纳米碳酸钙;改性后,粒子的分散性得到了进一步的提高。     

从伯方煤矸石中提取SiO2的试验研究

以伯方煤矸石酸浸提取A12O3后的残渣为原料制备SiO2,讨论了反应温度、反应时间、碱渣比、液固比对SiO2浸出率的影响.实验结果表明,反应时间、碱渣比、液固比对SiO2浸出率影响较大.经正交试验确定了最佳工艺条件:反应温度90℃,反应时间90 min,碱渣比1.4,液固比3∶1,此时SiO2浸出率达56.37％.XRD分析发现,所得产品为非晶态白炭黑,与标准SiO2 XRD衍射图谱相比可知,实验得到的白炭黑孔多、比表面大.SEM分析表明,制得的白炭黑是由小颗粒团聚而成的不规则球形颗粒,平均粒度为250 nm左右,白炭黑颗粒与颗粒相互连接,形成三维的网状结构.     

锌-钆抗菌白炭黑粉体的改性及抗菌性能研究

通过溶胶-凝胶法制备了锌-钆抗菌白炭黑.通过添加表面活性剂对材料进行改性,并探究了材料改性前后的粒径、比表面积和抗菌性能变化.采用粒度分析、BET、SEM和EDS等手段对样品进行表征.结果表明改性后材料的粒径减小,粒度分布相对集中,比表面积增大至275.20209m2/g.并对材料进行抗菌性能检测,结果表明改性后材料的抗菌性能有一定的增强,锌-钆抗菌白炭黑的杀菌率可达90.29％.     

Effect of different drying techniques on silaning efficiency

Colloidal drying is a method that is used in many areas but leads to particle agglomeration. In this study, the effects of drying methods on the agglomeration, dispersion, and silanization efficiency of silica nanoparticles (NSp) were investigated using vacuum oven dryer (VOD), rotary evaporator (RE), and freeze-dryer (FD) methods. In addition, dried silica nanoparticles were mechanically ground using a conventional ball mill system, and the relationship between grinding effect and agglomeration was investigated. The results of the SEM analysis showed that the surface energy, which increased with the reduction of the grain size as a result of the prolongation of the grinding time, caused the agglomeration of the grains. BET analysis, it was observed that the surface areas of silica nanoparticles vary depending on the drying method. Contact angle measurement was performed to investigate the silanization ability of silica nanoparticles and it was determined that silica nanoparticles with the low surface area had the lowest contact angle. Therefore, the silanization ability of silica nanoparticles was observed to increase with the reduction of agglomeration. As a result, the VOD technique, which allows the production of low surface area silica nanoparticles, was chosen as the best method for increasing the silanization efficiency.     

添加剂对气凝胶孔径分布的影响

以稻壳灰为硅源,在适宜的凝胶形成条件下,加入不同添加剂(羟基类和酰胺类有机物),通过溶胶-凝胶、溶剂置换过程及超临界二氧化碳干燥工艺制备了硅气凝胶. 结果表明,丙三醇、乙二醇添加量为15%~20%时调控作用显著,凝胶孔洞变小且分布更均匀,比表面积增大、平均孔径减小;聚乙二醇使凝胶化时间缩短,孔径分布较均匀;二甲基甲酰胺、甲酰胺调控效果最显著,所得样品孔径集中分布于20~40 nm,比表面积均在750 m2/g以上. 聚乙烯吡咯烷酮可加快缩聚速率,使小孔比例大幅增加,网络结构致密.     

Impact of agitated drying on the powder properties of an active pharmaceutical ingredient

In this study, the impact of agitated drying on the physical and bulk powder properties of an active pharmaceutical ingredient (API) is presented. The effects of different agitated drying conditions such as agitation rate, drying temperature, drying time pre-agitation, drying time during agitation and number of solvent wash cycles on the bulk density, millability, flow and specific surface area is reported. The crystal morphology is altered from fibrous needles to agglomerates when switching from tray to agitated drying. An increase in bulk density and specific surface area was evident when using agitated drying compared to tray drying as hard coarse granules were produced with an increase in the number of fine particles < 10 μm. The bulk density was found to increase with an increase in agitation speed, drying time and number of solvent wash cycles used during filtration. Controlling both fine and coarse particle size of the granules for this API during agitated drying was difficult to achieve due to the fibrous crystal habit. However, the increase in the bulk density observed has the potential to facilitate improvements in the ease of drug product development. In the case of this system further particle size control was required through the use of dry milling.     

Effects of Solvent Exchange Period and Heat Treatment on Physical and Chemical Properties of Rice Husk Derived Silica Aerogels

In this study, hydrophobic silica aerogels were synthesized from rice husk ash-derived sodium silicate through sol-gel processing, solvent exchange, surface modification and ambient pressure drying. By volume, 10% of trimethylchlorosilane (TMCS) in 90% of n-hexane was used as a hydrophobic solution in the surface modification process. The physical and chemical properties of silica aerogels were characterized by density and porosity measurements, scanning electron microscopy (SEM), Fourier transforms infrared (FTIR) spectroscopy, Brunauer–Emmett–Teller theory (BET) and dynamic scanning calorimetry (DSC). The hydrogels prepared were in the form of 2.5 ± 0.5 mm beads and then converted into alcogels through solvent exchange with ethanol for repetition of 3, 6 and 9 days. It is found that the optimal quality of silica aerogels with the BET surface area as high as 668.82 m²/g was obtained from the alcogels of the solvent exchange period of 9 days. Depending on the size of the gel’s block, a longer solvent exchange period will ensure adequate removal of pore water. Post heat treatment on silica aerogels obtained from the 9 days of solvent exchange at 200, 300 and 400 °C for 2 h results in slight decreased of aerogel’s density from 0.048 g/cm³ to 0.039 g/cm³ and the hydrophobicity of the aerogels is decreased above 380 °C as confirmed by DSC analysis.

     

Effect of aging temperature on the porosity characteristics of subcritically dried silica aerogels

Silica aerogels were synthesised by subcritical drying technique which involves controlled solvent exchange and aging of the wet gel in silane solution followed by drying under controlled conditions. Effect of temperature of aging in silane solution on the porosity characteristics of silica aerogels and the thermal pore stability of the resultant gels were investigated. Aging in silane solution leads to an increased degree of condensation reactions, siloxane crosslinking and the dissolution and reprecipitation of silica monomers to the gel structure and enhances the total strength of the gel. Thermal aging of the wet gel have a pronounced effect on bulk density, linear drying shrinkage, surface area and pore volume. As the temperature of aging increases the bulk density decreases whereas the surface area and pore volume were found to increase. We could achieve a surface area of 1040 m²/g, pore volume 1.2 cc/g and an average pore size of 49 Å corresponding to an aging temperature of 70 °C. Thermal pore stability of the gel was found to be up to 700 °C above which densification of SiO₂ gel starts. The novel findings will help in tailoring the process parameters to prepare mesoporous oxides from sol–gel precursors with specific pore features.     

二氧化硅气凝胶的制备和表征

以正硅酸四乙酯为硅源，通过采取老化、表面修饰、溶剂置换和分级干燥等一系列抑制二氧化硅气凝胶干燥中出现缩裂的有效措施，以非超临界干燥技术最终获得了大块无裂纹的二氧化硅气凝胶。该气凝胶的孔径较小且分布均匀，比表面积为684m^2／g，孔体积可达1．38cm^3／g，最可几孔径为3．221nm，平均孔径达2．871m。同时在实验和理论分析的基础上总结二氧化硅气凝胶缩裂的主要原因和抑制缩裂的有效措施。     

Effect of sodium bicarbonate solution on methyltrimethoxysilane-derived silica aerogels dried at ambient pressure

Here we present an economical ambient pressure drying method of preparing monolithic silica aerogels from methyltrimethoxysilane precursor while using sodium bicarbonate solution as the exchanging solvent. We prepared silica aerogels with a density and a specific surface area of 0.053 g∙cm⁻³ and 423 m²∙g⁻¹, respectively. The average pore diameter of silica aerogels is 23 nm as the pore specific volume is 1.11 cm³∙g⁻¹. Further, the contact angle between water droplet and the surface of silica aerogels in specific condition can be as high as 166°, which indicates a super-hydrophobic surface of aerogels.     

Preparation of silica aerogel from oil shale ash by fluidized bed drying

The silica aerogel with high specific surface area and large pore volume was successfully synthesized using oil shale ash (OSA) via ambient pressure drying. The oil shale ash was burned and leached by sulfuric acid solution, and then was extracted using sodium hydroxide solution to produce a sodium silicate solution. The solution was neutralized with sulfuric acid solution to form a silica gel. After washing with water, the solvent exchange with n-hexane, and the surface modification with hexamethyldisilazane (HMDZ), the aged gel was dried by fluidization technique and also using a furnace to yield silica aerogels. The physical and textural properties of the resultant silica aerogels were investigated and discussed. The results have been compared with silica aerogel powders dried in a furnace. From the results, it is clear that the properties of silica powders obtained in fluidized bed are superior to that of powders dried in the furnace. Using fluidization technique, it could produce silica aerogel powders with low tapping density of 0.0775 g/cm³, high specific surface area (789 m²/g) and cumulative pore volume of 2.77 cm³/g.     

有机-无机杂化柔性硅气凝胶的制备与表征

以甲基三甲氧基硅烷（MTMS）和四乙氧基硅烷（TEOS）为混合硅源、甲醇为溶剂,通过酸碱两步催化溶胶-凝胶法制备湿凝胶,经超临界流体干燥得到块状二氧化硅气凝胶。用扫描电镜、氮气吸附脱附测试以及热重分析等手段对气凝胶的微观形貌、比表面积、孔径分布、弯曲性、压缩性、热稳定性等进行研究,结果表明：MTMS/TEOS比例会影响气凝胶的微观结构、弯曲和压缩性以及热稳定性,以MTMS/TEOS=8/1制得的气凝胶密度为0.11 g·cm^-3、孔隙率为94.2%、比表面积为693.3 m²·g^-1、最大弯曲角可达92°、最大压缩比例可达41.2%、压缩回弹率为100%。