水滑石催化尿素与1,2-丙二醇合成碳酸丙烯酯研究

研究了几种不同阳离子组合的类水滑石对尿素与1,2-丙二醇醇解反应的催化性能.结果表明,类水滑石对尿素醇解反应有一定的催化活性,其焙烧产物的催化活性明显提高.当温度为170℃、1,2-丙二醇与尿素的摩尔比为41,催化剂浓度为1.0%,反应时间5 h时,Zn-Al水滑石焙烧产物的催化活性最佳,碳酸丙烯酯的收率95.6%.     

焙烧水滑石对Cr(Ⅵ)的去除性能研究

采用共沉淀法制备了Mg/Al-CO3水滑石,经焙烧得CLDH,用傅里叶红外光谱仪对物相进行表征;利用水滑石焙烧后在一定条件下可重新吸收水和阴离子,从而部分恢复层状结构的结构记忆效应,考察了不同温度焙烧的水滑石去除铬离子[Cr(Ⅵ)]的性能。实验结果表明,400℃下焙烧的水滑石对Cr(Ⅵ)的去除率最高。     

Mg-Al类水滑石催化大豆油酯交换制备生物柴油

采用共沉淀法制备了不同n(Mg)/n(Al)比的Mg-Al类水滑石,在不同温度下焙烧得到复合氧化物,作为大豆油与甲醇反应制备生物柴油的催化剂。结果表明,未焙烧Mg-Al类水滑石的催化活性较差,而n(Mg)/n(Al)=3的类水滑石在450℃焙烧时具有极高的催化活性。在反应温度65℃,醇/油15,催化剂用量为大豆油质量的2%,反应3 h,生物柴油产率可达97.4%。催化剂回收再用性能良好,重复使用3次,生物柴油收率仍在90%左右。     

焙烧水滑石对水泥-粉煤灰胶凝材料水化及力学性能的影响

通过改变粉煤灰掺量,观察了焙烧水滑石增强的胶凝材料力学性能、水化及微观结构特性。抗压强度测试表明,焙烧水滑石能极大提高水泥-粉煤灰砂浆抗压强度。通过X射线衍射及综合热分析实验对硬化水泥浆体相组成进行了测试,结果显示焙烧水滑石能促进水泥-粉煤灰胶凝材料水化,进而提高了水化产物含量。通过扫描电子显微镜观察到,焙烧水滑石能促进粉煤灰溶解,且其成核作用有利于水化产物的生成。     

水滑石焙烧产物对阴离子染料靛蓝胭脂红的吸附特性

碳酸根型水滑石焙烧产物对阴离子染料具有特异的吸附性能。该研究考察了两种具有不同镁铝摩尔比的镁铝复合氧化物对靛蓝胭脂红的吸附性能,并探讨了焙烧温度、投加量、初始染料浓度、溶液初始pH以及共存阴离子这几个因素的影响。结果表明经过500℃焙烧处理后的水滑石对染料的去除效果最好,去除率高达95%,平衡吸附量高达811.5 mg/g（1.74 mmol/g）;且吸附过程不受初始溶液pH和共存阴离子的影响。水滑石焙烧产物直接用于印染废水处理,脱色率达68%~84%。     

响应面法优化焙烧Mg/Al水滑石同时吸附水中F~-和硬度

采用焙烧Mg/Al水滑石同时去除微污染水体中的F~-和硬度。通过Plackett-Burman实验设计选出影响F~-和硬度去除率的主要因素,利用响应面法中Box-Behnken实验设计进行优化设计并得到回归模型。结果表明,pH、反应时间、焙烧Mg/Al水滑石投加量对F~-和硬度的去除率均有显著影响,最佳吸附条件:pH为9.40,反应时间为239.33 min,焙烧Mg/Al水滑石投加量为5.61 g/L。在此最优条件下,F~-和硬度的去除率分别为97.55%、58.09%。     

去除水中腐殖酸的磁性焙烧态类水滑石制备与表征

采用共沉淀法一步合成系列类水滑石负载磁性粒子的颗粒,经煅烧得到磁性焙烧产物.利用焙烧产物吸附水中腐殖酸,得到磁性焙烧态锌铝类水滑石去除腐殖酸效果较好.考察了磁性焙烧态锌铝类水滑石制备条件对腐殖酸去除效果的影响,通过正交试验优化了制备条件.静态吸附实验表明:吸附剂投加量0.2 g/L, 30 min内20 mg/L腐殖酸去除率为97.96%.X射线衍射(XRD)、红外光谱(FT-IR)、热重-差热(TG-DSC)和比表面积(SSA)表征结果表明:一定量的磁性基质掺入并没有破坏锌铝类水滑石典型的层状结构;焙烧态产物为氧化物,磁性保持良好;比表面积达80.00 m2/g.磁性焙烧态锌铝类水滑石在水中因"记忆效应"而结构重建通过表面吸附和腐殖酸结构中小尺寸的官能团插层快速去除腐殖酸.     

Zn-Al水滑石及其焙烧产物对水中磷的吸附研究

用水热法制备了不同尿素浓度下的Zn-Al水滑石,焙烧后制得焙烧态水滑石,用XRD、SEM 、BET、FTIR等方法对样品进行了表征,考察了水滑石及焙烧产物对水中磷酸盐的吸附性能.结果表明:水滑石对磷酸盐的吸附基本符合假二级动力学方程和Langmuir吸附等温式,当尿素浓度为0.6 mol/L,150℃水热24h,300...     

类水滑石催化剂催化合成碳酸二丙酯

采用共沉淀法,在500 ℃烘干焙烧制备了类水滑石催化剂,采用X射线衍射（XRD）、红外光谱（FT-IR）、BET分析对催化剂进行了表征。将类水滑石催化剂应用于碳酸二甲酯（DMC）与正丙醇酯交换合成碳酸二丙酯（DPC）。研究结果表明：镁铝摩尔比为2∶1,在500 ℃焙烧后,类水滑石对反应有较高的催化活性;当丙醇∶DMC =3∶1（摩尔比）、催化剂用量为反应物总质量的1%、反应温度为90 ℃、反应时间为5 h时,DPC的收率为46.87%。     

晶种诱导法水热合成滑石

以乙酸镁、偏硅酸钠为原料、低品位滑石矿为晶种，采用晶种诱导法水热合成滑石。研究了低品位滑石矿焙烧产物在不同焙烧温度和时间条件下的活性，得出适宜的低品位滑石矿焙烧温度并获得高活性滑石矿晶种；以低品位滑石焙烧矿为晶种，考察原料配比、醋酸用量、水热温度、水热时间、晶种用量、p H等对合成滑石的纯度、结晶度的影响。结果表明：在焙烧温度为700℃、焙烧时间为1.5 h条件下获得的低品位滑石焙烧矿晶种的活性最佳；在乙酸镁与偏硅酸钠的物质的量比为3∶4、pH为7、水热温度为180℃、水热反应时间为48 h、加入一定量的低品位滑石焙烧矿晶种的条件下，可以制备出结晶度良好的滑石。     

Thermal shielding performances of nano-structured intumescent coatings containing organo-modified layered double hydroxides

Cone calorimetry tests performed at 50 kW/m² heat flux have been exploited for assessing the fire resistant properties of nano-structured intumescent coatings containing modified layered double hydroxides (hydrotalcites, LDHs) and deposited on steel plates. The effects of different types of modified hydrotalcites (i.e. magnesium–aluminum lactate hydrotalcite, magnesium–aluminum gluconate hydrotalcite, magnesium–aluminum hydrotalcite modified with a fatty acid, magnesium–aluminum hydrotalcite modified with rosin) on the thermal shielding performances of the intumescent coatings and their intumescent degree have been thoroughly discussed and compared with the pristine unfilled counterparts.More specifically, the coatings containing organo-modified LDHs showed better thermal shielding performances with respect to the reference intumescent coating; on the contrary, the use of unmodified hydrotalcite in the intumescent formulations was found detrimental. The thermal shielding performances of the coatings filled with modified LDHs were found to be strictly related to the intumescent degree developed during the cone calorimetry tests. In addition, it was possible to compare the thermal shielding performances of the nanofilled coatings by evaluating the temperatures achieved after 2000 s exposure to the 50 kW/m² heat flux of the cone: the thermal shielding performance sequence was LDH-GL > LDH-RS > LDH-LA > LDH-FA > LDH).Finally, the intumescent degree of the modified coatings was found to decrease with increasing the hydrotalcite content, hence lowering their thermal shielding performances.     

新型催化热分解脱酸催化剂研究

催化热分解脱酸是一种方便且成本低廉的脱酸方法，但脱酸率较低，限制了工业化。通过采用氧化镁、氧化锌、镁铝水滑石和H-ZSM-5作为催化剂活性组分进行脱酸实验，发现镁铝水滑石对催化热分解脱酸具有较高的活性，可作为催化剂的活性组分，从机理方面证明具有催化石油酸分解的作用。对不同制备工艺制备的催化剂进行评价，得出最佳的催化剂制备工艺为：采用机械混合制球法，镁铝水滑石用量为催化剂质量的30%，活性氧化铝为载体，焙烧温度500 ℃。将中海油减二线馏分油与脱酸后油品进行红外分析，表明脱酸后油品中的环烷酸消失，证明镁铝水滑石催化剂具有良好的脱酸效果。     

一种非离子表面活性剂合成工艺的研究

以硝酸镁晶体和硝酸铝晶体为原料,在弱碱性条件下,通过共沉淀法合成出具有水滑石类结构的含Mg-Al基复合物酸/碱双活性位催化剂。该催化剂经过花生酸改性后,用XRD、NH_3-TPD和CO_2-TPD测试表征发现,改性后的催化剂相比未改性的在性能方面有明显提高。通过固定床反应器对醋酸丁酯的乙氧基化催化工艺进行了研究,结果表明自制Mg-Al基复合物酸/碱双活性位催化剂经过花生酸改性后反应活性明显提高,产物乙二醇丁醚醋酸酯1-EBAC和2-EBAC含量显著增大,产品分布变窄。     

铝镁复盐法去除工业废水中硫酸盐的试验研究

以氢氧化镁和水合铝盐作为沉淀剂,采用实验室配制的模拟工业废水,对废水中硫酸根的去除进行研究。考察溶液中氢氧化镁投加量、铝离子的投加量、反应时间、硫酸根的初始浓度、反应温度等因素对硫酸根去除率的影响,并且设置三因素三水平正交试验,在SO_4~(2-)初始质量浓度为2 000 mg/L,溶液体积为50 m L的情况下,得出最佳工艺条件为Mg(OH)_2投加量1.4 g,Al3+投加量0.284 g,反应时间40 min,去除率95.84%;工艺最高去除率可达97.68%。经XRD分析测得沉淀物为镁铝水滑石。     

Characterization of hybrid sol–gel coatings doped with hydrotalcite-like compounds to improve corrosion resistance of AA2024-T3 alloys

The inhibition effect of hydrotalcite addition to hybrid sol–gel coatings applied on AA2024-T3 alloy was evaluated. Hydrotalcite belongs to the anionic clay family with wide applications, most of them based on its anion exchange capacity due to its double layered structure. In this work hydrotalcite (HT) powder was prepared by the classical co-precipitation method using magnesium and aluminum nitrates as precursors. Different weight percentages (1, 5 and 10%, w/w) of hydrotalcite with Mg/Al ratio of 2.5 were added to hybrid sols prepared by copolymerization of 3-Glycydoxypropyltrimethoxysilane (GPTMS) and tetra-n-propoxyzirconium (TPOZ). The sol–gel coatings were deposited by dip-coating method on AA2024-T3 substrate. Scanning electron microscopy (SEM) and mechanical profilometry measurements revealed the heterogeneous particle sizes and the distribution of the agglomerates. Hydrotalcite additions significantly increased the bond strength between metal and coating, according to pull-off test results.The corrosion performance was evaluated by the salt spray fog chamber test and by Electrochemical Impedance Spectroscopy (EIS). The results showed a marked improvement of the corrosion resistance on the aluminum alloy when HT was added to the hybrid sol–gel coating. This positive effect was more evident at higher weight percentages of hydrotalcite.     

改性活性炭脱硫剂脱硫性能的研究

对煤质活性炭改性,包括加压水热活化、浸渍铜氨络合液,通过正交实验对改性活性炭脱硫剂的脱硫性能进行研究。结果表明,改性活性炭脱硫剂的最佳制备工艺条件为:加压水热活化压力为4.052 MPa,CuO/C为2.5%,煅烧温度为500℃,脱硫温度为25℃。各因素对改性活性炭脱硫活性的影响顺序为加压水热活化>煅烧温度>CuO/C>脱硫温度。     

镁铝复合氧化物表面酸碱性对丙酮缩合反应的影响

采用共沉淀法制备不同镁铝比的系列水滑石样品HLDs,水滑石焙烧得到系列镁铝复合氧化物LDOs.分别以吡啶和乙酸为探针分子,采用Fr-IR法对系列LDOs样品的表面酸碱性进行测定,考察镁铝复舍氧化物表面酸碱性对其催化丙酮缩合反应性能的影响.研究结果表明,镁铝物质的量比为3的复合氧化物催化性能较好,丙酮转化率最高可达36....     

活性炭改性对用于甲酸分解的Pd/活性炭催化剂的影响

采用磁力搅拌法和水浴振荡法制备应用于甲酸分解的Pd/活性炭(AC)催化剂,研究了活性炭载体改性和制备方法对催化剂分解甲酸性能的影响。采用恒温水浴振荡装置,在80℃水浴中进行甲酸催化分解反应,以甲酸的催化分解率评价催化剂催化活性。结果表明,以经过不同的酸、碱、盐溶液改性后的活性炭为载体采用不同方法制备的Pd/AC催化剂对甲酸的催化分解效果不同,以Na2CO3改性的活性炭为载体采用磁力搅拌法制备的催化剂活性最好,甲酸水溶液的分解率达85%以上,含甲酸的工业废水的分解率达70%。     

Synthesis of 3-glycidoxypropyltrimethoxysilane modified hydrotalcite bearing molybdate as corrosion inhibitor for waterborne epoxy coating

Zinc aluminum hydrotalcite intercalated with molybdate (HTM) and modified by 3-glycidoxypropyltrimethoxysilane (HTM-GS) was prepared and incorporated into a waterborne epoxy coating. The synthesized HTM-GS was characterized by FTIR, XRD, SEM, and TEM. The inhibitive action of HTM-GS on carbon steel was evaluated using electrochemical measurement and SEM/EDX analysis. The corrosion protection of the waterborne epoxy coating containing HTM-GS was evaluated and compared to that of the pure waterborne epoxy coating and the waterborne epoxy coating containing HTM by salt spray test and adhesion measurement. It was shown that the molybdate was intercalated in the hydrotalcite structure and the molybdate contents in HTM and HTM-GS were 16.0 and 13.2 wt%, respectively. The polarization curves obtained on the carbon steel electrode showed that HTM and HTM-GS are anodic corrosion inhibitors, and their inhibition efficiencies at concentration of 3 g/l were 92.0 and 94.7%, respectively. Additionally, HTM and HTM-GS at concentration of 0.5 wt% improved corrosion resistance and adhesion of waterborne epoxy coatings. Surface modification by 3-glycidoxypropyltrimethoxysilane ameliorated the dispersion of HTM in epoxy matrix and the effect of HTM on protection properties of waterborne epoxy coating.     

Studies on Hydrotalcite‐Catalyzed Synthesis of Poly(ethylene terephthalate)

Summary: The hydrotalcite‐catalyzed synthesis of PET was studied to clarify the effect of hydrotalcite properties on its catalytic activity. Hydrotalcite was modified by various treatments to tune its activity as a polycondensation catalyst. Hydrotalcite activity was found to decrease upon calcination. However, rehydration of the calcinated hydrotalcite resumed the catalytic activity. The hydrotalcite activity depends on the ratio of magnesium to aluminum cations in its composition, and highest activity occurs at a molar ratio of 2:1. Replacement of the carbonate anions of hydrotalcite by more nucleophilic ones like hydroxide and alkoxide groups resulted in improved catalytic activity. Hydrotalcite has two assembly orders: primary lamination of sheets into plates and secondary agglomeration of plates into particles. Hydrotalcite with larger sheet size showed lower activity. On the other hand, milling of hydrotalcite particles did not affect its activity as it probably enters the reaction on a plate level, which is not affected by milling. Polycondensation resulted in expansion of the hydrotalcite sheets under the effect of formed polymer. Reuse of hydrotalcite after polycondensation followed by depolycondensation resulted in a large activity enhancement.

High‐resolution SEM micrograph of calcinated HT after rehydration.