KOH活化木屑生物炭制备活性炭及其表征

以木屑热裂解的生物质炭为原料,氢氧化钾为活化剂,采用化学活化法制备活性炭,探讨了碱炭比、活化温度和活化时间对活性炭吸附亚甲基蓝吸附值的影响。 利用N2吸附实验、XRD和FTIR等实验技术,对原料与制备活性炭的结构与性能进行了表征。 结果表明,在碱炭质量比为1.5、活化温度750 ℃、活化时间2 h的条件下,所制备的活性炭对亚甲基蓝吸附值为255 mg/g,BET总比表面积为1514 m2/g,中孔比表面积为110 m2/g,吸附总孔容为0.821 cm3/g,中孔孔容为0.117 cm3/g,吸附平均孔径为2.170 nm。     

KOH活化糠醛渣制备活性炭机理与表征

以糠醛渣为原料、KOH为活化剂,采用两步活化法制备了活性炭。考察了活化温度、活化时间、碱炭比和浸渍时间对活性炭孔结构及吸附性能的影响。采用低温N2吸附、BET、BJH及DFT理论对活性炭孔结构进行了表征分析,利用傅里叶变换红外-拉曼光谱仪检测其表面官能团,分别使用扫描电镜和X射线衍射对其进行表观形貌观察和晶型分析。结果表明,制备活性炭的最佳工艺条件为:活化温度800℃、活化时间3h、碱炭比3∶1、浸渍时间12h。所制备的糠醛渣活性炭的吸附孔径分布集中,吸附孔容为0.8825cm2/g,DFT总比表面积为3290.5m2/g,其碘吸附值和亚甲基蓝吸附值分别为2107.32mg/g和39.67mL/0.1g。     

KOH活化糠醛渣制备活性炭及其表征

以糠醛渣为原料、KOH为活化剂,采用两步活化法制备了活性炭。考察了活化温度、活化时间、碱炭比和浸渍时间对活性炭孔结构及吸附性能的影响。采用低温N2吸附、BET、BJH及DFT理论对活性炭孔结构进行了表征分析,利用傅里叶变换红外-拉曼光谱仪检测其表面官能团,分别使用扫描电镜和X射线衍射对其进行表观形貌观察和晶型分析。结果表明,制备活性炭的最佳工艺条件为:活化温度800℃、活化时间3h、碱炭比3∶1、浸渍时间12h。所制备的糠醛渣活性炭的吸附孔径分布集中,吸附孔容为0.8825cm2/g,DFT总比表面积为3290.5m2/g,其碘吸附值和亚甲基蓝吸附值分别为2107.32mg/g和39.67mL/0.1g。     

水蒸气活化制备烟杆基颗粒活性炭的研究

以烟杆废弃物为原料,以木焦油为主的复合粘结剂,通过水蒸气活化制备了烟杆基颗粒活性炭.对影响颗粒活性炭吸附性能和收率的因素如活化温度、活化时间、水蒸气流量进行了系统研究,得到了最佳工艺条件:活化温度为900℃,活化时间为60 min,水蒸气流量为3.31 g/min.该工艺条件下,烟杆基颗粒活性炭对碘的吸附值为1028 mg/g,对亚甲基蓝的吸附值为285 mg/g,收率为24.39%.同时,测定了该活性炭氮吸附,通过BET计算了活性炭的比表面积,并通过密度函数理论(DFT)表征了活性炭的孔结构.结果表明,该活性炭为微孔型,BET比表面积为1073 m2/g,总孔容为0.8152 ml/g.     

利用除尘灰制备活性炭的工艺研究

以除尘灰为原料，用物理活化法制备活性炭．研究了活化温度、活化时间、活化剂流量对活性炭性能的影响．实验结果表明，活化温度和活化时间对活性炭的BET比表面积和吸附性能有很大影响；该方法可制得1nm以下微孔和10nm以下中孔均比较发达的活性炭．     

微波辐射在制备竹节活性炭中的应用研究

研究了以竹节废料为原料，采用微波辐射氯化锌法制备优质活性炭的可行性．探讨了微波功率．活化时间及氯化锌浓度对产品各项指标的影响．得到了微波辐射氯化锌法制备活性炭的最佳工艺：微波功率350W、活化时间5min、氯化锌浓度40%．用此工艺制得的活性炭碘吸附值1088．4mg／g、亚甲基蓝脱色力22．0ml/0．1g．得率39．2％．该工艺所需活化时间为传统方法的1／36，产品活性炭亚甲基蓝脱色力为国家一级标准的1．83倍(GB/T13496.10-1999)．微波辐射法所制活性炭比传统方法所制活性炭具有更加发达的孔隙结构，且孔隙的分布更加均匀．     

活化赤泥对染料废水吸附性能研究

以赤泥为原料,十二烷基苯磺酸钠为活化剂,制备出活化赤泥吸附剂,并对亚甲基蓝(MB)染料废水吸附性能进行研究。结果表明,活化赤泥对亚甲基蓝的吸附效果有一定提高。振荡时间15min,活化赤泥6g·L~(-1),中性条件下,对40mg·L~(-1)亚甲基蓝吸附率可达90%。吸附符合Langmuir和Freundlich吸附等式,最大吸附量为16.37mg·g~(-1)。活化赤泥吸附亚甲基蓝为放热反应,低温利于亚甲基蓝吸附。     

关于亚甲基蓝在活性炭表面吸附投影面积σA的探讨

溶液吸附法测定活性炭比表面积是大学本科基础物理化学实验中一个较重要的实验.亚甲基蓝在活性炭表面的吸附符合Langmuir单分子层吸附,但按照实验教科书及文献介绍的溶液吸附法测定活性炭比表面积的方法,大量学生实验的测定结果比活性炭实际比表面积偏低很多.本文以BET表面吸附装置测定活性炭比表面积,再以溶液吸附法测定了亚甲基蓝在活性炭表面的最大吸附量Γ∞,计算了亚甲基蓝在活性炭表面吸附投影面积σA.结果表明亚甲基蓝在活性炭表面可能不是端基吸附,而是平面吸附,分子的投影面积σA应为1.35×10-18 m2.     

微波辐射紫茎泽兰制备优质活性炭的研究

以紫茎泽兰为原料,碳酸钾为活化剂,采用超声波浸渍,微波辐射法制备活性炭.研究了浸渍方式与时间、微波功率、微波辐射时间、剂料比对活性炭吸附性能和得率的影响.得到了本实验条件下的优化工艺条件:超声波浸渍20min、120℃脱水2h,微波功率700W、微波辐射时间12min、剂料比1.25∶1.优化工艺条件下制备的活性炭碘吸附值为1470.27mg/g,亚甲基蓝吸附值为300mL/g,得率为16.35%.浸渍时间极大的缩短,微波辐射时间只有传统法活化时间的1/15左右,活性炭的吸附指标超过了国标GB/T 13803.1-1999和GB/T 13803.2-1999一级品的标准,其中碘吸附值是国家一级标准的1.47倍,亚甲基蓝吸附值是国家一级标准的2.73倍.同时,测定了该活性炭氮吸附,其BET比表面积为1540.97m2/g,总孔容为0.7393mL/g,并通过DFT表征了活性炭的孔径分布,结果表明该活性炭为微孔型活性炭.     

棕榈纤维制备活性炭纤维及其对水中三氯生的吸附研究

以棕榈纤维为原材料、磷酸为活化剂制备活性炭纤维,通过单因素实验和正交实验深入探讨反应条件对活性炭纤维吸附性能的影响,并确定最佳制备条件。系统研究三氯生在活性炭纤维上的吸附热力学、动力学以及溶液p H值对吸附的影响,并研究比较乙醇洗脱与加热煅烧法对吸附饱和后的活性炭纤维的再生效果。结果表明,磷酸溶液质量分数和碳化温度对活性炭纤维吸附性能影响较大,活化剂浸渍时间对其影响较小,活性炭纤维的最佳制备条件为:磷酸溶液浓度25%,碳化温度400℃,活化时间36h。所制备的活性炭纤维的BET比表面积为1358.478m~2/g、微孔面积为1240.131m~2/g、平均孔径为1.886nm。活性炭纤维对三氯生的吸附等温线符合Langumuir方程,吸附是放热反应。动力学研究表明,吸附反应符合准二级动力学方程,且在5h后基本达到平衡。随着p H值的升高,材料对三氯生的吸附量略有下降。乙醇洗脱和加热煅烧均可有效再生吸附饱和后的活性炭纤维。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

Microwave-assisted copper-catalyzed stereoselective ring expansion of three-membered heterocycles with α-diazo-β-dicarbonyl compounds

Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular S_N2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.