固体酸催化合成乙酸环己酯评述

固体酸是有机合成中能够替代硫酸的良好催化剂。评述了磺酸、无机盐、固体超强酸、杂多酸和分子筛等固体酸催化合成乙酸环己酯的方法。认为甲烷磺酸盐、氨基磺酸、强酸性阳离子交换树脂、结晶硫酸氢钠、固体超强酸和杂多酸适合催化合成乙酸环己酯。     

环己烯水合生成环己醇过程研究

本文以阳离子交换树脂A-36为催化剂,在高压间歇反应釜中研究了添加异佛尔酮作为助溶剂的环己烯直接水合制备环己醇工艺,以得到环己烯水合反应较佳的工艺条件。实验表明,环己烯水合反应的最优化工艺条件为反应温度120℃、催化剂浓度15%、搅拌器转速1000r/min阳离子交换树脂的粒径在小于0.6mm,水油两相比为4∶1,环己醇收率达到15.87%。     

阳离子交换树脂催化制备顺丁烯二酸二乙酯

顺丁烯二酸二乙酯是高效低毒农药——马拉松的重要中间体。目前国内大都采用硫酸催化,苯、酒精、水三元共沸脱水的方法生产。为了消除生产过程中苯的泄漏对操作车间的污染并减化生产工艺,我们采用阳离子交换树脂为催化剂,制备顺丁烯二酸二乙酯。磺酸型阳离子交换树脂,具有可交换基团——SO_3H,凡能被H_2SO_4催化的有机反应,原则上均可被磺酸型阳子交换树脂催化,根据这个原理,我们采用几种不同类型的磺酸     

阳离子交换树脂催化合成丙烯酸环己酯

以丙烯酸和环己烯为原料,磺酸基苯乙烯系强酸性阳离子交换树脂为催化剂合成丙烯酸环己酯,考察了反应温度、催化剂用量、烯酸摩尔比、反应时间对酯化反应的影响.结果表明,合成丙烯酸环己酯的最佳条件为:反应温度85℃,催化剂质量分数5%,n(酸)∶n(烯)=2∶1,反应时间5h.在最佳工艺条件下,环己烯转化率为87.2%,丙烯酸环...     

离子交换法治理尾矿水可溶性盐的研究

工业废水的脱盐方法主要是:电渗析、反渗透、离子交换及相变。某磷矿选矿尾矿水含盐4356毫克/升,选用磺酸型阳离子交换树脂,脱除尾矿水中的阳离子,而将树脂上的氢还原并与水中SO_4~(2-)形成硫酸又返回浮选作来,代替了选别作业中硫酸,这样,把浮选作业与尾矿水脱盐治理视为一个封闭     

固体酸催化合成丁酸戊酯

评述了强酸性阳离子交换树脂、磺化聚氯乙烯、六水三氯化铁、树脂固载三氯化铁、五水四氯化锡、二水氯化亚锡、氯化锌、树脂固载三氯化铝、水合硫酸铁、复合硫酸铁、硫酸铜、硫酸镓、一水硫酸氢钠、硫酸氢钾、固体超强酸、杂多酸和分子筛等催化合成丁酸戊酯的方法。认为强酸性阳离子交换树脂、磺化聚氯乙烯、树脂固载三氯化铁、树脂固载三氯化铝、复合硫酸铁、一水硫酸氢钠、固体超强酸、杂多酸和分子筛等是合成丁酸戊酯具有实用价值的催化剂。     

固体酸催化环己醇脱水制备环己烯

评述了对甲苯磺酸，五水四氯化锡、二水氯化亚锡、六水三氯化铁、一水合硫酸氢钠、Ti^4＋-、阳离子交换树脂、固体超强酸、杂多酸和沸石分子筛催化环己醇脱水制备环已烯的方法，并指出固体超强酸、条多酸和沸石分子筛是环己醇脱水制备环己烯的优良催化剂。     

丙酸烯丙酯合成用催化剂述评

评述硫酸、六水三氯化铁、二水氯化亚锡、十二水合硫酸铁铵、硫酸铜、一水硫酸氢钠和强酸性阳离子交换树脂催化合成丙酸烯丙酯的方法。综合评价后认为,六水三氯化铁、二水氯化亚锡和强酸性阳离子交换树脂是在合成丙酸烯丙酯中具有实用价值的催化剂。     

(四) Lewatit S100 (200-4)

氢型Tewatit S100离子交换树脂再生剂:硫酸(H_2SO_4) Tewatit S100为带磺酸酒柱荃西的聚苯乙烯阳离子交换树脂。其特点是具有高的交换容量,特别好的化学稳定性及好的机械强度。     

离子交换树脂磺化后处理新工艺的研究

本文介绍了001×7强酸性苯乙烯系阳离子交换树脂磺化后处理一种新的工艺,即采用碱性食盐水处理磺酸球。该新工艺具有不产生低浓度废硫酸、治理公害、节约水资源降低成本等特点。     

固体酸催化合成乙酸异戊酯研究进展

综述了对甲苯磺酸及对甲苯磺酸钙、氨基磺酸、甲磺酸、甲磺酸铜、阳离子交换村脂、Hβ型沸石、FeY、硫酸锌、硫酸钛、氯化铁、十二水硫酸铁铵、一水合硫酸氢钠、五水四氯化锡、硫酸铝钾、杂多酸和固体超强酸催化合成乙酸异戊酯的方法。指出了上述固体催化剂是合成乙酸异戊酯的优良催化剂。     

Methanesulfonic acid catalyzed additions to oleic acid and cyclohexene. III. Addition of acids and substituted phenols

Benzoic acid adds to oleic acid in methanesulfonic acid as catalyst-solvent to form an addition product in 30% yield. Saponification studies on the product reveal that the addition is made via the carboxyl group and no rearrangement of the initial product takes place. A number of substituted benzoic acids were also tried but the yield of addition product was nil. Data are included for the experiments with a number of phenols not previously reported. These include: o-chlorophenol,2,6-di-tert.-butylphenol, 2,4,6-trichlorophenol, resorcinol, 5-n-pentadecylresorcinol, hydroquinone, methyl salicylate, and 3-n-pentadecylphenol. Good yields of addition products of cyclohexene are obtained using methanesulfonic acid as catalyst-solvent and the same nucleophiles employed previously. Presented at the AOCS meeting in Toronto, Canada, 1962. A laboratory of the E. Utiliz. Res. & Dev. Div., ARS, U.S.D.A.     

Synthesis of Aromatic Polyketones by Direct Polycondensation Between Terephthalic Acid and Diaryl Compounds

A convenient method for the synthesis of a new series of polyarylketones with relatively high molecular weights has been investigated. The polymers were prepared readily by direct polycondensation of terephthalic acid with a series of diaryl compounds using phosphorous pentoxide/trifluoromethanesulfonic acid (w/w = 1/10), phosphorous pentoxide/methanesulfonic acid (w/w = 1/10), and aluminum chloride/phosphorous oxychloride (w/v = 1/3) as condensing agents. Among the three, the phosphorous pentoxide/trifluoromethanesulfonic acid pair was found to be most efficient and was studied in detail. The thermal and crystalline properties of the resulting polyarylketones were characterized. All of the polyketones prepared in the present study are crystalline and their glass transition temperatures and melting points depend greatly on the structure of the diaryl compounds employed.     

液晶单体4-(反-4-正丙基环己基)-氟苯的合成

以新蒸馏过的环己烯和丙酰氯为原料,与三氯化铝和氟苯一起采用“一锅法”制备4-(4-丙酰基环己基)-氟苯。首先将环己烯与丙酰胺的混合物在搅拌下于-10℃逐滴加入到三氯化铝的氟苯悬浮液中,而后将该反应混合物在40℃下搅拌反应2h即可得4-(4-丙酰基环己基)-氟苯。环己烯、丙酰氯、三氯化铝、氟苯投料摩尔比为1∶1∶1.5∶2。第二步反应是用黄鸣龙法将4-(4-丙酰基环己基)-氟苯还原为4-(反-4-正丙基环己基)-氟苯。最后经减压蒸馏和数次重结晶得到纯度大于99.5%的产品4-(反-4-正丙基环己基)-氟苯。     

Lucas试剂催化环己醇脱水制备环己烯的研究

lucas试剂通常作为醇的氯化试剂,但当在适当的条件下——催化环己醇反应,可以作为脱水剂生成环己烯。本文探索了lucas试剂作为环己醇的催化脱水试剂的最佳实验条件。当催化剂中盐酸(V)∶氯化锌(M)为1∶1,反应时间为83 min,环己烯的收率约为68%。     

Aluminum bisphenoxides: Promising challengers for a catalyzed copolymerization of cyclohexene oxide with CO2

Reacting triethyl aluminum and diethyl aluminum chloride with the chelating bisphenol ligands mdtbpH2 and mmcpH2 [mmcpH2: 2,2′-methylenebis(4-methyl-6-(1-methyl-cyclohexyl)phenol); mdtbpH2: 2,2′-methylenebis(4,6-di-tert-butyl-phenol)] afforded monomeric and dimeric aluminum bisphenoxides with reactive Al–Cl and Al–C₂H₅ moieties. We present here the X-ray structure determination of some of the isolated compounds as well as the preliminary catalytic tests in copolymerization reactions with cyclohexene oxide and carbon dioxide.     

1-甲基-1,2,3,4-四氢异喹啉的合成工艺改进

以苯乙胺为原料,经乙酰化反应得乙酰苯乙胺(3),在甲基磺酸的作用下环合得1-甲基-3,4-二氢异喹啉(4),经硼氢化钠还原得1-甲基-1,2,3,4-四氢异喹啉(1)。改进了合成工艺,总收率达80.8%。     

Study of TATP: Spontaneous Transformation of TATP to DADP

TATP, prepared in the presence of catalysts methanesulfonic, perchloric, or sulfuric acid, has been found to undergo transformation to DADP. However, no transformation occurs if TATP is purified or prepared involving catalysts such as hydrochloric acid, tin(IV) chloride, and nitric acid. The transformation has been monitored by the methods of DTA and HPLC.     

Isomeric linear phenylalkanes and sodium alkylbenzenesulfonates

Linear phenylalkanes made from 12, 14, 16 and 18 carbon α-olefins and benzene, with aluminum chloride or methanesulfonic acid as the condensing agent, were found by gas-liquid chromatography of the acetophenone homologs obtained by chromic acid oxidation to be a mixture of all possible internal position isomers. Product distribution measured by the relative amounts of acetophenone homologs must be corrected in the case of the 2- and 3-phenylalkanes because of unequal oxidative scission and differing ease of oxidation. The 2-phenyl isomer, formed in largest amount and presumably the highest melting isomer, was separated by low temperature crystallization from acetone. The phenylalkane product mixtures and the isolated 2-phenyl isomers were sulfonated and detergent and surface active properties were compared. The sodiump-alkylbenzenesulfonates from the 2-phenylalkanes were more biodegradable than the mixtures in the river water die-away test. Presented in part at the AOCS Meeting, Cincinnati, October, 1965. E. Utiliz. Res. Dev. Div., ARS, USDA.     

聚合氯化铝的合成

介绍了以铝灰和盐酸为原料制备聚合氯化铝的方法,讨论了投料比、加水量,反应时间,盐酸浓度等对产品的影响。