4-(6′甲基苯并噻唑-2′-偶氮)-3,5-二氨基吡唑与钯显色反应的研究和应用

对6种苯并噻唑偶氮吡唑化合物的分析特性进行了探讨,着重研究了4—(6′—甲基苯并噻唑-2′-偶氮)-3,5-二氨基吡唑(MBTAP)与钯离子显色反应的光度性质。在非离子表面活性剂 Brij35存在下与钯离子形成橙红色的配合物。适宜的 pH 值范围为9.0～10.5.配合物的最大吸收波长为510nm,表观摩尔吸光系数为3.01×10~4L·mol~(-1)·cm~(-1)。钯在0～14μg/25mL,范围内服从比尔定律.显色体系可稳定11h。在柠檬酸存在下可消除 Fe~(3+)、Co~(2+)、Cu~(2+)、Ni~(2+)等离子的干扰。     

Alkylation of Benzene with Isopropyl Alcohol over SAPO-5 Catalyst in an Integral Pressure Reactor

The alkylation of benzene with isopropyl alcohol was studied in an integral pressure reactor over silicon substituted aluminophosphate molecular sieves, SAPO-5. The influence of various process parameters such as temperature, pressure, time on stream, weight hourly space velocity, and mole ratio of reactants on cumene yield and selectivity were investigated. The activity of SAPO-5 was compared with that of Hbeta for this reaction under similar conditions and in the same reactor. At pressures higher than atmospheric, almost the theoretical maximum yields of cumene were achieved on this SAPO-5. Among the diisopropyl benzenes formed by the alkylation of cumene, the meta-isomer was found to form in a significant amount followed by the para-isomer. The ortho-isomer with relatively high strain energy of 4.26 kcal/mol was almost negligible. The cumene yield goes through a maximum in the temperature range 498-543 K studied. Cumene selectivity was found to decrease at higher temperatures, higher pressures and lower benzene to isopropanol mole ratios.     

"十五"期间国内石油化学工业发展梗概

概述了我国目前石油和化学工业的现状,与发达国家相比存在的主要差距,以及"十五"期间发展思路和规划目标.     

Adsorption of chromate by surfactant-modified zeolites and MCM-41 molecular sieve

Synthetic and natural zeolites, modified by the quaternary amines, i.e. hexadecyltrimethylammonium (HDTMA) bromide and n-cetylpyridinium bromide (CPB) as well as MCM-41 molecular sieve were employed for removal of chromate from aqueous solution. Obtained data from chromate adsorption experiments over the mentioned materials were compared. It was shown that adsorption data for modified zeolite using the amine was consistent with Langmuir isotherm equation. The maximum chromate adsorption over as synthesized MCM-41 was much greater than that of the natural clinoptilolite and ZSM-5 zeolites.     

5-硝基愈长木酚的合成

5-硝基愈创木酚作为高效、低毒植物调节剂,一直倍受关注.它的合成目前主要采用愈创木酚硝化法,以发烟硝酸和冰醋酸混酸做硝化剂.本文由愈创木酚为起始原料,经酚酯化、硝化、水解等步骤合成了5-硝基愈刨木酚.酚酯化采用碱催化法,收率可达96%以上;硝化反应则采用乙酸酐和硝酸混合物为硝化剂.5-硝基愈创木酚最高收率可达到91%.     

Structural significance of the alkyl substituent at the C-4 of (+)-trans-verbenyl acetate in sex pheromonal activity of the American cockroach

The significance of the alkyl group at the C-4 of (+)-trans-verbenyl acetate, which is the sex pheromone mimic of the American cockroach, was investigated. Seven alcohols possessing an ethyl, propyl, or dimethyl group at this position of the 6,6-dimethylbicyclo[3.1.1]heptane skeleton were synthesized and evaluated by behavioral assay. All of the alcohols were inactive, while three of four acetates of the 2-alcohols induced sexual behavior in male cockroaches at the 0.02 or 0.5 mg dosage level, either of which is many orders of magnitude higher than the threshold level of the natural sex pheromones (10^–8 mg). Among the acetates, the compounds with a methyl group or an -oriented ethyl group at C-4 showed the highest activity. The results are discussed in terms of spatial requirements of the molecules for interactions with the receptor.Studies on the sex pheromone mimic of the American cockroach, (+)-trans-verbenyl acetate. Part VIII. For Part VII, seeComp. Biochem. Physiol.,70A: 229–234 (1981).     

5’-单磷酸腺苷在乙醇-水中介稳区性质研究

针对5’-单磷酸腺苷(5’-AMP)在溶析结晶中易出现爆发结晶的问题,分别采用静态法和激光法测定了293—323 K下5’-AMP在纯水以及溶剂体积比为0.3—2.0的乙醇-水体系中的溶解度和超溶解度,以指数经验关联式建立了超溶解度关联式,并在试验条件下考察了温度、乙醇流速、pH值和搅拌速率对介稳区宽度的影响。运用中心复合设计预测了5’-AMP在本溶析结晶体系中介稳区间,并用扫描电镜观察了5’-AMP在结晶条件优化前后晶体形态的变化情况,为工业生产中提高结晶产品质量提供了理论指导。     

Study on the polymerization of ϵ‐caprolactam in the interlamellar spaces of [TEACOOH]–montmorillonite intercalations complex and its characterization

The polymerization of ?‐caprolactam between the interlamellar spaces of the [TEACOOH]–montmorillonite intercalations complex was attempted using Na–montmorillonite and 10‐carboxy‐n‐decyltriethylammonium bromide to achieve [TEACOOH]–polycaprolactam–montmorillonite, in which montmorillonite (inorganic polymer) is chemically bonded with the polycaprolactam (organic polymer). The results of X‐ray and IR analysis for the samples obtained after polymerization showed that the polymerization reaction has been successfully accomplished. For the purpose of studying the polymeric reaction product more precisely, we have isolated the polymerized product from the silicate layers and analyzed it with X‐ray diffractometer and IR spectrometer. Comparison of the results of X‐ray and IR analysis between the isolated polymer and the polymer that was synthesized by the reaction of ?‐caprolactam only with the organic cation without montmorillonite showed that both obtained polymers are the same compounds. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 1904–1910, 2003     

Platyphylloside: Metabolism and digestibility reductionin vitro

The metabolism of platyphylloside [(5S)-5-hydroxy-1,7-bis-(4-hydroxyphenyl)-3-heptanone-5-O--d-glucopyranosidel]—known to reduce digestibility—was studiedin vitro in sheep rumen liquor. Platyphylloside is hydrolyzed to 5-hydroxy-3-platyphyllone [(5S)-5-hydroxy-1,7-bis-(4-hydroxyphenyl)-3-heptanone], which is reduced to centrolobol [1,7-bis-(4-hydroxyphenyl)-3-heptanol], via 3-platyphyllone [7-bis-(4-hydroxyphenyl)-3-heptanone]. The digestibility-reducing effect was shown to be correlated with the concentration of centrolobol.     

钒钼酸铵分光光度法快速测定磷酸二铵中有效五氧化二磷

为了快速测定磷铵中P2O5含量,将0.1mol/LEDTA预热至80±2℃作为DAP有效P2O5的提取液,提取时间25min以上。鉴于正磷酸根在酸性介质中与钼酸盐及偏钒酸盐生成稳定的黄色化合物,在400nm波长下,利用示差法测定P2O5仅需50～55min。该方法的相对标准偏差(RSD)为0.13%～0.28%,回收率99.1%～101.1%,精密度和准确度好。