固体超强酸S2O28-/TiO2-MoO3催化合成丙酸苄酯

以氯化钛为主要原料，采用沉淀-浸渍法制备新型固体超强酸催化剂S2O8^2- -／TiO2-MoO3，并用于丙酸苄酯的合成反应。该催化剂制备的最优条件为：焙烧温度为500℃，（NH4）2S2O8浸渍浓度0．5mol／L，钼酸铵浸渍浓度为0．1mol／L时，焙烧时间为2．5h。采用该催化剂通过正交试验得到合成丙酸苄酯的最佳条件为：n（苄醇）：n（丙酸）=1．5：1．0，催化剂用量为0．6g（以0．2mol丙酸为准），带水剂环己烷用量为12mL，反应时间为2．5h，其酯化率可达96％以上。该催化剂具有催化活性高、不污染环境、可重复使用等特点。     

环境友好催化合成苯乙酮1,2-丙二醇缩酮

以硫酸铁和硝酸钴为主要原料,采用沉淀-浸渍法制备新型固体超强酸催化剂SO42-/CoFe2O4,并用于苯乙酮1,2-丙二醇缩酮的合成反应。该催化剂制备的最优条件为:焙烧温度为500℃(,NH4)2SO4浸渍浓度0.6mol/L,焙烧时间为2.5 h。采用该催化剂通过正交试验得到合成苯乙酮1,2-丙二醇缩酮的最佳条件为:n(醇)∶n(酮)=1.6∶1.0,催化剂用量为0.6 g,带水剂甲苯用量为12 mL,反应时间为2.0 h,其收率可达89.7%以上。该催化剂具有催化活性高、不污染环境、可重复使用等特点。     

复合固体超强酸SO2-4/Fe2O3-MoO3催化合成乙酸辛酯

以硝酸铁和钼酸铵为原料,柠檬酸为络合剂,采用溶胶-凝胶法,制备固体超强酸SO2-4/Fe2O3 MoO3.催化剂制备的最佳条件为:浸泡液浓度为0.5 mol/L,焙烧温度为350 ℃, 焙烧时间为3.5 h.用该催化剂通过正交试验合成乙酸辛酯的最佳条件为:酸醇摩尔比为1.35∶1.0,催化剂用量为0.8 g(以0.15 mol正辛醇为准),带水剂用量为12 mL,反应时间为2.5 h,其酯收率可达95%以上.     

复合固体超强酸SO_4~(2-)/Fe_2O_3-MoO_3催化合成乙酸辛酯

以硝酸铁和钼酸铵为原料,柠檬酸为络合剂,采用溶胶-凝胶法,制备固体超强酸SO_4~(2-)/Fe_2O_3-MoO_3。催化剂制备的最佳条件为:浸泡液浓度为0.5mol/L,焙烧温度为350℃,焙烧时间为3.5h。用该催化剂通过正交试验合成乙酸辛酯的最佳条件为:酸醇摩尔比为1.35∶1.0,催化剂用量为0.8g(以0.15mol正辛醇为准),带水剂用量为12mL,反应时间为2.5h,其酯收率可达95%以上。     

固体超强酸S_2O_8~(2-)/Fe_2O_3-MoO_3催化合成丁醛乙二醇缩醛

以硝酸铁和钼酸铵为原料,柠檬酸为络合剂,采用溶胶-凝胶法,制备固体超强酸催化剂S2O82-/Fe2O3-MoO3。催化剂制备的最佳条件为:浸泡液浓度为0.5 mol/L,焙烧温度为350℃,焙烧时间为3.0 h。用该催化剂通过试验合成丁醛乙二醇缩醛的最佳条件为:醇醛摩尔比为1.5∶1.0,催化剂用量为0.6 g,带水剂用量为10 mL,反应时间为1.0 h,缩醛收率可达89.3%以上。     

复合固体超强酸SO4^2-/Fe2O3-MoO3催化合成苯乙酮环乙二缩酮

以硝酸铁和钼酸铵为原料,柠檬酸为络合剂,采用溶胶-凝胶法,制备固体超强酸SO4^2-/Fe2O3-MoO3。催化剂制备的最佳条件为,浸泡液浓度0.5 mol/L,焙烧温度350℃,焙烧时间3.0 h。用该催化剂通过正交试验合成苯乙酮环乙二缩酮的最佳条件为,醇酮摩尔比1.7∶1.0,催化剂用量0.9 g（以0.10 mol苯乙酮为准）,带水剂用量15 mL,反应时间2.5 h,其收率可达88%以上。     

稀土固体超强酸S2O82-/Sb2O3/La3+的制备及催化性能研究

以SbCl3为原料经醇化水解制得Sb2O3前体氧化物,通过浸渍一定量的(NH4)2S2O8和掺杂La(NO3)3制备了一种新型催化剂S2O82-/Sb2O3/La3+.以催化合成乙酸苄酯为探针反应,考察了不同制备条件对催化剂性能的影响.结果表明,1.5 mol/L的(NH4)2S2O8和2.71% La(NO3)3混合溶液浸渍锑前体氧化物,经110℃烘干后,于500℃焙烧3h所得催化剂(SSL2.71-3-500)活性较好.同时,考察了催化剂的稳定性以及对不同酯化反应的作用规律.用Hammett,IR,DTA/TGA,XRD等手段对催化剂进行了表征.     

稀土固体超强酸SO42-/SnO2- Nd2O3催化合成棕榈酸甲酯

采用溶胶-凝胶法制备稀土固体超强酸催化剂SO4-/SnO2- Nd2O3,以工业棕榈酸和甲醇为原料催化合成棕榈酸甲酯.考察了氧化钕添加量、焙烧温度、硫酸浓度、醇酸质量比、催化剂用量和反应时间对酯化反应的影响.结果表明,当氧化钕添加量为5％,以2.0 mol/L硫酸浸渍后,于550℃下焙烧3h制备的催化剂性能最好.正交实验结果表明,合成棕榈酸甲酯的优化条件为:醇酸质量比为15∶25,催化剂用量为棕榈酸质量的6.0％,反应时间5h.在此条件下,酯化率为90.1％.     

含铈固体超强酸SO42-/SnO2-CeO2-kaolin催化合成异丁酸异丁酯

以质量比为1:9:20的硝酸铈铵、高岭土和SnCl4·5H2O制备了含铈固体超强酸催化剂SO42- -/SnO2-CeO2-kaolin,制备条件为促进剂H2SO4浓度2.0mol/L,浸渍12h,350℃焙烧3h,并采用Hammett指示剂法和XRD对其进行了酸强度和表面性能表征.适宜反应条件是催化剂用量为反应物总质量的2.5%,醇酸摩尔比1.4、反应时间100min,甲苯10mL,酯收率94.5%,重复使用6次酯收率仍高于80%.     

稀土固体超强酸Gd3+- SO2-4/ZrO2催化合成乙酸正丁酯

采用乙酸、正丁醇为原料,以固体超强酸Gd3+ -SO2-4/ZrO2作为催化剂,催化合成乙酸正丁酯.用固体超强酸Gd3+ -SO2-4/ZrO2和SO2-4/ZrO2进行催化活性对比试验,考察浸渍硫酸浓度、浸渍时间、焙烧温度对催化剂活性的影响以及原料酸醇比、反应时间、催化剂用量对酯化率的影响,从而确定固体超强酸的最佳制备条件.试验结果表明:在反应温度105～110℃,催化剂用量1.5g,n(正丁醇)∶n(乙酸)=2.5∶1,反应时间2.5h条件下,酯化率可达98.86％;催化剂重复使用效果明显;加Gd3+的固体超强酸的催化活性明显增强.     

CeO2对不锈钢基SiO2-BaO-Al2O3-Cr2O3陶瓷涂层性能的影响

采用高温熔烧法于1Cr18Ni9Ti不锈钢基材表面制备掺CeO2的SiO2-BaO-Al2O3-Cr2O3陶瓷涂层,研究了不同含量CeO2对涂层的抗氧化性、抗热震性和硬度的影响。研究结果表明,含CeO2的不锈钢基SiO2-BaO-Al2O3-Cr2O3陶瓷涂层能有效阻止不锈钢基体的氧化增重,提高涂层的抗热震性能及硬度。本实验条件下,CeO2含量2.8%时,涂层具有最好的抗氧化性能和抗热震性能。     

Synthesis and biological investigations of 1-(tetrahydropyran-2'-yl)- and 1-(tetrahydrofuran-2'-yl)benzimidazoles and 1/2-(tetrahydropyran-2'-yl)- and 1/2-(tetrahydrofuran-2'-yl)benzotriazoles

Sets of benzimidazole and benzotriazole derivatives bearing on position 1 or 2 a tetrahydrofuranyl or tetrahydropyranyl moieties were prepared through the addition of the suitable benzazoles on 2,3-dihydrofuran and 3,4-dihydro-2H-pyran. The reactions were carried on either without solvent or in carbon tetrachloride solution. In the last case some peculiar chlorinated side products were isolated and characterized. Twenty compounds were screened for in vitro antitumoral and anti-HIV-1 activities and found poorly active or completely inactive. On the other hand several compounds exhibited good tracheal relaxant activity in vitro; compound 8, 11, 16, 24 and 26 resulted more active than theophylline in this test, while compound 11 was comparable to amrinone till the concentration of 3 micrograms/ml. Finally, compound 5 resulted endowed with a strong diuretic and saluretic activity at the dose of 3 mg/Kg, thus representing a new lead for discovering new diuretic agents.     

Texture and residual strain in two SiC/Ti-6-2-4-2 titanium composites

Residual strain and texture variations were measured in two titanium matrix composites reinforced with silicon carbide fibers (Ti/SiC) of similar composition but fabricated by different processing routes. Each composite comprised a Ti-6242 α/β matrix alloy containing vol 35 pct continuous SiC fibers. In one, the matrix was produced by a plasma sprayed (PS) route, and in the other by a wiredrawn (WD) process. The PS and WD composites were reinforced with SCS-6 (SiC) and Trimarc (SiC) fibers, respectively. The texture in the titanium matrices differed significantly. The titanium matrix for the PS material exhibited random texture pre and post fabrication of the composite. For the WD material, the starting texture of the monolithic titanium matrix was ≈17 times random, but after consolidation into composite form, it was ≈6 times random. No significant differences were noted in the fiber-induced matrix residual strains between the composites prepared by the two procedures. However, the Trimarc (WD) fibers recorded higher (≈1.3 times) compressive strains than the SCS-6 (PS) fibers. Stresses and stress balance results are reported. Plane-specific elastic moduli, measured in load tests on the unreinforced matrices, showed little difference. This article is based on a presentation made in the Symposium “Mechanisms and Mechanics of Composites Fracture” held October 11–15, 1998, at the TMS Fall Meeting in Rosemont, Illinois, under the auspices of the TMS-SMD/ASM-MSCTS Composite Materials Committee.     

Texture and residual strain in two SiC/Ti-6-2-4-2 titanium composites

Residual strain and texture variations were measured in two titanium matrix composites reinforced with silicon carbide fibers (Ti/SiC) of similar composition but fabricated by different processing routes. Each composite comprised a Ti-6242 α/β matrix alloy containing vol 35 pct continuous SiC fibers. In one, the matrix was produced by a plasma sprayed (PS) route, and in the other by a wiredrawn (WD) process. The PS and WD composites were reinforced with SCS-6 (SiC) and Trimarc (SiC) fibers, respectively. The texture in the titanium matrices differed significantly. The titanium matrix for the PS material exhibited random texture pre and post fabrication of the composite. For the WD material, the starting texture of the monolithic titanium matrix was ≈17 times random, but after consolidation into composite form, it was ≈6 times random. No significant differences were noted in the fiber-induced matrix residual strains between the composites prepared by the two procedures. However, the Trimarc (WD) fibers recorded higher (≈1.3 times) compressive strains than the SCS-6 (PS) fibers. Stresses and stress balance results are reported. Plane-specific elastic moduli, measured in load tests on the unreinforced matrices, showed little difference. This article is based on a presentation made in the Symposium “Mechanisms and Mechanics of Composites Fracture” held October 11–15, 1998, at the TMS Fall Meeting in Rosemont, Illinois, under the auspices of the TMS-SMD/ASM-MSCTS Composite Materials Committee.     

Biochemical basis for a cholesterol-lowering activity of 2-[2"-(1",3"-dioxolane)]-2-methyl-4-(2'-oxo-1'-pyrrolidinyl)-6- nitro-2H-1-benzopyran (SKP-450), a novel antihypertensive agent

Administration (p.o.) of SKP-450, 2-[2"-(1",3"-dioxolane)]-2-methyl-4-(2'-oxo-1'-pyrrolidinyl)-6-nitro-2H- 1-benzopyran, a novel antihypertensive agent, to hypercholesterolemic Syrian hamsters led to a significant reduction in plasma lipids in a dose-dependent manner, i.e., a 10.8% to 29% reduction in low-density lipoprotein cholesterol at doses of 0.3 to 10 mg/kg of SKP-450. SKP-450 was found to specifically inhibit the hepatic microsomal lanosterol 14alpha-methyl demethylase (14alpha-DM) in a competitive manner (Ki:2.65 microM). Furthermore, a dose-dependent decrease in the 14alpha-DM activity by SKP-450 parallelled the cholesterol synthetic rate in vitro in both the rat hepatic S10 fractions (supernatants at 10,000 g; IC50:20 microM) and Chinese hamster ovary cells (IC50:23 microM). However, this phenomenon was not seen in AR45 cells, which are deficient in 14alpha-DM, suggesting that 14alpha-DM is the major target for the inhibitory action of SKP-450 in regard to cholesterol biosynthesis.     

The free energies of mixing of melts in the systems 2FeO-SiO2-2MnO-SiO2 and 2.33FeO-TiO2-2.33MnOTiO2

The free energies of mixing in melts in the system 2FeO · SiO₂-2MnO · SiO₂ at 1450°C and the system 2.33FeO · TiO₂-2.33MnO · TiO₂ at 1475°C have been obtained from measurement of the equilibrium Mn + FeO = Fe + MnO established between the melts and ironmanganese foils. Both systems exhibit ideal silicate mixing. The phase diagram for the system 2FeO-SiO₂-2MnO ·SiO₂ is calculated.     

新显色剂2-(2-咪唑偶氮)-5-二乙氨基酚光度法测定铁(Ⅲ)

研究了新显色剂2-（2-咪唑偶氮）-5-二乙氨基酚（简称IZAPN）与Fe     

Synthesis and biological investigations of 2-(tetrahydropyran-2'-yl) and 2-(tetrahydrofuran-2'-yl)benzimidazoles

A set of benzimidazole derivatives bearing on position 2 a tetrahydropyranyl or tetrahydrofuranyl residue was prepared and tested for antitumoral, anti HIV-1 and other pharmacological activities. While the anti-HIV activity was completely lacking, moderate antitumoral activity was found in a few compounds; particularly the 5,6-dichloro-2-(tetrahydropyran-2-yl)-benzimidazole (8) was able to inhibit the growth of 19 cell lines of humane tumors at near micromolar concentration. On the other hand compounds 4, 6-8 and 10 exhibited significant tracheal relaxant activity in vitro at concentration 3-10 micrograms/ml, thus resulting superior to theophylline and comparable to amrinone.     

Electrical properties of phases in the ZrO2 - Y2O3 - La2O3 system

An investigation was made of the electrical properties of phases with the cubic fluorite, pyrochlor, and C-Y₂O₃ structures, and the tetragonal ZrO₂ structure (T-ZrO₂) in the ternary system ZrO₂ - Y₂O₃ - La₂O₃. For comparison, the electrical conductivity of a number of specimens with the fluorite structure in the binary system ZrO₂ - Y₂O₃ and with the pyrochlor structure in the ternary system HfO₂ - Y₂O₃ - La₂O₃ was also studied. The specimens were prepared from nanocrystalline powders synthesized by the hydrolysis of zirconium salts in an acid medium at high temperatures. Conductivity was measured over the range 300–950°C in air. It was shown that phases with the fluorite and T-ZrO₂ structures in the investigated systems possess the highest electrical conductivities. Translated from Poroshkovaya Metallurgiya, Nos. 3/4(412), pp. 40–46, March–April, 2000.     

2-(2-咪唑偶氮)-5-二甲氨基苯甲酸分光光度法测定铜

研究了新显色剂2-(2-咪唑偶氮)-5-二甲氨基苯甲酸(IZDBA)与铜的显色反应。结果表明,在pH 4.0的HAc-NaAc缓冲溶液中,IZDBA与Cu(Ⅱ)形成稳定的摩尔比为2∶1的紫红色络合物,其最大吸收波长为600 nm,表观摩尔吸光系数为3.62×104L.mol-1.cm-1,Cu(Ⅱ)质量浓度在0.08~0.8 mg/L范围内符合比尔定律。本方法可不经分离直接测定铝合金和镁合金样品中微量的铜,测定结果与认定值相符。