对叔丁基杯[4]及杯[6]芳烃的合成及其对铜离子的萃取研究

以对叔丁基苯酚和甲醛为原料,分别对对叔丁基杯[4]及杯[6]芳烃的合成和萃取性质进行了研究．结果表明,在本研究范围内,以KOH为催化剂,对叔丁基杯[6]芳烃的最高产率为77．8％;以NaOH为催化剂,对叔丁基杯[4]芳烃的最高产率为47．3％。对于对叔丁基杯[4]和杯[6]芳烃,最佳的反应回流温度都为140℃。对叔丁基杯[6]芳烃对模拟废水中的铜离子具有一定的萃取效果,最高萃取率为70．3％。     

前驱体对熔盐法合成Bi2WO6光催化剂及其性能的影响

分别以Bi(NO3)3和Na2WO4溶液直接混合所得沉淀、加氨水所得沉淀及Bi(NO3)3×5H2O+Na2WO4×2H2O为前驱体,采用熔盐法合成Bi2WO6光催化剂粉体,研究了不同前驱体所制粉体的物相、形貌,以其为催化剂,在可见光照射下降解罗丹明B溶液. 结果表明,用后二者为前驱体均可得到薄片状纯相Bi2WO6粉体. 加氨水所得沉淀为前驱体所制Bi2WO6粉体的光催化性能最好,在可见光照射下对0.01 mmol/L RhB溶液的降解率在60 min内达99%.     

2-氨基-6-羟基-3,5-二硝基吡啶的合成探索

2-氨基-6-羟基-3,5-二硝基吡啶(AHDNP)是合成聚对苯亚乙基吡啶并咪 二唑(PPIO)重要前体.本文以2,6-二氯吡啶为原料经单硝化、单氨解、再硝化先合成中间体2-氨基-6-氯-3,5-二硝基吡啶(ACDNP),纯度为95.60%,总收率41.00%以上;最后在K₂CO₃的碱性水溶液中70℃条件下单水解,成功合成出AHDNP,提纯后总收率为82.07%,纯度为98.13%.AHDNP的结构经过FT-IR、MS、¹³C NMR 准确定性和表征.合成过程操作方便、产品质量优异、经济性良好及易于产业化,为进一步研发合成新型高性能材料PPIO及其新单体提供技术基础及中间体来源.     

Butanol isomer separation using polyamide-imide/CD mixed matrix membranes via pervaporation

Mixed matrix membranes (MMMs) comprising polyamide-imide (PAI) and α-, β- or γ-cyclodextrin (CD) have been investigated experimentally and computationally for isomeric n-butanol/tert-butanol (n-BuOH/t-BuOH) separation via pervaporation. Consistent with molecular simulation, experimental results show that the CD inclusion ability and butanol discrimination ability are dependent on both CD cavity size and butanol molecular size. The PAI membrane incorporated with α-CD has the smallest cavity and has the highest discrimination ability for the n-BuOH/t-BuOH pair but with a low butanol flux. The mixed matrix membrane embedded with γ-CD has the lowest selectivity and the highest flux. The PAI/β-CD membrane has a comparable selectivity and flux, and exhibits preferential sorption and diffusion selectivity toward n-BuOH. A maximum separation factor of 1.53 with a corresponding flux of 4.4 g/m² h are obtained at an optimal β-CD loading of 15 wt%. Further increments in the CD content eventually lead to a decrease in separation performance because of CD agglomeration and severe phase separation. To better understand the influence of CD on the separation performance of mixed matrix membranes, SEM, FTIR and XRD have been employed for membrane characterizations. The effect of n-butanol/t-butanol ratio in the feed composition has also been studied. It is found that both flux and separation factor decrease with increasing n-butanol content in the feed. The decline is attributed to the change in total vapor pressure at the upstream and the mutual drag effect of isomeric butanol molecules.     

2-甲氧基-6-(2′-萘基)丙酸-(2,″2″-二甲基-3″-溴)丙酯水解反应制备萘普生

用氢氧化钠水溶液水解2-甲氧基-6-(2′-萘基)丙酸-(2,″2″-二甲基-3″-溴)丙酯得到萘普生,以萘普生收率为主要指标,用均匀设计和单因素实验方法,考察了NaOH质量分数,物料摩尔比,水解时间对水解反应的影响。结果表明:在水解温度(110±5)℃,水解反应时间60~90 m in,w(NaOH)=40%,n(氢氧化钠)∶n(原料)=4.4∶1的条件下,萘普生收率可达99.19%。同时确定了高效液相色谱分析萘普生的分析方法。     

尼龙-6的拉伸多次屈服行为及球晶形态的研究

研究了不同拉伸速度下尼龙-6的多次屈服成颈行为,并采用生物显微镜研究了尼龙-6的球晶形貌。结果表明：在拉伸速率低于50m／min的条件下,可观察到尼龙-6明显的多次屈服成颈行为,这应与拉伸条件下球晶演变形成的微纤维的缺陷有关：采用生物显微镜,可观察到尼龙-6球晶中的发射状微纤、球晶形貌和晶界。     

一种移动IPv6下防火墙技术的研究与实现

随着计算机网络在政治、经济、文化等诸多方面的飞速发展,网络安全技术也越来越受到前所未有的重视。本文针对移动节点在外地网络与家乡网络通信的透明性,以及传输的安全性问题,设计了一种对防火墙和移动节点之间的通信进行IPSEC信息验证的方法,解决了移动IPv6下移动节点在外地网络与家乡网络通信穿越防火墙的问题。     

2,6-二甲基-3,4-二氢-4-氧代喹唑啉的合成研究

2,6-二甲基-3,4-二氢-4-氧代喹唑啉是合成抗癌药物雷替曲塞及其衍生物的重要中间体。其合成方法主要是以对甲基苯胺为原料经3步反应可制得2-氨基-5-甲基苯甲酸,然后环化生成2,6-二甲基-3,4-二氢-4-氧代喹唑啉。对该过程进行改进,反应中用乙酰胺代替硫代乙酰胺,减少污染,降低了成本。     

聚合物浓度对PA6／氯化钙冻胶体系结构与性能的影响

以氯化钙为络合剂,将聚酰胺6（PA6）粉末与氯化钙溶解在甲酸,氯仿混合溶液中制得冻胶样品,采用DTA、XRD、FTIR、SEM等方法对冻胶结构与性能进行分析,探讨了PA6质量浓度对冻胶样品结构和性能的影响。结果表明,氯化钙可以部分屏蔽PA6的氢键,降低其结晶能力;随着PA6浓度的增大,冻胶样品的分子间作用力增强,熔点升高,不同浓度间的冻胶样品结构和性能以及络合剂的络合效果有一定的差异。     

Adsorption and inhibition effect of 6-benzylaminopurine on cold rolled steel in 1.0 M HCl

The adsorption and inhibition effect of 6-benzylaminopurine (BAP) on cold rolled steel (CRS) in 1.0 M HCl at 25-50 °C was studied by weight loss and potentiodynamic polarization methods. The results showed that BAP was a good inhibitor in 1.0 M HCl, and the inhibition efficiency (IE) increased with the inhibitor concentration. The adsorption of BAP on the CRS surface obeyed the Langmuir adsorption isotherm equation. Both thermodynamic parameters (adsorption heat ΔH⁰, adsorption free energy ΔG⁰ and adsorption entropy ΔS⁰) and kinetic parameters (apparent activation energy E_a and pre-exponential factor A) were calculated and discussed. Polarization curves showed that BAP acted as a mixed-type inhibitor in hydrochloric acid. Good agreement between weight loss and polarization methods was obtained. The adsorbed film on CRS surface containing optimum dose of BAP was investigated by Fourier transform infrared spectroscopy (FTIR) and atomic force microscope (AFM). Quantum chemical calculation was applied to elucidate the adsorption mode of the inhibitor molecule onto steel surface. Depending on the results, the inhibitive mechanism was proposed from the viewpoint of adsorption theory.