固定床中液-固相连续催化反应合成2-苯硫基乙醇

采用无机多孔材料负载碱金属盐作为催化剂,在固定床反应器中,以苯硫酚(PhSH)和碳酸乙烯酯(EC)为原料合成了2-苯硫基乙醇,优化工艺条件为:常压,120℃,n(EC)/n(PhSH)=1.05/1,体积空速0.75~1.50 h^-1。在此条件下,苯硫酚转化率99.9%,2-苯硫基乙醇选择性99.9%。催化剂连续运转168 h,PhSH转化率和2-苯硫基乙醇的选择性均大于99%。

温和条件下催化合成2-苯硫基乙醇

以苯硫酚和碳酸乙烯酯为原料,1,5-二氮杂二环[4.3.0]壬-5-烯(DBN)为催化剂,合成了2-苯硫基乙醇。研究了催化剂种类及其物质的量、反应时间、反应温度等条件对反应的影响。结果表明,在DBN为催化剂、n(苯硫酚)/n(DBN)=100、反应时间为10 min、反应温度为50℃时,2-苯硫基乙醇的转化率达到90%以上;当反应温度为90℃时,可获得100%的转化率,该合成路线催化剂的选择性均为100%。根据软硬酸碱理论对反应机理进行了探讨。

异辛酸硫基乙醇酯型有机锡化合物及其制备方法和应用

本发明涉及异辛酸巯基乙醇酯型有机锡化合物及其制备方法和应用。该化合物的结构式为RnSnX4-n其中R为烷基，其碳原予数为1～30，或R为β-烷氧基羰烷基，其烷基的碳原子数为1～10；X为异辛酸巯基乙醇酯，n为1或2。制备时，将异辛酸巯基乙醇酯、烷基或酯基氯化锡和有机溶剂加热回流，同时加入催化剂，然后通过分液，保留有机层，再对有机层进行减压蒸等步骤制得所述化合物；本发明合成工艺简单，转化率大于95％，反应在常压条件下，反应温度低，从而降低了能耗，减少了污染，所制备的化合物具有反应活性高和毒性小的特点。

色谱—原子荧光光度计联用技术的新进展及其在食品、环境领域中的应用

本文详细介绍了高效液相色谱(HPLC)、离子色谱(IC)和气相色谱(GC)与国产的蒸气发生—原子荧光光度计(VG-AFP)联用技术,用于元素形态分析的特点,及其在紫外(UV)在线消解、专用的气—液分离器和接口技术等关键部件的研究成果。此外,还对研制成功的HPLC—UV—VG—AFP、IC—UV—VG—AFP和GC—AFP联用仪在食品、环境领域中砷、汞和硒等元素形态分析的应用进行了阐述。

试制SG8PVC树脂初步经济评价

根据小试结果对分别采用巯基乙酸（２乙基）己酯和巯基乙醇作链转移剂生产ＳＧ８ＰＶＣ树脂进行了经济分析，为工业生产中采用巯基乙醇作链转移剂提供了依据。

Ternary System of Fe-based Ionic Liquid,Ethanol and Water for Wet Flue Gas Desulfurization

Fe-based ionic liquid （Fe-IL） was synthesized by mixing FeCl3·6H2O and 1-butyl-3-methylimidazolium chloride [Bmim]C1 in this paper. The phase diagram of a ternary Fe-IL, ethanol and water system was investigated to construct a ternary desulfurization solution for wet flue gas desulfurization. The effects of flow rate and concentration of SO2, reaction temperature, pH and Fe-IL fraction in aqueous desulfurization solution on the desulfiariza- tion efficiency were investigated. The results shows that the best composition of ternary desulfurization solution of Fe-IL, ethanol and water is 1 ： 1.5 ： 3 by volume ratio, and pH should be controlled at 2.0. Under such conditions, a desulfurization rate greater than 90% could be obtained. The product of sulfuric acid had inhibition effect on the wet desulfurization process. With applying this new ternary desulfurization solution, not only the catalyst Fe-IL can be recycled and reused, but also the product sulfuric acid can be separated directly from the ternary desulfurization system.

Synthesis and Crystal Structure of a Complex Bimetallic Salt [Ni(trans_[14]diene)] [Ni (mnt)_2]

The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-diene and mnt2- = cis-1, 2-dicyano-1,2-ethylenedithiolato. Its crystal structure has been determined by X-raycrystallography analysis with 4827 independent reflections (Fo>4σ(F0). The bimetallic complex salt [Ni (trans [14] diene )] [Ni (mnt )2] (C24 H32N8Ni2S4, Mr = 678. 24 )crystallizes in the triclinic system with space group P1, a = 9. 2911 (9), b= 11. 7075(12), c=15. 799(2) A, α=68. 384(7), β=79. 324(7), γ=67. 581(6)°, V=1474. 9(3) A3, Dc=1. 527 Mg/m3, Z=2, λ=0. 71073 A, μ=1. 589mm-1, F(000) =704,R=0. 0367. The structure consists of slightly distorted Square planar units [Ni(trans[14]diene)]2+ and [Ni(mnt)2]2-.

丙烯酸-2,4,6-三硝基苯乙酯的合成及热分解

以TNT、甲醛为原料,在弱碱性条件下反应合成得到2,4,6-三硝基苯乙醇(PicCH2CH2OH);PicCH2CH2OH在浓硫酸催化下和丙烯酸在甲苯中回流反应24h,合成得到丙烯酸-2,4,6-三硝基苯乙酯,产率为62%。采用紫外可见光谱(UV-Vis)、核磁共振氢谱(1HNMR)、红外光谱(FTIR)、质谱(MS)以及元素分析等对产物结构进行了表征。利用热重分析(TG)对产物热稳定性进行了研究,采用Kissinger方法和Ozawa方法计算其热分解活化能Ea分别为99.78,102.96kJ·mol-1。