吡唑啉酮衍生物的合成初探

以1-苯基-3-甲基-5-吡唑啉酮与苯甲酰氯进行的反应，探讨了合成高产率吡唑啉酮衍生物的简易方法。并通过TLC对产物进行了初步鉴定。     

离子液体中正丁基苯基醚的绿色合成方法

制备了1-甲基-3-正丁基咪唑氟硼酸盐([bmim]BF_4)和N-正丁基吡啶氟硼酸盐([bpy]BF_4)两种离子液体,并作为溶剂和催化剂用于正丁基苯基醚的合成。考察了反应条件对正丁基苯基醚产率的影响,探讨了正丁基苯基醚的合成反应机理。在反应条件为65℃、2 h、氯代正丁烷与苯酚钠摩尔比为1∶1.2、离子液体与反应物的质量比为2∶1时,分别以[bmim]BF_4、[bpy]BF_4和混合离子液体([bmim]BF_4和[bpy]BF_4的摩尔比为1∶1)为溶剂和催化剂时,正丁基苯基醚的产率分别为80.2%、85.1%和96.9%。结果表明,混合离子液体因提高了与极性相异反应物的相溶性而明显提高了正丁基苯基醚的产率,并且具有良好的重复使用性能。     

二段生物接触氧化法处理香精污水的生产性工艺研究

本文论述二段生物接触氧化法处理香精污水的经济合理工艺 ,生产性实验结果表明 :在一氧接触时间t1=8hrs左右 ,二氧接触时间t2 =3hrs左右 ,水气比r=1∶2 4左右 ,初、二沉淀时间t3 =44 =1.5hrs左右 ,气浮时间t5=1.0hr左右和BOD有机负荷 3 0 0— 3 18,处理后的香精污水可达到国家二级排放标准 (GB8978— 1996 )。CODCr去除率达到 93%～ 95 % ,BOD5去除率达到 88%～ 91% ,SS去除率达到 86 %～ 90 %     

Synthesis and characterization of poly(urethane‐co‐imidine)s having pendent phenyl and benzylidene groups using bisphthalides,bislactones and blocked polyurethane prepolymers

Poly(urethane‐co‐imidine)s were prepared using amine blocked polyurethane (PU) prepolymer. The PU prepolymer was prepared by the reaction of poly(propylene glycol) (PPG₂₀₀₀) and 2,4‐tolylene diisocyanate (TDI) and end capped with N‐methyl aniline. The PU prepolymer was then reacted with bisphthalides and bislactones, until the evolution of carbon dioxide ceased. Polymerization reactions with bispthalides and bislactone took more time than with dianhydrides. Polymers were characterized by FTIR, GPC, TG and DSC analyses. Molecular weights of the poly(urethane‐co‐imidine)s were found to be lower than that of poly(urethane‐co‐imide)s. Compared to poly(urethane‐co‐imide)s all poly(urethane‐co‐imidine)s showed high glass transition temperature and crystallization peak in DSC. The thermal stability of the polyurethanes was found to increase with the introduction of imidine component. © 2001 Society of Chemical Industry     

催化加氢制备三(4-氨基苯基)硫代磷酸酯工艺条件的改进

以对硝基苯酚和三氯硫磷合成反应制得的三(4-硝基苯基)硫代磷酸酯为原料,催化加氢还原制备三(4-氨基苯基)硫代磷酸酯。通过对溶剂种类、催化剂型号及用量、反应温度、反应压力等工艺条件的研究,得出如下较佳的工艺条件:以甲醇为溶剂,Raney-N i为催化剂,反应温度70℃、反应压力2.0~3.0M Pa。所得成品纯度大于94%。通过补加少量新鲜催化剂,催化剂能够重复使用并且性能稳定。     

Monomer conversion in a light‐cured dental resin containing 1‐phenyl‐1,2‐ propanedione photosensitizer

The efficiency of 1‐phenyl‐1,2‐propanedione (PPD) photosensitizer for the photopolymerization of a dental resin based on 2,2‐bis[4‐(2‐hydroxy‐3‐methacryloxyprop‐1‐oxy)phenyl]propane/triethylene glycol dimethacrylate was assessed. Experimental formulations containing PPD or/and camphorquinone (CQ) in combination with dimethylaminoethyl methacrylate (DMAEMA), ethyl‐4‐dimethylaminobenzoate (EDMAB), 4‐(N,N‐dimethylamino)phenethyl alcohol (DMPOH) and N,N‐3,5‐tetramethylaniline (TMA) at different concentrations were studied. The photopolymerization was carried out by means of a commercial light‐emitting diode (LED) curing unit. Near‐infrared spectroscopy was used to follow the consumption of double bonds versus irradiation time. No significant differences in the conversion values among formulations prepared with PPD in combination with DMAEMA, DMPOH and TMA were found. In contrast, the conversion was markedly increased by the presence of EDMAB. At low concentrations of photosensitizer, when used in combination with DMAEMA and EDMAB, PPD resulted in a final conversion equivalent to CQ. However, when DMPOH and TMA were used, PPD was found to be less efficient than CQ. In addition, at high photoinitiator concentration, the effectiveness of PPD was less than that of CQ independently of the co‐initiator used. The replacement of some CQ by an equivalent amount of PPD resulted in similar final monomer conversion as formulations having the same amount of CQ alone. The LED light source employed emitted in the wavelength range 410–490 nm with a peak around 470 nm, whereas the maximum molar absorbance of PPD was in the UV region. However, the small overlap of the spectral distribution of the LED curing lamp and the PPD absorption spectrum was compensated by the large extinction coefficient of PPD. Copyright © 2007 Society of Chemical Industry     

Clean synthesis of methyl N‐phenyl carbamate over ZnO‐TiO2 catalyst

BACKGROUND: Methyl N‐phenyl carbamate (MPC) is an intermediate for the preparation of methylene diphenyl diisocyanate (MDI), which is an important monomer for polyurethane synthesis. The synthesis of MPC by the reaction of aniline and dimethyl carbonate (DMC) is becoming more and more attractive. However, most of the catalysts used in MPC synthesis are homogeneous and not environment‐friendly. Therefore, it is important and necessary to develop a new kind of oxide catalyst, that is not only friendly to the environment, but also exhibits higher activity and longer service time. RESULTS: A new heterogeneous catalyst, ZnO‐TiO₂, was prepared for MPC synthesis. ZnO‐TiO₂ catalyst with a molar ratio Ti/Zn = 2 and calcined at 673 K exhibited good catalytic activity: aniline conversion was 96.9% and MPC yield 66.7%. CONCLUSION: ZnO‐TiO₂ exhibits better catalytic activity than ZnO or TiO₂ alone, which may result from the formation of ZnTiO₃ and Zn₂TiO₄. Compared with ZnTiO₃, Zn₂TiO₄ has better selectivity for MPC synthesis. Lewis acid sites with weaker acid strength favour MPC synthesis. The catalyst activity can be recovered almost completely by calcination. Copyright © 2008 Society of Chemical Industry     

壬基酚聚氧乙烯醚琥珀酸酯合成条件的研究

在原有合成壬基酚聚氧乙烯醚琥珀酸酯方法的基础上,讨论了催化剂种类、原料配比及其他反应条件对反应的影响,确定了壬基酚聚氧乙烯醚琥珀酸酯的最佳合成条件:催化剂为自制催化剂,原料摩尔比1.00:1.04,反应温度(94±2)℃,真空度15.5 kPa,反应时间3 h。     

Combination of chemical oxidation‐membrane filtration processes for the elimination of phenyl‐ureas in water matrices

BACKGROUND: Phenyl‐urea herbicides are found in surface waters and wastewaters as a consequence of their extensive use in agriculture. Due to their pollutant power, the removal of phenyl‐ureas is a priority objective in water treatment technologies. RESULTS: Four selected phenyl‐ureas herbicides (linuron, diuron, chlortoluron and isoproturon), dissolved in two water matrices (a groundwater and and a reservoir water), were subjected to sequential combinations of chemical treatments and membrane filtration processes. Two specific sequences were conducted: first, a chemical oxidation stage (where UV radiation, ozone and ozone plus hydrogen peroxide were used) followed by a nanofiltration process; and second, a membrane filtration stage (using UF and NF membranes) followed by an ozonation stage. Values for the herbicide removals in the oxidation stages and for the rejection coefficients in the filtration stages are provided, and the partial contribution of the different stages is established for each combined treatment. CONCLUSIONS: High removals (over 80%) were reached for phenyl‐ureas elimination by most of the combined processes tested. In the combined chemical oxidation/nanofiltration processes, the most effective was an ozonation pretreatment ([O₃]₀ = 1.5 mg L^?1)) followed by a NF step. In the opposite sequence filtration/chemical oxidation, the most effective was a NF pretreatment followed by the ozonation ([O₃]₀ = 2 mg L^?1). Copyright © 2009 Society of Chemical Industry     

Study on Oligomerization of Phenyl Isocyanate Catalyzed by Bis(methylcyclopentadienyl)samarium Complex

Ｐｏｌｙｉｓｏｃｙａｎａｔｅｓｈａｖｅｒｅｃｅｉｖｅｄａｇｒｅａｔｄｅａｌｏｆａｔｔｅｎｔｉｏｎｉｎｒｅｃｅｎｔｙｅａｒｓｏｗｉｎｇｔｏｔｈｅｉｒｃｈｉｒａｌｈｅｌｉｃａｌｓｔｒｕｃｔｕｒｅｓ ,ｌｉｑｕｉｄｃｒｙｓｔａｌｌｉｎｅｐｒｏｐｅｒ ｔｉｅｓ ,ｅｔｃ .Ｓｉｎｃｅｗｅｆｏｕｎｄｔｈａｔｄｉｖａｌｅｎｔｂｉｓ(ｐｈｅｎｏｘｏ)ｓａｍａｒｉｕｍｃｏｍｐｌｅｘｃａｎｅｆｆｅｃｔｉｖｅｌｙｃａｔａｌｙｚｅｔｈｅｏｌｉｇｏｍｅｒｉｚａｔｉｏｎｏｆｐｈｅｎｙｌｉｓｏ ｃｙａｎａｔｅ[1 ] ,ｉｓｏｃｙａｎａｔ…