丁醇催化氨化合成丁腈催化剂及工艺的研究

筛选出由丁醇催化氨化合成丁腈的催化剂Co20.0-Ni3.0/-Al2O3,并对其结构进行了表征。在固定床反应器上对该催化剂催化的由正丁醇（异丁醇）合成正丁腈（异丁腈）的工艺及稳定性进行了研究。当反应在410 ℃（420 ℃）、氨醇物质量比3 : 1、液时空速LHSV 0.3 h-1（0.2 h-1）及常压条件下进行时,正丁醇（异丁醇）的转化率达100 %,正丁腈（异丁腈）收率达81.6 %（80.6 %）。连续运转100 h,催化剂活性几乎没有变化,正丁腈（异丁腈）的选择性下降不足1 %。结果表明该催化剂具有优良的催化性能和良好的稳定性。     

催化丁醇氨化合成丁腈催化剂及工艺的研究

筛选出由催化丁醇氨化合成丁腈的催化剂Co20.0-Ni3.0/γ-Al2O3,并对其结构进行了表征。在固定床反应器上对该催化剂催化的由正丁醇(异丁醇)合成正丁腈(异丁腈)的工艺及稳定性进行了研究。当反应在410℃(420℃)、氨醇摩尔比3∶1、液时空速LHSV0.3h-1(0.2h-1)及常压条件下进行时,正丁醇(异丁醇)的转化率达100%,正丁腈(异丁腈)收率达81.6%(80.6%)。连续运转100h,催化剂活性几乎没有变化,正丁腈(异丁腈)的选择性下降不足1%。结果表明,该催化剂具有优良的催化性能和良好的稳定性。     

年产10吨合成异丁腈单管放大试验

一、前言异丁腈是合成农药杀虫剂“地亚农”的主要原料。“地亚农”是有机磷农药中较大吨位的产品。为了支援农业生产,我们对异丁腈的合成进行了研究。异丁腈的合成,有美国的依斯曼公司由异丁醛经缩合的异丁酸异丁酯为原料合成异丁腈的方法已工业化;异丁醇或异丁醛直接催化一步合成的路线也有中试规模性的报道;其他处于研究阶段的方法也有所报道。若以原料划分,主要有以下几种路线:     

农药、医药及中间体

六、农药、医药及中间体异丁腈的合成中试研究异丁腈是新农药“地亚农”的主要原料，该农药目前国内尚无生产厂家。为开发这一新农药，省科委先后批准了异丁腈小试和年产３０吨中试的合成研究。该项目主要原料为异丁醇（或异丁醛）、液氨和催化剂。中试研究１９８５年通过...     

美国、日本部分化工产品价格

品 名美国价格(95.04)美国交货量美元/kg品名日本价格(95.03)日本交货量日元/kg 氢溴酸 盐酸 氢氟酸 溴化氢 氯化氯 氟化氢过氧化氢过氧化氢过氧化氢 硫化氢 氢醌 氢醌 羟基乙酸 碘 碘 铁蓝 铁红 异戊醇丁酸异戊酯水杨酸异戊酯乙酸异丁酯丙烯酸异丁酯 异丁醇 异丁烯 异丁醛 异丁醛 异丁酸 异丁酸 异丁腈 异丁腈 异丙胺醋酸异丙酯 异丙醇 异丙醇 异丙醚 丁酸 乳酸 乳酸 乳酸 羊毛脂 48%,桶装20deg,Be,槽车水溶液,70%,桶装 无水,钢瓶装 无水,钢瓶装 无水,槽车 35%,工业槽车 50%。槽车 70%,槽车99.25%,】70磅钢瓶 照相级 工业,桶装工业。70%,…     

低含量偶氮二异丁腈的色谱定量分析方法研究

偶氮二异丁腈受热易分解,通过用气相色谱法定量分析偶氮二异丁腈分解产物异丁基自由基,达到对偶氮二异丁腈进行定量分析的目的,分析方法简单、快速、准确。采用气相色谱-质谱联用仪进行定性分析,通过气相色谱法分析建立w(偶氮二异丁腈)=0.002 01%~9.95%的工作曲线。结果表明,w(偶氮二异丁腈)与其分解产物异丁基自由基的峰面积成线性关系,相关系数为0.999;采用气相色谱法外标法进行定量分析,其分析结果的相对标准偏差为13%。     

异丁醛生产应注重深加工开发

异丁醛作为一种重要的有机化工原料,可以开发出数十种高附加值的下游衍生产品,具有巨大的市场潜力。———农用化学品。异丁醛和尿素在酸催化剂存在下经缩合反应后得异丁叉二脲,这是一种性能良好的有机缓释控制肥料,一次施用可维持整个生长期的需要。由异丁醛制得的异丁醇与氨作用后催化脱水得异丁胺,可作为生产农用杀虫剂的原料。异丁醛氨化可制取异丁腈,是合成高效低毒有机磷农药三嗪农的主要原料。以异丁腈为原料生产的盐酸异丁腈也是制取高效杀虫剂的中间体。———饲料添加剂。异丁醛和尿素制取的异丁叉二脲也是一种安全型非蛋白…     

生物法合成异丁酰胺的研究

研究了生物法合成异丁酰胺的方法。采用腈水合酶催化异丁腈与水反应合成异丁酰胺,在20℃,发酵液体积分数为2.5%(v%)的条件下,获得最大反应速度为17.85714 mol(L.h),此时异丁腈的最大浓度约为0.18 mol/L。通过对反应液进行膜分离、精制和结晶,获得异丁酰胺的纯度大于99.9%,产品收率在98%以上。根据研究结果,生物法合成异丁酰胺具有产品收率高和纯度大的特点,适合生产高纯度异丁酰胺。     

异丁醇的催化氨化研究

本研究是以异丁醇为起始原料,液氨为氨化剂,在临氢气相条件和催化剂M的存在下氨化合成异丁胺、二异丁胺、三异丁胺.研究了反应温度、反应时间、压力、氨醇比对收率的影响,获得了较佳合成工艺;当温度为160～170℃,压力为10Kgf/cm2时异丁醇的单程转化率为最高.     

偶氮异丁腈甲酰胺的合成研究

以水合肼和尿素反应制得氨基脲,再与丙酮氰醇反应,经过氧化脱氢合成了偶氮异丁腈甲酰胺.研究了反应条件对反应的影响,确定了反应的最佳工艺条件:水合肼与尿素在98～101 ℃反应4 h,制得氨基脲;n(氨基脲):n(丙酮氰醇)＝1.05:1.0,反应4 h得偶氮异丁腈肼甲酰胺,在20～25℃,用双氧水将其氧化,制备了偶氮异丁腈甲酰胺,收率91.2%,含量98%以上.产品经元素分析、核磁共振和红外光谱等进行了确认.     

IBN partition between st monomer/polymer and water and its application in miniemulsion polymerization initiated by AIBN

Isobutyronitrile has been selected as a stable substitute for the 2‐cyano‐2‐propyl radical originating from 2,2′‐azobis(isobutyronitrile) to study the behavior of this radical in miniemulsion polymerization. The partition of isobutyronitrile between styrene monomers/polymers and water has been investigated by carrying out equilibrium experiments under different conditions. Prediction based on a published kinetic model using the newly measured partition coefficient has also been compared with published experimental data and prediction based on the partition coefficient of 2,2′‐azobis(isobutyronitrile). The partition coefficients for isobutyronitrile were found to be 10.98 for the styrene/water system and 4.34 for the polystyrene/water system, respectively. The partition coefficient was found to be unaffected by selected conditions. The model prediction based on the partition coefficient of isobutyronitrile agreed well with the published experimental data, thus, indicating that the partition coefficient of the primary radical should be used in theoretical calculations rather than that of the initiator. © 2011 American Institute of Chemical Engineers AIChE J, 58: 3135–3143, 2012     

A Practical Way to Prepare Isobutyronitrile Amides through Reactions between Carboxylic Acids and Azobisisobutyronitrile

A practical and efficient synthesis of N‐isobutyronitrile amides has been achieved through the direct condensation of carboxylic acid and azobisisobutyronitrile (AIBN). Carboxylic acids bearing variously substituted phenyl rings and cinnamic or phenylpropiolic acids were employed to furnish both tertiary and secondary isobutyronitrile amides in moderate to high yields. A radical pathway was proposed. The methodology presented here requires no catalysts and additives, and represents the first practical approach to a variety of valuable amides containing the isobutyronitrile structural unit.

     

锚固处理对SiO_2/CE复合材料静态力学性能的影响

采用偶联剂SEA-171对纳米SiO2表面进行了处理(M-1),再由偶氮异丁腈对M-1进行锚固表面处理(M-2),对产物进行了红外,元素分析和热失重分析。研究了上述2种纳米SiO2的含量对其氰酸酯树脂复合材料静态力学性能的影响,并采用扫描电镜和透射电镜分析研究了材料界面结构特征,探讨了其作用机理。结果表明,当M-1的添加质量分数为3%时,复合材料的冲击强度增长61.9%;弯曲强度增长44.2%,添加4%M-2时,增幅分别为89.0%和53.8%。经锚固处理后,纳米SiO2颗粒团聚程度减小,在高分子有机相中的分散更加均匀。     

Observation of nitriles formed in the oxidative dehydrogenation of carboxylic acids over metal-oxygen cluster catalysts

At reaction temperatures of 300–350 °C isobutyronitrile and methacrylonitrile, in addition to the expected products of oxidative dehydrogenation, methacrylic acid, acetone, propene, CO and CO₂, are produced from isobutyric acid passed over ammonium salts of 12-molybdophosphoric acid.     

Synthesis and property of hydrogel membranes consisting of fumaramate with phosphorylcholine group

Fumaramate bearing a phosphoryl choline group, isopropyl‐2‐[2′‐(trimethylammonium) ethyl phosphoryl] ethyl fumaramate (IPTPFA), was radically copolymerized with 2‐hydroxyethylmethacrylate (HEMA) in the presence of various crosslinking agents, water, and 2,2′‐azobis(isobutyronitrile) to obtain hydrogel membranes. The obtained hydrogel membranes adsorbed bovine serum albumin (BSA) much less than those of poly(HEMA), and the values of water content (H) were higher than those of poly(HEMA). The values of tensile strength and tensile elongation of the hydrogel were 68.4 g/mm² and 239%, respectively. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 2552–2557, 2004     

Synthesis of well‐defined poly(methyl methacrylate) nanoparticles by reverse atom transfer radical polymerization in a microemulsion

Well‐defined poly(methyl methacrylate) (PMMA) with an α‐isobutyronitrile group and an ω‐bromine atom as the end groups was synthesized by the microemulsion polymerization of methyl methacrylate (MMA) at 70°C with a 2,2′‐azobisisobutyronitrile/CuBr₂/2,2′‐bipyridine system. The conversion of the polymerization reached 81.9%. The viscosity‐average molecular weight of PMMA was high (380,000), and the polydispersity index was 1.58. The polymerization of MMA exhibited some controlled radical polymerization characteristics. The mechanism of controlled polymerization was studied. The presence of hydrogen and bromine atoms as end groups of the obtained PMMA was determined by ¹H‐NMR spectroscopy. The shape and size of the final polymer particles were analyzed by scanning probe microscopy, and the diameters of the obtained particles were usually in the range of 60–100 nm. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 3670–3676, 2006     

Controlled radical polymerization of methyl methacrylate in the presence of 2-bromoethanol

Summary The radical polymerization of methyl methacrylate (MMA) and styrene (St) initiated by 2,2’-azobis(isobutyronitrile) (AIBN) at 60 °C in the presence of haloalkyl alcohol are studied. The influence of structure and concentration of haloalkyl alcohol as a transfer agent are investigated. For the radical polymerization of MMA in the presence of large amount of 2-bromoethanol, controlled radical polymerization is proceeded. The 2-bromoethanol is, thus, one of the transfer agents for radical polymerization to control the molecular weight and the structure of poly(MMA).     

丙烯腈与丙烯酸氨基酯的溶液共聚动力学研究

采用膨胀计法,研究了丙烯腈（AN）和丙烯酸氨基酯（F）溶液共聚反应过程。N,N-二甲基甲酰胺（DMF）为溶剂,偶氮二异丁腈（AIBN）为引发剂。由动力学分析得到单体反应总级数和引发剂的反应级数分别为2和0．9561,其共聚合反应的表观活化能Ea=53．2kJ／mol。