二(二甲苯基)丙烷合成工艺的研究

二氯丙烷(DCP)与二甲苯在混合金属氯化物催化剂(HD90)作用下合成二(二甲苯基)丙烷,生产过程简单,产品收率高。在60—80℃的温度下,二甲苯与二氯丙烷摩尔比为6∶1,HD用量50克/摩尔DCP的条件下反应5—6小时,二(二甲苯基)丙烷的收率可达88％以上。     

Performance of the polymer- and oxide-supported triphase catalysts and effect of ultrasound on their stabilities

In this study, several trialkylamines were immobilized on chloromethylated polystyrene (CMPS), silica gel, and alumina to prepare triphase catalysts for catalyzing the etherification reaction of allyl bromide (the organic reactant) and sodium phenolate (the aqueous reactant). The reactor was agitated mechanically or with the aid of ultrasonic vibration. Performances of the prepared catalysts were compared, and the effect of imposing ultrasound was investigated based on the activity, selectivity, and stability of the catalyst. Experimental results show that tri-n-propylamine is the best active species when CMPS is used as the support, while tri-n-butylamine is the best when SiO₂ and Al₂O₃ are employed as the supports. The CMPS-supported catalyst is far better than the SiO₂- and Al₂O₃-supported catalysts in activity and selectivity but not in stability. Imposing the ultrasound can effectively increase the reaction rate. Mechanical agitation at a low speed with the imposition of ultrasonic vibration not only results in a conversion slightly higher than the case with a high mechanical agitation speed without ultrasonic vibration, but also gives a constant stability for the CMPS-supported catalyst.     

OPS和OPC系列稠油乳化降黏剂的研制

以工业品烷基酚聚氧乙烯醚OP-n（n=4,6,8,10,15）为起始原料,合成了烷基酚聚氧乙烯醚乙酸盐OPC-n和磺酸盐OPS-n两个系列的阴-非离子表面活性剂。以酸值和黏度不同的胜利单家寺和陈庄稠油为实验油样。将OPC-n和OPS-n溶于矿化度5811 mg/kg的胜利标准盐水和NaCl、CaCl2盐水中作为水相,按油、水质量比7∶3在50℃用玻棒搅拌混合,观察是否形成水包油乳状液并测黏度进行确认。在胜利标准盐水溶液中,OPC-n和OPS-n乳化稠油所需的最低质量分数,随稠油、表面活性剂类型及氧乙烯链节数n而变,一般而言,OPC-n系列中的OPC-8和OPS-n系列中的OPS-4乳化稠油的性能最好,该最低质量分数值分别为0.05%或0.025%和0.025%。在NaCl盐水溶液中,OPC-n的该最低质量分数值与稠油和n有关,均随盐含量增加而增大,在盐含量≤15%时,抗盐性最好的OPC-8和OPC-10的该值≤0.05%;OPS-n的抗盐性好于OPC-n。OPC-n的抗钙性良好,钙盐含量为2%时该最低质量分数≤0.1%;OPS-n的抗钙性更好,钙盐含量为2%和3%时该最低质量分数仅为0.025%或0.05%。表6参5。     

BIOFUMIGANT COMPOUNDS RELEASED BY FIELD PENNYCRESS (<Emphasis Type="Italic">Thlaspi arvense</Emphasis>) SEEDMEAL

Defatted field pennycress (Thlaspi arvense L.) seedmeal was found to completely inhibit seedling germination/emergence when added to a sandy loam soil containing wheat (Triticum aestivum L.) and arugula [Eruca vesicaria (L.) Cav. subsp. sativa (Mill.) Thell.] seeds at levels of 1.0% w/w or higher. Covering the pots with Petri dishes containing the soil-seedmeal mixture decreased germination of both species at the lowest application rate (0.5% w/w), suggesting that the some of the phytotoxins were volatile. CH₂Cl₂, MeOH, and water extracts of the wetted seedmeal were bioassayed against wheat and sicklepod (Senna obtusifolia (L.) H. S. Irwin & Barneby) radicle elongation. Only the CH₂Cl₂ extract was strongly inhibitory to both species. Fractionation of the CH₂Cl₂ extract yielded two major phytotoxins, identified by gas chromatography–mass spectrometry and NMR as 2-propen-1-yl (allyl) isothiocyanate (AITC) and allyl thiocyanate (ATC), which constituted 80.9 and 18.8%, respectively, of the active fraction. When seeds of wheat, arugula and sicklepod were exposed to volatilized AITC and ATC, germination of all three species was completely inhibited by both compounds at concentrations of 5 ppm or less. In field studies, where seedmeal was applied at 0.50, 1.25, and 2.50 kg/m² and tarped with black plastic mulch, all of the treatments significantly reduced dry weight of bioassay plants compared to the tarped control, with the highest seedmeal rate decreasing dry matter to less than 10% of the control 30 d after seedmeal application. Field pennycress seedmeal appears to offer excellent potential as a biofumigant for high-value horticultural crops for both conventional and organic growers.Names are necessary to report factually on available data; however, the USDA neither guarantees nor warrants the standard of the product, and the use of the name by USDA implies no approval of the product to the exclusion of others that may also be suitable.     

苯乙酸溶解度测定及提取工艺研究

为了提取6-氨基青霉烷酸(6-APA)、7-ADCA生产过程中产生的副产物苯乙酸,采用物理法测定了苯乙酸在水、水-乙醇、水-丙酮中的溶解度及其在水中的溶解速率,由此确定了水法多次提取的工艺方案。结果表明,在提取温度(60±2)℃,时间10~15 m in,水用量1 500 mL,提取次数3~4次时,苯乙酸收率为90.8%,纯度为99.3%。该法污染少、成本低,所得PAA产品质量好。     

亚砜基改性纤维素膜的SO2气体渗透性能研究

分别使用二甲基亚砜浸泡的物理方法及苯基乙烯基亚砜加成的化学方法对纤维素膜进行了改性,并对改性膜的性能进行了测试.结果表明改性后纤维素膜仍为致密结构,SO2的渗透性能及其对N2的分离性能明显提高,其中改性液中添加二甲基亚砜的均相化学加成反应所得的改性膜具有较好的SO2渗透稳定性.     

奈非西坦药物的合成研究

以碳酸钠为缚酸剂,摩尔比为1︰1的2,6-二甲基苯胺与氯乙酰氯反应合成了中间体2-氯-N-(2,6-二甲基苯基)乙酰胺;在强碱乙醇钠作用下,2-吡咯烷酮再与2-氯-N-(2,6-二甲基苯基)乙酰胺经亲核取代合成了目标化合物奈非西坦。探讨了影响中间体和奈非西坦产率的因素,在乙醇钠、2-氯-N-(2,6-二甲基苯基)乙酰胺和2-吡咯烷酮的摩尔比为2︰1︰2、反应时间为2 h的较佳工艺条件下,产品总收率达81%。     

过氧化氢氧化苯甲醛制苯甲酸的研究

以过氧化氢为氧化剂,十六烷基三甲基钨磷杂多酸铵为催化剂,催化氧化苯甲醛制苯甲酸.考察了反应温度、催化剂用量、30%过氧化氢用量和反应时间对苯甲酸产率的影响.结果表明：苯甲醛10.1 mL,30%过氧化氢11.5 mL,催化剂0.16 g,90℃下反应6 h,苯甲酸的产率可达到74.9%.     

新显色剂4—（2—苯并噻唑偶氮）邻苯二酚—钼（Ⅵ）—OP体系的分光光度研究

在ｐＨ５．０～５．７范围内，新显色剂４－（２－苯并噻唑偶氮）邻苯二酚（ＢＴＡＰＣ）与钼（Ⅵ）和非离子表面活性剂ＯＰ反应，形成稳定的、带负电荷的、紫红色三元胶束配合物。该配合物中Ｍｏ（Ⅵ）与ＢＴＡＰＣ的组成比为１∶２；其λｍａｘ为５６０ｎｍ，对比度（Δλ）为１２８ｎｍ；在２０℃、ｐＨ５．２和μ０．１时，配合物的表观稳定常数为３．０２×１０１０，表观摩尔吸光系数ε５６０为８．１１×１０４Ｌ·ｍｏｌ－１·ｃｍ－１，真实ε５６０为７．６７×１０４Ｌ·ｍｏｌ－１·ｃｍ－１。钼含量在０～０．７２ｍｇ／Ｌ范围内遵从比耳定律。建议了配合物的结构。本法简便、快速、准确，用于合金钢试样中痕量或小量钼的测定，取得了满意的结果。     

1-苯基-3-甲基-5-吡唑啉酮的合成工艺研究

在无水乙醇的存在下，乙酰乙酸乙酯和苯肼为原料合成标题化合物、采用单因素实验法，得到最佳配比为乙酰乙酸乙酯：苯肼=1.05(摩尔比)，无水乙醇50m，反应温度70℃，反应2小时，再回流7小时，收率90．9％，产品纯度99.0％以上。