N-氰乙基对甲苯胺的合成研究

用三氯化铝作催化剂,对甲苯胺与丙烯腈反应合成N-氰乙基对甲苯胺。研究了反应体系中各因素对反应的影响,实验结果表明：合成N-氰乙基对甲苯胺较适宜的工艺条件是：n（对甲苯胺）：n（丙烯腈）=1．2：1,催化剂用量为对甲苯胺的10％,反应温度为68℃-70℃,反应时间为24小时,目标产物的产率高达89．4％,纯度高于94％。     

邻硝基对甲苯胺合成工艺的研究

研究了邻硝基对甲苯胺(红色基GL,简称GL)的合成工艺,以四氯化碳为溶剂,对甲苯胺为原料,经酰化、硝化、水解三步反应制得。采用单因素实验,通过考察反应条件,确定了最佳工艺条件:对甲苯胺与乙酸酐的摩尔比为1∶1.17,对甲苯胺与发烟硝酸的摩尔比为1∶2.5,溶剂四氯化碳的用量为150 mL,硝化反应时间为1 h,硝化反应温度为42~44℃,GL的产率可达90.5%。     

2-氨基-5-甲基苯甲酸合成工艺的改进

对甲苯胺与水合氯醛、盐酸羟胺反应制得异亚硝基乙酰对甲苯胺,于浓硫酸中脱水成环得到5-甲基靛红,然后在碱性条件下以双氧水为氧化介质合成2-氨基-5-甲基苯甲酸。通过正交实验得到了一、二步反应的较佳工艺条件,三步反应总收率以对甲苯胺计算达61.7%。通过FTIR和1HNMR对最终产品进行了表征。     

邻硝基对甲苯胺的合成及其应用

一、前言邻硝基对甲苯胺,又称红色基GL、GL培司或油红培司。它是一种重要的中间体,国内外均有一定的用量,国内已有生产。邻硝基对甲苯胺纯品为桔红色结晶,熔点117℃,密度1.312,微溶于水,溶于乙醇、浓硫酸、乙醚和苯。在碱中溶解度比在酸中小得多,氨基易被氧化。工业品外观为桔红色或褐红色湿料,熔点112～115℃,干品含量可达98％。国内生产的邻硝基对甲苯胺,大部分为湿料,含量在50％以上。     

N-氰乙基对甲苯胺的合成研究

用三氯化铝作催化剂,对甲苯胺与丙烯腈反应合成N-氰乙基对甲苯胺.研究了反应体系中各因素对反应的影响,实验结果表明:合成N-氰乙基对甲苯胺较适宜的工艺条件是:n(对甲苯胺):n(丙烯腈)＝1.2:1,催化剂用量为对甲苯胺的10%,反应温度为68℃～70℃,反应时间为24小时,目标产物的产率高达89.4%,纯度高于94%.     

邻硝基对甲苯胺的合成

以对甲苯胺为原料,合成了邻硝基对甲苯胺(红色基GL)。改进了合成工艺,将酰化、硝化、水解三步合为一锅反应,总收率可达88.8%。用发烟硝酸硝化,加入二氯乙烷作溶剂,溶剂可回收利用。通过实验确定了物料的最佳配比为:n(对甲苯胺)∶n(乙酐)=1∶1.15,n(对甲苯胺)∶n(发烟硝酸)=1∶2.6,二氯乙烷的用量为105 mL(0.1 mol对甲苯胺)。     

中国2B酸发展与展望

2B酸(3-氯对甲苯胺-6-磺酸)是一种重要的有机颜料中间体，其工业化生产工艺是以对硝基甲苯为原料，经过氯化、结晶分离、还原、磺化焙烧、精制而得。     

高纯度对溴甲苯

以对甲苯胺为原料,采用两步反应法制备出高纯度对溴甲苯。该工艺在传统工艺的基础上采用独特的工艺方法,改变反应条件,抑制了邻溴甲苯、间溴甲苯的生成。产品收率76％,产品含量≥99.9％,单一杂质含量≤0.1％。南京金陵化工厂已建立了100t/a的生产装置。     

硅胶铜催化加氢气相合成对甲苯胺

对甲苯胺为白色有光泽片状或叶状结晶体，比重1．046，熔点45℃。沸点200.3℃，可溶于醇、醚、二硫化碳和油类，微溶于水，是一种重要的有机合成原料，主要用作医药、荧光增白剂的中间体以及4B酸、木质素、亚硝酸盐的试剂。近几年，对甲苯胺的国内外市场需求较大，以每年7％的速度增长。目前国内对甲苯胺的生产厂家有十余家，如江苏淮河化工厂、上海染化九厂等，生产工艺都是以对硝基甲苯还原制得。对甲苯肢的生产方法主要有：（1）硫化钠还原法。这是目前国内普遍采用的生产方法，采用63.5wt％Na2S和对硝基甲苯为原料，伴随大量的废水排…     

溶剂法制备对甲苯胺－2－磺酸

研究了溶剂法制备对甲苯胺－２－磺酸的工艺，选定了优惠工艺条件（对甲苯胺与浓硫酸的摩尔比为１∶１．０５，磺化时间７ｈ，磺化温度８０～１００℃）。确定浓硫酸为适宜磺化剂，并确认溶剂可以回收，循环使用。     

脱氢枞酸单离方法的比较研究

以歧化松香为原料、气相色谱为分析手段进行了脱氢枞酸单离方法的比较。分别采用胺化法、皂化法和超声波强化胺化反应结晶耦合法单离脱氢枞酸,并对不同的歧化松香原料进行了单离脱氢枞酸的研究,实验结果表明,采用自制的歧化松香为原料,超声波强化胺化反应结晶耦合法在 40℃ 时单离脱氢枞酸的效果最好,纯度达 99.99%,收率达 55.37%,并用GC、UV、IR、熔点仪和旋光仪对所制备的高纯度脱氢枞酸进行了分析鉴定,实验值与文献值基本一致。     

枞酸标准样品的研制

研究了从马尾松松香中分离得到的95%纯度的枞酸制备枞酸标准样品,用DB-5毛细管石英柱对枞酸样品进行气相色谱定量分析,并运用统计学分析法检验了标准样品的均匀性。枞酸标准样品的稳定性较好,-16℃下稳定时间达到8个月。     

Back extraction of propionic acid from loaded organic phase

Study of back extraction and hence regeneration of the acid from the loaded organic phase is essential for the design of a complete reactive extraction process. In this paper, the backextraction of propionic acid from the loaded organic phase (tri-n-octylamine (TOA)+diluent) was studied using different techniques, like, temperature and diluent swing, using NaOH or trimethyl amine. It was found that temperature swing regeneration could result in recovery as high as 88% of acid in two stages from organic phase, TOA+MIBK. However, from TOA+alcohols, the recovery by this technique was average. Diluent swing is not successful in efficiently recovering acid from the organic phases employed. NaOH, in stoichiometric ratio, could completely recover the acid, but in the form of sodium propionate. The 100% acid recovery was accomplished using trimethylamine (TMA), when used in stoichiometric ratio slightly higher than (1:1). Along with the complete recovery acid can be easily separated from TMA as the base is volatile. Kinetics of backextraction of propionic acid using TMA was also studied and it was found to be fast.     

固定化产氨短杆菌连续生产L—苹果酸的研究

本文研究了K-卡拉胶固定化产氨短杆菌连续生产L-苹果酸技术。用0.4％胆酸处理固定化细胞,能有效地抑制反应副产物生成。在固定化介质中添加1.5％多胺试剂,可以提高延胡索酸酶活性50％。采用柱式反应器连续生产L-苹果酸,37 C稳定工作40天,空间流速0.22小时,转化率在85％以上。固定化细胞酶的半衰期为100天,转化液经多步提纯得列白色晶体,提取收率55％。产品经纸层析,红外光谱分析和熔点测定与L-苹果酸标准品一致。     

Production of biodiesel from soapstock using an ion-exchange resin catalyst

The feasibility of biodiesel production from soapstock containing high water content and fatty matters by a solid acid catalyst was investigated. Soapstock was converted to high-acid acid oil (HAAO) by the hydrolysis by KOH and the acidulation by sulfuric acid. The acid value of soapstock-HAAO increased to 199.1 mg KOH/g but a large amount of potassium sulfate was produced. To resolve the formation of potassium sulfate, acid oil was extracted from soapstock and was converted to HAAO by using sodium dodecyl benzene sulfonate (SDBS). The maximum acid value of acid oil-HAAO was 194.2 mg KOH/g when the mass ratio of acid oil, sulfuric acid, and water was 10: 4: 10 at 2% of SDBS. In the esterification of HAAO using Amberylst-15, fatty acid methyl ester (FAME) concentration was 91.7 and 81.3% for soapstock and acid oil, respectively. After the distillation, FAME concentration became 98.1% and 96.7% for soapstock and acid oil. The distillation process decreased the total glycerin and the acid value of FAME produced a little.     

微波辅助合成5-硝基水杨酸的研究

以醋酸和醋酸酐的混和液为溶剂、浓硝酸为硝化剂,在冰浴中微波辐射下一步法直接合成5-硝基水杨酸,粗产率可达88．3％。经50％乙醇重结晶得到淡黄色粉状固体,产率为82．6％,产物结构经IR,1H NMR表征并得到确认。     

钛铁矿制备钛白副产废硫酸浓缩回用研究

在废酸浓缩装置中利用水蒸汽加热钛白生产过程中产生的废硫酸,使其质量分数由20％提高到37％,与98％的硫酸混合配制成80％的硫酸,作为酸解钛矿的操作酸。研究表明．酸解率由93％下降到90％,工艺流程顺畅．废硫酸回用率由12％提高到25％,每t钛白成本下降873．6元。     

Synthesis of fatty acid esters from acid oils using lipase B from Candida antarctica

Esterification of corn and sunflower acid oils with straight‐ and branched‐chain alcohols were conducted using lipase B from Candida antarctica (Novozym 435) in n‐hexane. Sunflower acid oil consisted of 55.6% free fatty acids and 24.7% triacylglycerols, while the free fatty acids and triacylglycerols contents of corn acid oil were 75.3% and 8.6%, respectively. After 1.5 h of methanolysis of sunflower acid oil, the highest fatty acid methyl ester content (63.6%) was obtained at 40 °C and the total fatty acid/methanol molar ratio was 1/1, using 15% enzyme based on acid oil weight. The conversion of both acid oils with straight‐ and branched‐chain alcohols was not significantly affected by the chain length of the alcohols. However, the lowest fatty acid methyl ester content (50%) was obtained in the reaction of corn acid oil with methanol. Sunflower acid oil was converted to fatty acid esters using primer alcohols such as n‐propanol, i‐ and n‐butanol, n‐amylalcohols, n‐octanol, and a mixture of amylalcohol isomers, resulting in a fatty acid ester content of about 70% at 40 °C.     

钨酸催化氧化环己醇合成己二酸

以钨酸-酸性添加剂为催化体系,在无有机溶剂和相转移剂的情况下,催化30%过氧化氢氧化环己醇合成己二酸。结果表明,当钨酸用量为2．5mmol,钨酸：酸性添加剂：环己醇：过氧化氢为1：1：40：176(摩尔比)时,酸性添加剂中,以磺酸水杨酸氧化环己醇效果最佳,反应8h己二酸分离产率达87．8%、纯度为99．9%;而单独以钨酸为催化剂时,己二酸分离产率达65．6%、纯度为97．3%;以酚类-弱酸性化合物为添加剂时,己二酸分离产率均在80%以上。钨酸-磺酸水杨酸催化体系重复使用至第5次,己二酸分离产率仍可达81．5%。     

5-单硝酸异山梨醇酯的合成研究(Ⅱ)

山梨醇经脱水、酯化、硝酸酯化及皂化,合成了５ 单硝酸异山梨醇酯。山梨醇脱水反应：山梨醇与硫酸质量比为１∶００１４,二甲苯作带水剂,反应温度１４０℃,反应时间３５ｈ,得异山梨醇（Ⅰ）,收率６９％;酯化反应：异山梨醇、冰乙酸及对甲基苯磺酸的质量比为１∶０４９∶００３４,溶剂Ｓ兼作带水剂,回流反应,得２ 乙酸异山梨醇酯混合物（Ⅱ）;在１０℃,Ⅱ与硝酸质量比为１∶０３６,２ｈ内进行硝酸酯化,得２ 乙酸 ５ 硝酸异山梨醇酯混合物（Ⅲ）;Ⅲ在５０℃、ｐＨ＝１０～１２条件下皂化１５ｈ,得５ 单硝酸异山梨醇酯。总收率２５％。