一种弱酸性绿光黑染料的合成研究

本文对一种弱酸性绿光黑染料的合成进行了研究。合成工艺为对硝基苯胺经重氮化后,在酸性条件下与H酸偶合,合成一次偶合物;4,4'-二氨基苯磺酰替苯胺重氮盐在碱性条件下分别与上述一次偶合物和间苯二酚偶合,合成绿光黑染料。经测试,该染料牢度性能优于直接黑RN和直接耐晒黑G。     

芳香胺的重氮偶合反应 N-偶合和 C-偶合之间的竞争

作者对芳香胺(过量)与苯胺重氮盐在无水乙腈中的重氮化和偶合反应在三个温度以及不同胺浓度条件下作了研究。N-偶合和 C-偶合反应各自都生成重氮氨基化合物和氨基偶氮化合物。但是,在强碱及Cl存在下,只生成重氮氨基化合物。     

KN型双偶氮活性蓝色染料的制备及其染色性能研究

以对硝基苯胺重氮盐与1-氨基-8-萘酚-3,6-二磺酸(H酸)在酸性条件下偶合首先制备了红色单偶氮染料,接着与对(β-硫酸酯乙基砜)苯胺重氮盐在中性条件下与单偶氮红色染料偶合制备了KN型双偶氮活性蓝色染料,通过红外、紫外-可见吸收光谱和质谱对产物结构进行了表征。通过浸染工艺,将该KN型双偶氮活性蓝色染料用于棉纤维的染色研究,结果表明染色棉纤维的干/湿摩擦牢度分别为4和3～4级,日晒牢度4级,水洗牢度4～5级。     

分散橙SE—3GL合成研究

本文介绍了分散橙ＳＥ－３ＧＬ的合成工艺，研究了利用甲醛、亚硫酸氢钠加成物与邻甲氧基苯胺的氨基形成Ｗ盐，与对硝基苯胺重氮盐偶合的反应条件。     

C.I.分散蓝257及其中间体的合成

研究了以间乙酰氨基苯胺和对甲苯磺酸-β-甲氧基乙酯为原料,在缚酸剂氧化镁的作用下合成间乙酰氨基-N,N-二(β-甲氧基乙基)苯胺的工艺路线,然后与2-氰基-4-硝基-6-溴苯胺的重氮盐偶合反应合成C.I.分散蓝257,总收率80%,并对产品进行上染性能测试.合成中间体间乙酰氨基-N,N-二(β-甲氧基乙基)苯胺较佳工艺条件为:水与对甲苯磺酸-β-甲氧基乙酯及间乙酰氨基苯胺摩尔比为10∶ 2.2∶ 1,且采用分段升温.     

C．I．分散蓝257及其中间体的合成

研究了以间乙酰氨基苯胺和对甲苯磺酸-β-甲氧基乙酯为原料,在缚酸剂氧化镁的作用下合成间乙酰氨基-N,N-二（β-甲氧基乙基）苯胺的工艺路线,然后与2-氰基-4-硝基-6-溴苯胺的重氮盐偶合反应合成C．I．分散蓝257,总收率80％,并对产品进行上染性能测试。合成中间体间乙酰氨基-N,N-二（β-甲氧基乙基）苯胺较佳工艺条件为：水与对甲苯磺酸-β-甲氧基乙酯及间乙酰氨基苯胺摩尔比为10：2、2：1,且采用分段升温。     

苯胺重氮盐与间苯二酚的偶合反应

苯胺重氮盐与间苯二酚的偶合反应会生成一个由一偶氮物、二偶氮物和三偶氮物组成的混合物,其中二偶氮物(4,6-二苯基偶氮间苯二酚)是合成4,6-二氨基间苯二酚的关键中间体,因此控制偶合反应的条件,高选择性地得到4,6-二苯基偶氮间苯二酚是非常有意义的。考察了反应温度、间苯二酚与苯胺重氮盐的摩尔比、间苯二酚与NaOH的摩尔比对生成4,6-二苯基偶氮间苯二酚的影响。研究发现,当反应温度在-7℃～-5℃,间苯二酚∶苯胺重氮盐的摩尔比=1∶2.3,间苯二酚∶NaOH的摩尔比=1∶16.8时,反应产物未经纯化处理,其4,6-二苯基偶氮间苯二酚的含量即可达92%以上,收率80%左右。     

分散橙SE—3GL合成研究

本文介绍了分散橙ＳＥ－３ＧＬ的合成工艺，研究了利用甲醛、亚硫酸氢钠加成物与邻甲氧基苯胺的的氨基形成Ｗ盐，与对硝基苯胺重氮盐偶合的反应条件。     

C.I.分散黄163绿色合成工艺研究

介绍了C.I.分散黄163新的合成方法:以2,6-二氯-4-硝基苯胺为原料,在醇醚溶剂中用亚硝酰硫酸对其进行重氮化,采用萘磺酸稳定剂与之形成复盐,重氮盐以固体形态析出。再将其与N,N-二氰乙基苯胺偶合,得到最终染料产品。对N,N-二氰乙基苯胺预先进行了细化处理,在不加入酸的条件下进行偶合反应,针对偶合组分细化处理条件对偶合反应的影响进行了研究,得到了较好的反应条件。     

弱酸性黑NB-G染料合成工艺

本文介绍了4,4-二氨基苯磺酰苯胺(简称DASA)双重氮化,在酸性条件下与H-酸偶合,苯胺重氮化,与上述所得产物在碱性条件下偶合,然后再与间苯二胺偶合,合成出弱酸性黑NB-G染料合成工艺,并对工艺条件进行了研究.     

活性黑RL染料合成工艺研究

通过实验确定活性黑RL染料的合成工艺。本文采用γ酸重氮化后,在低温酸性条件下与1-(4-磺酸基苯基)-3-羧基-5-吡唑啉酮偶合,2,5-二甲氧基对位酯重氮化后与上述产物进行第二次偶合,偶合产物经Cu络合后盐析、干燥得到活性黑RL染料成品。最佳工艺条件为:重氮反应温度控制在0～5℃、偶合反应时pH=7.5～8、Cu络合反应时温度控制在110℃、pH=6～6.2。     

酸性红P-L的合成研究

本文介绍了2-甲基-5-氨基-N-乙基苯磺酰苯胺重氮化后,在酸性条件下与γ-酸偶合而制得酸性红P-L的方法.讨论了合成工艺路线的优化,并对染料的应用性能进行了测定.     

Oleic acid esterification with ethanol under continuous water removal conditions

The production of ethyl ester was investigated using a new reaction system consisting of a reactor coupled to an adsorption column. The adsorption system was used to shift the equilibrium toward ethyl ester production by removing the water from commercial ethanol and the water produced during the esterification reaction. A condenser placed above the adsorption column was responsible to condensate the vapor, returning water free ethanol to the reactor. Ethyl ester was produced by esterification of oleic acid and ethanol using sulfuric acid as catalyst. The results showed a yield of 99.9%. The best operating condition was found operating the reactor at 110 °C, 1% of catalyst (w/w) and with an oleic acid to ethanol ratio of 1:3.     

HPLC-ELSD法测定缬氨酸样品中杂质氨基酸的含量

建立了反相高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定缬氨酸样品中杂质氨基酸含量的方法.采用Hypersil BDS C18色谱柱(4.6×250mm,5μm),以0.1%三氟乙酸乙腈溶液-0.1%三氟乙酸水溶液为流动相进行线性梯度洗脱,流速为0.8mL·min-1,在漂移管温度60℃,氮气流量1.5L·m...     

ICP-OES法测定高温合金中的铌

建立了用电感耦合等离子体发射光谱法（ICP-OES）测定高温合金钢中铌的测定方法。比较了用盐、硝混合酸溶样加硫、磷混酸发烟后测定以及盐、硝混合酸溶样加硫酸发烟后再进行测定的效果。对溶液酸度进行了研究,结果表明5%的硫酸介质测定效果较好。考察了测定用仪器的等离子观测方式以及铌的分析谱线与共存元素的干扰问题。最终选定径向观测、分析线波长Nb309.418 nm,用于高温合金钢样品的测定,相对标准偏差小于2%,加标回收率为102.2%～107.0%。结果较好。     

Polarization and impedance studies on zinc phosphate coating developed using galvanic coupling

Galvanic coupling technique is capable of producing coatings of desired thickness. Good quality coatings can be produced at low temperature. Galvanic coupling of mild steel (MS) with the other cathode materials such as titanium (Ti), copper (Cu), brass (BR), nickel (Ni), and stainless steel (SS) accelerates iron dissolution, enables quicker consumption of free phosphoric acid and facilitates an earlier attainment of point of incipient precipitation, resulting in a higher amount of coating formation. In the present investigation, potentiodynamic polarization and electrochemical impedance spectra on MS substrates phosphated using galvanic coupling are studied. This study reveals that MS substrates phosphated under galvanically coupled condition possess better corrosion resistance than the substrates phosphated under uncoupled condition.     

微波消解-电感耦合等离子体原子发射光谱法测定酚醛树脂合成材料中铝钙硼镁锌

提出了微波消解电感耦合等离子体原子发射光谱法测定酚醛树脂合成材料中铝、钙、硼、镁、锌的分析方法。在密闭容器中,用硝酸和氢氟酸混酸做溶剂在微波状态下消解酚醛树脂合成材料样品,样品溶解完毕泄压后,定容,用电感耦合等离子体原子发射光谱仪测定铝、钙、硼、镁、锌的含量。同时考察了微波消解称样量、溶剂用量及共存离子对分析结果的影响,其样品的测定结果与化学法测定值一致。本法适应于酚醛树脂合成材料中铝、钙、硼、镁、锌的测定。     

Adsorption of 2-naphthalenesulfonic acid/sulfuric acid/sulfurous acid from aqueous solution by iron-impregnated weakly basic resin:Equilibrium and model

Commercial grade weakly basic resin D301 was impregnated with iron through a simple method using ferric chloride. Experiments for single, bisolute and trinary competitive adsorption were carried out to investigate the adsorption behavior of 2-naphthalenesulfonic acid (NSA), sulfuric acid and sulfurous acid from their solution at 298K onto the novel hybrid iron impregnated D301(Fe-D301). Adsorption affinity of NSA on Fe-D301 was found to be much higher than that of sulfuric acid, while adsorption affinity of sulfuric acid was slightly higher than that of sulfurous acid. The data of single-solute adsorption were fitted to the Langmuir model and the Freundlich adsorption model. The non-ideal competitive adsorbed model coupled with the single-solute adsorp-tion models were used to predict the bisolute and trinary-solute competitive adsorption equilibria. The NICM coupled with the Langmuir model yields the favorable representation of the bisolute and trinary-solute compet-itive adsorption behavior.     

酸性红S—GN的合成研究

4-氯-2-氨基苯酚重氮化后,分别与1-（4’-磺酸基）苯基-3-甲基-5-吡唑酮和1-苯基-3-甲基-5-吡唑酮偶合,得到偶氮物I和偶氮物Ⅱ;偶氮物I和氧化铬铬化反应得到络合物Ⅲ;络合物Ⅲ再与偶氮物Ⅱ在碱性条件下反应得到红色不对称金属络合染料（酸性红S—GN）。本文介绍了该染料的化学结构及合成方法。     

2-萘磺酸/硫酸在弱碱性树脂上的吸附平衡研究

Experiments for single and bisolute competitive adsorption were carried out to investigate the adsorption behavior of β-naphthalenesulfonic acid(NSA and sulfuric acid from their solution at 25℃ onto weakly basic resin D301R,Adsorption affinity of sulfuric acid on D301R was found to be much higher than that of NSA.The data of single-solute adsorption were fitted to the Langmuir model and the Freundlich adsorption model.The ideal adsorbed solution theory(IAST) coupled with the single-solute adsorption models were used to predict the bisolute competitive adsorption equilibria.The IAST coupled with the Langmuir and the Freundlich model for sulfuric acid and NSA.Respectively,yields the favorable representation of the bisolute competitive adsorption behavior.