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催化加氫法制備對(duì)苯二甲胺的研究

發(fā)布時(shí)間:2018-05-26 12:16

  本文選題:對(duì)苯二腈 + 對(duì)苯二甲胺。 參考:《河北師范大學(xué)》2011年碩士論文


【摘要】:對(duì)苯二甲胺屬于芳香胺類化合物,此類化合物是一種用途廣泛的化工原料和精細(xì)化工中間體,目前在藥物、染料、涂料、尼龍、人造樹脂、添加劑、固化劑、纖維整理劑、防銹劑、鰲合劑、潤(rùn)滑劑、表面活性劑等許多方面都有廣泛的應(yīng)用。隨著對(duì)苯二甲胺用途的逐漸增多,對(duì)于它的生產(chǎn)工藝研究具有重要的應(yīng)用價(jià)值。目前,關(guān)于對(duì)苯二甲胺的生產(chǎn)工藝的研究比較少,本文主要研究對(duì)苯二甲腈經(jīng)催化加氫制備對(duì)苯二甲胺的工藝條件。 腈基的還原通常比較困難,腈的催化加氫反應(yīng)不僅具有理論研究上的重要意義而且在有機(jī)合成反應(yīng),精細(xì)化學(xué)品合成中具有重要的應(yīng)用。催化劑是影響腈基加氫還原反應(yīng)的主要因素。本文選用了雷尼鎳、鈀碳和鎳鋁鐵鉻合金三種催化劑催化氫化對(duì)苯二甲腈制備對(duì)苯二甲胺。其中鎳鋁鐵鉻合金催化劑為自制,通過XRD、BET、熒光等方法對(duì)其進(jìn)行了表征。 本文分別選用雷尼鎳、鈀碳、鎳鋁鐵鉻合金作為催化加氫反應(yīng)的催化劑,分別考察每種催化劑催化加氫反應(yīng)時(shí)的反應(yīng)條件,考察了溶劑、溶劑用量、催化劑用量、反應(yīng)時(shí)間、反應(yīng)溫度、反應(yīng)壓力等條件對(duì)于催化加氫反應(yīng)產(chǎn)物收率的影響,并且還對(duì)催化劑的使用壽命及再生進(jìn)行了研究。通過對(duì)比三種催化劑催化加氫反應(yīng)的最佳反應(yīng)條件和產(chǎn)物收率,并結(jié)合工業(yè)化生產(chǎn)的實(shí)際,得出鈀碳的催化加氫效果最好,得到的最佳工藝條件為:以鈀碳為催化劑,甲醇作溶劑,原料/甲醇=1:15(質(zhì)量比) ,溫度為65℃,壓力為2MPa,反應(yīng)時(shí)間為1小時(shí),產(chǎn)物對(duì)苯二甲胺的收率為81.3%,這個(gè)工藝條件比較適合工業(yè)化生產(chǎn),因此本論文對(duì)于對(duì)苯二甲腈催化加氫制備對(duì)苯二甲胺的研究具有非常重要的應(yīng)用價(jià)值。
[Abstract]:P-phenylenediamine is an aromatic amine compound, which is a widely used chemical raw material and fine chemical intermediate, and is currently used in drugs, dyes, paints, nylon, artificial resins, additives, curing agents, fiber finishing agents, Antirust agents, chelating agents, lubricants, surfactants and many other aspects have been widely used. With the increasing use of p-phenylenediamine, it has important application value for the study of its production technology. At present, there are few studies on the production process of p-phenylenediamine. In this paper, the process conditions of catalytic hydrogenation of p-phenylenediamine were studied. The reduction of nitrile group is usually difficult. The catalytic hydrogenation of nitrile not only has important significance in theoretical research but also has important applications in organic synthesis and fine chemical synthesis. Catalyst is the main factor affecting the hydrogenation reduction of nitrile group. In this paper, the catalytic hydrogenation of p-phenylenedionitrile to p-phenylenediamine was carried out on three catalysts: Raney nickel, palladium carbon and Ni-Al-Fe-Cr alloy. The Ni-Al Fe Cr alloy catalyst was prepared and characterized by XRDX BETand fluorescence method. In this paper, Reni nickel, palladium carbon, nickel, aluminum, iron and chromium alloys were selected as catalysts for hydrogenation. The reaction conditions of each catalyst were investigated, and the solvent, catalyst dosage, reaction time and solvent were investigated. The effect of reaction temperature and reaction pressure on the yield of the product was also studied. The service life and regeneration of the catalyst were also studied. By comparing the optimum reaction conditions and product yields of the three catalysts, and combining with the industrial production practice, it is concluded that the catalytic hydrogenation effect of palladium carbon is the best, and the optimum process conditions are as follows: palladium carbon as catalyst, palladium carbon as catalyst. Methanol as solvent, raw material / methanol 1: 15 (mass ratio), temperature 65 鈩,

本文編號(hào):1937203

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