[EN] PROCESS FOR PREPARING TRIALKYLGALLIUM COMPOUNDS<br/>[FR] PROCÉDÉ POUR LA PRÉPARATION DE COMPOSÉS DE TYPE TRIALKYLGALLIUM
申请人:UMICORE AG & CO KG
公开号:WO2013083450A1
公开(公告)日:2013-06-13
The invention relates to a process for preparing trialkylgallium compounds of the general formula R3Ga. The process is based on the reaction of gallium trichloride (GaCh), optionally in a mixture with partially alkylated products, with an alkylaluminium compound of the type RaAICIb (where R = C1-C5-alkyl, a = 1, 2 or 3, b = 0, 1 or 2 and a + b = 3) in the presence of at least two alkali metal halides (e.g. NaCI and KCI) as auxiliary base. Preference is given to using alkylaluminium sesquichloride (R3AI2CI3) or trialkylaluminium (R3AI). The reaction mixture is heated to a temperature in the range from 120°C to 250°C and the trialkylgallium compound formed is separated off via a separator which is operated at a temperature which is more than 30°C below the boiling point of the most volatile partially alkylated product. Complete alkylation is achieved here and partially alkylated products are recirculated to the reaction mixture. In a further step, the reaction mixture can be heated to a maximum of 350°C and the remaining fully alkylated and partially alkylated products can be separated off. The process provides a high yield of trialkylgallium compound and displays high gallium utilization; the products are used, e.g., as precursors for MOCVD processes.
该发明涉及一种制备一般式为R3Ga的三烷基镓化合物的过程。该过程基于氯化镓(GaCl3)与一种类型为RaAlClb(其中R = C1-C5-烷基,a = 1、2或3,b = 0、1或2,a + b = 3)的烷基铝化合物反应,可选地与部分烷基化产物混合,同时在至少两种碱金属卤化物(例如NaCl和KCl)的辅助碱存在下进行。优选使用烷基铝酮三氯化物(R3Al2Cl3)或三烷基铝(R3Al)。将反应混合物加热至120°C至250°C的温度范围,并通过在沸点最易挥发的部分烷基化产物的沸点以下30°C以上的温度下操作的分离器将生成的三烷基镓化合物分离出来。在这里实现了完全烷基化,部分烷基化产物被重新循环到反应混合物中。在进一步的步骤中,反应混合物可以加热至最高350°C,并且可以分离出剩余的完全烷基化和部分烷基化产物。该过程提供了高产率的三烷基镓化合物,并显示出高镓利用率;这些产物可用作MOCVD过程的前体。