N,N′-二仲丁基对苯二胺抗氧剂的合成

Synthesis of N,N′-Di-sec-butyl-p-phenylenediamine

以对苯二胺、丁酮为原料,在自制的铜铬催化剂和氢气存在下合成了N,N'-二仲丁基对苯二胺.研究了催化剂的制作工艺,并考察了催化剂用量、反应温度、压力、反应时间对产物收率的影响,寻找到合适的催化剂制作工艺条件及抗氧剂的制备条件:硝酸铜、硝酸铬、硝酸钡按10:10:1质量比混合后,于400℃下分解1.5 h,然后经水洗活化制得催化剂;催化剂加入量占对苯二胺的质量分数为4%;反应温度160℃,压力3.3～5.6MPa,反应时间12 h,N,N'-二仲丁基对苯二胺收率超过95%.将合成的N,N'-二仲丁基对苯二胺加入汽油(30μg·g-1)中,汽油诱导期较加入常规的抗氧化剂明显增加.

N,N′-di-sec-butyl-p-phenylenediamine was synthesized by using p-phenylenediamine, methyl ethyl ketone and hydrogen as raw materials in the presence of Cu-Cr catalyst. The preparation conditions of the catalyst and the effects of the reaction condi- tions such as catalyst dosage, reacting temperature, pressure and reaction time on the yield of product were studied. The appropriate preparation conditions of catalyst were as follows： re（copper nitrate） ： re（chromium nitrate） ： m（ barium nitrate）=10 ： 10 ：1, decomposed for 1.5 h at 400℃ , then washed with water and dried at 300℃. The optimum reacting conditions were as follows： catalyst dosage 4wt% （based on p-phenylenediamine）, reacting temperature 160 ℃, reacting pressure 3.3 ～5.6 MPa and reacting time 12 h. Under above conditions, the yield of product was over 95%. When the product （30μg·g^-1）was added in gasoline the induction time of gasoline became much longer.