CAJ | 학술논문

以三氯化磷、季戊四醇及2，4-二叔丁基苯酚为原料，采用二步法合成抗氧剂626。首先由三氯化磷与季戊四醇反应生成二氯代季戊四醇亚磷酸酯（Ⅰ），然后再与2，4-二叔丁基苯酚反应生成抗氧剂626（Ⅱ）。研究了原料配比、反应温度、反应时间、溶剂及催化剂等因素对原料转化率和产物收率的影响，利用正交设计对二步反应的工艺条件进行了优化，得到了合成抗氧剂626的优化工艺条件：原料物质的量之比为季戊四醇∶三氯化磷∶2，4-二叔丁基苯酚＝1.0∶2.25∶2.52；第1步反应温度为（60±3）℃，反应时间8 h；第2步反应温度（62±3）℃，反应时间10 h；催化剂用量为原料总投料质量的3％；溶剂为二甲苯，体系压力为0.08～0.09 MPa，结晶溶剂为异丙醇，洗涤溶剂为甲醇；以2，4-二叔丁基苯酚计目标产品，收率约为75％。
이삼록화린、계무사순급2，4-이숙정기분분위원료，채용이보법합성항양제626。수선유삼록화린여계무사순반응생성이록대계무사순아린산지（Ⅰ），연후재여2，4-이숙정기분분반응생성항양제626（Ⅱ）。연구료원료배비、반응온도、반응시간、용제급최화제등인소대원료전화솔화산물수솔적영향，이용정교설계대이보반응적공예조건진행료우화，득도료합성항양제626적우화공예조건：원료물질적량지비위계무사순∶삼록화린∶2，4-이숙정기분분＝1.0∶2.25∶2.52；제1보반응온도위（60±3）℃，반응시간8 h；제2보반응온도（62±3）℃，반응시간10 h；최화제용량위원료총투료질량적3％；용제위이갑분，체계압력위0.08～0.09 MPa，결정용제위이병순，세조용제위갑순；이2，4-이숙정기분분계목표산품，수솔약위75％。
Using phosphorus trichloride,pentaerythritol and 2,4-di-tertiary-butyl phenol as raw ma-terials,antioxidant 626 was synthesized in two steps.In the first step,pentaerythritol reacted with phos-phorus trichloride to form dichloro pentaerythritol phosphite (Ⅰ),then I continually reacted with 2,4-di-tertiary-butyl phenol to produce antioxidant 626 (Ⅱ).The influences of raw material ratio,reaction temperature,reaction time,solvent and catalyst on the conversion of raw material and product yield in two reactions were thoroughly investigated,process conditions of two reactions were optimized according to the orthogonal design.The optimization of process conditions of synthetic antioxidant 626 were ob-tained as follows:the ratio of the amount of raw material for pentaerythritol/phosphorus trichloride/2,4-di tertiary butyl phenol was equal to 2.52/1.0/2.25;the first reaction temperature was (60±3)℃,the reaction time 8 h,the second reaction temperature was (62±3)℃,reaction time 10 h;catalyst accoun-ted for 3% of the total feeding quality,Solvent was xylene,reaction system pressure was 0.08~0.09 MPa,crystallization solvent is isopropyl alcohol and cleaning solvent was methanol,and under the above optimization conditions,the antioxidant 626 yield was about 75%.