反应一:酚醛反应
(1).前期准备:研磨多聚甲醛及催化剂无水草酸。
(2). 将多聚甲醛,二甲苯,三乙胺,加入三口烧瓶中通过机械搅拌混合均匀解聚0.5-1h。
(3). 将1004A,三乙胺在烧杯中混合搅拌均匀,通过注射机将其滴注到(2)的烧瓶中,速率为1ml/min。待滴完反应一段时间停止反应。用真空泵在55℃的条件下去除剩余的三乙胺,甲醛,二甲苯,得到羟甲基化中间产物。
反应二:酚醇反应
(4). 称取(3)中的中间产物(约0.1mol),加入二甲苯 机械搅拌+超声30分钟后备用(完全溶解)。
(5). 将28.2g苯酚(n(苯酚):n(腰果酚中间产物)=3:1),与充分研磨的草酸混合放入三口烧瓶(100ml),机械搅拌活化0.5-1h。
(6).将(4)中备用的溶液通过注射机滴注到(5)的烧瓶中。速率为1.1ml/min。滴完反应15分钟,停止。
(7).将(6)中产品通过用60℃的去离子水多次水洗至溶液呈中性
(8).最后用真空泵去除剩余的二甲苯和苯酚。得到多元酚。
Reaction 1: Phenol-formaldehyde reaction
(1). Preparation: grinding paraformaldehyde and catalyst anhydrous oxalic acid.
(2). Add paraformaldehyde, xylene, triethylamine, into a three-necked flask by mechanical stirring and mixing uniformly to depolymerise for 0.5-1h.
(3). Mix 1004A, triethylamine in a beaker with homogeneous mixing, and drop it into the flask of (2) through a syringe machine at a rate of 1 ml/min. stop the reaction for a period of time until the drop is finished. The remaining triethylamine, formaldehyde, and xylene were removed with a vacuum pump to obtain the hydroxymethylated intermediate.
Reaction II: Phenol alcohol reaction
(4). Weigh the intermediate product (about 0.1 mol) from (3), add xylene Mechanical stirring + sonication for 30 min and set aside (completely dissolved).
(5). Mix 28.2 g of phenol (n(phenol):n(cashew phenol intermediate) = 3:1), with well ground oxalic acid into a three-necked flask (100 ml) and activate with mechanical stirring for 0.5-1h.
(6). The solution reserved in (4) was injected dropwise into the flask of (5) via a syringe. The rate was 1.1 ml/min. the reaction was stopped after 15 min of dripping.
(7). The product in (6) was passed through washing with deionised water at 60°C several times until the solution was neutral.
(8). Finally, the remaining xylene and phenol were removed by vacuum pump. Polyphenols were obtained.