磺甲基酚醛树脂的制备

以亚硫酸氢钠/亚硫酸钠为磺化剂、苯酚和甲醛为原料,经苯酚磺甲基化反应和缩聚反应制备了磺甲基酚醛树脂。分别考察了羟甲基磺酸钠的合成反应、苯酚磺甲基化反应和缩聚反应的主要影响因素,羟甲基磺酸钠较佳合成工艺为n(NaHSO_3):n(Na_2SO_3):n(HCHO)=1:1:2:3,反应温度60℃,反应3h;苯酚磺甲基化反应的较佳反应条件为n(羟甲基磺酸钠):n(苯酚)=0.7:1,反应温度90℃,反应1h,pH=9;缩聚反应的较佳反应条件为:n(羟甲基磺酸钠):n(苯酚):n(甲醛)=0.7:1:1.2,pH=9,反应温度100℃,反应时间为3h。产物较佳干燥温度为100℃,较佳条件下磺甲基酚醛树脂产物的平均收率为102.7%,质量分数为10%水溶液的平均粘度为5.84 mPa·s,不溶物质量分数≤3%。对羟甲基磺酸钠和磺甲基酚醛树脂进行了红外光谱表征。

PREPARATION OF SULFOMETHYLATED PHENOL FORMALDEHYDE RESIN

Using sodium bisulfite, sodium sulfite, phenol and formaldehyde as raw materials, sulfom- ethylated phenol formaldehyde resin(SMP)was prepared by phenolic sulfomethylation and condensa- tion polymerization. The optimum conditions for preparing sodium hydroxymethylsulfonate were n (sodium bisulfite):n(sodium sulfite):n(formaldehyde)=1:1:2.3, reaction temperature 60℃and reaction time 3h. The optimum conditions for phenolic sulfomethylation were n(sodium hydroxy- methylsulfonate):n(phenol)=0.7:1, reaction temperature 90℃, reaction time 1h and pH=9. The optimum condensation polymerization conditions were n(sodium hydroxymethylsulfonate):n (phenol):n(formaldehyde)=0.7:1:1.2, pH=9, reaction temperature 100℃and reaction time 3 h. Under these conditions, the average yield of SMP was 102.7% with the average viscosity of 5.84 mPa·s(10% aqueous solution).