微波辐射下P(BMA/2-EHM/St)复合凹凸棒高吸油树脂的制备

Preparation of High Oil-absorbing Resin of P(BMA/2-EHM/St) Composite Attapulgite under Microwave Irradiation

以甲基丙烯酸丁酯（BMA）、甲基丙烯酸异辛酯（2-EHM）和苯乙烯（St）为原料,过氧化二苯甲酰（BPO）为引发剂,聚乙烯醇（PVA）为分散剂,二乙烯基苯（DVB）为交联剂,改性凹凸棒（OATP）为无机添加物,在微波辐射下合成了高吸油树脂。探讨了St、BPO和OATP质量分数以及微波功率、反应温度和反应时间等对树脂吸油倍率的影响,用响应面法对合成工艺进行了优化,采用FTIR、TGA、SEM等对产物进行了结构表征与性能测试。结果表明：当St用量为52.54%（以单体的总质量为基准,下同）、m（2-EHM）∶m（BMA）=1.0∶1.5、BPO用量为1.95%（以单体的总质量为基准,下同）、DVB加入量为0.60%（以单体的总质量为基准,下同）、PVA加入量为3.00%（以单体的总质量为基准,下同）、OATP用量为2.00%（以单体的总质量为基准,下同）,聚合温度82℃、反应时间70 min、微波功率为700 W时,所制得的高吸油树脂吸油倍率最大,对四氯化碳、二氯甲烷、甲苯和二甲苯的吸油倍率分别达到37.24、30.50、19.64、16.81 g/g;添加OATP后树脂的热分解温度提高了32℃。

A kind of high oil-absorption resin was prepared using butyl methacrylate（BMA）,2-ethylhexyl methacrylate（2-EHM） and styrene（St） as raw materials,polyvinyl alcohol（PVA） as dispersant agent,benzoyl peroxide（BPO） as initiator,divinylbenzene（DVB） as crosslinking agent,modified attapulgite as inorganic additive under microwave irradiation. The influences of St mass fraction,BPO mass fraction,OATP mass fraction,reaction temperature,microwave power and reaction time on the oil-absorptivity of the as-prepared resin were studied. Furthermore,the synthetic process was optimized by response surface methodology. The structure and performance of oil-absorbing resin were characterized by FTIR,TGA and SEM. The results showed that when the content of St was 52.54%（based on the total mass of monomers,the same below）,the mass ratio of 2-EHM to BMA was 1.0∶1.5,the BPO dosage was 1.95%,the content of DVB was 0.60%,the content of PVA was 3.00%,the OATP dosage was 2.00%,the reaction temperature was 82 ℃,the reaction time was 70 min,and the microwave power was 700 W,the resulting oil-absorbing resin exhibited an excellent oil-absorbing property. The maximum oil-absorptivity of resin for carbon tetrachloride,dichloromethane,toluene and xylene was 37.24,30.50,16.94 and 16.81 g/g,respectively. In addition,the thermal decomposition temperature of the resin containing OATP was an improvement of 32 ℃ compared with that of the resin without OATP.