安徽理工大学学报(自然科学版)
安徽理工大學學報(自然科學版)
안휘리공대학학보(자연과학판)
Journal of Anhui University of Science and Technology (Natural Science)
2015年
3期
44-49
,共6页
陈明强%李文婷%杨忠连%刘珂%甘子玉
陳明彊%李文婷%楊忠連%劉珂%甘子玉
진명강%리문정%양충련%류가%감자옥
木质素%酚化%环氧树脂%环氧值
木質素%酚化%環氧樹脂%環氧值
목질소%분화%배양수지%배양치
lignin%phenolation%epoxy resin%Epoxy Value ( EV)
以离子液体为溶剂,对甲苯酚为酚化剂,浓硫酸为催化剂,对碱木质素( LG )进行酚化改性,然后再以NaOH为催化剂,酚化木质素(PLG)与环氧氯丙烷(ECH)进行环氧化反应,合成木质素基环氧树脂( LGEP)。利用傅里叶红外光谱对木质素及其改性和合成产物进行表征分析,示差紫外光谱法对PLG的酚羟基含量进行测定,环氧异丙醇法测定LGEF的环氧值,并设计正交实验,对酚化工艺及环氧树脂合成工艺进行了探究。实验表明:对甲苯酚的用量为10 mL/g,催化剂质量分数为60%的浓硫酸的用量为10 mL/g,改性温度为80℃,改性时间为3 h,酚化效果最佳,产物酚羟基含量达到1.4532 mmol/g;pH=9,n(酚羟基):n(ECH)=1∶2.5,反应温度90℃,反应时间5 h,环氧效果最好,最高环氧值为0.431。
以離子液體為溶劑,對甲苯酚為酚化劑,濃硫痠為催化劑,對堿木質素( LG )進行酚化改性,然後再以NaOH為催化劑,酚化木質素(PLG)與環氧氯丙烷(ECH)進行環氧化反應,閤成木質素基環氧樹脂( LGEP)。利用傅裏葉紅外光譜對木質素及其改性和閤成產物進行錶徵分析,示差紫外光譜法對PLG的酚羥基含量進行測定,環氧異丙醇法測定LGEF的環氧值,併設計正交實驗,對酚化工藝及環氧樹脂閤成工藝進行瞭探究。實驗錶明:對甲苯酚的用量為10 mL/g,催化劑質量分數為60%的濃硫痠的用量為10 mL/g,改性溫度為80℃,改性時間為3 h,酚化效果最佳,產物酚羥基含量達到1.4532 mmol/g;pH=9,n(酚羥基):n(ECH)=1∶2.5,反應溫度90℃,反應時間5 h,環氧效果最好,最高環氧值為0.431。
이리자액체위용제,대갑분분위분화제,농류산위최화제,대감목질소( LG )진행분화개성,연후재이NaOH위최화제,분화목질소(PLG)여배양록병완(ECH)진행배양화반응,합성목질소기배양수지( LGEP)。이용부리협홍외광보대목질소급기개성화합성산물진행표정분석,시차자외광보법대PLG적분간기함량진행측정,배양이병순법측정LGEF적배양치,병설계정교실험,대분화공예급배양수지합성공예진행료탐구。실험표명:대갑분분적용량위10 mL/g,최화제질량분수위60%적농류산적용량위10 mL/g,개성온도위80℃,개성시간위3 h,분화효과최가,산물분간기함량체도1.4532 mmol/g;pH=9,n(분간기):n(ECH)=1∶2.5,반응온도90℃,반응시간5 h,배양효과최호,최고배양치위0.431。
With ionic liquids as solvents , p-cresol as phenolic agent and concentrated sulfuric acid as catalyst , the alkali lignin (LG ) was modified by p -cresol.Then with NaOH as catalyst , lignin -based epoxy resin ( LGEP) was synthesized via the epoxidation reaction between the phenol lignin ( PLG)and 3-Chloro-1,2-epoxypropane (ECH).The structure of LG, PLG and LGEP were characterized by Fourier Transform -Infrared ( FT-IR) .The method of differential ultaviolet spectrophotometry was used to determine the phenoliehydroxyl group of PLG.The method of hydrochloric acid -isopropylalcohol was used to determine the Epoxy Value (EV) of LGEP.The orthogonal tests were designed to explore the optimal conditions for the phenolation of lignin and synthesis of LGEP process .The experimental results showed that the optimal conditions for the phenolation of lig-nin, which was 1.453 2mmol/g, were determined as follows:the dosage of p -cresol was 10 mLg/, and 60%sulfuric acid ,which was catalyst , was 10 mL/g, with the reaction temperature was 80℃and reaction time was 3 h.The optimal conditions for the synthesis of LGEP , which epoxy value was 0.431 , were determined as fol-lows:pH was 9, and molar ratio of phenolic hydroxyl group to ECH was 1∶2.5, with the reaction temperature was 90℃and the reaction time 5 h.