高校化学工程学报
高校化學工程學報
고교화학공정학보
JOURNAL OF CHEMICAL ENGINEERING OF CHINESE UNIVERSITIES
2013年
2期
259-265
,共7页
蒋平平%李成成%董玉明%苗红艳%张萍波
蔣平平%李成成%董玉明%苗紅豔%張萍波
장평평%리성성%동옥명%묘홍염%장평파
环氧聚酯%增塑剂%环氧化%环保塑化剂
環氧聚酯%增塑劑%環氧化%環保塑化劑
배양취지%증소제%배양화%배보소화제
epoxy polyester%plasticizer%epoxidation%environmental plasticizer
以四氢苯酐、二甘醇、2-乙基己醇、双氧水为原料,钛酸四正丁酯、甲酸为催化剂,分别经酯化和环氧化两步合成功能化环氧聚酯增塑剂环氧聚四氢苯酐二甘醇酯.考察了酯化反应温度、时间、醇酸摩尔比、封端剂用量、催化剂用量以及环氧化反应温度、时间、双氧水用量、甲酸用量对环氧聚四氢苯酐二甘醇酯合成的影响.采用红外光谱仪(FT-IR)、核磁共振仪(1H-NMR)、热重分析仪(TGA)对产品的结构和热稳定性等进行了表征.结果显示,最佳酯化反应条件为:四氢苯酐、二甘醇、2-乙基己醇的摩尔比为1.0:1.25:0.50,催化剂用量为酸酐质量的0.80%,反应温度200℃,反应时间6 h.最佳环氧化条件为:聚四氢苯酐二甘醇酯、甲酸、H2O2的质量比为1.0:0.50:0.90,反应温度50℃,反应时间1 h.产品环氧值>1.40%,碘值<4.0 g?(100g)?1,具有较好的流动性和热稳定性,加入PVC树脂中后,有效地提高了PVC的热稳定性.
以四氫苯酐、二甘醇、2-乙基己醇、雙氧水為原料,鈦痠四正丁酯、甲痠為催化劑,分彆經酯化和環氧化兩步閤成功能化環氧聚酯增塑劑環氧聚四氫苯酐二甘醇酯.攷察瞭酯化反應溫度、時間、醇痠摩爾比、封耑劑用量、催化劑用量以及環氧化反應溫度、時間、雙氧水用量、甲痠用量對環氧聚四氫苯酐二甘醇酯閤成的影響.採用紅外光譜儀(FT-IR)、覈磁共振儀(1H-NMR)、熱重分析儀(TGA)對產品的結構和熱穩定性等進行瞭錶徵.結果顯示,最佳酯化反應條件為:四氫苯酐、二甘醇、2-乙基己醇的摩爾比為1.0:1.25:0.50,催化劑用量為痠酐質量的0.80%,反應溫度200℃,反應時間6 h.最佳環氧化條件為:聚四氫苯酐二甘醇酯、甲痠、H2O2的質量比為1.0:0.50:0.90,反應溫度50℃,反應時間1 h.產品環氧值>1.40%,碘值<4.0 g?(100g)?1,具有較好的流動性和熱穩定性,加入PVC樹脂中後,有效地提高瞭PVC的熱穩定性.
이사경분항、이감순、2-을기기순、쌍양수위원료,태산사정정지、갑산위최화제,분별경지화화배양화량보합성공능화배양취지증소제배양취사경분항이감순지.고찰료지화반응온도、시간、순산마이비、봉단제용량、최화제용량이급배양화반응온도、시간、쌍양수용량、갑산용량대배양취사경분항이감순지합성적영향.채용홍외광보의(FT-IR)、핵자공진의(1H-NMR)、열중분석의(TGA)대산품적결구화열은정성등진행료표정.결과현시,최가지화반응조건위:사경분항、이감순、2-을기기순적마이비위1.0:1.25:0.50,최화제용량위산항질량적0.80%,반응온도200℃,반응시간6 h.최가배양화조건위:취사경분항이감순지、갑산、H2O2적질량비위1.0:0.50:0.90,반응온도50℃,반응시간1 h.산품배양치>1.40%,전치<4.0 g?(100g)?1,구유교호적류동성화열은정성,가입PVC수지중후,유효지제고료PVC적열은정성.
Using tetrahydrophthalic anhydride(THPA), ethylene diglycol (DEG), 2-ethyl-hexanol and hydrogen peroxide as raw materials, tetra-n-butyl titanate and formic acid as catalysts, epoxided poly(diglycol tetrahydrophthalic anhydride) (EPTA-2) was prepared via esterification and epoxidation reaction. The influences of esterification and epoxidation reaction conditions, such as reaction temperature, reaction time, stuff ratio, amount of used chain-ending reagent, catalyst dosage and the amounts of H2O2 and formic acid, on the two reactions were investigated. The structure and thermostability of product were characterized by FT-IR, 1H-NMR, TGA, respectively. The results show that the optimized reaction conditions of esterification are as follows: the molar ratio of THPA, DEG and 2-ethyl-hexanol is 1.0:1.25:0.50, amount of catalyst 0.8%(based on the mass of THPA), reaction temperature 200 ℃and time 6 h. The optimized conditions of epoxidation are as follows:the mass ratio of PTA-2, formic acid and H2O2 is 1.0:0.50:0.90, reaction temperature 50℃ and time 1 h. The epoxy value of product is above 1.40% and residual iodine value is below 4.0 g?(100g)?1. The product is with higher flowability and thermostability. The addition of the prepared EPTA-2 to PVC improves the thermal stability of PVC effectively.