化工技术与开发
化工技術與開髮
화공기술여개발
TECHNOLOGY & DVELOPMENT OF CHEMICAL INDUSTRY
2014年
1期
9-12
,共4页
钱慧娟%王依璨%宋立武%赵介堂%任成锋%高清河
錢慧娟%王依璨%宋立武%趙介堂%任成鋒%高清河
전혜연%왕의찬%송립무%조개당%임성봉%고청하
钨酸盐催化剂%环氧琥珀酸%合成规律%产率测定%提纯%表征
鎢痠鹽催化劑%環氧琥珀痠%閤成規律%產率測定%提純%錶徵
오산염최화제%배양호박산%합성규률%산솔측정%제순%표정
tungstate catalyst%epoxysuccinic acid%synthesis regularity%determination of yield%purification%characterization
以马来酸酐为原料,过氧化氢为氧化剂,钨酸盐为催化剂合成环氧琥珀酸,考察了反应温度、反应时间、物料配比、氧化剂及催化剂用量对环氧化反应和水解反应的影响规律,研究了提纯方法。结果表明,反应温度65℃,反应时间1.5h,催化剂用量3%(wt%),氢氧化钠与马来酸酐摩尔比2∶1,过氧化氢与马来酸酐质量比1.2∶1,环氧琥珀酸收率88%。采用间接法计算环氧琥珀酸产率,可精确计算收率。甲醇重结晶法可以提纯环氧琥珀酸,所得产率与间接法计算结果基本一致。经红外光谱仪分析确定产物为环氧琥珀酸。
以馬來痠酐為原料,過氧化氫為氧化劑,鎢痠鹽為催化劑閤成環氧琥珀痠,攷察瞭反應溫度、反應時間、物料配比、氧化劑及催化劑用量對環氧化反應和水解反應的影響規律,研究瞭提純方法。結果錶明,反應溫度65℃,反應時間1.5h,催化劑用量3%(wt%),氫氧化鈉與馬來痠酐摩爾比2∶1,過氧化氫與馬來痠酐質量比1.2∶1,環氧琥珀痠收率88%。採用間接法計算環氧琥珀痠產率,可精確計算收率。甲醇重結晶法可以提純環氧琥珀痠,所得產率與間接法計算結果基本一緻。經紅外光譜儀分析確定產物為環氧琥珀痠。
이마래산항위원료,과양화경위양화제,오산염위최화제합성배양호박산,고찰료반응온도、반응시간、물료배비、양화제급최화제용량대배양화반응화수해반응적영향규률,연구료제순방법。결과표명,반응온도65℃,반응시간1.5h,최화제용량3%(wt%),경양화납여마래산항마이비2∶1,과양화경여마래산항질량비1.2∶1,배양호박산수솔88%。채용간접법계산배양호박산산솔,가정학계산수솔。갑순중결정법가이제순배양호박산,소득산솔여간접법계산결과기본일치。경홍외광보의분석학정산물위배양호박산。
Epoxysuccinic acid was synthesized using maleic anhydride as raw material, hydrogen peroxide as oxidizer and tungstate as catalyst. The effects of reaction temperature, reaction time, ratio of materials, dosage of oxidizer and catalyst on epoxidation and hydrolysis reaction were investigated. Purification method of epoxysuccinic acid was also researched. The results showed that the yield of epoxysuccinic acid was 88%when the reaction conditions were as followed:reaction temperature 65℃, reaction time 1.5h, catalyst dosage 3%(wt%), molar ratio of sodium hydrate to maleic anhydride 2:1, mass ratio of hydrogen peroxide to maleic anhydride 1.2:1. The yield of epoxysuccinic acid was indirectly obtained. This indirect method could calculate the yield of epoxysuccinic acid precisely and overcome the disadvantage of obtaining inpure product by recrystallization method. Methanol recrystallization method could purify epoxysuccinic acid which had a same conclusion with indirect method. Infrared spectrometer demonstrated that the product was epoxysuccinic acid.