浙江师范大学学报(自然科学版)
浙江師範大學學報(自然科學版)
절강사범대학학보(자연과학판)
JOURNAL OF ZHEJIANG NORMAL UNIVERSITY(NATURAL SCIENCES)
2014年
3期
317-322
,共6页
严晓阳%孔黎春%张红娣%朱霄鹏%何卫国%何斌%郑绍成%宣日荣
嚴曉暘%孔黎春%張紅娣%硃霄鵬%何衛國%何斌%鄭紹成%宣日榮
엄효양%공려춘%장홍제%주소붕%하위국%하빈%정소성%선일영
光稳定剂%间苯二酚单苯甲酸酯%间苯二酚%苯甲酰氯%酯化%结晶
光穩定劑%間苯二酚單苯甲痠酯%間苯二酚%苯甲酰氯%酯化%結晶
광은정제%간분이분단분갑산지%간분이분%분갑선록%지화%결정
light stabilizer%resorcinol monobenzoate%resorcinol%benzoyl chloride%esterification%crystallization
研究了以苯甲酰氯和间苯二酚为原料、液碱为除酸剂,酯化合成然后精制得间苯二酚单苯甲酸酯的工艺.研究了酯化反应中温度、物料配比、pH、间苯二酚水溶液的浓度和反应时间等条件对反应的影响,获得了较佳的酯化工艺条件:苯甲酰氯与间苯二酚的摩尔比为1.15∶1;pH值为7.5;反应温度为25℃;反应时间为1.5 h;间苯二酚溶液的质量分数为10%.酯化反应收率为88.6%.考察了结晶溶剂配比、温度对产品质量和收率的影响,经实验评估得到了较佳的结晶工艺条件:结晶溶剂甲苯的体积(/mL)与初产物的质量(/g)之比为2.5∶1,结晶温度为30℃,结晶收率为95.0%.优化工艺条件下产品的总收率为84.2%.
研究瞭以苯甲酰氯和間苯二酚為原料、液堿為除痠劑,酯化閤成然後精製得間苯二酚單苯甲痠酯的工藝.研究瞭酯化反應中溫度、物料配比、pH、間苯二酚水溶液的濃度和反應時間等條件對反應的影響,穫得瞭較佳的酯化工藝條件:苯甲酰氯與間苯二酚的摩爾比為1.15∶1;pH值為7.5;反應溫度為25℃;反應時間為1.5 h;間苯二酚溶液的質量分數為10%.酯化反應收率為88.6%.攷察瞭結晶溶劑配比、溫度對產品質量和收率的影響,經實驗評估得到瞭較佳的結晶工藝條件:結晶溶劑甲苯的體積(/mL)與初產物的質量(/g)之比為2.5∶1,結晶溫度為30℃,結晶收率為95.0%.優化工藝條件下產品的總收率為84.2%.
연구료이분갑선록화간분이분위원료、액감위제산제,지화합성연후정제득간분이분단분갑산지적공예.연구료지화반응중온도、물료배비、pH、간분이분수용액적농도화반응시간등조건대반응적영향,획득료교가적지화공예조건:분갑선록여간분이분적마이비위1.15∶1;pH치위7.5;반응온도위25℃;반응시간위1.5 h;간분이분용액적질량분수위10%.지화반응수솔위88.6%.고찰료결정용제배비、온도대산품질량화수솔적영향,경실험평고득도료교가적결정공예조건:결정용제갑분적체적(/mL)여초산물적질량(/g)지비위2.5∶1,결정온도위30℃,결정수솔위95.0%.우화공예조건하산품적총수솔위84.2%.
A new process for preparation of resorcinol monobenzoate starting from benzoyl chloride and resor -cinol by esterification, extraction and crystallization was studied .The influence of temperature , pH, reaction time, resorcinol solution concentration and molar ratio of reactants on the yield of esterification was investiga -ted.The optimum reaction conditions were evaluated and selected as follows:the molar ratio of benzoyl chlo-ride to resorcinol was 1.15∶1, the pH value was 7.5, reaction temperature was 25 ℃, reaction time was 1.5 h, resorcinol solution concentration was 10%, under the optimum condition the yield of esters was about 88 .6%.The dosage of crystallization solvent and the temperature of crystallization were experimented also . The results of the experiments showed that the temperature of crystallization was 30 ℃.The ratio of solvent and reaction product was 2 .5∶1 .The yield of esterification product was about 95 .0%.The total yield was 84 .2%.