林产化学与工业
林產化學與工業
림산화학여공업
CHEMISTRY AND INDUSTRY OF FOREST PRODUCTS
2015年
4期
41-47
,共7页
黄旭娟%刘鹤%商士斌%齐帆
黃旭娟%劉鶴%商士斌%齊帆
황욱연%류학%상사빈%제범
过氧乙酸%环氧化%环氧脱水蓖麻油
過氧乙痠%環氧化%環氧脫水蓖痳油
과양을산%배양화%배양탈수비마유
peracetic acid%epoxidation%epoxidized dehydrated castor oil
以蓖麻油( CTO)为原料,先制备脱水蓖麻油( DCO),再以磷酸为催化剂,过氧乙酸为氧化剂,进行环氧化反应制备环氧脱水蓖麻油( EDCO),通过单因素和正交试验优化不同条件对产品环氧值的影响。结果表明,制备EDCO较佳工艺条件为反应温度30℃、反应时间3.5 h、DCO与过氧乙酸物质的量之比5.5∶1、磷酸用量0.5%,此条件下所得EDCO的环氧值达到4.82%。采用FT-IR和1H NMR表征了蓖麻油、脱水蓖麻油以及环氧脱水蓖麻油的化学结构,结果证实EDCO中C—C被环氧化后基本消失,生成了环氧键。通过黏度测定、热重分析(TG)等方法对产品的性能进行了分析,得到CTO黏度为1100.0 mPa·s,DCO黏度为299.5 mPa·s,EDCO黏度为1896.0 mPa·s;产品的热稳定性顺序为EDCO>DCO>CTO。
以蓖痳油( CTO)為原料,先製備脫水蓖痳油( DCO),再以燐痠為催化劑,過氧乙痠為氧化劑,進行環氧化反應製備環氧脫水蓖痳油( EDCO),通過單因素和正交試驗優化不同條件對產品環氧值的影響。結果錶明,製備EDCO較佳工藝條件為反應溫度30℃、反應時間3.5 h、DCO與過氧乙痠物質的量之比5.5∶1、燐痠用量0.5%,此條件下所得EDCO的環氧值達到4.82%。採用FT-IR和1H NMR錶徵瞭蓖痳油、脫水蓖痳油以及環氧脫水蓖痳油的化學結構,結果證實EDCO中C—C被環氧化後基本消失,生成瞭環氧鍵。通過黏度測定、熱重分析(TG)等方法對產品的性能進行瞭分析,得到CTO黏度為1100.0 mPa·s,DCO黏度為299.5 mPa·s,EDCO黏度為1896.0 mPa·s;產品的熱穩定性順序為EDCO>DCO>CTO。
이비마유( CTO)위원료,선제비탈수비마유( DCO),재이린산위최화제,과양을산위양화제,진행배양화반응제비배양탈수비마유( EDCO),통과단인소화정교시험우화불동조건대산품배양치적영향。결과표명,제비EDCO교가공예조건위반응온도30℃、반응시간3.5 h、DCO여과양을산물질적량지비5.5∶1、린산용량0.5%,차조건하소득EDCO적배양치체도4.82%。채용FT-IR화1H NMR표정료비마유、탈수비마유이급배양탈수비마유적화학결구,결과증실EDCO중C—C피배양화후기본소실,생성료배양건。통과점도측정、열중분석(TG)등방법대산품적성능진행료분석,득도CTO점도위1100.0 mPa·s,DCO점도위299.5 mPa·s,EDCO점도위1896.0 mPa·s;산품적열은정성순서위EDCO>DCO>CTO。
Dehydrated castor oil( DCO) was firstly prepared by using castor oil( CTO) as raw material via dehydration reaction, and epoxidized dehydrated castor oil( EDCO) was synthesized using phosphoric acid as catalyst and acetic acid peroxide as the oxidant by epoxidation reaction afterwards. The influences of different parameters on the epoxy value of EDCO were investigated through single factor and orthogonal experiments. The results indicated that the optimal preparation conditions of EDCO were 3. 5 h reaction time, 30℃ reaction temperature, 5. 5∶1 molar ratio of peracetic acid to DCO and 0. 5% phosphoric acid dosage. The epoxy value of EDCO could be up to 4. 82% under these conditions. In addition, the chemical structures of CTO, DCO, and EDCO were characterized by FT-IR and 1H NMR . It was confirmed that the C—C double bonds in EDCO almost disappeared and the epoxy bonds were formed during the epoxidation. The properties of the products were also studied by viscosity measurement and thermogravimetric analysis( TG) . Viscosity measurement showed that the viscosities of CTO, DCO, and EDCO were 1 100. 0, 299. 5 and 1 896. 0 mPa·s, respectively. TG analysis demonstrated that the descending order of thermal stability of the products was EDCO>DCO>CTO.