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化妆品用改性山茶油制备工艺研究 |
Preparation technology of modified camellia oil for cosmetics |
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DOI:10.12166/j.zgyz.1003-7969/2020.06.009 |
中文关键词: 改性山茶油 化妆品;山茶油水解产物;酯化 |
英文关键词:modified camellia oil cosmetics camellia oil hydrolyzate esterification |
基金项目:福建省科技厅产学研项目(2017N5007);福建省科技厅公益性项目(2019R1009-8);福建省林业厅项目(闽林科(2017)3号) |
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中文摘要: |
以山茶油水解产物和聚乙二醇600(PEG600)为原料,在高温下进行酯化反应制备改性山茶油。考察了催化剂种类和用量、反应温度、投料比及反应时间对酯化反应的影响。根据单因素试验得出制备改性山茶油的最佳工艺条件为:预热温度80 ℃,预热时间5 min,4 型分子筛为催化剂,催化剂用量0.4%,反应温度160 ℃,投料比(PEG600与山茶油水解产物摩尔比)1∶ 1.2,反应时间6.5 h。在最佳工艺条件下,酯化率为93.16%,产物改性山茶油能与水以任意比例互溶。对产物分离纯化后,经定性试验以及红外光谱和超高效液相色谱-质谱(UPLC-MS)分析,发现改性山茶油的主要成分是聚乙二醇单、双酯。同时对产物的各项性能进行测试,其含水率为0.67%、皂化值(KOH)为110.2 mg/g、过氧化值为4.6 mmol/kg、临界胶束浓度为1.5 g/L(此时表面张力为32.01 mN/m)、HLB值为14、乳化最大分水时间为9.8 min。 |
英文摘要: |
The modified camellia oil was prepared by esterification reaction at high temperature using camellia oil hydrolyzate and polyethylene glycol 600(PEG600) as raw materials. The effects of catalyst type and dosage, reaction temperature, feed ratio and reaction time on the esterification reaction were investigated. According to the single factor experiment, the optimal conditions for preparing modified camellia oil were obtained as follows: preheating tempreture 80 ℃,preheating time 5 min, 4 molecular sieve as catalyst, dosage 0.4%, reaction temperature 160 ℃, feed ratio(molar ratio of PEG600 to camellia oil hydrolyzate) 1∶ 1.2, reaction time 6.5 h. Under these conditions, the esterification rate was 93.16%, and the obtained product could be mutually soluble in water at any ratio. After separating and purifying the product, qualitative tests, infrared spectrum and ultra high performance liquid chromatography-mass spectrometry (UPLC-MS) analysis showed that the main components of the modified camellia oil were polyethylene glycol mono-esters and glycol di-esters. The properties of the product were tested and the water content was 0.67%, the saponification value was 110.2 mgKOH/g, the peroxide value was 4.6 mmol/kg, and the critical micelle concentration was 1.5 g/L(with the surface tension 32.01 mN/m), the HLB value was 14, and the maximum water separating time of emulsification was 9.8 min. |
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