脂肪酸酰胺蜡的研究
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摘要
本课题首先以乙二胺和硬脂酸为主要原料,在常压下一步法制备乙撑双硬脂酰胺,通过添加抗氧剂解决了产品颜色发黄的问题。实验结果表明最佳工艺条件为：n(硬脂酸)：n(乙胺)=1：0.56,乙二胺滴加温度100℃,滴加时间40min,反应温度204℃,反应时间4.5h,催化剂为磷酸其用量为硬脂酸质量的0.5%,抗氧剂的用量为硬脂酸质量的0.4%。抗氧剂的加入能够显著提高产品的颜色。
其次,以硬脂酸和二乙烯三胺为原料,通过加入添加剂利用催化合成反应制备了能够用于肥料表面做缓释剂的酰胺蜡。实验结果表明最佳合成工艺条件为：n(硬脂酸)：n(二乙烯三胺)=1：1.05,反应温度145℃,反应时间2.5h,催化剂质量分数0.5%,添加剂的质量分数0.5%,抗氧剂的质量分数0.5%。在该工艺条件下产品的颜色为白色,酸值5.13mgKOH/g,滴熔点81℃,针入度2.2(0.1mm),胺值143.42mgKOH/g。经用户使用表明该产品可以替代国外同类产品,而且价格低于国外同类产品。
最后,以硬脂酸和二乙醇胺为主要原料,通过分步、催化合成法制备了烷醇酰胺蜡,通过对反应条件进行考察,得出最佳工艺条件为：第一步n(硬脂酸)：n(二乙醇胺)=1：0.45,第二步n(硬脂酸)：n(二乙醇胺)=1：0.65第一步反应时间4h,第二步反应时间4h,第一步反应温度175℃,第二步反应温度105℃,催化剂用量为硬脂酸质量的0.5%。在此工艺条件下,制备的产品的颜色为淡黄色,酸值2.16mgKOH/g,胺值27.56mgKOH/g,滴熔点52℃,针入度15.37(0.1mm)。
Firstly, In this study, with ethylene diamine and stearic acid as raw material, ethylene bistearamide were prepared by adding antioxidant to solve the problem of yellow color, at normal pressure. Experimental results showed that the optimum technology condition were as follows:n(stearic acid):n(Ethylenediamine)=1:0.56; the temperature and rang of time of ethylenediamine dropping were 100℃and 40 min; the optimum temperature and reaction time were 204℃and 4.5h; phosphoric acid as the catalyst for the dosage of the quality of the stearic acid 0.5%; antioxidant for the dosage of the quality of the stearic acid 0.4%. Antioxidant can significantly improve the color of product.
Secondly, with stearic acid and diethylenetrianmine as raw materials, the amide wax was prepared using catalytic synthesis reaction by adding additives, which was used as the surface slow release agent of fertilizer. Experimental results showed that the optimum technology conditions were as follows:n(stearic acid):n(diethylenetriamine)=1:1.05, the reaction temperature 145℃, the reaction time about 2.5h,0.5% of mass percent of the catalyst,0.5% of mass percent of both the additive and antioxidant. In these conditions, the color of product was white, the acid number was 5.13mgKOH/g, the dropping point was 81℃, the penetration degree was 2.2(0.1mm), and the amine value was about 143.42mgKOH/g. The feedback information of users showed that the product can substitute for foreign like products and the price of the product is lower than the prices of foreign like products.
Finally, with stearic acid and diethanolamine as raw materials, the alkanolamide wax was prepared according to two steps and catalytic synthesis. Experimental results showed that the optimum technology conditions were as follows:the first step n(stearic acid): n(diethanolamine)=1:0.45 and the second step n(stearic acid):n(diethanolamine)=1:0.65; The first step reaction time was 4.5h and the second step reaction time was 4h also;the first step reaction temperature was 175℃and the second reaction temperature was 105℃;The amount of catalyst is 0.5% of stearic acid, In this condition, the color of the product was light yellow,acid value was 2.16mgKOH/g and amine number was 27.56 mgKOH/g, dropping point was 52℃and the penetration degree was 15.37(0.1mm).
其次,以硬脂酸和二乙烯三胺为原料,通过加入添加剂利用催化合成反应制备了能够用于肥料表面做缓释剂的酰胺蜡。实验结果表明最佳合成工艺条件为：n(硬脂酸)：n(二乙烯三胺)=1：1.05,反应温度145℃,反应时间2.5h,催化剂质量分数0.5%,添加剂的质量分数0.5%,抗氧剂的质量分数0.5%。在该工艺条件下产品的颜色为白色,酸值5.13mgKOH/g,滴熔点81℃,针入度2.2(0.1mm),胺值143.42mgKOH/g。经用户使用表明该产品可以替代国外同类产品,而且价格低于国外同类产品。
最后,以硬脂酸和二乙醇胺为主要原料,通过分步、催化合成法制备了烷醇酰胺蜡,通过对反应条件进行考察,得出最佳工艺条件为：第一步n(硬脂酸)：n(二乙醇胺)=1：0.45,第二步n(硬脂酸)：n(二乙醇胺)=1：0.65第一步反应时间4h,第二步反应时间4h,第一步反应温度175℃,第二步反应温度105℃,催化剂用量为硬脂酸质量的0.5%。在此工艺条件下,制备的产品的颜色为淡黄色,酸值2.16mgKOH/g,胺值27.56mgKOH/g,滴熔点52℃,针入度15.37(0.1mm)。
Firstly, In this study, with ethylene diamine and stearic acid as raw material, ethylene bistearamide were prepared by adding antioxidant to solve the problem of yellow color, at normal pressure. Experimental results showed that the optimum technology condition were as follows:n(stearic acid):n(Ethylenediamine)=1:0.56; the temperature and rang of time of ethylenediamine dropping were 100℃and 40 min; the optimum temperature and reaction time were 204℃and 4.5h; phosphoric acid as the catalyst for the dosage of the quality of the stearic acid 0.5%; antioxidant for the dosage of the quality of the stearic acid 0.4%. Antioxidant can significantly improve the color of product.
Secondly, with stearic acid and diethylenetrianmine as raw materials, the amide wax was prepared using catalytic synthesis reaction by adding additives, which was used as the surface slow release agent of fertilizer. Experimental results showed that the optimum technology conditions were as follows:n(stearic acid):n(diethylenetriamine)=1:1.05, the reaction temperature 145℃, the reaction time about 2.5h,0.5% of mass percent of the catalyst,0.5% of mass percent of both the additive and antioxidant. In these conditions, the color of product was white, the acid number was 5.13mgKOH/g, the dropping point was 81℃, the penetration degree was 2.2(0.1mm), and the amine value was about 143.42mgKOH/g. The feedback information of users showed that the product can substitute for foreign like products and the price of the product is lower than the prices of foreign like products.
Finally, with stearic acid and diethanolamine as raw materials, the alkanolamide wax was prepared according to two steps and catalytic synthesis. Experimental results showed that the optimum technology conditions were as follows:the first step n(stearic acid): n(diethanolamine)=1:0.45 and the second step n(stearic acid):n(diethanolamine)=1:0.65; The first step reaction time was 4.5h and the second step reaction time was 4h also;the first step reaction temperature was 175℃and the second reaction temperature was 105℃;The amount of catalyst is 0.5% of stearic acid, In this condition, the color of the product was light yellow,acid value was 2.16mgKOH/g and amine number was 27.56 mgKOH/g, dropping point was 52℃and the penetration degree was 15.37(0.1mm).
引文
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[20]李明,李玉芳.乙撑双硬脂酰胺的生产和应用前景[J].精细化工原料及中间体.2007,(6)：31-33
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[22]韩金山.我国EBS的市场前景和应用进展[J].化工中间体.2004,(15)：15-16
[23]徐群,陈朝晖,田文霞.乙撑双硬脂酰胺的合成[J].齐齐哈尔大学学.2000,16(4)：74-76
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