超声辅助下皂脚加压水解制备脂肪酸

doi:10.16085/j.issn.1000-6613.2022-0540

摘要/Abstract

摘要：

为了回收利用油脂精炼过程中产生的副产品皂脚中的有效成分，利用超声波辅助技术将皂脚一步转化为脂肪酸，意在考量超声波辅助技术在皂脚酸化水解过程中的作用，并在超声辅助下探究工艺条件的影响。以产物酸价和得率作为考察目标，探究了超声辅助酸化水解对产物分布的影响。结果表明，超声的分散搅拌作用使得产物的酸价和得率得到提升。通过单因素和正交设计实验探究各因素对产物酸价和得率的影响，进而确定制备脂肪酸的最佳反应条件。实验结果表明，以甲酸为酸催化剂，在反应温度220℃、反应时间110min、超声功率1050W、超声持续时间7s的反应条件下，产物酸价和得率均得到最高值，分别为184mg KOH/g和79.9%；影响产物得率的因素从主到次：反应温度>超声持续时间>超声功率>反应时间。经气相色谱质谱联用仪分析表明，产物中脂肪酸含量达到97.4%；产物质量指标测定结果表明产物具有较高的质量，皂化值达到190mg KOH/g，碘值达到157g I/100g，不皂化物含量达到0.54%。

关键词: 超声波辅助, 皂脚, 回收, 水解, 脂肪酸

Abstract:

To recycle the valuable by-product of the oil refining industry, ultrasonic assisted technology was used to produce fatty acids in one step from the soapstock. The goal was to test the acidification hydrolysis of soapstock by the ultrasonic assisted technology, and to explore the influence of process conditions with ultrasonic assistance. The acid value and yield of the product were taken as the inspection targets, and the influence of ultrasonic assistance on the product distribution was explored. Experimental results indicated that the acid value and yield of fatty acids were improved because of the enhanced dispersion and stirring of ultrasound. In order to determine the optimal reaction conditions, the effects of each factor on the acid value and yield of the product through single factor and orthogonal design experiments were discussed. Results showed that with formic acid as the catalyst, under the conditions of reaction temperature 220℃, reaction time 110min, ultrasonic power 1050W and ultrasonic duration 7s, the highest acid value and yield of the product were 184mg KOH/g and 79.9%, respectively. The order of factors affecting the yield of product from primary to secondary were reaction temperature, ultrasonic duration, ultrasonic power, and reaction time. The GC-MS analysis showed that the fatty acid content in the product reached 97.4%. The results of product quality index test showed that the product had high quality with saponification value 190mg KOH/g, iodine value 157g I/100g, and unsaponifiable matter content 0.54%.

Key words: ultrasound assisted, soapstock, recovery, hydrolysis, fatty acids

中图分类号:

TQ645.6

李栋先, 王佳, 蒋剑春. 超声辅助下皂脚加压水解制备脂肪酸[J]. 化工进展, 2023, 42(1): 409-416.

LI Dongxian, WANG Jia, JIANG Jianchun. Producing aliphatic acids via pressurized hydrolysis of soapstock assisted by ultrasound[J]. Chemical Industry and Engineering Progress, 2023, 42(1): 409-416.

图/表 9

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变量	酸价/mg KOH·g^-1	得率/%
无超声	181	35.7
有超声^②	184	63.4

变量	酸价/mg KOH·g^-1	得率/%
无超声	181	35.7
有超声^②	184	63.4

水平	反应温度（A）/℃	反应时间（B）/min	超声功率（C）/W	超声持续时间（D）/s
1	180	70	600	6
2	200	90	825	7
3	220	110	1050	8

水平	反应温度（A）/℃	反应时间（B）/min	超声功率（C）/W	超声持续时间（D）/s
1	180	70	600	6
2	200	90	825	7
3	220	110	1050	8

编号	反应温度（A）/℃	反应时间（B）/min	超声功率（C）/W	超声持续时间（D）/s	产率 /%
1	180	70	600	6	63.5
2	180	90	825	7	66.9
3	180	110	1050	8	66.2
4	200	70	825	8	69.1
5	200	90	1050	6	71.3
6	200	110	600	7	75.2
7	220	70	1050	7	77.5
8	220	90	600	8	75.2
9	220	110	825	6	72.2
K₁	196.6	210.1	213.9	207	—
K₂	215.6	213.4	208.2	219.6	—
K₃	224.9	213.6	215	210.5	—
k₁	65.5	70.0	71.3	69.0	—
k₂	71.9	71.1	69.4	73.2	—
k₃	75.0	71.2	71.7	70.2	—
R	9.5	1.2	2.3	4.2	—
最佳条件	A₃	B₃	C₃	D₂	—