亚临界萃取棉酚工艺研究

doi:10.11924/j.issn.1000-6850.casb2021-0675

摘要/Abstract

摘要：

试验利用亚临界萃取技术探究棉籽仁中游离棉酚萃取的合适提取工艺条件,为棉酚的工业化生产提供依据。以高酚棉籽为提取原料,分析前处理方式和萃取过程中温度、时间、料液比、次数等因素对提取率的影响,并采取正交试验优化提取工艺条件。结果表明,预处理试验中,粉碎过40目筛轧胚提取率最高,为57.6%;单因素试验中,棉酚提取率随着温度的升高先升高后降低,20℃时达到最高58.2%,随着时间的增加逐渐升高,30 min后增长趋于平缓,随着次数的增加逐渐升高,4次后增长趋于平缓,随着料液比的增加逐渐变大,在1:12后增长趋于平缓。正交试验结果得到亚临界萃取棉酚的最佳工艺为：温度20℃,时间40 min,次数4次,料液比1:14,此时提取率为68.9%。

关键词: 棉酚, 亚临界萃取, 单因素试验, 正交试验

Abstract:

The experiment aims to use subcritical extraction technology to explore the optimal extraction condition of free gossypol in cotton kernels, and provide a basis for the industrial production of gossypol. Using high-phenol cottonseed as the raw material for extraction, the influence of factors such as the pretreatment method and the temperature, time, material-to-liquid ratio, and times of extraction on the extraction rate were analyzed, and orthogonal experiments were conducted to determine the optimal extraction condition. The results showed that in the pretreatment experiment, the extraction rate of crushed embryos through 40 mesh sieve was the highest, which was 57.6%; In the single factor experiment, the extraction rate of gossypol first increased and then decreased with the increase of temperature, reaching the highest 58.2% at 20 ℃. With the time increasing gradually, the growth of the extraction rate tended to be flat after 30 minutes, and gradually increased along with the number of extraction times, the growth tended to be flat after 4 times. The extraction rate gradually increased along with the material-to-liquid ratio, and became flat after the ratio reached 1:12. Orthogonal test results showed that the optimal condition for subcritical extraction of gossypol was: temperature at 20℃, time duration of 40 min, 4 times of extraction, and the material-liquid ratio of 1:14, under this condition, the extraction rate was 68.9%.

Key words: gossypol, subcritical extraction, single-factor experiment, orthogonal test

中图分类号:

荣梦杰, 金云倩, 王延琴. 亚临界萃取棉酚工艺研究[J]. 中国农学通报, 2021, 37(26): 9-14.

Rong Mengjie, Jin Yunqian, Wang Yanqin. Subcritical Extraction Technology of Gossypol[J]. Chinese Agricultural Science Bulletin, 2021, 37(26): 9-14.

图/表 9

参考文献 26

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溶剂	甲醇	乙醇	丙酮	二甲醚	液氨
分子式	CH₃OH	C₂H₅OH	CH₃COCH₃	C₂H₆O	NH₃
分子量	32	46	58	46	17
沸点/℃	64.7	78	56.5	-23	-33.5
临界温度/℃	240	243.1	235.5	127	132.3
临界压力/KPa	7950	6380	4720	5330	11300
性状	无色有酒精气味	无色有味	无色有辛辣气味	无色有味	无色有刺激性气味
常温状态	液态	液态	液态	气态	气态
介电常数	33.7	25.7	20	5.02	16.2
爆炸极限/%	6~36.5	3.3~19	2.5~12.8	不燃	16~25
蒸气压(20℃,kPa)	12.3	5.333	24.711	0.495	882
价格/（元/t）	1600	6300	12000	2300	4200

溶剂	甲醇	乙醇	丙酮	二甲醚	液氨
分子式	CH₃OH	C₂H₅OH	CH₃COCH₃	C₂H₆O	NH₃
分子量	32	46	58	46	17
沸点/℃	64.7	78	56.5	-23	-33.5
临界温度/℃	240	243.1	235.5	127	132.3
临界压力/KPa	7950	6380	4720	5330	11300
性状	无色有酒精气味	无色有味	无色有辛辣气味	无色有味	无色有刺激性气味
常温状态	液态	液态	液态	气态	气态
介电常数	33.7	25.7	20	5.02	16.2
爆炸极限/%	6~36.5	3.3~19	2.5~12.8	不燃	16~25
蒸气压(20℃,kPa)	12.3	5.333	24.711	0.495	882
价格/（元/t）	1600	6300	12000	2300	4200

试验序号	试验因素				棉酚萃取率
试验序号	A	B	C	D	棉酚萃取率
1	1	1	1	1	54.40
2	1	2	2	2	60.20
3	1	3	3	3	68.90
4	2	1	2	3	60.50
5	2	2	3	1	46.10
6	2	3	1	2	54.20
7	3	1	3	2	45.00
8	3	2	1	3	44.70
9	3	3	2	1	18.80
K1	183.500	159.900	153.300	119.300	452.80
K2	160.800	151.000	139.500	159.400
K3	108.500	141.900	160.000	174.100
k1	61.167	53.300	51.100	39.767
k2	53.600	50.333	46.500	53.133
k3	36.167	47.300	53.333	58.033
R	25.000	6.000	6.833	18.267
主次顺序	A>D>C>B
优水平	A1	B1	C3	D3
优组合	A1B1C3D3

试验序号	试验因素				棉酚萃取率
试验序号	A	B	C	D	棉酚萃取率
1	1	1	1	1	54.40
2	1	2	2	2	60.20
3	1	3	3	3	68.90
4	2	1	2	3	60.50
5	2	2	3	1	46.10
6	2	3	1	2	54.20
7	3	1	3	2	45.00
8	3	2	1	3	44.70
9	3	3	2	1	18.80
K1	183.500	159.900	153.300	119.300	452.80
K2	160.800	151.000	139.500	159.400
K3	108.500	141.900	160.000	174.100
k1	61.167	53.300	51.100	39.767
k2	53.600	50.333	46.500	53.133
k3	36.167	47.300	53.333	58.033
R	25.000	6.000	6.833	18.267
主次顺序	A>D>C>B
优水平	A1	B1	C3	D3
优组合	A1B1C3D3

因素	变差平方和	自由度	F值	F_0.05(2,2)	F_0.01(2,2)	显著性
A	986.176	2	13.539	19.00	99.00	—
B	54.002	2	0.741	19.00	99.00	—
C	72.842	2	1.000	19.00	99.00	—
D	536.349	2	7.363	19.00	99.00	—
误差	54.002	2				—