阅读说明：本技术 一种大蒜毛油膜过滤提纯工艺 (Membrane filtration purification process for garlic crude oil ) 是由 张士伟 王益友 王晖 于 2020-08-04 设计创作，主要内容包括：本发明公开了一种大蒜毛油膜过滤提纯工艺,包括如下步骤：大蒜毛油的制备、大蒜毛油粗过滤、微滤、超滤、反渗透浓缩、大蒜精油制取。本发明提纯得到的大蒜精油各项指标均符合国家标准要求,同时本发明提纯得到的大蒜精油得率达到了0.4%左右,大蒜精油得率明显高于传统方法,且本发明采用过滤与蒸馏结合,整个过程没有添加有机溶剂,同时大大减少了蒸馏时间,最大程度保留了大蒜精油的有效活性成分,值得推广使用。(The invention discloses a membrane filtration and purification process of garlic crude oil, which comprises the following steps: preparing garlic crude oil, coarse filtering garlic crude oil, micro-filtering, ultra-filtering, reverse osmosis concentrating, and preparing garlic essential oil. The garlic essential oil obtained by purification meets the national standard requirements in all indexes, the yield of the garlic essential oil obtained by purification reaches about 0.4%, the garlic essential oil yield is obviously higher than that of the garlic essential oil obtained by the traditional method, and the method adopts the combination of filtration and distillation, does not add an organic solvent in the whole process, greatly reduces the distillation time, retains the effective active ingredients of the garlic essential oil to the maximum extent, and is worthy of popularization and application.)

1. A membrane filtration purification process for garlic crude oil is characterized by comprising the following steps:

s1, preparing garlic crude oil: selecting high-quality garlic cloves, removing garlic skins, cleaning the garlic cloves, removing water on the surfaces of the garlic cloves, crushing the garlic cloves, adding deionized water for fermentation, and performing filter pressing on fermented garlic pulp to obtain filtrate, namely garlic raw oil;

s2, coarse filtration of garlic crude oil: coarse filtration treatment is carried out on the garlic crude oil through a filter bag, and waste residue impurities in the garlic crude oil are removed to obtain primary filtrate;

s3, microfiltration: microfiltration is carried out on the primary filtrate obtained in the step S2 through a microfiltration membrane technology, residual impurities, macromolecular substances and the like are further removed, secondary filtrate is obtained, the temperature in the microfiltration process is controlled to be 30-35 ℃, the pressure of equipment is adjusted to be 0.1-0.3MPa, and the aperture of the microfiltration membrane is 0.2-0.6 um;

s4, ultrafiltration; carrying out ultrafiltration on the secondary filtrate obtained in the step S3 by using an ultrafiltration membrane technology, wherein the molecular weight cut-off of the ultrafiltration membrane is 500-1000Da, the temperature in the ultrafiltration process is controlled at 30-35 ℃, the equipment pressure is regulated to 1-2.5MPa, and the garlic polysaccharide with the molecular weight larger than that of the garlic oil is cut off by the ultrafiltration membrane to remove the garlic polysaccharide in the filtrate so as to obtain a tertiary filtrate;

s5, reverse osmosis concentration: filtering and concentrating the tertiary filtrate obtained in the step S4 by a reverse osmosis membrane technology, wherein the diameter of surface micropores of the reverse osmosis membrane is 0.5-10nm, the temperature in the reverse osmosis process is controlled at 30-35 ℃, the pressure of equipment is regulated to 3.1-3.4MPa, the retentate is garlic oil concentrated solution, the filtrate is clear water, and the concentration multiple is controlled to be 7-9 times;

s6, preparing garlic essential oil: and (5) distilling, cooling and performing oil-water separation on the garlic oil concentrated solution obtained in the step (S5) to obtain the garlic essential oil.

2. The membrane filtration purification process of garlic crude oil according to claim 1, wherein: the aperture of the filter bag in the step S2 is 3-5 um.

3. The membrane filtration purification process of garlic crude oil according to claim 1, wherein: the retentate from S4 was spray dried to make garlic polysaccharide powder.

4. The membrane filtration purification process of garlic crude oil according to claim 1, wherein: the reverse osmosis membrane in the step S5 is a disc tube reverse osmosis membrane.

5. The membrane filtration purification process of garlic crude oil according to claim 1, wherein: and cleaning the membrane element once every 30min when reverse osmosis is performed in the step S5.

6. The membrane filtration purification process of garlic crude oil according to claim 1, wherein: the clear water obtained by filtering in the step S5 is recycled for fermentation in the step S1.

7. The membrane filtration purification process of garlic crude oil according to claim 1, wherein: the distillation temperature in the step S6 is 100-120 ℃, the distillation time is 30-40min, the outlet temperature of the cooling water is controlled to be less than or equal to 30 ℃, and the outlet temperature of the distillate is controlled to be less than or equal to 25 ℃.

Technical Field

The invention belongs to the field of garlic processing, and particularly relates to a membrane filtration and purification process for garlic crude oil.

Background

The garlic oil is a special substance in garlic, presents bright transparent amber liquid, is the most important substance extracted from garlic, contains important active sulfide, and is helpful for general health and cardiovascular health.

At present, the garlic oil is purified and produced by mainly adopting a water vapor distillation method in the industry, but the yield of the garlic oil is only about 0.2 percent, the yield is low, the distillation temperature is over 100 ℃, the whole process adopts distillation, and the long-time high-temperature purification easily damages effective active ingredients in the garlic oil, so that a new garlic oil purification process is needed.

Disclosure of Invention

The invention aims to overcome the problems in the prior art and provide a membrane filtration and purification process of garlic raw oil, which can not only improve the yield of garlic essential oil, but also maximally retain the effective active ingredients of the garlic essential oil.

In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:

a membrane filtration purification process for garlic crude oil comprises the following steps:

s1, preparing garlic crude oil: selecting high-quality garlic cloves, removing garlic skins, cleaning the garlic cloves, removing water on the surfaces of the garlic cloves, crushing the garlic cloves, adding deionized water for fermentation, and performing filter pressing on fermented garlic pulp to obtain filtrate, namely garlic raw oil;

s2, coarse filtration of garlic crude oil: coarse filtration treatment is carried out on the garlic crude oil through a filter bag, and waste residue impurities in the garlic crude oil are removed to obtain primary filtrate;

s3, microfiltration: microfiltration is carried out on the primary filtrate obtained in the step S2 through a microfiltration membrane technology, residual impurities, macromolecular substances and the like are further removed, secondary filtrate is obtained, the temperature in the microfiltration process is controlled to be 30-35 ℃, the pressure of equipment is adjusted to be 0.1-0.3MPa, and the aperture of the microfiltration membrane is 0.2-0.6 um;

s4, ultrafiltration; carrying out ultrafiltration on the secondary filtrate obtained in the step S3 by using an ultrafiltration membrane technology, wherein the molecular weight cut-off of the ultrafiltration membrane is 500-1000Da, the temperature in the ultrafiltration process is controlled at 30-35 ℃, the equipment pressure is regulated to 1-2.5MPa, and the garlic polysaccharide with the molecular weight larger than that of the garlic oil is cut off by the ultrafiltration membrane to remove the garlic polysaccharide in the filtrate so as to obtain a tertiary filtrate;

s5, reverse osmosis concentration: filtering and concentrating the tertiary filtrate obtained in the step S4 by a reverse osmosis membrane technology, wherein the diameter of surface micropores of the reverse osmosis membrane is 0.5-10nm, the temperature in the reverse osmosis process is controlled at 30-35 ℃, the pressure of equipment is regulated to 3.1-3.4MPa, the retentate is garlic oil concentrated solution, the filtrate is clear water, and the concentration multiple is controlled to be 7-9 times;

s6, preparing garlic essential oil: and (5) distilling, cooling and performing oil-water separation on the garlic oil concentrated solution obtained in the step (S5) to obtain the garlic essential oil.

Further, the aperture of the filter bag in the step S2 is 3-5 um.

Further, the retentate in S4 was made into garlic polysaccharide powder by spray drying.

Further, the reverse osmosis membrane in the step S5 is a disc tube reverse osmosis membrane.

Further, the membrane elements are cleaned every 30min when reverse osmosis is performed in the step S5.

Further, the clear water filtered in the step S5 is recycled for fermentation in the step S1.

Further, the distillation temperature in the step S6 is 100-120 ℃, the distillation time is 30-40min, the outlet temperature of the cooling water is controlled to be less than or equal to 30 ℃, and the outlet temperature of the distillate is controlled to be less than or equal to 25 ℃.

The invention has the beneficial effects that:

the garlic essential oil obtained by purification meets the national standard requirements in all indexes, the yield of the garlic essential oil obtained by purification reaches about 0.4%, the garlic essential oil yield is obviously higher than that of the garlic essential oil obtained by the traditional method, and the method adopts the combination of filtration and distillation, does not add an organic solvent in the whole process, greatly reduces the distillation time, retains the effective active ingredients of the garlic essential oil to the maximum extent, and is worthy of popularization and application.

Detailed Description

All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.