CN113652302B - Method for preparing skin-care tea seed oil by separating unsaturated fatty acid from tea seed oil - Google Patents

Method for preparing skin-care tea seed oil by separating unsaturated fatty acid from tea seed oil Download PDF

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CN113652302B
CN113652302B CN202111022327.5A CN202111022327A CN113652302B CN 113652302 B CN113652302 B CN 113652302B CN 202111022327 A CN202111022327 A CN 202111022327A CN 113652302 B CN113652302 B CN 113652302B
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seed oil
tea seed
fatty acid
unsaturated fatty
oil
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CN113652302A (en
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刘国功
李心善
余光明
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Anhui Shanmei Biotechnology Co ltd
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Anhui Shanmei Biotechnology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/008Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B7/00Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/74Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses a method for preparing skin-care tea seed oil by separating unsaturated fatty acid from tea seed oil, which relates to the technical field of skin-care product processing, and adopts a mode of combining low-temperature freezing and natural tempering, and the tea seed oil with the unsaturated fatty acid content of more than 98% is separated from edible tea seed oil; according to the invention, the camellia seed oil is processed into the skin care camellia seed oil, so that deep processing of the camellia seed oil is realized, and the economic benefit of the product is greatly improved, thereby promoting the healthy development of enterprises.

Description

Method for preparing skin-care tea seed oil by separating unsaturated fatty acid from tea seed oil
Technical field:
the invention relates to the technical field of skin care product processing, in particular to a method for preparing skin care tea seed oil by separating unsaturated fatty acid from tea seed oil.
The background technology is as follows:
the wild camellia oil is also called camellia seed oil and camellia oil, the camellia tree grows in a wet climate zone of a subtropical south mountain, and auxiliary means such as chemical fertilizers and pesticides are not needed in the whole growth process, so that the wild camellia oil belongs to pure natural high-grade woody edible oil. The oil tea seed oil is obtained from mature seeds of camellia oleifera of Theaceae or small She Youcha, and is obtained by extracting with oil extraction method such as squeezing method and leaching method. The camellia oleosa seed oil is one of the oldest woody edible vegetable oil in China and also one of the four woody vegetable oils in the world.
The camellia seed oil contains rich unsaturated fatty acid, and researches show that the higher the content of the unsaturated fatty acid is, the better the affinity of the camellia seed oil with human skin is, the more easily the camellia seed oil is absorbed by the skin, so that the effects of diminishing inflammation, resisting oxidation, sterilizing and the like are exerted.
The components of the camellia seed oil are complex, if the camellia seed oil is directly used as skin care oil, the expected skin care effect cannot be obtained, so that the camellia seed oil needs to be separated and purified, and the unsaturated fatty acid content of the camellia seed oil is improved. However, the separation and purification method adopted at present is complicated, has high cost and is not suitable for popularization and application.
The invention comprises the following steps:
the technical problem to be solved by the invention is to provide the method for preparing the skin care tea seed oil by separating the unsaturated fatty acid from the tea seed oil, which is simple and convenient to operate, can enable the unsaturated fatty acid content to reach more than 98%, obviously improves the economic benefit of the tea seed oil and ensures the skin care effect of the tea seed oil.
The technical problems to be solved by the invention are realized by adopting the following technical scheme:
the invention aims to provide a method for preparing skin care tea seed oil by separating unsaturated fatty acid from tea seed oil, which comprises the following preparation steps:
(1) Freezing edible-grade camellia seed oil at a low temperature to enable all liquid camellia seed oil to be converted into solid;
(2) Naturally returning to the temperature, and immediately extracting the upper liquid oil tea seed oil when 80-85% of the solid oil tea seed oil is returned to the temperature to be converted into the liquid state;
(3) Filtering the extracted liquid oil tea seed oil by filter paper to obtain oil tea seed oil with unsaturated fatty acid content up to more than 98%;
(4) Standing the obtained camellia seed oil, and returning to the normal temperature state;
(5) Adding edible essence to obtain skin care tea seed oil.
The low-temperature freezing temperature is-25 to-15 ℃.
The low-temperature freezing time is 5-8 hours. The low-temperature freezing time is adjusted according to the actual form of the camellia seed oil, so that the camellia seed oil is ensured to be completely changed from a liquid state to a solid state.
The temperature return time is 8-12 h.
The mesh number of the filtration is 100-200 mesh. The number of filter paper meshes is selected in consideration of not only the filtering effect but also the filtering efficiency. The smaller the pore diameter is, the better the filtering effect is, but the longer the filtering time is, and the unnecessary loss of the oil tea seed oil can be caused.
The addition amount of the edible essence is 1-3 per mill. The flavor of the tea seed oil is improved by adding the edible essence, the sensory experience of the skin care tea seed oil is enriched, and meanwhile, the use safety of the essence is ensured.
The filter paper filtration belongs to a common filtration means in the field, has the characteristics of simple and convenient operation and low cost, but can only remove impurity particles in the camellia seed oil to different degrees through the adjustment of the pore size of the filter paper, and can not selectively filter unsaturated fatty acids, so that the unsaturated fatty acid content in the camellia seed oil is required to be further and substantially improved, and the filtration cannot be performed only by the filter paper.
The inventors know that membrane filtration is a precise separation means, and that two-phase separation is performed by utilizing the permselectivity of membrane pores. Therefore, in order to further substantially increase the unsaturated fatty acid content in the camellia seed oil, the inventor tries to perform membrane filtration on the camellia seed oil filtered by the filter paper in the step (3) by using a commercially available microporous membrane, but does not obtain the expected effect of increasing the unsaturated fatty acid content to more than 99%, so that the inventor wants to self-prepare a microporous membrane to achieve the expected filtration effect, but the research and development process is very difficult, the problems of incapability of forming the membrane, poor filtration effect and low filtration efficiency are successively generated, the inventor does not give up, and actively teaches professionals about the encountered problems and adjusts the preparation process of the membrane according to actual conditions, so that the microporous membrane applicable to the camellia seed oil is finally prepared.
Another object of the present invention is to provide a method for preparing skin care tea seed oil by separating unsaturated fatty acid from tea seed oil, comprising the following preparation steps:
(1) Freezing edible-grade camellia seed oil at a low temperature to enable all liquid camellia seed oil to be converted into solid;
(2) Naturally returning to the temperature, and immediately extracting the upper liquid oil tea seed oil when 80-85% of the solid oil tea seed oil is returned to the temperature to be converted into the liquid state;
(3) Sequentially filtering the extracted liquid camellia seed oil by using filter paper and microporous filter membrane to obtain camellia seed oil with unsaturated fatty acid content up to more than 99%;
the preparation method of the microporous filter membrane comprises the following steps: adding vinyl tributyl ketoxime silane and azodiisobutyronitrile into acetone under the protection of nitrogen, heating to react, defoaming after the reaction is finished to obtain casting solution, uniformly coating the casting solution on a glass plate by using a scraper, and drying to obtain a microporous filter membrane;
(4) Standing the obtained camellia seed oil, and returning to the normal temperature state;
(5) Adding edible essence to obtain skin care tea seed oil.
The low-temperature freezing temperature is-25 to-15 ℃.
The low-temperature freezing time is 5-8 hours.
The temperature return time is 8-12 h.
The mesh number of the filtration is 100-200 mesh.
The addition amount of the edible essence is 1-3 per mill.
The volume ratio of the acetone to the vinyl tributylketoxime silane is (3-8): 1. The vinyl tributyl ketoxime silane generates a polymer under the initiation of the azo-bis-isobutyronitrile, and then the polymer is used for preparing the microporous filter membrane.
The dosage of the azodiisobutyronitrile is 0.5-2% of the mass of the vinyl tributylketoxime silane.
The microporous filter membrane with the film thickness of 0.2-0.3mm and the pore diameter of 0.28-0.36 mu m is prepared by the technical proposal.
The beneficial effects of the invention are as follows:
(1) The invention adopts a mode of combining low-temperature freezing and natural tempering, and separates the edible camellia seed oil to obtain the camellia seed oil with the unsaturated fatty acid content of more than 98 percent.
(2) According to the invention, the camellia seed oil is processed into the skin care camellia seed oil, so that deep processing of the camellia seed oil is realized, and the economic benefit of the product is greatly improved, thereby promoting the healthy development of enterprises.
The specific embodiment is as follows:
the invention is further described in connection with the following embodiments in order to make the technical means, the creation features, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
(1) Freezing 5L edible oil tea seed oil at-20deg.C for 7 hr to make all the liquid oil tea seed oil into solid;
(2) Naturally heating for 10h, and immediately extracting the upper liquid oil tea seed oil when 85% of the solid oil tea seed oil is converted into liquid state;
(3) Filtering the extracted liquid camellia seed oil by using 120-mesh filter paper to obtain camellia seed oil with unsaturated fatty acid content up to more than 98%;
(4) Standing the obtained camellia seed oil, and returning to the normal temperature state;
(5) Adding 2%o edible essence to obtain skin care tea seed oil.
Example 2
(1) Freezing 5L edible oil tea seed oil at-25deg.C for 5h to make all liquid oil tea seed oil into solid;
(2) Naturally tempering for 12h, and immediately extracting the upper liquid oil tea seed oil when 80% of the solid oil tea seed oil is tempered to be liquid;
(3) Filtering the extracted liquid camellia seed oil by using 120-mesh filter paper to obtain camellia seed oil with unsaturated fatty acid content up to more than 98%;
(4) Standing the obtained camellia seed oil, and returning to the normal temperature state;
(5) Adding 1%edible essence to obtain skin care tea seed oil.
Example 3
(1) Freezing 5L edible oil tea seed oil at-20deg.C for 8 hr to make all the liquid oil tea seed oil into solid;
(2) Naturally heating for 10h, and immediately extracting the upper liquid oil tea seed oil when 80% of the solid oil tea seed oil is converted into liquid state;
(3) Filtering the extracted liquid camellia seed oil by 140-mesh filter paper to obtain camellia seed oil with unsaturated fatty acid content up to more than 98%;
(4) Standing the obtained camellia seed oil, and returning to the normal temperature state;
(5) Adding 3%o edible essence to obtain skin care tea seed oil.
Example 4
(1) Freezing 5L edible oil tea seed oil at-15deg.C for 8 hr to make all the oil tea seed oil in liquid state into solid state;
(2) Naturally heating for 8h, and immediately extracting the upper liquid oil tea seed oil when 85% of the solid oil tea seed oil is converted into liquid state;
(3) Filtering the extracted liquid camellia seed oil by 140-mesh filter paper to obtain camellia seed oil with unsaturated fatty acid content up to more than 98%;
(4) Standing the obtained camellia seed oil, and returning to the normal temperature state;
(5) Adding 2%o edible essence to obtain skin care tea seed oil.
Example 5
The procedure (3) of example 1 was followed by filtration with a microporous membrane to give example 5, and the remaining procedure was identical to example 1.
Preparation of microporous filter membrane: under the protection of nitrogen, adding 100mL of vinyl tributyl ketoxime silane and azo-diisobutyronitrile into 500mL of acetone, wherein the use level of the azo-diisobutyronitrile is 1% of the mass of the vinyl tributyl ketoxime silane, heating to a boiling state, carrying out reflux reaction for 3h, defoaming after the reaction is finished to obtain a casting solution, uniformly coating the casting solution on a glass plate by using a scraper, and drying to obtain the microporous filter membrane with the film thickness of 0.22mm and the aperture of 0.34 mu m.
Example 6
The procedure (3) of example 1 was followed by filtration with a microporous membrane to give example 6, and the remaining procedure was identical to example 1.
Preparation of microporous filter membrane: under the protection of nitrogen, adding 100mL of vinyl tributyl ketoxime silane and azo-diisobutyronitrile into 400mL of acetone, wherein the use level of the azo-diisobutyronitrile is 2% of the mass of the vinyl tributyl ketoxime silane, heating to a boiling state, carrying out reflux reaction for 2 hours, defoaming after the reaction is finished to obtain casting solution, uniformly coating the casting solution on a glass plate by using a scraper, and drying to obtain the microporous filter membrane with the film thickness of 0.28mm and the aperture of 0.30 mu m.
Comparative example 1
The procedure (3) of example 1 was followed by filtration with a microporous membrane to give comparative example 1, and the remaining procedure was identical to example 1.
The microporous filter membrane adopts polyvinylidene fluoride microporous filter membrane (Zun) with pore diameter of 0.22 μm.
Comparative example 2
The procedure (3) of example 1 was followed by filtration with a microporous membrane to give comparative example 2, and the remaining procedure was identical to example 1.
The microporous filter membrane adopts a polypropylene microporous filter membrane (Jinteng) with the pore diameter of 0.22 mu m.
And (3) determining the unsaturated fatty acid content of the camellia seed oil prepared in the step (3) by referring to a standard GB/T22223-2008 method for determining total fat, saturated fatty (acid) and unsaturated fatty (acid) in foods by a hydrolysis extraction-gas-phase gas-chromatography, wherein the determination results are shown in Table 1.
TABLE 1 unsaturated fatty acid content of oil tea seed oil
Unsaturated fatty acid content/%
Example 1 98.16
Example 2 98.21
Example 3 98.29
Example 4 98.05
Example 5 99.47
Example 6 99.31
Comparative example 1 98.40
Comparative example 2 98.28
According to the invention, the edible oil tea seed oil is processed into the skin care oil tea seed oil, so that the price per ton is increased by 5 times, and the economic benefit is more than 4.5 times of that of the edible oil tea seed oil.
The skin care tea seed oil finally prepared by the invention meets the requirements of Q/SMSW 004-2021 standard.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (3)

1. The method for preparing the skin care tea seed oil by separating unsaturated fatty acid from the tea seed oil is characterized by comprising the following preparation steps of:
(1) Freezing edible-grade camellia seed oil at a low temperature to enable all liquid camellia seed oil to be converted into solid;
(2) Naturally returning to the temperature, and immediately extracting the upper liquid oil tea seed oil when 80-85% of the solid oil tea seed oil is returned to the temperature to be converted into the liquid state;
(3) Sequentially filtering the extracted liquid camellia seed oil by using filter paper and microporous filter membrane to obtain camellia seed oil with unsaturated fatty acid content up to more than 99%;
the preparation method of the microporous filter membrane comprises the following steps: adding vinyl tributyl ketoxime silane and azodiisobutyronitrile into acetone under the protection of nitrogen, heating to react, defoaming after the reaction is finished to obtain casting solution, uniformly coating the casting solution on a glass plate by using a scraper, and drying to obtain a microporous filter membrane;
(4) Standing the obtained camellia seed oil, and returning to the normal temperature state;
(5) Adding edible essence to obtain skin care tea seed oil;
the volume ratio of the acetone to the vinyl tributylketoxime silane is (3-8) 1;
the dosage of the azodiisobutyronitrile is 0.5-2% of the mass of the vinyl tributylketoxime silane;
the temperature of the low-temperature freezing is minus 25 to minus 15 ℃;
the low-temperature freezing time is 5-8 hours;
the tempering time is 8-12 h;
the membrane thickness of the microporous filter membrane is 0.2-0.3mm, and the pore diameter is 0.28-0.36 mu m.
2. The method for preparing skin care tea seed oil by separating unsaturated fatty acid from tea seed oil according to claim 1, wherein the method comprises the following steps: the mesh number of the filtration is 100-200 mesh.
3. The method for preparing skin care tea seed oil by separating unsaturated fatty acid from tea seed oil according to claim 1, wherein the method comprises the following steps: the addition amount of the edible essence is 1-3 per mill.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604735A (en) * 2012-03-12 2012-07-25 国家***桉树研究开发中心 Method for extracting unsaturated fatty acids from eucalyptus leaves
CN103074158A (en) * 2013-01-29 2013-05-01 北京普仁生物工程技术有限公司 Separation method of unsaturated fatty acid
CN104789353A (en) * 2015-03-31 2015-07-22 赖琼玮 Low-temperature purified -full-bodied camellia oil and preparation method thereof
CN109433027A (en) * 2018-12-20 2019-03-08 长春工业大学 A kind of hydrophilic antipollution ultrafiltration membrane and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604735A (en) * 2012-03-12 2012-07-25 国家***桉树研究开发中心 Method for extracting unsaturated fatty acids from eucalyptus leaves
CN103074158A (en) * 2013-01-29 2013-05-01 北京普仁生物工程技术有限公司 Separation method of unsaturated fatty acid
CN104789353A (en) * 2015-03-31 2015-07-22 赖琼玮 Low-temperature purified -full-bodied camellia oil and preparation method thereof
CN109433027A (en) * 2018-12-20 2019-03-08 长春工业大学 A kind of hydrophilic antipollution ultrafiltration membrane and preparation method thereof

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