NL2026853B1 - Plant squalene composition, preparation method and application thereof, and product using the same - Google Patents

Abstract

The present disclosure relates to the field of preparation of cosmetic raw materials, and in particular to a plant sgualene composition, a preparation method and application thereof, and a product using the same. The present disclosure provides a preparation method of a plant sgualene composition, which comprises the following steps: introducing raw materials rich in plant sgualene into a falling—film evaporator continuously and cyclically; enabling the obtained steam to enter a rectifying tower to be separated; collecting fatty acid and/or fatty acid methyl ester at a pressure of lO—lOOOPa and a temperature of 160— 220°C, and then rising the temperature to 220—260°C; and collecting the plant sgualene composition containing plant sgualene. The method is not limited by the type and composition of raw materials, has simple process flow, low cost and relatively stable ingredients. The prepared plant sgualene composition has good safety. In addition to plant sgualene, the plant sgualene composition also contains effective active substances such as natural vitamin E and plant sterols, and can be used for the preparation of cosmetics after simple refining.

Description

P664/NLpd PLANT SQUALENE COMPOSITION, PREPARATION METHOD AND APPLICATION THEREOF, AND PRODUCT USING THE SAME

TECHNICAL FIELD The present disclosure relates to the field of preparation of cosmetic raw materials, and in particular to a plant squalene com- position, a preparation method and application thereof, and a product using the same.

BACKGROUND ART Squalene is a highly unsaturated hydrocarbon compound. The chemical name of squalene is 2,6,10,15,19, 23-hexamethyl- 2,6,10,14,18,22-tetracosahexaenoic acid which has a molecular for- mula of C30H50 and belongs to terpenoids. Squalene is widely dis- tributed in animals and plants. In view of its special chemical structure, squalene has many functions such as resisting oxida- tion, promoting skin health and cardiovascular health, assisting in the prevention and treatment of tumors, and improving the human body's ability to withstand hypoxia, and is widely used in the fields of medicine and cosmetics. The application of the squalene in the field of health products has gradually expanded in recent years. Squalene has excellent phytochemical properties, is highly compatible with skin, has softening and moisturizing properties, and is thus widely used in cosmetic formulations.

The squalene on the market is mainly extracted from liver oil of deep-sea sharks. At present, the number of deep-sea sharks is gradually decreasing, and some species are on the verge of extinc- tion, making this source increasingly scarce. Therefore, it is very important to find new squalene resources and develop corre- sponding extraction methods. There have been many reports on the discovery of squalene resources in recent years. In particular, deodorized distillates of vegetable oils are most widely extract- ed. The deodorized distillates are by-products in the process of oil deodorization and are good sources of plant squalene. However, the independent extraction of squalene from the deodorized distil-

lates of vegetable oils alone still has many defects.

SUMMARY OF THE INVENTION The present disclosure is directed to provide a plant squa- lene composition and a preparation method thereof, so as to alle- viate at least one technical problem in the prior art.

In order to achieve the above purposes of the present disclo- sure, it adopts the following technical solution: The present disclosure provides a preparation method of a plant squalene composition, comprising the following steps: intro- ducing raw materials rich in plant squalene into a falling-film evaporator continuously and cyclically and performing evaporation processing, enabling the obtained steam to enter a rectifying tow- er to be separated, and then recycling light components to obtain the plant squalene composition containing plant squalene, the process conditions of the falling-film evaporator com- prises: a system pressure is 10-1000Pa and a temperature is 160 - 260°C, wherein fatty acid and/or fatty acid methyl ester are col- lected in the case that the temperature of the falling-film evapo- rator is 160-220°C and the temperature is then risen to 220-260°C, and the plant squalene composition containing plant squalene is collected.

Further, the rectifying tower comprises a packed tower or a plate tower.

Optionally, the raw materials rich in plant squalene include the following components in percentage by weight: 5%-30% of plant squalene, 1%-30% of natural vitamin E, and 13-10% of plant ster- ols.

Preferably, the raw materials rich in plant squalene include one or a mixture of two or more of deodorized distillates of vege- table oils.

Preferably, the raw materials rich in plant squalene include by-products obtained by extracting one or a mixture of two or more of deodorized distillates of vegetable oils with natural vitamin E and/or plant sterols.

Preferably, the raw materials rich in plant squalene include a low-content natural vitamin E raw material obtained by esterifi-

cation, cold precipitation and distillation of one or a mixture of two or more of deodorized distillates of vegetable oils.

Preferably, the low-content natural vitamin E raw material contains the following components in percentage by weight: 5%-50% of natural vitamin E, 5%-30% of squalene, 1%-20% of sterol, and the balance of other inevitable impurities.

Preferably, the vegetable oils include soybean oil, palm oil, corn oil, cottonseed oil, rice bran oil, sunflower oil, and/or rapeseed oil.

The present disclosure also provides a plant squalene compo- sition prepared by the preparation method.

Optionally, the plant squalene composition comprising the following components in percentage by weight: 50%-90% of plant squalene, 1%-10% of natural vitamin E, 1%-5% of phytosterol and 1%-10% vegetable wax.

Preferably, the plant squalene composition has an iodine val- ue of 150-350, a saponification value of 10-50mg KOH/g, and an ac- id value of not more than 5mg KOH/g.

The present disclosure further provides an application of the plant squalene composition in a cosmetic, the plant squalene com- position is used to prepare a cosmetic after being refined, and the refining process includes winterization, decolorization and deodorization.

Optionally, the refined plant squalene composition has a melting point of 0-5°C, and a peroxide value of not more than 5 milliequivalents.

The present disclosure finally provides a cosmetic containing the plant squalene composition, the plant squalene composition is refined, and the refining process includes winterization, decolor- ization and deodorization.

Optionally, the cosmetic comprising lip balm and a moisturiz- er.

Preferably, the cosmetic further comprising cosmetic accesso- ries.

Optionally, the lip balm comprises the following components in percentage by weight: 10%-50% of vegetable wax and 50%-90% of the vegetable squalene composition, the plant squalene composition is refined, and the refining process includes winterization, de- colorization and deodorization.

Optionally, the moisturizer comprises the following compo- nents in percentage by weight: 2%-60% of the plant squalene compo- sition and the balance of water, the plant squalene composition is refined, and the refining process includes winterization, decolor- ization and deodorization.

Compared with the prior art, the present disclosure has the following beneficial effects: the present disclosure provides a preparation method of a plant squalene composition, which comprises the following steps: introducing raw materials rich in plant squalene into a falling- film evaporator having a pressure of 10-1000Pa and a temperature of 160-260°C continuously and cyclically and performing evapora- tion treatment; enabling the obtained steam to enter a rectifying tower to be separated; collecting fatty acid and/or fatty acid me- thyl ester in the case that the temperature of the falling-film evaporator is 160-220°C and then rising the temperature to 220- 260°C; and collecting the plant squalene composition containing plant squalene. This method is not limited by the types and ingre- dients of raw materials, has simple process flow, low cost and relatively stable ingredients, and can realize the preparation of the plant squalene composition through the first-stage rectifica- tion. The prepared plant squalene composition has stable ingredi- ents. In addition to plant squalene, the plant squalene composi- tion also contains effective active substances such as natural vitamin E and plant sterols, and can be used for the preparation of cosmetics after simple refining This method is suitable for the preparation of the plant squalene composition used in the produc- tion of cosmetics on a large scale.

The plant squalene composition prepared by the above prepara- tion method provided in the present disclosure has relatively sta- ble ingredients and can be directly applied to the production of cosmetics.

The cosmetics provided by the present disclosure include the above-mentioned plant squalene composition, and have high- efficiency lubricating and moisturizing effects.

DETAILED DESCRIPTION The embodiments of the present disclosure will be described in detail below in conjunction with examples, but those skilled in 5 the art will understand that the following examples are only used to illustrate the present disclosure and should not be regarded as limiting the scope of the present disclosure. If specific condi- tions are not indicated in the examples, these examples shall be carried out in accordance with conventional conditions or condi- tions recommended by manufacturers.

At present, since deodorized distillates are relatively low in squalene content and are mainly used to extract natural vitamin E and plant sterols with higher added value, it is economically unreasonable to extract squalene from deodorized distillates of vegetable oils alone. Therefore, the current researches focus on using by-products of natural vitamin E and plant sterols as raw materials to extract squalene, using low-content natural vitamin E as a raw material to extract squalene, natural vitamin E and some plant sterols at the same time, and using deodorized distillates of vegetable oils as raw materials directly to extract squalene in a few cases. The current process for preparing plant squalene needs to make use of the technologies such as saponification ex- traction, cold precipitation and crystallization, silica gel chro- matography, multi-stage molecular distillation, ion exchange chro- matography, rectification, solvent extraction, activated carbon adsorption and high-speed countercurrent chromatography. The raw materials of squalene extracted and prepared by the above methods are diverse, and the extraction methods are different, resulting in poor versatility and relatively narrow scope of application.

In order to solve one of the technical problems in the prior art, the present disclosure provides a preparation method of a plant squalene composition. The plant squalene method comprises the following steps: introducing raw materials rich in plant squa- lene into a falling-film evaporator continuously and cyclically and performing evaporation treatment, enabling the obtained steam to enter a rectifying tower to be separated, and then recycling a light component to obtain the plant squalene composition contain-

ing plant squalene.

Optionally, the process conditions of the falling-film evaporator comprises: a system pressure of 10-1000Pa and a temperature of 160-260°C.

Optionally, fatty acid and/or fat- ty acid methyl ester are/is collected in the case that the temper- ature of the falling-film evaporator is 160-220°C and the tempera- ture is then risen to 220-260°C, and the plant squalene composi- tion containing plant squalene is collected.

Raw materials rich in plant squalene are introduced into the stable falling-film evaporator having a specific pressure continu- ously and cyclically.

The obtained steam enters the rectifying tower to be separated.

The fatty acid and/or fatty acid methyl es- ter are/is collected in the case that the temperature of the fall- ing-film evaporator is 160-220°C and the temperature is then risen to 220-260°C.

The plant squalene composition containing plant squalene is collected.

In addition to the main component, i.e., the plant squalene, the plant squalene composition may also fur- ther a small amount of natural vitamin E, plant sterols and plant wax.

This method is not limited by the types and ingredients of raw materials, has simple process flow, low cost and relatively stable ingredients, and can realize the preparation of the plant squalene composition through the first-stage rectification.

The prepared plant squalene composition has good safety.

In addition to plant sgualene, the plant squalene composition also contains effective active substances such as natural vitamin E and plant sterols, and can be used for the preparation of cosmetics after simple refining This method is suitable for the preparation of the plant squalene composition used in the production of cosmetics on a large scale.

It should be noted that the system pressure is typically but not limited to 10Pa, 50Pa, 100Pa, 200Pa, 300Pa, 400Pa, 500Pa, ¢00Pa, 700Pa, 800Pa, 900Pa or 1000Pa; the temperature is typically but not limited to 160°C, 170°C, 180°C, 190°C, 200°C, 210°C, 220°C, 230°C, 240°C, 250°C or 260°C.

In an optional example of the present disclosure, the raw ma- terials rich in plant squalene include the following components in percentage by weight: 54-303 of plant squalene, 1%-30% of natural vitamin E, and 1%-10% of plant sterols.

The raw materials rich in plant squalene are more conducive to the extraction and prepara- tion of the plant squalene composition.

The content of the plant squalene in raw materials rich in plant squalene is typically but not limited to 52, 10%, 153, 20%, 25% or 30%; the content of the natural vitamin E is typically but not limited to 1%, 5%, 10%, 15%, 20%, 25% or 30%; and the content of the plant sterols is typ- ically but not limited to 1%, 5% or 10%. In an optional embodiment of the present disclosure, the preparation raw material can be any raw material rich in plant squalene, and is not limited to a specific source.

The raw materi- al rich in plant squalene may be one or a mixture of two or more of deodorized distillates of vegetable oils.

When the deodorized distillates of vegetable oils are directly used as the raw materi- al, the light component obtained when the temperature of the fall- ing-film evaporator is 160-220°C is mainly fatty acid.

Alternatively, the raw material rich in plant squalene may be a by-product of one or a mixture of two or more of the deodorized distillates of vegetable oils from which natural vitamin E and/or plant sterols are extracted.

The utilization efficiency of the de- odorized distillates is improved to maximize the utilization of effective ingredients.

The light component obtained from this raw material when the temperature of the falling film evaporator is 160-220°C is mainly fatty acid methyl ester.

Alternatively, the raw material rich in plant squalene may be a low-content natural vitamin E raw material obtained by esterifi- cation, cold precipitation and distillation of one or a mixture of two or more of deodorized distillates of vegetable oils.

The uti- lization efficiency of the deodorized distillates is improved to maximize the utilization of effective ingredients.

The light com- ponent obtained from this raw material when the temperature of the falling film evaporator is 160-220°C is mainly fatty acid methyl ester.

Alternatively, the raw material rich in plant squalene may be a low-content natural vitamin E raw material, which contains the following components in percentage by weight: 5%-50% of natural vitamin E, 5%-30% of squalene, 1%-20% of sterols, and the balance of other unavoidable impurities.

The light component obtained from this raw material when the temperature of the falling-film evapo- rator is 160-220°C is mainly fatty acid methyl ester. Waste liquid obtained after natural vitamin E and/or plant sterols are/is ex- tracted contains a large amount of plant squalene, which may also be used as a raw material of the present disclosure, thereby achieving the full utilization of materials. The content of the natural vitamin E in the low-content natural vitamin E raw materi- al is typically but not limited to 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50%; the content of the squalene is typically but not limited to 5%, 10%, 15%, 20%, 25% or 30%; the content of the sterols is typically but not limited to 1%, 5%, 10%, 15% or 20%.

In a preferred embodiment of the present disclosure, the veg- etable oils include soybean oil, palm oil, corn oil, cottonseed oil, rice bran oil, sunflower oil and/or rapeseed oil. A large amount of deodorized distillates which are rich in natural vitamin E and plant squalene and other effective ingredients will be pro- duced from the above plants while preparing vegetable oils. There- fore, the deodorized distillates can be directly used in the pre- sent disclosure to produce the plant squalene composition, or used in other processes to produce natural vitamin E and/or plant ster- ols first, and then produce the plant squalene composition.

In the case that the deodorized distillates of vegetable oils are directly used to produce the plant squalene composition, after the plant squalene composition is collected by vaporization, heavy components are mainly a concentrate of natural vitamin E. The heavy components are then subjected to molecular distillation through a molecular distiller under the conditions of a system pressure of 1-10Pa and a temperature of 210-240°C to obtain natu- ral vitamin E and vegetable pitch. At this time, the natural vita- min E and the plant squalene composition can be directly produced. The system pressure of the molecular distiller is typically but not limited to 1 Pa, 2 Pa, 3 Pa, 4 Pa, 5 Pa, 6 Pa, 7 Pa, 8 Pa, 3 Pa or 10Pa; and the temperature is typical but not limited to 210°C, 220°C, 230°C or 240°C.

The present disclosure also provides a plant squalene compo- sition prepared by the above preparation method. The plant squa- lene composition has relatively stable ingredients, and can be di-

rectly applied to the production of cosmetics through simple re- fining treatment.

In an optional embodiment of the present disclosure, the plant squalene composition comprises the following components in percentage by weight: 50%-90% of plant squalene, 1%-10% of natural vitamin E, 1%-5% of plant sterols and 1%-10% of vegetable wax.

The content of the plant squalene in the plant squalene composition is typically but not limited to 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85% or 90%; the content of the natural vitamin E is typically but not limited to 1%, 3%, 5%, 8% or 10%; the content of the plant sterols is typically but not limited to 1%, 2%, 3%, 4% or 5%; the content of the plant wax is typically but not limited to 1%, 3%, 5%, 7% or 10%. In an optional embodiment of the present disclosure, the plant squalene composition has an iodine value of 150-350, a sa- ponification value of 10-50mg KOH/g, and an acid value of not more than 55mg KOH/g.

The iodine value is typically but not limited to 150, 200, 250, 300 or 350; the saponification value is typically but not limited to 10mg KOH/g, 15mg KOH/g, 20mg KOH/g, 25mg KOH/ g, 30mg KOH/g, 35mg KOH/g, 40mg KOH/g, 45mg KOH/g or 50mg KOH/g; and the acid value is typically but not limited to Omg KOH/g, 1mg KOH/g, 2mg KOH/g, 3mg KOH/g, 4mg KOH/g, or 5mg KOH/g.

The present disclosure further provides an application of the above-mentioned plant squalene composition in cosmetics.

The plant squalene composition is used to prepare cosmetics after being re- fined.

The refining process includes but is not limited to winter- ization, decolorization and deodorization.

The refined plant squa- lene composition has a melting point of 0-5°C and a peroxide value of not more than 5 millieguivalents.

The refining process may re- fer to conventional vegetable oil refining steps such as winteri- zation, decolorization and deodorization (such as Bailey's oil chemistry and technology, Edition 5, Vol. 4, Chapter 1, Oil Pro- cessing Technology, translated by Xu Shenggeng, Qiu Aiyong, China Light Industry Press). The melting point is typically but not lim- ited to 0°C, 2°C, 4°C, 6°C, 8°C or 10°C; the peroxide value is typically but not limited to 0 milliequivalent, 1 milliequiwvalent, 2 milliequivalents, 3 milliequivalents, 4 milliequivalents, or 5 milliequivalents.

The present disclosure finally provides a cosmetic comprising the above-mentioned plant squalene composition. The plant squalene composition is refined, and the refining process includes winteri- zation, decolorization and deodorization. The cosmetic containing the above-mentioned plant squalene composition has high-efficiency lubricating and moisturizing effects.

In an optional embodiment of the present disclosure, the cos- metic includes a lip balm and a moisturizer.

In an optional embodiment of the present disclosure, the cos- metic product further includes cosmetic accessories.

In an opticnal embodiment of the present disclosure, the lip balm includes the following components in percentage by weight: 104-50% of vegetable wax and 50%-90% of the plant squalene compo- sition, wherein the plant squalene composition is refined, and the refining process includes winterization, decolorization and deo- dorization. The content of the vegetable wax is typically but not limited to 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50%; the con- tent of the plant squalene composition is typically but not lim- ited to 50% %, 55%, 60%, 65%, 70%, 75%, 80%, 85% or 90%.

In an optional embodiment of the present disclosure, the moisturizer includes the following components in percentage by weight: 2%-60% of the plant squalene composition and the balance of water, wherein the plant squalene composition is refined, and the refining process includes winterization, decolorization and deodorization. The content of the plant squalene composition is typically but not limited to 2%, 10%, 20%, 30%, 40%, 50% or 60%.

In order to facilitate a clearer understanding of the content of the present disclosure, it is now described in detail with ref- erence to specific examples. However, these examples are only ex- emplary and do not constitute any limitation to the scope of the present disclosure.

Example 1 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres-

sure of 500Pa and a temperature of 200°C, introducing soybean oil deodorized distillate to a falling-film evaporator continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light compo- nent, i.e., fatty acid. The falling-film evaporator is then slowly heated 260°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 20Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 50.5% of plant squalene, 5% of natural vitamin E, 4.0% of plant sterols and 10% of plant wax.

Example 2 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 1000Pa and a temperature of 220°C, introducing rice bran oil deodorized distillate to a falling-film evaporator continuous- ly and cyclically to be vaporized continuously, such that materi- als are separated in a rectifying tower; and collecting a light component, i.e., fatty acid. The falling-film evaporator is then slowly heated 260°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 50Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 65.8% of plant squalene, 8.4% of natural vitamin E, 4.2% of plant sterols and 7.2% of plant wax.

Example 3 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 100Pa and a temperature of 190°C, introducing rice bran oil and palm oil deodorized distillate to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid. The falling-film evaporator is then slowly heated 250°C, and the materials continue to be sep- arated in the rectifying tower. When the system pressure is stable at 10Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 55.2% of plant squalene, 5.4% of natural vitamin E, 3.8% of plant sterols and 7.6% of plant wax.

Example 4 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 200Pa and a temperature of 200°C, introducing corn oil, sunflower oil and rapeseed oil deodorized distillate to a falling- film evaporator continuously and cyclically to be vaporized con- tinuously, such that materials are separated in a rectifying tow- er; and collecting a light component, i.e., fatty acid. The fall- ing-film evaporator is then slowly heated 240°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 10Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 52.3% of plant squalene, 7.6% of natural vitamin E, 4.9% of plant sterols and 1% of plant wax.

Example 5 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 150Pa and a temperature of 175°C, introducing a by- product, obtained from deodorized distillates of palm oil from which natural vitamin E is extracted, to a falling-film evaporator continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. The falling-film evaporator is then slowly heated 260°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 30Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 77.1% of plant squalene, 3.6% of natural vitamin E, 1.2% of plant sterols and 5.2% of plant wax. Example 6

This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 500Pa and a temperature of 215°C, introducing a by- product, obtained from deodorized distillates of soybean oil and corn oil from which natural vitamin E and plant sterols are ex- tracted, to a falling-film evaporator continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. The falling-film evaporator is then slowly heated 245°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 20Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 78.0% of plant squalene, 2.4% of natural vitamin E, 2.2% of plant sterols and 4.6% of plant wax.

Example 7 This example provides a preparation method of a plant squa- lene composition, including the following steps: performing ester- ification, cold precipitation and distillation on a deodorized distillate mixture of soybean oil and rice bran oil at a system pressure of 700Pa and a temperature of 220°C to obtain a low- content natural vitamin E solution; introducing the low-content natural vitamin E solution to a falling-film evaporator continu- ously and cyclically to be vaporized continuously, such that mate- rials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. The falling-film evapo- rator is then slowly heated 255°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 50Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 69.1% of plant squalene, 6.4% of natural vitamin E, 4.1% of plant sterols and 3.3% of plant wax.

Example 8 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres-

sure of 800Pa and a temperature of 210°C, introducing the low- content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. The falling-film evaporator is then slowly heated 235°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 10Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 63.4% of plant squalene, 2.5% of natural vitamin E, 1.3% of plant sterols and 6.9% of plant wax.

Example 9 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 100Pa and a temperature of 160°C, introducing the low- content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. The falling-film evaporator is then slowly heated 260°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 30Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 74% of plant squalene, 1.33 of natural vitamin E, 1.9% of plant sterols and 1.5% of plant wax.

Example 10 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 10Pa and a temperature of 180°C, introducing the low- content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. Adjusting the temperature to 220°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at

20Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 77.0% of plant squalene, 5.3% of natural vitamin E, 2.9% of plant sterols and 10.6% of plant wax.

Example 11 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 800Pa and a temperature of 220°C, introducing the low- content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. Adjusting the temperature to 250°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stable at 20Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 87.0% of plant squalene, 2.33 of natural vitamin E, 1.9% of plant sterols and 4.6% of plant wax.

Example 12 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 800Pa and a temperature of 160°C, introducing rice bran oil deodorized distillate to a falling-film evaporator continuous- ly and cyclically to be vaporized continuously, such that materi- als are separated in a rectifying tower; and collecting a light component to obtain fatty acid; adjusting the temperature to 240°C, and stabilizing the system pressure to 10Pa, wherein a light component collected at the top of the tower is the plant squalene composition.

Heavy components are conveyed to a molecular distiller, and subjected to molecular distillation at a system pressure of 1Pa and a temperature of 210°C to obtain a light component, i.e., nat- ural vitamin E and a heavy component, i.e., vegetable pitch.

Upon testing, the obtained plant squalene composition in- cludes 78% of plant squalene, 2.6% of natural vitamin E, 3.5% of plant sterols and 2.2% of plant wax.

Example 13 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 800Pa and a temperature of 160°C, introducing rice bran oil deodorized distillate to a falling-film evaporator continuous- ly and cyclically to be vaporized continuously, such that materi- als are separated in a rectifying tower; and collecting a light component to obtain fatty acid; adjusting the temperature to 260°C, and stabilizing the system pressure to 30Pa, wherein a light component collected at the top of the tower is the plant squalene composition.

Heavy components are conveyed to a molecular distiller, and subjected to molecular distillation at a system pressure of 10Pa and a temperature of 240°C to obtain a light component, i.e., nat- ural vitamin E and a heavy component, i.e., vegetable pitch.

Upon testing, the obtained plant squalene composition in- cludes 72.3% of plant squalene, 1.5% of natural vitamin E, 2.6% of plant sterols and 1.3% of plant wax.

Example 14 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 800Pa and a temperature of 170°C, introducing rice bran oil deodorized distillate to a falling-film evaporator continuous- ly and cyclically to be vaporized continuously, such that materi- als are separated in a rectifying tower; and collecting a light component to obtain fatty acid; adjusting the temperature to 230°C, and stabilizing the system pressure to 30Pa, wherein a light component collected at the top of the tower is the plant squalene composition.

Heavy components are conveyed to a molecular distiller, and subjected to molecular distillation at a system pressure of 5Pa and a temperature of 225°C to obtain a light component, i.e., nat- ural vitamin E and a heavy component, i.e., vegetable pitch.

Upon testing, the obtained plant squalene composition in- cludes 75.0% of plant squalene, 2.8% of natural vitamin E, 1.9% of plant sterols and 2.2% of plant waz.

Comparative Example 1 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 5Pa and a temperature of 200°C, introducing the low- content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. The falling-film evaporator is then slowly heated 250°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stabilized at 30Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 6.7% of plant squalene, 1.3% of natural vitamin E, 0.9% of plant sterols and 2.5% of plant wax.

Comparative Example 2 This example provides a preparation method of a plant squa- lene composition, including the following steps: performing ester- ification, cold precipitation and distillation on a deodorized distillate mixture of soybean oil and rice bran oil at a system pressure of 1200Pa and a temperature of 180°C to obtain a low- content natural vitamin E solution; introducing the low-content natural vitamin E solution, to a falling-film evaporator continu- ously and cyclically to be vaporized continuously, such that mate- rials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. The falling-film evapo- rator is then slowly heated 230°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stabilized at 40Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 92.1% of plant squalene, 1.0% of natural vitamin E, 1.2% of plant sterols and 1.3% of plant waz.

Comparative Example 3 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 800Pa and a temperature of 150°C, introducing the low-

content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester.

The falling-film evaporator is then slowly heated 220°C, and the materials continue to be separated in the rectifying tower.

When the system pressure is stabilized at 20Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 7.0% of plant squalene, 4.3% of natural vitamin E, 2.2% of plant sterols and 3.6% of plant wax.

Comparative Example 4 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 800Pa and a temperature of 230°C, introducing the low- content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester.

The falling-film evaporator is then slowly heated 260°C, and the materials continue to be separated in the rectifying tower.

When the system pressure is stabilized at 20Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 11.2% of plant squalene, 3.1%% of natural vitamin E, 1.1% of plant sterols and 2.6% of plant wax.

Comparative Example 5 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 800Pa and a temperature of 180°C, introducing the low- content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester.

The falling-film evaporator is then slowly heated 200°C, and the materials continue to be separated in the rectifying tower.

When the system pressure is stabilized at 30Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 6.2% of plant squalene, 1.4%% of natural vitamin E, 2.9% of plant sterols and 5.3% of plant wax.

Comparative Example 6 This example provides a preparation method of a plant squa- lene composition, including the following steps: at a system pres- sure of 800Pa and a temperature of 200°C, introducing the low- content natural vitamin E raw material to a falling-film evapora- tor continuously and cyclically to be vaporized continuously, such that materials are separated in a rectifying tower; and collecting a light component, i.e., fatty acid methyl ester. The falling-film evaporator is then slowly heated 280°C, and the materials continue to be separated in the rectifying tower. When the system pressure is stabilized at 40Pa, the light component collected at the top of the tower is the plant squalene composition.

Upon testing, the obtained plant squalene composition in- cludes 8.3% of plant squalene, 2.2%% of natural vitamin E, 1.7% of plant sterols and 6.6% of plant wax.

As can be seen from the above Examples 1-14, no matter what source the raw material is rich in plant squalene, the preparation method provided in the present disclosure can effectively extract the plant squalene composition. The plant squalene composition meets the raw material requirements for cosmetic preparation. In addition, the method is simple and easy to operate, low in cost, wide in raw material sources, and high in versatility, and can be widely promoted and applied. However, although the preparation method of the plant squalene composition provided by Comparative Examples 1-6 of the present disclosure includes the step of intro- ducing the raw materials rich in plant squalene into the falling- film evaporator continuously and cyclically for evaporation treat- ment, enabling the obtained steam to enter the rectifying tower to be separated and collecting the light component, all conditions used in this method are not within the scope defined in the pre- sent disclosure, and it can be seen from the results that the plant squalene composition cannot be effectively extracted.

Example 15

This example provides a lip balm, which includes 10% of vege- table wax, 90% of the vegetable squalene composition in Example 2.

The plant squalene composition in Example 2 is subjected to winterization, decolorization and deodorization refining process- es.

Example 16 This example provides a lip balm, which includes 50% of vege- table wax, 50% of the vegetable squalene composition in Example

10.

The plant squalene composition in Example 10 is subjected to winterization, decolorization and deodorization refining process- es.

Example 17 This example provides a lip balm, which includes 30% of vege- table wax, 60% of the vegetable squalene composition in Example 13, and 10% of sodium hyaluronate.

The plant squalene composition in Example 13 is subjected to winterization, decolorization and deodorization refining process- es.

Example 18 This embodiment provides a moisturizer, which includes 2% of the plant squalene composition in Example 11, and the balance of water.

The plant squalene composition in Example 11 is subjected to winterization, decolorization and deodorization refining process- es.

Example 19 This embodiment provides a moisturizer, which includes 60% of the plant squalene composition in Example 12, and the balance of water.

The plant squalene composition in Example 12 is subjected to winterization, decolorization and deodorization refining process- es.

Example 20 This embodiment provides a moisturizer, which includes 35% of the plant squalene composition in Example 14, 5% of emulsifier, and the balance of water.

The plant squalene composition in Example 14 is subjected to winterization, decolorization and deodorization refining process- es.

Example 21 This example provides a lip balm, which includes 30% of vege- table wax, 60% of the vegetable squalene composition in Example 13, and 10% of sodium hyaluronate.

The plant squalene composition in Example 13 is not subjected to a refining process.

Comparative Examples 7-9 This Comparative Example provides a lip balm, which includes 20% of vegetable wax, and 90% of the vegetable squalene composi- tion in Comparative Examples 1-3.

The plant squalene composition in Comparative Examples 1-3 are subjected to winterization, decolorization and deodorization refining processes.

Comparative Examples 10-12 This Comparative Example provides a moisturizer, which in- cludes 15% of the plant squalene composition in Comparative Exam- ples 4-6, 2% of emulsifier, and the balance of water, respective- ly.

The plant squalene composition in Comparative Examples 4-6 are subjected to winterization, decolorization and deodorization refining processes.

Experimental example In order to verify the effects of the plant squalene composi- tions prepared by the preparation methods of the plant squalene composition provided in the present disclosure as the cosmetics, 65 female volunteers are invited and randomly divided into 13 groups to evaluate their moisturizing properties of the cosmetics provided in Examples 15-21 and Comparative Examples 7-12, to be specific: The lip balms provided in Examples 15-17, 21 and Comparative Examples 7-9 are applied to the lips respectively, and the moist- urizers provided in Examples 18-20 and Comparative Examples 10-12 are applied to the whole faces. After 6 hours, the skin is tested for the water content with a skin moisture tester. The results are shown in the following table: Group Average water content | Average water content after before use (%) 6 hours of use (%) Example 1 Example 1 Example 17 Example 13 Example 19 Example 2 229 Example 2 228 Comparative Example 7 Comparative Example § Comparative Example 9 Comparative Example 10 Comparative Example 11 Comparative Example 12 239 It can be seen from the above table that the lip balms and the moisturizers provided in Examples 15-20 of the present disclo- sure have good moisturizing effects and improve the skin's mois- ture retention function.

Natural vitamin E, plant sterols and oth- er active substances make the lip balms and the moisturizers have repairing, soothing, calming and skin care effects, and suitable for users of all skin types.

The lip balm provided in Example 21 has the same raw materials as the lip balm provided in Example 17. However, the plant squalene composition in Example 21 has not been processed by the refining process, and its moisturizing effect is obviously inferior to that of Example 17, which indicates that the cosmetic obtained by applying the preferred method of the present invention to the raw materials through the refining process has a better moisturizing effect.

However, the cosmetics provided in Comparative Examples 7-12 respectively use the plant squalene com- position provided in Comparative Examples 1-6 of the present dis- closure respectively, and have relatively poor moisturizing ef-

fects. After 6 hours of use, the skin moisture content does not increase, or even decrease slightly. Although specific embodiments have been used to illustrate and describe the present disclosure, it should be appreciated that many other changes and modifications can be made without departing from the spirit and scope of the present disclosure. Therefore, this means that all these changes and modifications that fall within the scope of the present disclosure are included in the ap- pended claims.

Industrial applicability The preparation method of the plant squalene composition pro- vided by the present invention is not limited by the types of raw materials and ingredients, and is simple in process flow and low in cost. The prepared plant squalene composition has relatively stable ingredients. In addition to the plant squalene, the plant squalene composition also contains effective active substances such as natural vitamin E and plant sterols, and can be used for the preparation of cosmetics after simple refining. This method is suitable for the preparation of the plant squalene composition used in the production of cosmetics on a large scale.

Claims (19)

CONCLUSIONS A method for preparing a vegetable squalene composition, comprising the steps of: continuously and cyclically introducing raw materials rich in vegetable squalene into a falling film evaporator and performing an evaporation treatment, whereby the obtained steam in a rectification tower can be separated, and then the recycling of light components to obtain the vegetable squalene composition containing vegetable squalene, wherein the process conditions of the falling film evaporator include: a system pressure of 10-1000 Pa and a temperature of 160-260 °C, collecting fatty acid and/or fatty acid methyl ester in case the temperature of the falling film evaporator is 160-220 °C and the temperature is then raised to 220-260 °C, and the plant vegetable squalene composition containing vegetable vegetable squalene is collected. The method of claim 1, wherein the rectification tower is a packed tower or a plate tower. A method according to claim 1 or 2, wherein the raw materials rich in vegetable squalene contain the following components in percent by weight: 53-304 of vegetable squalene, 1%-30% of natural vitamin E, and 1%-10% of plant sterols. Process according to claim 1 or 2, wherein the raw materials rich in vegetable squalene contain one or a mixture of two or more deodorized distillates of vegetable oils. A method according to claim 1 or 2, wherein the raw materials rich in vegetable squalene comprise by-products obtained by extracting one or two or more deodorized distillates of vegetable oils with natural vitamin E and/or plant sterols. The method according to claim 1 or 2, wherein the vegetable squalene rich raw materials contain a low content natural vitamin E raw material obtained by esterification, cold precipitation and distillation of one or two or more deodorized distillates of vegetable oils. The method of claim 6, wherein the low content natural vitamin E raw material contains the following components in percent by weight: 5%-503 natural vitamin E, 5%-30% squalene, 1%-20% sterol , and otherwise other unavoidable impurities. A method according to any one of claims 4 to 6, wherein the vegetable oils are soybean oil, palm oil, corn oil, cottonseed oil, rice bran oil, sunflower oil and/or rapeseed oil. A vegetable squalene composition prepared according to the method according to any one of claims 1 to 8. A vegetable squalene composition according to claim 9, comprising the following components by weight: 50%-30% vegetable squalene, 1%-10% natural vitamin E, 1%-5% phytosterol and 1%-10% to vegetable wax. The vegetable squalene composition according to claim 9 or 10, wherein the vegetable squalene composition has an iodine value of 150-350, a saponification value of 10-50 mg KOH/g, and an acid number of not more than 5 mgKOH/g. Use of the vegetable squalene composition according to any one of claims 9 to 11 in a cosmetic product. Use according to claim 12, wherein the vegetable squalene composition is used to prepare a cosmetic product after being refined, and the refining process comprises wintering, decolorization and deodorization. Use according to claim 13, wherein the refined vegetable squalene composition has a melting point of 0-5 °C, and a peroxide value of not more than 5 milliequivalents. A cosmetic product containing the vegetable squalene composition according to any one of claims 9 to 11, wherein the vegetable squalene composition is refined, and the refining process comprises frigelization, decolorization and deodorization. A cosmetic product according to claim 15 comprising lip balm and a moisturizing cream. The cosmetic product of claim 16, further comprising cosmetic accessories. A cosmetic product according to claim 16 or 17, wherein the lip balm contains the following ingredients in percent by weight: 10%-50% of the vegetable wax and 50%-90% of the vegetable squalene composition. A cosmetic product according to claim 16 or 17, wherein the moisturizing cream contains the following components in percent by weight: 2%-60% of the vegetable squalene composition and the balance water.