A preparation method of squalene-rich cosmetic camellia oil

Abstract

The present invention belongs to the field of cosmetic camellia oil processing technology, and in particular to a preparation method of squalene-rich cosmetic camellia oil. The present invention steam distills camellia oil and wet-base camellia oil paste, and uses water vapor to bring out squalene in camellia oil and wet-base camellia oil paste; then the oil water vapor containing squalene is used to enrich camellia oil with squalene again, so as to increase the content of squalene in camellia oil; on the one hand, the steps of washing, alkali refining, degumming, vacuum decolorization, and deodorization are omitted in the refining process of camellia oil, and the camellia oil after enriching squalene is directly refined and winterized, and the wet-base camellia oil paste filled in the winterization filter column can be used to further supplement the squalene lost during the decolorization of the winterization oil in the winterization filter column. While the present invention can significantly increase the content of squalene, the oil is transparent and clear, tasteless and colorless, and fully meets the quality requirements of the national standard GB / T11765‑2018 of camellia oil.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetic camellia oil processing, and particularly relates to a preparation method of squalene-rich cosmetic camellia oil. Background Art

[0002] Cosmetic camellia oil is made from camellia oil, which is known as "Oriental olive oil", after being bleached by mixing white clay and activated carbon. It is colorless and odorless, rich in unsaturated fatty acids, and can effectively adhere to the skin surface to remove oxidative free radicals and repair damaged skin cells. It has the effects of moisturizing, anti-inflammatory, anti-oxidation, and repairing allergic damage. In recent years, as the cosmetics industry has become more and more aware of the efficacy of cosmetic camellia oil, most camellia oil companies have begun to produce cosmetic camellia oil. However, due to the large-scale loss of "squalene", which is known as the gold of cosmetic antioxidants, during the production of cosmetic camellia oil, the antioxidant effect of cosmetic camellia oil has been severely discounted. Therefore, the cosmetics industry has set a new standard for cosmetic camellia oil, requiring the squalene content to be greater than 50mg / kg, but no company's production process can meet this standard, resulting in the application of cosmetic camellia oil in the cosmetics field being gradually replaced by other chemical base oils.

[0003] At present, the production of cosmetic camellia oil generally needs to go through five production processes: water washing, alkali refining, bleaching, deodorization, and winterization refining. In the bleaching process, as the color of camellia oil decreases, the use of white clay and activated carbon gradually increases. However, excessive use of white clay and activated carbon to decolorize camellia oil, although the white camellia oil produced is colorless and tasteless and meets the appearance requirements of cosmetics, it removes a variety of biologically active ingredients in cosmetic camellia oil. The excessive use of white clay and activated carbon in the camellia oil refining and bleaching process leads to excessive adsorption of squalene, and the squalene content in cosmetic camellia oil seriously drops to 8mg / kg, affecting the efficacy of cosmetic camellia oil; however, if the content of squalene in cosmetic camellia oil needs to be guaranteed, the use of white clay and activated carbon decolorizers must be reduced, and the yellow and red colors of cosmetic camellia oil do not meet the standards. The unqualified rate of appearance quality of cosmetic camellia oil production reaches more than 98%, which seriously affects the production efficiency of camellia oil enterprises. Therefore, how to effectively remove the color of camellia oil, maximize the retention of squalene content in cosmetic camellia oil, effectively reduce production costs, improve production yields, and increase the competitiveness of cosmetic camellia oil in the camellia oil industry has become a key problem that needs to be solved in the application field of camellia oil cosmetics to break the product price competition. Summary of the invention

[0004] The object of the present invention is to provide a method for preparing squalene-rich cosmetic camellia oil. The squalene-rich cosmetic camellia oil prepared by the present invention meets the requirements of the cosmetic appearance characteristics of being colorless and odorless, and the squalene content is significantly improved.

[0005] In order to achieve the above object, the present invention provides the following technical solutions:

[0006] The present invention provides a method for preparing squalene-rich cosmetic camellia oil, comprising the following steps:

[0007] (1) mixing camellia oil and wet-based camellia dregs and squeezing them to obtain wet-based camellia seed paste; the mass ratio of the camellia oil to the wet-based camellia dregs is ≤2:3;

[0008] (2) mixing wet-base camellia seed paste and camellia seed oil to obtain a mixed oil; the mass ratio of the wet-base camellia seed paste to the camellia seed oil is ≤1:1; passing the water vapor into the mixed oil for vacuum distillation to obtain oil-water vapor; the temperature of the vacuum distillation is ≥ the boiling point of squalene; the oil-water vapor contains squalene;

[0009] (3) introducing the oil-water vapor into camellia oil to enrich squalene, and obtaining enriched oil after cooling;

[0010] (4) winterizing the enriched oil to obtain winterized oil;

[0011] (5) The winterized oil is loaded onto a winterized filter column for filtration to obtain squalene-rich cosmetic camellia oil; the filler in the winterized filter column is sequentially filled with a first decolorizing filler, a wet-based camellia seed paste, and a second decolorizing filler in the direction from the oil inlet to the oil outlet; the squalene content in the squalene-rich cosmetic camellia oil is ≥80 mg / kg.

[0012] Preferably, in step (1), the moisture content of the wet-based camellia oleifera seed residue is 20-30%.

[0013] Preferably, in step (1), the mass ratio of the camellia oil to the wet-based camellia residue is (2-4):(6-8).

[0014] Preferably, in step (2), the mass ratio of the wet-base camellia seed paste and camellia seed oil is (4-5):(5-6).

[0015] Preferably, the temperature of the vacuum distillation is 220 to 240° C., and the vacuum degree is -0.1 to -0.8 MPa.

[0016] Preferably, in step (3), the temperature for squalene enrichment is 160-180° C., the vacuum degree is -0.1-0.8 MPa, and the heat and pressure holding time is 3-5 h.

[0017] Preferably, in step (4), the winterization temperature is 4 to 6° C. and the insulation time is 24 to 48 hours.

[0018] Preferably, in step (5), the first decolorizing filler comprises silica sand; and the second decolorizing filler comprises activated carbon and diatomaceous earth.

[0019] Preferably, in step (5), the filler in the winterization filter column is filled with silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth in sequence from the oil inlet to the oil outlet; the mass ratio of the silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth is (2-6): (4:7): (1-5): (1-3).

[0020] Preferably, the squalene content in the squalene-rich camellia oil is 80-100 mg / kg; 2-3 Lovibond units for yellow, and 0.2-0.3 Lovibond units for red.

[0021] The present invention provides a method for preparing squalene-rich cosmetic camellia oil, comprising the following steps:

[0022] (1) mixing camellia oil and wet-based camellia residues for squeezing to obtain wet-based camellia paste; the mass ratio of the camellia oil to the wet-based camellia residues is ≤2:3; (2) mixing the wet-based camellia paste and camellia oil to obtain a mixed oil; the mass ratio of the wet-based camellia paste to the camellia oil is ≤1:1; passing the water vapor into the mixed oil for vacuum distillation to obtain oil-water vapor; the temperature of the vacuum distillation is ≥ the boiling point of squalene; the oil-water vapor contains squalene; (3 ) passing the oil-water vapor into camellia oil to enrich squalene, and obtaining enriched oil after cooling; (4) winterizing the enriched oil to obtain winterized oil; (5) loading the winterized oil onto a winterization filter column for filtration to obtain squalene-rich cosmetic camellia oil; the filler in the winterization filter column is sequentially filled with a first decolorizing filler, a wet-based camellia oil paste, and a second decolorizing filler in the direction from the oil inlet to the oil outlet; the squalene content in the squalene-rich cosmetic camellia oil is ≥80 mg / kg. On the one hand, the present invention is to steam distill camellia oil and wet-base camellia oil paste, and use steam to take out squalene in the camellia oil and the wet-base camellia oil paste; then use oil steam containing squalene to enrich the camellia oil with squalene, so as to increase the content of squalene in the camellia oil; on the other hand, the present invention omits the step of vacuum decolorization of the camellia oil, directly winterizes the camellia oil enriched with squalene, and then uses a winterization filter column to filter, and uses a first decolorization filler to simultaneously decolorize and oil-filter the winterized oil. Filter, and at the same time, the wet-based camellia oil seed paste filled in the winterization filter column can further supplement the squalene lost when the winterization oil is decolorized in the winterization filter column, and finally the second decolorization filler is used to remove the colored substances and impurities in the wet-based camellia oil paste brought out by the winterization oil separated from the wet-based camellia oil paste; in summary, the preparation method provided by the present invention can make the squalene content of cosmetic camellia oil ≥80 mg / kg, while significantly improving the squalene content, the oil is transparent and clear, odorless and colorless, and fully meets the quality requirements of the national standard GB / T 11765-2018 for camellia oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 A schematic diagram of the preparation process of squalene-rich cosmetic camellia oil provided in an embodiment of the present invention. DETAILED DESCRIPTION

[0024] The present invention provides a method for preparing squalene-rich cosmetic camellia oil, comprising the following steps:

[0025] (1) mixing camellia oil and wet-based camellia dregs and squeezing them to obtain wet-based camellia seed paste; the mass ratio of the camellia oil to the wet-based camellia dregs is ≤2:3;

[0026] (2) mixing wet-base camellia seed paste and camellia seed oil to obtain a mixed oil; the mass ratio of the wet-base camellia seed paste to the camellia seed oil is ≤1:1; passing the water vapor into the mixed oil for vacuum distillation to obtain oil-water vapor; the temperature of the vacuum distillation is ≥ the boiling point of squalene; the oil-water vapor contains squalene;

[0027] (3) introducing the oil-water vapor into camellia oil to enrich squalene, and obtaining enriched oil after cooling;

[0028] (4) winterizing the enriched oil to obtain winterized oil;

[0029] (5) The winterized oil is loaded onto a winterized filter column for filtration to obtain squalene-rich cosmetic camellia oil; the filler in the winterized filter column is sequentially filled with a first decolorizing filler, a wet-based camellia seed paste, and a second decolorizing filler in the direction from the oil inlet to the oil outlet; the squalene content in the squalene-rich cosmetic camellia oil is ≥80 mg / kg.

[0030] In the present invention, unless otherwise specified, all preparation raw materials / components are commercially available products well known to those skilled in the art.

[0031] The invention mixes camellia oil and wet-based camellia residues for squeezing to obtain wet-based camellia seed paste; the mass ratio of the camellia oil to the wet-based camellia residues is ≤2:3.

[0032] In the present invention, the preparation method of camellia oil and wet-based camellia residues comprises the following steps: squeezing fresh camellia fruits to obtain camellia oil and wet-based camellia residues.

[0033] In the present invention, the pressing is preferably screw pressing, and the present invention has no special requirements for the specific implementation process of the screw pressing.

[0034] In the present invention, the camellia seed oil is freshly pressed camellia seed oil.

[0035] In the present invention, the wet-based camellia oil seed residue is preferably a wet-based camellia oil seed cake.

[0036] In the present invention, the moisture content of the wet-based camellia seed residue is preferably 20-30%, and specifically preferably 20%, 25% or 30%.

[0037] In the present invention, the mass ratio of the camellia oil to the wet-based camellia residue is preferably (2-4):(6-8), and specifically preferably 4:6, 2:8 or 3:7.

[0038] The present invention has no special requirements on the specific implementation process of the squeezing.

[0039] The invention uses a wet-based camellia seed paste obtained by mixing camellia oil and wet-based camellia seed residues for squeezing, and the wet-based camellia seed paste is used for vacuum distillation of squalene and as a filler for a winterization filter column, respectively, and can effectively recover squalene in the wet-based camellia seed residues, avoid waste of squalene in the wet-based camellia seed residues, and improve the extraction rate of squalene, a cosmetic active ingredient, in fresh camellia fruit. In addition, the invention uses squeezing to squeeze the wet-based camellia seed residues into a paste, which is beneficial to the leaching of squalene in the wet-based camellia seed residues and improves the recovery rate of squalene.

[0040] In the present invention, the camellia oil is freshly squeezed camellia oil. The present invention adopts fresh camellia fruit to prepare camellia oil and wet-based camellia residue. The obtained camellia oil and wet-based camellia residue contain rich squalene.

[0041] After obtaining the wet-based camellia seed paste, the present invention mixes the wet-based camellia seed paste and camellia seed oil to obtain a mixed oil; the mass ratio of the wet-based camellia seed paste and the camellia seed oil is ≤1:1; the water vapor is introduced into the mixed oil for vacuum distillation to obtain oil-water vapor; the temperature of the vacuum distillation is ≥ the boiling point of squalene; and the oil-water vapor contains squalene.

[0042] In the present invention, the mass ratio of the wet-based camellia seed paste and the camellia seed oil is preferably (4-5):(5-6), and specifically preferably 4:6 or 5:5.

[0043] In the present invention, the temperature of the vacuum distillation is preferably 220-240°C, specifically preferably 220°C, 230°C or 240°C; the vacuum degree is preferably -0.1-0.8MPa, more preferably -0.1MPa or -0.8MPa. The time of the vacuum distillation is preferably 0.1-3h, more preferably 0.2h. In the present invention, the vacuum distillation is preferably carried out in a high-temperature distillation tower. The present invention preferably uses biomass fuel to heat the high-temperature distillation tower to the temperature of the vacuum distillation, stops the biomass fuel from heating the high-temperature distillation tower, and then the present invention passes water vapor into the mixed oil for vacuum distillation.

[0044] The present invention preferably heats and vaporizes the squalene in the mixed oil obtained by mixing the wet-base camellia seed paste and the camellia seed oil into a gaseous state through vacuum distillation, and entrains the gaseous squalene with water vapor to obtain wet-base oil water vapor.

[0045] The invention distills squalene after mixing the wet-based camellia seed paste and the camellia seed oil, thereby recovering the squalene in the wet-based camellia seed residue and improving the extraction rate of squalene.

[0046] After obtaining the oil-water vapor, the invention introduces the oil-water vapor into camellia oil to enrich squalene, and obtains enriched oil after cooling.

[0047] In the present invention, the temperature for the squalene enrichment is preferably 160-180°C, specifically preferably 175°C, 180°C, 160°C; the vacuum degree is preferably -0.1-0.8MPa, specifically preferably -0.1MPa; the heat preservation and pressure holding time is preferably 3-5h, specifically preferably 3h, 4h or 5h. In the present invention, the temperature for the squalene enrichment specifically refers to the temperature of the oil vapor and the temperature of the camellia oil.

[0048] When the squalene is enriched, the introduction rate of the oil-water vapor is preferably 5-10 mL / min. The ratio of the mass of the camellia seed oil to the volume of the oil-water vapor is preferably 1 g:3 mL.

[0049] The present invention preferably carries out the squalene enrichment in an enrichment tank.

[0050] The present invention preferably enriches squalene by using squalene obtained by vacuum distillation to supplement the squalene in camellia oil, thereby effectively increasing the content of squalene in the cosmetic camellia oil.

[0051] After obtaining the enriched oil, the present invention winterizes the enriched oil to obtain the winterized oil.

[0052] In the present invention, the winterization temperature is preferably 4-6°C, specifically preferably 5°C or 6°C; the insulation time is preferably 24-48h, more preferably 24h.

[0053] After obtaining the winterized oil, the present invention loads the winterized oil onto a winterization filter column for filtration to obtain squalene-rich cosmetic camellia oil; the filler in the winterization filter column is sequentially filled with a first decolorizing filler, a wet-based camellia seed paste, and a second decolorizing filler in the direction from an oil inlet to an oil outlet; the content of squalene in the squalene-rich cosmetic camellia oil is ≥80 mg / kg.

[0054] In the present invention, the first decolorizing filler preferably includes silica gel sand; the second decolorizing filler preferably includes activated carbon and diatomaceous earth.

[0055] In the present invention, the filler in the winterization filter column is preferably filled with silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth in sequence from the oil inlet to the oil outlet; the mass ratio of the silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth is preferably (2-6): (4:7): (1-5): (1-3).

[0056] In the present invention, the effects of the wet-based camellia seed paste in the winterization filter column include the following three aspects: first, reducing the flow rate of the winterization oil in the winterization filter column, enabling the winterization oil to fully contact with the first decolorizing filler, thereby fully removing the oil and colored substances in the winterization oil; second, further supplementing the squalene effective ingredient in the winterization oil; third, enhancing the fragrance of the winterization oil, making the smell of the cosmetic camellia oil more intense.

[0057] In the present invention, when the winterized oil is filtered through the winterization filter column, the first decolorizing filler can remove impurities such as free fatty acids, phospholipids, wax fats, yellow and red in the winterized oil, thereby achieving decolorization of the winterized oil; then, the filler in the winterization filter column includes wet-based camellia seed paste, and the squalene in the wet-based camellia seed paste can further supplement the squalene in the winterized oil. Finally, the second decolorizing filler can remove colored substances and impurities in the freshly pressed camellia seed oil brought out by the decolorized oil in the wet-based camellia seed paste, and further decolorize the winterized oil.

[0058] In the present invention, the content of squalene in the squalene-rich camellia oil is preferably 80-100 mg / kg; 2-3 Lovibond units for yellow, and 0.2-0.3 Lovibond units for red.

[0059] Compared with the existing technology, the preparation of the existing cosmetic camellia oil needs to go through six refining production process links of water washing, alkali refining, decolorization, deodorization and winterization, and there are many squalene loss links. The present invention uses freshly squeezed camellia oil to directly supplement with squalene steam, and then uses the decolorizing filler in the winterization filter column to filter and decolorize the winterized oil, directly removes impurities and colored substances such as free fatty acids, phospholipids, wax fats in the oil, and avoids the water washing in the prior art, the alkali refining process sodium chloride solution, sodium hydroxide solution, acid solution and other chemical substances in the oil, causing the loss of squalene in the oil, and the use of the cosmetic camellia oil of the present invention fully meets the quality requirements of the national standard GB / T 11765-2018 for camellia oil, squalene 80-100mg / kg, yellow 2.0-3.0 Lovibond units, red 0.2-0.3 Lovibond units.

[0060] In order to further illustrate the present invention, the technical solution provided by the present invention is described in detail below in conjunction with the accompanying drawings and embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0061] Example 1

[0062] according to Figure 1 The process shown is as follows: In this embodiment, fresh camellia fruit is squeezed in batches. In each batch of squeezing, 215g of freshly squeezed camellia seed oil and 624g of 20% moisture wet-based camellia seed cake are produced by spiral squeezing 1000g of fresh camellia fruit to obtain freshly squeezed camellia seed oil and wet-based camellia seed cake.

[0063] 156g of freshly pressed camellia oil and 624g of wet-based camellia seed cake are mixed in a mass ratio of 2:8 and pressed into a paste to produce 780g of wet-based camellia seed paste. 20g of wet-based camellia seed paste, silica gel sand, activated carbon and diatomaceous earth are added to a winterization filter column. The filling materials from the oil inlet to the oil outlet of the winterization filter column are silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth in sequence, with a mass ratio of 2:4:1:1. 480g of wet-based camellia seed paste enters a high-temperature distillation tower for distillation.

[0064] 480g wet-base camellia seed paste and 720g freshly pressed camellia seed oil are mixed in a mass ratio of 4:6 and enter a high-temperature distillation tower for distillation to produce wet-base oil water vapor. The high-temperature distillation tower is first heated to 220°C by biomass fuel, and then the biomass fuel is stopped and heated by hot steam instead. The mixed material is introduced into the distillation tower to keep warm at 220°C. The vacuum degree of the high-temperature distillation tower is -0.8MPa, and the wet-base oil water vapor is obtained by distillation for 0.2h.

[0065] 200g of freshly pressed camellia oil was sent to an enrichment tank, and 600mL of wet base oil water vapor was flushed into the freshly pressed camellia oil. The vacuum degree in the enrichment tank was -0.1MPa, the temperature was 160℃, the time was 5h, and it was cooled to room temperature.

[0066] The oil cooled to room temperature in the enrichment tank enters the 4°C winterization tank for winterization for 24 hours to become winterized oil. The winterized oil is then input into the winterization filter column for filtration. The winterized finished cosmetic camellia oil fully meets the quality requirements of the national standard GB / T 11765-2018 for camellia oil. The specific component analysis is shown in Table 1.

[0067] Example 2

[0068] according to Figure 1 The process shown is as follows: In this embodiment, fresh camellia fruit is squeezed in batches. In each batch of squeezing, 215g of freshly squeezed camellia seed oil and 624g of 20% moisture wet-based camellia seed cake are produced by spiral squeezing 1000g of fresh camellia fruit to obtain freshly squeezed camellia seed oil and wet-based camellia seed cake.

[0069] 156g of freshly pressed camellia oil and 234g of wet-based camellia seed cake are mixed in a mass ratio of 4:6 and squeezed into a paste to produce 390g of wet-based camellia seed paste. 25g of wet-based camellia seed paste, silica gel sand, activated carbon and diatomaceous earth are added to a winterization filter column. The filling materials from the oil inlet to the oil outlet of the winterization filter column are silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth in sequence, with a mass ratio of 6:7:5:3. 365g of wet-based camellia seed paste enters a high-temperature distillation tower for distillation.

[0070] 365g wet-base camellia seed paste and 365g freshly pressed camellia seed oil are mixed in a mass ratio of 5:5 and enter a high-temperature distillation tower for distillation to produce wet-base oil water vapor. The high-temperature distillation tower is first heated to 240°C by biomass fuel, and then the biomass fuel is stopped and heated by hot steam instead. The mixed material is introduced into the distillation tower to keep warm at 240°C. The vacuum degree of the high-temperature distillation tower is -0.1MPa, and distillation is performed for 0.2h to obtain wet-base oil water vapor.

[0071] 200g of freshly pressed camellia oil was sent to an enrichment tank, and 600mL of wet base oil water vapor was flushed into the freshly pressed camellia oil. The vacuum degree in the enrichment tank was -0.1MPa, the temperature was 180℃, the time was 3h, and it was cooled to room temperature.

[0072] The oil cooled to room temperature in the enrichment tank enters the 6°C winterization tank for winterization for 24 hours to become winterized oil. The winterized oil is then input into the winterization filter column for filtration. The winterized finished cosmetic camellia oil fully meets the quality requirements of the national standard GB / T 11765-2018 for camellia oil. The specific component analysis is shown in Table 1.

[0073] Example 3

[0074] according to Figure 1 The process shown is as follows: In this embodiment, fresh camellia fruit is squeezed in batches. In each batch of squeezing, 215g of freshly squeezed camellia seed oil and 624g of 20% moisture wet-based camellia seed cake are produced by spiral squeezing 1000g of fresh camellia fruit to obtain freshly squeezed camellia seed oil and wet-based camellia seed cake.

[0075] 156g of freshly pressed camellia oil and 364g of wet-based camellia seed cake are mixed in a mass ratio of 3:7 and squeezed into a paste to produce 520g of wet-based camellia seed paste. 20g of wet-based camellia seed paste, silica gel sand, activated carbon and diatomaceous earth are added to a winterization filter column. From the oil inlet to the oil outlet of the winterization filter column, the filling materials are silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth in sequence, with a mass ratio of 4:5:3:2. 500g of wet-based camellia seed paste enters a high-temperature distillation tower for distillation.

[0076] 500g wet-base camellia seed paste and 750g freshly pressed camellia seed oil are mixed in a mass ratio of 4:6 and enter a high-temperature distillation tower for distillation to produce wet-base oil water vapor. The high-temperature distillation tower is first heated to 230°C by biomass fuel, and then the biomass fuel is stopped and heated by hot steam instead. The mixed material is introduced into the distillation tower to keep warm at 230°C. The vacuum degree of the high-temperature distillation tower is -0.1MPa, and the wet-base oil water vapor is obtained by distillation for 0.2h.

[0077] 200g of freshly pressed camellia oil was sent to an enrichment tank, and 600mL of wet base oil water vapor was flushed into the freshly pressed camellia oil. The vacuum degree in the enrichment tank was -0.1MPa, the temperature was 175℃, the time was 4h, and it was cooled to room temperature.

[0078] The oil cooled to room temperature in the enrichment tank enters the 5℃ winterization tank for winterization for 24 hours to become winterized oil. The winterized oil is then input into the winterization filter column for filtration. The finished cosmetic camellia oil after winterization fully meets the quality requirements of the national standard GB / T 11765-2018 for camellia oil. The specific component analysis is shown in Table 1.

[0079] Comparative Example 1

[0080] 1. Water washing: Heat 720 g of camellia oil to 70°C, add 3% by mass fraction of sodium chloride aqueous solution according to 10% of the oil mass, wash for 1.5 hours, let it settle for 4 hours, release the water-washed impurities, and obtain water-washed oil.

[0081] 2. Alkali refining: Add 0.1 mol / L potassium hydroxide aqueous solution to the water-washed oil at 25°C. The acid value of the water-washed oil should be ≤4.0 mg / kg in terms of KOH. Stir at 60 rpm for 30 minutes. When the oil and soap separate, the temperature rises to 70°C. Continue stirring for 15 minutes and then stop. Remove the saponified product by centrifuge.

[0082] 3. Decolorization: The oil is heated to 120°C through a heat exchanger and enters a decolorization tower. Decolorizer (clay and activated carbon, mass ratio of 5:1) is added in an amount of 6% of the oil weight. The decolorization temperature is 105°C, the vacuum degree is -0.7MPa, the time is 45min, and the oil is filtered to filter out the clarified decolorized oil.

[0083] 4. Deodorization: The vacuum degree of the deodorization tower is -0.1MPa, the temperature of the bleached oil reaches 250℃, the bleached oil is heat exchanged with the outflowing finished oil in the spiral plate heat exchanger, the oil flow rate is 2000L / h, the time is 2.5h, the color, acid value, peroxide value, plasticizer and benzopyrene of the deodorized oil are in line with the national health standards.

[0084] 5. Winterization: The deodorized oil enters the winterization tank. After crystallization at 4°C for 24 hours, the plate and frame filter paper filters out the clear and transparent camellia oil without any suspended matter, which is the traditionally produced cosmetic camellia oil.

[0085] Comparative Example 2

[0086] In this comparative example, fresh camellia fruit is squeezed in batches. In each squeeze, 215g of freshly squeezed camellia seed oil and 624g of 20% moisture wet-based camellia seed cake are produced by spiral squeezing 1000g of fresh camellia fruit to obtain freshly squeezed camellia seed oil and wet-based camellia seed cake.

[0087] 156 g of freshly pressed camellia oil and 364 g of wet-based camellia cake were mixed in a mass ratio of 3:7 and pressed into a paste to produce 520 g of wet-based camellia paste.

[0088] 500g wet-base camellia seed paste and 720g freshly pressed camellia seed oil are mixed in a mass ratio of 4:6 and enter a high-temperature distillation tower for distillation to produce wet-base oil water vapor. The high-temperature distillation tower is first heated to 230°C by biomass fuel, and then the biomass fuel is stopped and heated by hot steam instead. The mixed material is heated to 230°C in the distillation tower and the vacuum degree of the high-temperature distillation tower is -0.1MPa. The wet-base oil water vapor is obtained by distillation for 0.2h.

[0089] 200g of freshly pressed camellia oil was sent to an enrichment tank, and 600mL of wet base oil water vapor was flushed into the freshly pressed camellia oil. The vacuum degree in the enrichment tank was -0.1MPa, the temperature was 175℃, the time was 4h, and it was cooled to room temperature.

[0090] The oil cooled to room temperature in the enrichment tank enters the 5℃ winterization tank for winterization for 24 hours to become winterized oil. The winterized oil is input into the winterization filter column for filtration. The filling materials from the oil inlet to the oil outlet of the winterization filter column are silica gel sand, activated carbon, and diatomaceous earth in sequence, with a mass ratio of 4:2:2. The finished cosmetic camellia oil after winterization fully meets the quality requirements of the national standard GB / T 11765-2018 for camellia oil. The specific component analysis is shown in Table 1.

[0091] Test Case

[0092] The cosmetic camellia oil prepared in Examples 1 to 3 has no significant difference in safety index, squalene content, yellow and red; compared with the cosmetic camellia oil prepared in Comparative Example 1, Example 2 has not only better safety index, but also significantly increased squalene content, and significantly reduced yellow and red; compared with the cosmetic camellia oil prepared in Comparative Example 1, Example 1 to 3 has not only better safety index, but also significantly increased squalene content, and significantly reduced yellow and red; compared with the cosmetic camellia oil prepared in Comparative Example 2, Example 1 to 3 has no significant difference in safety index, yellow and red, and significantly increased squalene content. The test results of the cosmetic camellia oil prepared in Example 1 to 3 compared with Comparative Examples 1 and 2 are shown in Table 1.

[0093] Table 1 Test results of cosmetic camellia oil prepared in Examples 1 to 3 compared with Comparative Examples 1 and 2

[0094]

[0095]

[0096] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention, not all of the embodiments. Other embodiments can be obtained based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A method for preparing squalene-rich cosmetic camellia oil, characterized in that: The following steps are involved: (1) mixing camellia oil and wet-based camellia dregs and squeezing them to obtain wet-based camellia seed paste; the mass ratio of the camellia oil to the wet-based camellia dregs is ≤2:3; (2) mixing wet-base camellia seed paste and camellia seed oil to obtain a mixed oil; the mass ratio of the wet-base camellia seed paste to the camellia seed oil is ≤1:1; passing water vapor into the mixed oil for vacuum distillation to obtain oil-water vapor; the temperature of the vacuum distillation is ≥ the boiling point of squalene; the oil-water vapor contains squalene; (3) passing the oil-water vapor into tea seed oil to enrich squalene, and obtaining enriched oil after cooling; (4) winterizing the enriched oil to obtain winterized oil; (5) The winterized oil is loaded onto a winterized filter column for filtration to obtain squalene-rich cosmetic camellia oil; the filler in the winterized filter column is sequentially filled with a first decolorizing filler, a wet-based camellia seed paste, and a second decolorizing filler in the direction from the oil inlet to the oil outlet; the squalene content in the squalene-rich cosmetic camellia oil is ≥80 mg / kg.

2. The preparation method according to claim 1, characterized in that: In step (1), the moisture content of the wet-based camellia oleifera seed residue is 20-30%.

3. The preparation method according to claim 2, characterized in that: In step (1), the mass ratio of the camellia oil to the wet-based camellia residue is (2-4):(6-8).

4. The preparation method according to claim 1, characterized in that: In step (2), the mass ratio of the wet-base camellia seed paste and camellia seed oil is (4-5):(5-6).

5. The preparation method according to claim 1, characterized in that: The temperature of the vacuum distillation is 220-240° C., and the vacuum degree is -0.1 MPa.

6. The preparation method according to claim 1, characterized in that: In step (3), the temperature for squalene enrichment is 160-180° C., the vacuum degree is -0.1 MPa, and the heat and pressure holding time is 3-5 hours.

7. The preparation method according to claim 1, characterized in that: In step (4), the winterization temperature is 4 to 6° C. and the insulation time is 24 to 48 hours.

8. The preparation method according to claim 1, characterized in that: In step (5), the first decolorizing filler includes silica gel sand; the second decolorizing filler includes activated carbon and diatomaceous earth.

9. The preparation method according to claim 8, characterized in that: In step (5), the filler in the winterization filter column is filled with silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth in sequence from the oil inlet to the oil outlet; the mass ratio of the silica gel sand, wet-based camellia seed paste, activated carbon and diatomaceous earth is (2-6): (4:7): (1-5): (1-3).

10. The preparation method according to claim 1, characterized in that: The squalene content in the squalene-rich camellia oil is 80-100 mg / kg; the yellow color is 2-3 Lovibond units, and the red color is 0.2-0.3 Lovibond units.

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