Preparation method of prickle fruit oil, its product and application in hair products

Through the cold pressing process, combined with mixed soil treatment of acidic white clay and diatomaceous earth, the problems of strong odor, dark color and many impurities of green thorn fruit oil are solved, and its application in daily chemical and hair products is expanded, achieving excellent color protection and soft repair effects.

CN116376630BActive Publication Date: 2025-08-12GUANGDONG THANMELIN BIOTECHNOLOGY CO LTD
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Patent Information

Application Number
CN202310109131.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-02-14
Publication Date
2025-08-12
Estimated Expiration
2043-02-14

AI Technical Summary

Technical Problem

The existing preparation methods for green thorn oil lead to strong oil odor, dark color and many impurities, affecting the application of daily chemical products, and have fewer applications in used products.

Method used

After the cold pressing process is used to produce crude oil of green thorn fruit, the mixed soil of acidic white clay and diatomaceous earth is used to decolorize, dehydrate and deodorize the taste treatment to avoid the saponification reaction caused by alkaline white clay and optimize the temperature and pressure conditions.

Benefits of technology

The produced green thorn oil has a light odor, light color and few impurities. It is suitable for daily chemical products and has excellent color protection, resistance to high temperature damage and soft repair effects on the hair.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a method for preparing prickle fruit oil, a product thereof, and application thereof in hair products. The preparation method comprises the following steps: drying prickle fruit seeds and then pressing them at room temperature to obtain crude oil; mixing the crude oil with acidic clay and diatomaceous earth, heating the oil, cooling the oil, and filtering the oil. The method first uses a cold pressing process to prepare the prickle fruit crude oil, and then uses a mixture of acidic clay and diatomaceous earth to decolorize, dehydrate, and remove odor. The refined prickle fruit oil obtained overcomes the drawbacks of the prickle fruit oil prepared in the prior art, such as strong odor, dark color, and high impurities, thereby increasing its compatibility in daily chemical products. The preparation method is simple in process, can be industrialized, and has the advantages of being non-toxic, highly effective, safe, and free of the introduction of exogenous solvents, thereby making it more widely applicable in the field of daily chemical products.
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Description

Technical Field

[0001] The invention belongs to the technical field of oil processing, and relates to a preparation method of prickle fruit oil, a product thereof, and an application of the oil in hair products, and in particular to a preparation method of prickle fruit oil, a product thereof, and an application of the oil in hair products with the functions of protecting color, resisting high-temperature damage, or softening and repairing hair. Background Art

[0002] Prinsepia utilis Royle, also known as Prinsepia utilis Royle in Chinese, belongs to the genus Prinsepia in the Rosaceae family, subfamily Prunaceae. Also known as green thorn tip and oil-beating fruit, it grows on hillsides, wastelands, farmlands, roadsides, and in shady thickets at altitudes of 1,800-3,000 meters, remaining remarkably resilient even in the cold of winter.

[0003] The fruit of the Chinese prickly ash tree has a wide range of uses and a long history of medicinal use. Its kernels and leaves contain numerous essential macro- and trace elements, and are high in crude fat. They have the potential to clear heat and detoxify, reduce inflammation, promote blood circulation, relieve pain, aid digestion, and strengthen the stomach. The fruit oil (also known as qingna oil) has been used for many years as a popular edible oil. It is a highly recommended, environmentally friendly food. Regular consumption can lower blood lipids, regulate blood pressure, promote microcirculation, and enhance the body's immune system. Furthermore, because it is rich in unsaturated fatty acids and has a composition similar to human sebum, it also has the potential to regenerate and repair the skin, slow aging, and maintain moisture.

[0004] CN110724591A discloses a method for processing prickle fruit oil. This invention utilizes hot pressing to extract the oil, adding water to the oil dregs and extracting them with a subcritical fluid. The oil is then combined and refined, yielding a yield of 20-28%. The prickle fruit obtained by hot pressing has a strong and fragrant aroma and a dark color, and the final refining process is not dehydrated. Because the color and odor affect the appearance and odor of the finished skin care product formula, and because the refining process does not involve dehydration, its application in the daily chemical industry is limited due to its easy impact on the odor of the finished product formula.

[0005] CN112175713A discloses a process for preparing prickle fruit oil with a prolonged oxidation induction time. This process utilizes supercritical CO2 extraction. While enriching fatty acids, it also extracts volatile terpenes, anthraquinones, and small-scale pigments contained in the prickle fruit. The resulting crude oil has a pungent flavor and is high in impurities, significantly increasing the difficulty of subsequent purification. Furthermore, the process uses alkaline clay for purification, which reacts with components in the oil to saponify, increasing the saponification value and affecting the quality and stability of the prickle fruit oil. Summary of the Invention

[0006] In view of the deficiencies in the prior art, the present invention aims to provide a method for preparing prickle fruit oil, a product thereof, and applications thereof in hair products, and in particular to provide a method for preparing prickle fruit oil, a product thereof, and applications thereof in hair products having color protection, resistance to high temperature damage, or softening and repairing effects.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a method for preparing utilitarian fruit oil, the preparation method comprising the following steps:

[0009] (1) drying the seeds of the utilitarian fruit and pressing them at a temperature of 10-40° C. to obtain crude oil;

[0010] (2) The crude oil obtained in step (1) is mixed with acidic white clay and diatomaceous earth, subjected to heat treatment, then cooled, and filtered to obtain the prickle oil.

[0011] The invention creatively adopts a cold pressing process to prepare crude prickle fruit oil, and then uses a mixture of acidic white clay and diatomaceous earth to perform decolorization, dehydration and deodorization treatment, so that the obtained refined prickle fruit oil overcomes the disadvantages of the prickle fruit oil prepared in the prior art, such as strong odor, dark color and many impurities, and improves its adaptability in daily chemical products. At the same time, the preparation method has a simple process, can realize industrial production, and has the advantages of being non-toxic, highly effective, safe and free of introduction of exogenous solvents, so that the refined prickle fruit oil is more widely used in the field of daily chemical products.

[0012] In addition, in the prior art, prickle fruit oil is primarily used for health care, skin care, and beauty. The oleic acid and linoleic acid contained in it have been shown to have anti-cancer activity. However, currently, prickle fruit oil is rarely used in hair products. The prickle fruit oil prepared using the preparation method of the present invention has excellent color protection, resistance to high temperature damage, and softening and repairing effects on hair. Therefore, it can be used as a raw material to prepare hair products with the above-mentioned effects, expanding the application field of prickle fruit oil.

[0013] Preferably, the moisture content of the dried utilitarian fruit seeds is 2-6%, for example, 2%, 3%, 4%, 5%, 6%, etc. Other specific values within this numerical range can be selected and will not be described in detail here.

[0014] The prickle fruit seed raw material used in the preparation method of the present invention preferably has a moisture content of 2-6% because if the moisture content is higher than 6%, the moisture content in the prickle fruit oil will be too high, accelerating the acidification of the prickle fruit oil; if the moisture content is lower than 2%, the structural water of the prickle fruit seeds will be destroyed, and the unsaturated fatty acids therein will accelerate oxidation and affect the quality of the prickle fruit oil, all of which will have a negative impact on the color protection, resistance to high temperature damage and softening and repairing effects of the prepared prickle fruit oil.

[0015] Preferably, the usage amount of the acidic clay and diatomaceous earth is 1-6% of the mass of the crude oil, for example 1%, 2%, 3%, 4%, 5%, 6%, etc. Other specific values within this numerical range can be selected and will not be described here one by one.

[0016] The amount of acidic white clay and diatomaceous earth used in the preparation method of the present invention is preferably 1-6% of the mass of the crude oil because if the amount used is further increased, the effects of the obtained prickle fruit oil in terms of smell, color, and hair efficacy will not be significantly improved, and if the amount used is further reduced, the effects of the obtained prickle fruit oil in terms of smell, color, and hair efficacy will be significantly reduced.

[0017] Preferably, the mass ratio of the acidic clay to diatomaceous earth is (2-4):1, such as 2:1, 2.5:1, 3:1, 3.5:1, 4:1, etc. Other specific values within this numerical range can be selected and will not be described here one by one.

[0018] The present invention specifically uses a mixture of acidic clay and diatomaceous earth to refine crude prickle oil. This, on the one hand, prevents saponification reaction between the alkaline clay and components in the oil, which would affect the quality and stability of the prickle oil. On the other hand, the combined advantages of the acidic clay and diatomaceous earth are utilized. The combined use of the acidic clay and diatomaceous earth has a significant synergistic effect in reducing the odor and color of the prickle oil and improving the hair efficacy of the prickle oil. This combined advantage is even more pronounced when the mass ratio of the acidic clay and diatomaceous earth is selected to be (2-4):1.

[0019] Preferably, the heat treatment is performed at 50-70° C. (e.g., 50° C., 53° C., 55° C., 58° C., 60° C., 63° C., 65° C., 68° C., 70° C., etc.) for 0.5-1.5 h (e.g., 0.5 h, 0.7 h, 0.8 h, 1.0 h, 1.2 h, 1.3 h, 1.4 h, 1.5 h, etc.). Other specific values within the above numerical range can be selected and will not be repeated here.

[0020] The above-mentioned heating treatment is preferably performed at 50-70° C. because if the temperature is further increased, unpleasant odor will be produced, and if the temperature is further decreased, the decolorization effect will be less obvious.

[0021] Preferably, the cooling refers to cooling to below 35°C, such as 35°C, 30°C, 28°C, 25°C, 20°C, 15°C, etc.

[0022] Preferably, the filtration is performed at 0.1-0.5 MPa (eg, 0.1 MPa, 0.2 MPa, 0.3 MPa, 0.4 MPa, 0.5 MPa, etc.) using a 0.2-1.0 μm membrane.

[0023] Other specific point values within the above numerical range can be selected and will not be described in detail here.

[0024] In a second aspect, the present invention provides prickle fruit oil prepared according to the preparation method of prickle fruit oil described in the first aspect.

[0025] The prickle fruit oil product prepared by the preparation method of the present invention has a light fragrance or is substantially odorless, a low Gardner chroma value, few impurities, and no precipitation; the composition ratio of polyunsaturated fatty acids, monounsaturated fatty acids, and saturated fatty acids is close to the structure of human fatty acids, which is conducive to skin absorption; and it is creatively found that the prickle fruit oil product has excellent effects of protecting hair color, resisting high-temperature damage, and softening and repairing hair.

[0026] In a third aspect, the present invention further provides use of the utilitarian fruit oil according to the second aspect in preparing hair products.

[0027] Preferably, the hair product is a hair product with color protection effect.

[0028] Preferably, the hair product is used in a hair product having the effect of resisting high temperature damage.

[0029] Preferably, the hair product is used in a hair product with softening and repairing effects.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] The invention creatively adopts a cold pressing process to prepare crude prickle fruit oil, and then uses a mixture of acidic white clay and diatomaceous earth to perform decolorization, dehydration and deodorization treatment, so that the obtained refined prickle fruit oil overcomes the disadvantages of the prickle fruit oil prepared in the prior art, such as strong odor, dark color and many impurities, and improves its adaptability in daily chemical products. At the same time, the preparation method has a simple process, can realize industrial production, and has the advantages of being non-toxic, highly effective, safe and free of introduction of exogenous solvents, so that the refined prickle fruit oil is more widely used in the field of daily chemical products.

[0032] The prickle fruit oil product prepared by the preparation method of the present invention has a light fragrance or is substantially odorless, a low Gardner chroma value, few impurities, and no precipitation; the composition ratio of polyunsaturated fatty acids, monounsaturated fatty acids, and saturated fatty acids is close to the structure of human fatty acids, which is conducive to skin absorption; and it is creatively found that the prickle fruit oil product has excellent effects of protecting hair color, resisting high-temperature damage, and softening and repairing hair. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a scanning electron micrograph of the hair cuticle of the control group in the heat protection efficacy test (magnification 500x);

[0034] Figure 2 This is a scanning electron micrograph of the hair cuticle of the control group in the heat protection efficacy test (magnification 1000x);

[0035] Figure 3 This is a scanning electron micrograph of the hair cuticle of the control group in the heat protection efficacy test (magnification 2000x);

[0036] Figure 4 This is a scanning electron micrograph (500x magnification) of the hair cuticle of the sample group in the heat protection efficacy test.

[0037] Figure 5 This is a scanning electron micrograph of the hair cuticle of the sample group in the heat protection efficacy test (magnification 1000x);

[0038] Figure 6 This is a scanning electron micrograph of the hair cuticle of the sample group in the heat protection efficacy test (magnification 2000x);

[0039] Figure 7 This is the electron micrograph of the hair cuticle of the control group before and after treatment;

[0040] Figure 8 These are electron microscope images of the hair scales of the sample group before and after treatment. DETAILED DESCRIPTION

[0041] The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the embodiments are merely to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0042] Example 1

[0043] This embodiment provides a kind of prickle fruit oil, and its preparation method is as follows:

[0044] (1) 150.23 g of prune prune seeds without leaves, branches, or stones, and without mold or corruption were selected and dried in a cool, ventilated place to a moisture content of 4% for subsequent use;

[0045] (2) The dried seeds of the fruit of the Chinese clava were squeezed at 23.6°C using a squeezer (WOP-KP0202, Jiangxi Westinghouse) to obtain crude oil;

[0046] (3) The crude oil obtained was mixed with acidic white clay and diatomaceous earth (mass ratio of 3:1) with a total amount of 3% of the crude oil, heated at 60° C. for 1 h, then cooled to 30° C., and filtered with a 0.45 μm membrane at a pressure of 0.3 MPa to obtain the prickle oil.

[0047] Example 2

[0048] This embodiment provides a kind of prickle fruit oil, and its preparation method is as follows:

[0049] (1) 150.22 g of prune prune seeds without leaves, branches, or stones, and without mold or corruption were selected and dried in a cool, ventilated place to a moisture content of 5% for subsequent use;

[0050] (2) The dried seeds of the fruit of the Chinese clava were squeezed at 15.5°C using a squeezer (WOP-KP0202, Jiangxi Westinghouse) to obtain crude oil;

[0051] (3) The obtained crude oil was mixed with acidic white clay and diatomaceous earth (mass ratio of 2:1) with a total amount of 6% of the crude oil, heated at 55° C. for 1.5 h, then cooled to 25° C., and filtered with a 0.45 μm membrane at a pressure of 0.4 MPa to obtain the prickle oil.

[0052] Example 3

[0053] This embodiment provides a kind of prickle fruit oil, and its preparation method is as follows:

[0054] (1) 150.04 g of pruinosa seeds without leaves, branches, or stones, and without mold or corruption were selected and dried in a cool, ventilated place to a moisture content of 3% for subsequent use.

[0055] (2) The dried seeds of the fruit of the Chinese clava were squeezed at 32.0°C using a squeezer (WOP-KP0202, Jiangxi Westinghouse) to obtain crude oil;

[0056] (3) The obtained crude oil was mixed with acidic white clay and diatomaceous earth (mass ratio of 4:1) with a total amount of 2% of the crude oil, heated at 65° C. for 0.5 h, then cooled to 25° C., and filtered with a 0.45 μm membrane at a pressure of 0.2 MPa to obtain the prickle oil.

[0057] Example 4

[0058] This embodiment provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that the mass ratio of the acidic white clay to the diatomaceous earth in step (3) is 1:3 and the total amount of the mixed soil is kept unchanged, and other processing methods remain the same.

[0059] Example 5

[0060] This embodiment provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that in step (3), the oil is heated at 80° C. for 0.5 h, and other treatment methods remain the same.

[0061] Example 6

[0062] This embodiment provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that the oil is heated at 40° C. for 1.5 h in step (3), and other treatment methods remain the same.

[0063] Comparative Example 1

[0064] This comparative example provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that in step (2), the dried prickle fruit seeds are squeezed at 129.8° C. using a squeezer (WOP-KP0202, Jiangxi Westinghouse), and other processing methods remain the same.

[0065] Comparative Example 2

[0066] This comparative example provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that an equal amount of acid clay in step (3) is replaced by activated carbon, and other processing methods remain the same.

[0067] Comparative Example 3

[0068] This comparative example provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that an equal amount of acidic clay in step (3) is replaced by alkaline clay, and other processing methods remain the same.

[0069] Comparative Example 4

[0070] This comparative example provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that an equal amount of diatomaceous earth in step (3) is replaced with silica gel, and other processing methods remain the same.

[0071] Comparative Example 5

[0072] This comparative example provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that in step (3), the obtained crude oil is mixed with acidic clay in a total amount of 3% of the crude oil, and other processing methods remain the same.

[0073] Comparative Example 6

[0074] This comparative example provides a prickle fruit oil, the preparation method of which differs from that of Example 1 only in that in step (3), the obtained crude oil is mixed with diatomaceous earth in an amount of 3% of the crude oil, and other processing methods remain the same.

[0075] Test Example 1

[0076] The fatty acid composition of the utilitarian fruit oil prepared in Examples 1-3 was determined by referring to the third method normalization method in "GB5009.168-2016 National Food Safety Standard Determination of Fatty Acids in Foods", and the results are shown in Table 1, Table 2, and Table 3, respectively:

[0077] Table 1

[0078]

[0079]

[0080] Table 2

[0081]

[0082] Table 3

[0083]

[0084] From the test results in Tables 1-3, it can be seen that the mass ratios of saturated fatty acids, monounsaturated fatty acids and saturated fatty acids in the prepared Prinus utilis oil are all close to the 1:1:1 structure of human fatty acids.

[0085] Test Example 2

[0086] The physicochemical properties of the utilitarian fruit oils obtained in Examples 1-6 and Comparative Examples 1-6 were measured, including Gardner color value, moisture content, odor, and appearance. The results are shown in Table 4:

[0087] Table 4

[0088]

[0089] As shown in Table 4, the pruinosa purpureus oil prepared by the preparation method of the present invention has the advantages of being odorless and light in color, which increases its adaptability in daily chemical products. The composition formula of the selected mixed soil and the processing temperature will affect the color and odor of the pruinosa purpureus oil.

[0090] Test Example 3

[0091] Color protection efficacy test:

[0092] 1. Test purpose: To test the color difference of dyed hair using a colorimeter and evaluate the effect of clavatica arborvitae oil on hair color protection.

[0093] 2. Test samples:

[0094] Control group: shampoo blank matrix (10% sodium lauryl ether sulfate aqueous solution)

[0095] Sample group: Shampoo containing 1% of the purpureus fruit oil prepared in Examples 1-6 and Comparative Examples 1-6 (99 g of shampoo blank matrix was weighed, and 1 g of purpureus fruit oil was added, stirred evenly, and set aside)

[0096] 3. Test materials:

[0097] Hair bundle specifications: dyed hair bundle 27cm×2.5cm×6g

[0098] 4. Test instruments:

[0099] Colorimeter CHROMA METER CR-400

[0100] 5. Test environment:

[0101] Constant temperature and humidity environment, temperature 21±1℃, humidity 50±10%

[0102] 6. Testing process:

[0103] (1) 39 dyed hair bundles were randomly divided into 13 groups, with 3 bundles in each group. Before the test, the chromaticity value of the hair bundles was measured using a colorimeter tester, and each hair bundle was measured 10 times (before treatment);

[0104] (2) After the measurement is completed, the hair bundles of the sample group are treated with purpureus purpureus oil shampoo at a dosage of about 0.2 g of sample per gram of hair bundle, evenly applied on the hair surface for 1 minute, and then rinsed clean; the hair bundles of the control group are treated with shampoo matrix and the treatment method is the same as the sample group;

[0105] (3) Wash the hair bundles 8 times according to step (2). After washing, place the hair bundles in a constant temperature and humidity environment (temperature 26±2°C; relative humidity 60±10%RH) to dry naturally.

[0106] (4) Use a colorimeter to measure the chromaticity value of the hair bundle, and measure each hair bundle 10 times (after treatment).

[0107] 7. Result analysis:

[0108] L, a, and b are the chromaticity values representing an object's color, or the color space coordinates of that color. L represents lightness and darkness (black and white), a represents red and green, and b represents yellow and blue. A colorimeter automatically compares the color difference between a sample and the object being inspected, outputting three sets of data: L, a, and b, along with the colorimetric delta E (ΔE). Smaller ΔE values indicate better color preservation. The results are shown in Table 5.

[0109] Table 5

[0110] Group Mean color difference Standard error control group 1.0594 0.0954 Example 1 1.0066 0.1229 Example 2 1.0103 0.0857 Example 3 1.0187 0.1455 Example 4 1.0257 0.0986 Example 5 1.0295 0.0889 Example 6 1.0310 0.1369 Comparative Example 1 1.0583 0.1377 Comparative Example 2 1.0502 0.0994 Comparative Example 3 1.0486 0.1232 Comparative Example 4 1.0514 0.1106 Comparative Example 5 1.0492 0.1283 Comparative Example 6 1.0528 0.0897

[0111] From the data results in Table 5, it can be seen that the pruning fruit oil prepared by the preparation method of the present invention has an excellent hair color protection effect, and the selected pressing temperature, the composition formula of the mixed soil and the processing temperature affect the color protection effect.

[0112] Test Example 4

[0113] Thermal protection efficacy test:

[0114] 1. Test Purpose: To observe the condition of the cuticle of damaged hair before and after using the product using a scanning electron microscope, analyze the hair heat absorption curve using a differential scanning calorimeter (DSC), and evaluate the product's effect on improving the hair's heat absorption state.

[0115] 2. Test materials:

[0116] Hair bundle specifications: slightly damaged hair bundle specifications: 17cm×1.5cm×2.5g

[0117] Basic shampoo: shampoo blank matrix (10% sodium lauryl ether sulfate aqueous solution)

[0118] 3. Test instruments:

[0119] Analytical balance, SEM scanning electron microscope, scanning differential thermal analyzer DSC2.1.4

[0120] 4. Test environment:

[0121] Constant temperature and humidity environment, temperature 21±1℃, humidity 50±10%

[0122] 5. Testing process:

[0123] (1) Hair scanning differential thermal analysis (DSC) test process:

[0124] (1.1) Thirty-nine hair bundles were randomly divided into 13 groups, each containing 3 bundles. The following treatments were performed:

[0125] Control group: Mildly damaged hair was washed with basic shampoo and then the surface moisture was wiped dry;

[0126] Sample group: After washing slightly damaged hair with basic shampoo, wipe off the surface moisture. When the hair is half dry, apply the purpureus utilis oil samples prepared in Examples 1-6 and Comparative Examples 1-6 (0.2 g sample per gram of hair) respectively, and massage along the direction of the hair scales for 3 minutes. Do not wash;

[0127] The control group and the sample group were blown with a hair dryer (high temperature, high wind speed, 10 cm away from the hair bundle) for 3 minutes respectively.

[0128] (1.2) Cut the processed hair into pieces of about 1.0 mm.

[0129] (1.3) Use a differential scanning calorimeter (DSC) to measure the DSC curve of the hair and calculate the absorption peak temperature (Td) and average absorption peak area (ΔHd) in the temperature range of 230°C-250°C.

[0130] (2) Hair scale scanning electron microscope testing process:

[0131] (2.1) Take two hair bundles, one for the control group and one for the sample group of Example 1, and perform the following treatments:

[0132] Control group: Mildly damaged hair was washed with basic shampoo and then the surface moisture was wiped dry;

[0133] Sample group: After washing slightly damaged hair with basic shampoo, wipe off the surface moisture. When the hair is half dry, apply the utilitarian fruit oil sample prepared in Example 1 (0.2g sample per gram of hair) and massage along the direction of the hair scales for 3 minutes. Do not wash.

[0134] The control group and the sample group were blown with a hair dryer (high temperature, high wind speed, 10 cm away from the hair bundle) for 3 minutes respectively.

[0135] (2.2) Randomly select 2 hairs from each of the control group and sample group for scanning electron microscopy.

[0136] 6. Result analysis:

[0137] (1) Hair scanning differential scanning calorimetry (DSC) analysis results and analysis

[0138] The DSC curve of hair α-keratin shows an endothermic peak between 230°C and 250°C, labeled the α-helix peak. The peak temperature (Td) is defined as the denaturation temperature of the α-helix peak. The peak area (ΔHd) represents the denaturation enthalpy, which refers to the energy required for denaturation of the α-helix peak (heat absorbed per gram of dry hair). ΔHd is used to calculate RHC (relative helical content): RHC = 100 × (ΔHd sample / ΔHd control)%. The smaller the peak area in the sample, the smaller the RHC, indicating greater α-keratin damage. The mean peak temperature and mean peak area of the hair helix peak are shown in Table 6.

[0139] Table 6

[0140] Group Peak temperature (℃) Peak area (J / g) control group 238.5 11.54 Example 1 237.8 17.34 Example 2 237.9 17.33 Example 3 237.9 17.27 Example 4 238.2 13.88 Example 5 238.6 13.79 Example 6 238.3 13.54 Comparative Example 1 242.2 12.89 Comparative Example 2 245.5 12.05 Comparative Example 3 246.9 12.02 Comparative Example 4 244.4 12.93 Comparative Example 5 243.7 12.85 Comparative Example 6 249.1 12.21

[0141] It can be seen from the data in Table 6 that the pruning fruit oil prepared by the preparation method of the present invention has an excellent effect of protecting hair from heat damage, and the selected pressing temperature, the composition formula of the mixed soil and the processing temperature affect the heat protection effect.

[0142] (2) Scanning electron microscopy test results and analysis of hair scales

[0143] The electron microscope scanning images of the control group are as follows Figure 1-3 As shown (magnifications are 500 times, 1000 times, and 2000 times, respectively); the electron microscope scanning images of the sample group of Example 1 are shown as follows Figure 4-6 As shown (magnifications are 500 times, 1000 times, and 2000 times, respectively).

[0144] As can be seen from the figure, the cuticles of the control group's hair bundles are irregularly arranged, while the cuticles of the sample group's hair bundles are more regularly arranged. The degree of cuticle closure is different between the hair bundles treated with the product and those not treated with the product. This indicates that the utilising the utilising fruit oil prepared in this invention has a repairing effect on the cuticles (cuticle closure) of hair bundles damaged by hair dryers.

[0145] Test Example 5

[0146] Softening and repairing efficacy test:

[0147] 1. Test Purpose: To evaluate the effectiveness of prickle fruit oil in improving combability, detangling, smoothness, and repairing hair scales by testing the dry combing, wet combing, friction, and hair scale conditions of the test sample and control before and after treatment.

[0148] 2. Test samples:

[0149] Control group: cyclopentasiloxane (solvent control);

[0150] Sample group: 98 g of cyclopentasiloxane was weighed, and 2.0 g of the prickle oil prepared in Examples 1-6 and Comparative Examples 1-6 were added respectively, and the mixture was stirred and mixed to prepare a prickle oil sample with a concentration of 2%, which was set aside.

[0151] 3. Test materials:

[0152] Hair bundle specifications: slightly damaged hair bundle (2.5g, 6 inches)

[0153] Basic shampoo (10% sodium lauryl ether sulfate aqueous solution)

[0154] 4. Test instruments:

[0155] Analytical balance; carding instrument (fibra.one); scanning electron microscope (ZEISS sigma500)

[0156] 5. Test environment:

[0157] Constant temperature and humidity environment, temperature 21±1℃, humidity 50±10%

[0158] 6. Testing process:

[0159] (1) Hair pretreatment: Wet the hair at 37.0±2℃, apply 1mL of basic shampoo evenly, rub gently to create rich foam for 1min, remove the oil on the hair surface, rinse at a constant flow rate, comb the hair 10 times on each side with a flat narrow-tooth comb, hang the hair in a constant temperature and humidity chamber for balance, and let it dry naturally.

[0160] (2) Dry combing test:

[0161] (2.1) Thirteen identical hair bundles (2.5 g, 6 inches) were randomly divided into 13 groups;

[0162] (2.2) Treat the hair bundles of the sample group and the control group according to the following method:

[0163] Sample hair bundle treatment method: Add sample to the pre-treated hair bundle at a rate of 0.1g / g, gently rub for 3 minutes, and test after air drying;

[0164] Treatment method for control hair bundles: Add the control to the pre-treated hair bundles at a rate of 0.1g / g sample, rub gently for 3 minutes, and test after air drying;

[0165] (2.3) After completion, hang the hair bundle to dry in a constant temperature and humidity chamber at 21±1°C and 50±10% RH, and allow to air dry.

[0166] (2.4) After natural drying, use fibra.one to measure the dry combing strength and work parameter values of the hair bundle.

[0167] (3) Wet comb test:

[0168] (3.1) Thirteen identical hair bundles (2.5 g, 6 inches) were randomly divided into 13 groups;

[0169] (3.2) Treat the hair bundles of the sample group and the control group according to the following method:

[0170] Sample hair bundle treatment method: Add sample to the pre-treated hair bundle at a rate of 0.1g / g, gently rub for 3 minutes, and test after air drying;

[0171] Treatment method for control hair bundles: Add the control to the pre-treated hair bundles at a rate of 0.1g / g sample, rub gently for 3 minutes, and test after air drying;

[0172] (3.3) After completion, use fibra.one to measure the wet combing strength and work parameter values of the hair bundle.

[0173] (4) Friction test:

[0174] (4.1) Thirteen identical hair bundles (2.5 g, 6 inches) were randomly divided into 13 groups;

[0175] (4.2) Treat the hair bundles of the sample group and the control group according to the following method:

[0176] Sample hair bundle treatment method: Add sample to the pre-treated hair bundle at a rate of 0.1g / g, gently rub for 3 minutes, and test after air drying;

[0177] Treatment method for control hair bundles: Add the control to the pre-treated hair bundles at a rate of 0.1g / g sample, rub gently for 3 minutes, and test after air drying;

[0178] (4.3) After completion, hang the hair bundle in a constant temperature and humidity chamber at 21±1°C and 50±10% RH to balance and air dry. After air drying, use fibra.one to measure the friction work parameter value of the hair bundle.

[0179] (5) Hair scale repair test:

[0180] (5.1) Two identical hair bundles (2.5 g, 6 inches) were randomly divided into a control group and a sample group according to Example 1;

[0181] (5.2) Cut a few hairs from the sample group and the control group before treatment and take electron micrographs (initial values);

[0182] (5.3) Treat the hair bundles of the sample group and the control group according to the following method:

[0183] Sample group hair bundle treatment method: After pre-treatment, add the sample prepared in Example 1 at a sample amount of 0.1g / g, gently rub for 3 minutes, and test after natural drying;

[0184] Treatment method for control hair bundles: Add the control to the pre-treated hair bundles at a rate of 0.1g / g sample, rub gently for 3 minutes, and test after air drying;

[0185] (5.4) After completion, hang the hair bundle to dry in a constant temperature and humidity chamber at 21±1°C and 50±10% RH, and allow to air dry.

[0186] (5.5) After air drying, cut a few hairs from each of the treated sample group and the control group and take electron microscope photos (after using the sample).

[0187] 7. Result analysis:

[0188] The test results of dry combing intensity (J / g), dry combing work (mJ), wet combing intensity (J / g), wet combing work (mJ), and friction work (mJ) of each group are shown in Table 7.

[0189] Table 7

[0190]

[0191]

[0192] It can be seen from the data in Table 7 that the pruning fruit oil prepared by the preparation method of the present invention has excellent hair softening and repairing effects, and the selected pressing temperature, the composition formula of the mixed soil and the processing temperature affect the softening and repairing effects.

[0193] The results of the hair scale repair test for the control group and the sample group of Example 1 are shown in the following figures: Figure 7 and Figure 8 As shown in the figure, the cuticles of normal hair are arranged from root to tip like fish scales from head to tail. When hair is damaged, the tail end of the cuticles will lift up and detach from the hair. The greater the lifting, the more the cuticles open and close. In severe cases, the entire cuticle will fall off the hair. The surface of the cuticle is relatively smooth. In normal hair, the cuticles are tightly arranged on the hair body, giving the hair a smooth and shiny appearance. When the cuticles lift up, open and close, or fall out, the hair becomes rough and loses its luster.

[0194] After the sample group was treated, the opening and closing of the hair scales was smaller, and the hair scales did not fall off; after the control group was treated, there was no obvious change in the opening and closing of the hair scales, and the hair scales did not fall off, indicating that the clavatica oil involved in the present invention has excellent effect of repairing hair scales.

[0195] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the preparation method of the utilitarian fruit oil, the product thereof, and its application in hair products. However, the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments in order to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent replacements of various raw materials in the product of the present invention, addition of auxiliary ingredients, selection of specific methods, etc., are all within the scope of protection and disclosure of the present invention.

[0196] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the scope of protection of the present invention.

[0197] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any appropriate manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A method for preparing prickle fruit oil for hair products, characterized in that: The preparation method comprises the following steps: (1) drying the prickle fruit seeds in a cool and ventilated place; the moisture content of the prickle fruit seeds after drying is 3-5%; (2) pressing the dried pruinosa seeds at a temperature of 15.5-32°C to obtain crude oil; (3) mixing the crude oil obtained in step (2) with acidic clay and diatomaceous earth, heating the mixture at 55-65° C. for 0.5-1.5 h, cooling the mixture to below 25-30° C., and filtering the mixture using a 0.45 μm membrane at 0.2-0.4 MPa to obtain the prickle oil; The usage amount of the acid clay and diatomaceous earth is 2-6% of the mass of the crude oil; the mass ratio of the acid clay and diatomaceous earth is (2-4):

1.

2. the prickle fruit oil that the preparation method of prickle fruit oil according to claim 1 makes.

3. Use of the utilitarian fruit oil according to claim 2 in preparing hair products.

4. The use according to claim 3, characterized in that The hair product is a hair product with color protection effect.

5. The use according to claim 3, characterized in that The hair product is a hair product with the effect of resisting high temperature damage.

6. The use according to claim 3, characterized in that The hair product is a hair product with softening and repairing effects.

Citation Information

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