A method for dewaxing tung oil, its products and applications
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-10
- Publication Date
- 2026-08-14
AI Technical Summary
目前关于山桐子蜡的系统研究仍属空白,特别是在脱蜡工艺优化等产业化应用基础研究领域的不足,直接影响了山桐子油脂的脱蜡工艺及加工副产品的高效开发利用
(1)本发明提供了一种山桐子油的脱蜡方法,可有效提高油得率,并降低山桐子油的蜡含量,提高山桐子油的品质。
Smart Images

Figure CN121343667B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of oil processing technology, and in particular to a dewaxing method for tung oil, its products, and applications. Background Technology
[0002] As a newly emerging woody edible oil, *Vernicia fordii* oil is rich in unsaturated fatty acids such as linoleic acid and oleic acid, and also contains various bioactive components such as tocopherols, sterols, and squalene. It exhibits significant effects in preventing cardiovascular and cerebrovascular diseases and in anti-oxidation, making it a current hot topic in functional oil research. However, this oil is prone to turbidity and precipitation during long-term storage or at low temperatures, a quality deterioration that severely hinders its commercialization. Preliminary research indicates that wax may be a key factor inducing precipitation. Currently, systematic research on *Vernicia fordii* wax is lacking, particularly in basic research on industrial applications such as dewaxing process optimization. This deficiency directly affects the dewaxing process of *Vernicia fordii* oil and the efficient development and utilization of processing by-products. Therefore, developing an efficient dewaxing process for *Vernicia fordii* oil and strategies for the efficient utilization of dewaxing by-products is essential. Summary of the Invention
[0003] The purpose of this invention is to provide a dewaxing method for tung oil, its products, and their applications, in order to solve the problems existing in the prior art.
[0004] To achieve the above objectives, the present invention provides the following solution: One of the technical solutions of the present invention: a method for dewaxing tung oil, comprising the following steps: Crude tung oil is subjected to degumming pretreatment, deacidification pretreatment and decolorization pretreatment in sequence to obtain decolorized tung oil; the decolorized tung oil is heated to melt wax and then cooled to 20-25 ℃ (i.e., room temperature), and then perlite is added to grow crystals; after the crystal growth is completed, it is filtered to obtain dewaxed tung oil and tung oil wax paste.
[0005] Degumming, deacidification, and decolorization pretreatments can remove high-melting-point fatty acids from crude *Vernicia fordii* oil, reducing its viscosity at low temperatures. This promotes wax crystallization and grain growth, thereby increasing oil yield and reducing the wax content in dewaxed *Vernicia fordii* oil. Perlite facilitates wax crystal aggregation and growth and can also adsorb trace impurities and colloids in the oil, thus improving the dewaxing rate. In summary, the dewaxing method of this invention can effectively increase oil yield and reduce wax content.
[0006] Tung oil contains fatty acids with high melting points, which easily crystallize and solidify at lower temperatures. Since the tung oil is not degummed or deacidified, its viscosity increases at low temperatures during dewaxing, which is detrimental to wax crystallization and grain growth. The higher viscosity also reduces fluidity, significantly slowing down filtration and resulting in a relatively high wax content in the final product.
[0007] Furthermore, the temperature at which the wax is heated and melted is 90°C.
[0008] Furthermore, the amount of perlite added is 2-3 wt% of the decolorized tung oil.
[0009] Furthermore, the crystal growth temperature is -5 to 5 °C, and the time is 18 to 30 h.
[0010] Preferably, the amount of perlite added is 2 wt% of the decolorized tung oil; the crystal growth temperature is -5℃ and the time is 18 h.
[0011] Further, the degumming pretreatment step includes: heating the crude tung oil to 60-90 ℃, adding a citric acid solution with a concentration of 0.16 g / mL, mixing well, adding hot distilled water at a mass of 8% of the crude tung oil mass, stirring evenly, and finally adding an EDTA-2Na solution with a concentration of 0.14 mol / L and an SDS (sodium dodecyl sulfate) solution with a concentration of 0.06 mol / L, reacting for 15 min, removing and allowing to stand, and centrifuging at 5000 r / min for 20 min to obtain degummed tung oil.
[0012] Furthermore, the ratio of the crude tung oil, the citric acid solution, the EDTA-2Na solution, and the SDS solution is 25 g:0.4 mL:2 mL:2 mL.
[0013] Furthermore, the temperature of the hot distilled water is 70 °C.
[0014] Further, the deacidification pretreatment step includes: heating the degummed tung oil to 35 ℃, adding a sodium hydroxide solution with a concentration of 0.15 g / mL, and then adding 0.25% sodium hydroxide solution (concentration of 0.15 g / mL) based on the mass of the degummed tung oil as superalkali. Continue stirring for 45 min, remove and let stand, centrifuge at 5000 r / min for 20 min, remove the supernatant oil and wash it with water (water temperature of 60 ℃, added amount of 20 wt% of the degummed tung oil), and rotary evaporate to obtain deacidified tung oil.
[0015] Furthermore, the ratio of the degummed tung oil to the sodium hydroxide solution is 25 g: 2 mL.
[0016] Further, the decolorization pretreatment step includes: heating the deacidified tung oil to 94 ℃, adding activated clay at 17% of the mass of the deacidified tung oil and stirring for 94 min, and then filtering to obtain decolorized tung oil.
[0017] The second technical solution of the present invention: a dewaxed tung oil obtained by the above-mentioned dewaxing method for tung oil.
[0018] The third technical solution of the present invention: a tung oil wax paste obtained by the above-mentioned dewaxing method of tung oil.
[0019] The fourth technical solution of the present invention: a method for refining the above-mentioned *Vernicia fordii* oil and wax paste, comprising the following steps: mixing the *Vernicia fordii* oil and wax paste with hexane, refluxing at 65 °C for 90 min, then filtering while hot, and filtering out insoluble matter after the filtrate cools to 20 °C; dissolving the insoluble matter in isopropanol, refluxing at 80 °C for 30 min, then cooling to 20-25 °C (i.e., room temperature), filtering, and drying to obtain defatted *Vernicia fordii* wax; adding petroleum ether to the defatted *Vernicia fordii* wax, then adding an adsorbent, and heating at 80 °C for 60 min to obtain a primary decolorization product; adding petroleum ether and an adsorbent again to the primary decolorization product, and heating again at 80 °C for 60 min to obtain a secondary decolorization product; filtering and concentrating the secondary decolorization product to obtain decolorized *Vernicia fordii* wax; washing and drying the decolorized *Vernicia fordii* wax to obtain refined *Vernicia fordii* wax.
[0020] This invention addresses the issue that *Vernicia fordii* oil wax paste contains numerous impurities such as moisture, oil, pigments, and odors. It also addresses the characteristics of the wax being unstable, soft, and having a low melting point, which causes it to melt at high temperatures. The invention employs a combined degreasing-decolorizing-deodorizing process, specifically using hexane and isopropanol solvent extraction for degreasing, an adsorbent for decolorizing, and water washing to remove residual solvent odors. The result is a high-purity, low-color refined wax product, achieving excellent wax paste refining results.
[0021] Furthermore, the ratio of the amount of *Vernicia fordii* oil wax paste to the amount of hexane is 1 g: 7 mL.
[0022] Furthermore, the ratio of the insoluble substance to the isopropanol is 1 g: 7 mL.
[0023] Furthermore, the ratio of the defatted tung oil wax to the petroleum ether added each time is 1 g: 20 mL.
[0024] Furthermore, the adsorbent comprises activated carbon and diatomaceous earth in a mass ratio of 3:2.
[0025] Activated carbon can significantly improve the decolorization rate, but its bleaching effect is relatively poor, and powdered activated carbon is difficult to filter. Diatomaceous earth, on the other hand, has a good bleaching effect, and its larger particles make it easier to filter. Using diatomaceous earth and activated carbon in combination can improve decolorization efficiency while reducing the limitations of using a single adsorbent.
[0026] Furthermore, the amount of adsorbent added each time is 5 wt% of the defatted tung oil wax. The dewaxing method for tung oil of the present invention is essentially a dewaxing and refining method for crude tung oil. After obtaining dewaxed tung oil through dewaxing treatment, the dewaxed tung oil can be further deodorized to obtain refined tung oil that can be sold directly.
[0027] The fifth technical solution of the present invention: a refined tung oil wax obtained according to the above-mentioned refining method of tung oil wax paste.
[0028] The sixth technical solution of the present invention: a method for preparing an oleogel, comprising the following steps: The refined tung oil wax was mixed with the base oil and heated until completely dissolved. After cooling to 20-25 ℃ (i.e., room temperature), it was placed at 4±2 ℃ for 24 h to obtain the oil gel.
[0029] Furthermore, the amount of refined tung oil wax added is 12-21 wt% of the base oil.
[0030] Preferably, the amount of refined tung oil wax added is 21 wt% of the base oil.
[0031] The seventh technical solution of the present invention: an oleogel obtained according to the above-described method for preparing oleogel.
[0032] The present invention discloses the following technical effects: (1) The present invention provides a dewaxing method for tung oil, which can effectively improve the oil yield and reduce the wax content of tung oil, thereby improving the quality of tung oil.
[0033] (2) This invention uses decolorized *Vernicia fordii* oil as raw material, and focuses on the dewaxing yield and wax content of the dewaxed *Vernicia fordii* oil. The dewaxing process of *Vernicia fordii* oil was optimized, and the physicochemical properties and main fatty acid content of the dewaxed *Vernicia fordii* oil were tested. The results showed that the optimal dewaxing conditions for *Vernicia fordii* oil were: perlite addition of 2 wt%, crystal growth temperature of -5 ℃, and crystal growth time of 18 h. Under these conditions, the dewaxed *Vernicia fordii* oil yield and wax content were 93.69% and 32.79 mg / kg, respectively. The dewaxed *Vernicia fordii* seed oil obtained by this method has a color of Y6.5, R1.1, which is reddish-brown; an acid value of 0.09 mg KOH / g, less than 3 mg / g; a peroxide value of 0.05 g / 100g, less than 0.25 g / 100g; an iodine value of 129.76 g / 100g, within the range of 125-146 g / 100g; a saponification value of 195.38 mg / g, within the range of 190-205 mg / g; a moisture and volatile matter content of 0.05%, less than 0.1%; and an insoluble impurity content of 0.02%, less than 0.05%. Its transparency and freezing test results meet the standards of the grain and oil industry. The fatty acids are mainly composed of linoleic acid, palmitic acid, oleic acid, palmitoleic acid, stearic acid, linolenic acid, and erucic acid, with linoleic acid being the most abundant.
[0034] (3) This invention employs a two-step method to prepare refined *Vernicia fordii* wax. The final refined *Vernicia fordii* wax has an acid value of 6.48 mg KOH / g, a saponification value of 84.15 mg / kg, and a purity of 95.87%, all lower than rice bran wax but higher than beeswax; its moisture and volatile matter content is 0.55%, and its whiteness value is 34.78, lower than both rice bran wax and beeswax. Differential scanning calorimetry analysis shows that the melting temperature and crystallization temperature of the refined *Vernicia fordii* wax are 84.32 ℃ and 74.64 ℃, respectively, higher than both rice bran wax and beeswax, making it suitable for high-temperature applications. This invention provides a basis for extracting and separating special compounds from *Vernicia fordii* wax and utilizing its byproducts.
[0035] (4) The refined tung oil wax obtained by the present invention can be used as a gelling agent for oleogels and has good thermal stability.
[0036] (5) This invention studies the optimization of the dewaxing process of tung oil, the refining of wax and the application of refined wax in oil gel, providing a certain theoretical basis for the industrial refining of tung oil and the high-value utilization of by-products. Attached Figure Description
[0037] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0038] Figure 1 This is the standard curve for determining the wax content of dewaxed oil using a turbidimeter method in this invention.
[0039] Figure 2 The effect of different crystal growth times (6, 12, 18, 24, 30, 36, 42, 48 h) on the yield and wax content of dewaxed tung oil was investigated in Example 1 under the conditions of crystal growth temperature of 5 ℃ and perlite addition of 2.5 wt%.
[0040] Figure 3 In Example 2, under the conditions of a crystallization time of 24 h and a perlite addition of 2.5 wt%, the effects of different crystallization temperatures (-10, -5, 0, 5, 10, 15, 20 ℃) on the yield and wax content of dewaxed tung oil were investigated.
[0041] Figure 4 In Example 3, under the conditions of crystal growth time of 24 h and dewaxing temperature of 5 ℃, the effects of different perlite addition amounts (1, 1.5, 2, 2.5, 3, 3.5, 4 wt%) on the yield and wax content of dewaxed tung oil were investigated.
[0042] Figure 5 DCS melting and crystallization curves for refined tung oil wax (IPMW), rice bran wax (RBW), and beeswax (BW) are given, where a is the crystallization curve and b is the melting curve.
[0043] Figure 6 The DCS melting and crystallization curves of *Vernicia fordii* wax oil gel and beeswax oil gel are shown, where a is the crystallization curve of *Vernicia fordii* wax oil gel, b is the melting curve of *Vernicia fordii* wax oil gel, c is the crystallization curve of beeswax oil gel, and d is the melting curve of beeswax oil gel. Detailed Implementation
[0044] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.
[0045] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Any stated value or intermediate value within a stated range, as well as each smaller range between any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.
[0046] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.
[0047] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be apparent to those skilled in the art. This specification and embodiments are merely exemplary.
[0048] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.
[0049] It should be noted that any aspects not described in detail in this invention are conventional practices in the field and are not the focus of this invention.
[0050] In the following embodiments and comparative examples of the present invention, room temperature refers specifically to 20-25 °C.
[0051] Unless otherwise specified, all raw materials used in the following embodiments and comparative examples of this invention are commercially available products.
[0052] Example 1 A method for dewaxing tung oil, the steps of which are as follows: (1) Degumming pretreatment Weigh 25 g of crude tung oil, heat the oil to 60 ℃, add 0.4 mL of 0.16 g / mL citric acid solution, mix well, then add hot distilled water (70 ℃) at 8% of the mass of crude tung oil, stir evenly, and finally add 2 mL each of 0.14 mol / L EDTA-2Na solution and 0.06 mol / L SDS solution. React for 15 min, remove and let stand, then centrifuge at 5000 r / min for 20 min to obtain degummed tung oil.
[0053] (2) Deacidification pretreatment Weigh 25 g of degummed tung oil, keep the oil temperature at 35 ℃, add 2 mL of sodium hydroxide solution with a concentration of 0.15 g / mL, and then add 0.25% sodium hydroxide solution (concentration of 0.15 g / mL) based on the mass of the degummed tung oil as the superalkali amount. Continue stirring for 45 min, remove and let stand, centrifuge at 5000 r / min for 20 min, remove the supernatant oil and wash it with water (water temperature at 60 ℃, the amount added is 20 wt% of the degummed tung oil) and rotary evaporate (temperature at 70 ℃) to obtain deacidified tung oil.
[0054] (3) Decolorization pretreatment Weigh a certain amount of deacidified tung oil, heat the oil to 94 ℃, keep it at a constant temperature, add 17% of the mass of the deacidified tung oil and stir for 94 min, then transfer it to a vacuum filtration flask for vacuum filtration to obtain decolorized tung oil.
[0055] (4) Dewaxing treatment Weigh 100 g of decolorized tung oil and place it in a 250 mL beaker. Heat it to 90 °C to melt the wax, then cool it to room temperature. Add a certain amount of perlite and stir for 30 min. Place it in a refrigerator and allow it to crystallize at a certain temperature for a period of time. Then filter it to obtain dewaxed tung oil and tung oil wax paste.
[0056] Under the conditions of crystallization temperature of 5 ℃ and perlite addition of 2.5 wt% of decolorized *Vernicia fordii* oil, the crystallization time was varied to 6, 12, 18, 24, 30, 36, 42, and 48 h, resulting in multiple groups of dewaxed *Vernicia fordii* oil and *Vernicia fordii* oil wax paste. This represents a multi-group single-factor experiment with crystallization time as the variable.
[0057] Example 2 Similar to Example 1, the only difference is that in the dewaxing step, under the conditions of a crystal growth time of 24 h and a perlite addition of 2.5 wt% of the decolorized *Vernicia fordii* oil, the crystal growth temperature was changed to -10, -5, 0, 5, 10, 15, and 20 °C, resulting in multiple groups of dewaxed *Vernicia fordii* oil and *Vernicia fordii* oil wax paste. That is, multiple single-factor experiments were conducted with crystal growth temperature as the variable.
[0058] Example 3 Similar to Example 1, the only difference is that in the dewaxing step, under the conditions of a crystal growth time of 24 h and a dewaxing temperature of 5 ℃, the amount of perlite added was varied to 1, 1.5, 2, 2.5, 3, 3.5, and 4 wt% of the decolorized *Vernicia fordii* oil, resulting in multiple groups of dewaxed *Vernicia fordii* oil and *Vernicia fordii* oil wax paste. That is, multiple single-factor experiments were conducted with the amount of perlite added as the variable.
[0059] Test Example 1 I. Test Items and Test Methods 1. Determination of dewaxed oil yield Weigh the tung oil before and after dewaxing treatment, and calculate the dewaxed oil yield according to formula (1).
[0060] (1) 2. Dewaxing oil wax content determination The wax content of the dewaxed oil was determined by a turbidimeter, and the specific steps are as follows: (1) Raw material preparation Preparation of pure *Vernicia fordii* oil wax: 100g of *Vernicia fordii* oil wax paste (provided by the National Engineering Research Center for Processing and Comprehensive Utilization of *Vernicia fordii* in Forestry and Grassland) was weighed, extracted by Soxhlet extraction in diethyl ether at 55 ℃ for 5 h, and then dried in an oven at 105 ℃ for 1 h to obtain an oil-wax mixture. Five times the volume of butanone was added to the oil-wax mixture and stirred until homogeneous. The mixture was cooled at 0 ℃ for 0.5 h, filtered while cold, and repeated until the filter cake turned white to obtain pure *Vernicia fordii* oil wax.
[0061] Preparation of wax-free refined tung oil: Winterized refined tung oil (provided by the National Engineering Research Center for Processing and Comprehensive Utilization of Tung Oil) was left to stand for 5 days in an environment below 4 ℃, and then filtered three times with double-layer filter paper in a constant temperature oven at 4 ℃ to obtain wax-free refined tung oil.
[0062] (2) Preparation of waxy standard solution Weigh 0.1 g (accurate to 0.0001 g) of pure tung oil wax and add it to 200 g of refined tung oil without wax. Heat to 130 °C. The wax concentration of this solution is 500 mg / kg. Using this as the base solution, wax standard solutions with final concentrations of 50, 100, 150, 200, 250, and 300 mg / kg are prepared by gradually diluting the base solution.
[0063] (3) Plotting the standard curve A 1:1 ratio of wax standard solution to acetone was placed in a colorimetric bottle, totaling 30 mL. After thorough mixing, the mixture was heated in a water bath until clear and then cooled to room temperature. The mixture was then transferred to an ice bath (0 °C) for 5 minutes. The colorimetric bottle was removed from the ice bath, rinsed with acetone, and the outer wall was gently wiped clean. It was then placed at room temperature for 5 minutes. The rinsing and wiping of the outer wall with acetone was repeated. The colorimetric bottle was then placed in a Hach 2100 AN turbidimeter, and the "READ" button was pressed to obtain the measurement results immediately. The readings on the turbidimeter were recorded sequentially for wax standard solutions with wax contents of 50, 100, 150, 200, 250, and 300 mg / kg. A standard curve was plotted based on these readings, and the corresponding regression equation was calculated. Figure 1 As shown.
[0064] (4) Oil sample determination The turbidity of the oil sample to be tested (i.e., dewaxed tung oil) was determined by the method described in (3), and then the standard curve obtained by the method was used to calculate the wax content in the oil sample.
[0065] II. Test Results 1. Effect of crystal growth time on the yield of dewaxed tung oil (i.e., dewaxed oil) and the wax content in dewaxed tung oil. Figure 2 This study investigated the effects of different crystallization times (6, 12, 18, 24, 30, 36, 42, and 48 h) on the yield and wax content of dewaxed *Vernicia fordii* oil under the conditions of a crystallization temperature of 5 °C and a perlite addition of 2.5 wt%. The results showed that the wax content of the dewaxed *Vernicia fordii* oil decreased with increasing crystallization time. The wax content was relatively high at 6 h, and significantly decreased when the crystallization time exceeded 6 h. However, the decrease in wax content was not significant after 24 h. This is because sufficient time is required for crystal nuclei to form large and solid crystals. Therefore, a short crystallization time leads to a high wax content in the dewaxed *Vernicia fordii* oil, while a long dewaxing time prevents crystal growth, resulting in a less significant decrease in wax content. Rapid wax crystallization in the early stages of crystallization caused a sharp drop in oil yield. In the middle stages, the wax separation rate slowed down, and the decrease in oil yield became more gradual. In the later stages, wax separation was essentially complete, and the oil yield tended to stabilize. Taking all factors into consideration, a crystal growth time of 18-30 hours is more appropriate.
[0066] 2. Effect of crystallization temperature on the yield of dewaxed *Vernicia fordii* oil and the wax content in the dewaxed *Vernicia fordii* oil Figure 3 This study investigated the effects of different crystallization temperatures (-10, -5, 0, 5, 10, 15, 20 °C) on the yield and wax content of dewaxed *Vernicia fordii* oil under the conditions of a crystallization time of 24 h and a perlite addition of 2.5 wt%. It can be seen that as the crystallization temperature increases, the wax content in the oil initially decreases and then increases, while the oil yield initially increases and then decreases. At lower temperatures, the oil has high viscosity and poor fluidity, making it difficult for wax crystals to grow sufficiently and resulting in more entrained oil, leading to poor separation, higher wax content, and lower oil yield. As the temperature increases, the oil viscosity decreases, allowing for more complete wax crystal formation and growth, improving separation, reducing wax content, and increasing oil yield. However, excessively high temperatures increase the solubility of wax in the oil, making it difficult for wax crystals to form or redissolve, resulting in poorer separation and a higher wax content. Considering all factors, a crystallization temperature of -5 to -5 °C is more suitable.
[0067] 3. Effect of perlite addition on the yield and wax content of dewaxed *Vernicia fordii* oil. Figure 4 This study examines the effects of different perlite addition amounts (1, 1.5, 2, 2.5, 3, 3.5, 4 wt%) on the yield and wax content of dewaxed *Vernicia fordii* oil under the conditions of a crystal growth time of 24 h and a dewaxing temperature of 5 °C in Example 3. It can be seen that different perlite addition amounts affect the dewaxing effect of *Vernicia fordii* oil. The dewaxed oil yield in *Vernicia fordii* oil decreases with increasing perlite content. The decrease is more significant when perlite content is less than 2.5%, while the change is less pronounced when perlite content is greater than 2.5%. This is because as the amount added continues to increase, the adsorption capacity of perlite gradually becomes saturated, and its adsorption of waxes no longer significantly enhances. Continuously increasing the amount of perlite is not conducive to wax crystallization and precipitation. Furthermore, uneven dispersion of perlite in the system may affect the oil-wax separation effect, leading to some waxes not being effectively separated, thus causing a rebound in wax content and a decrease in oil yield. Excessive perlite can also impart an off-odor to the finished oil. Considering all factors, a perlite addition of 2-3 wt% is more appropriate.
[0068] Example 4 Orthogonal experimental design Based on the single-factor experimental results of Examples 1-3, a three-factor, three-level orthogonal experiment was conducted. The yield of dewaxed *Vernicia fordii* oil and wax content were used as evaluation indicators. Perlite (A), crystal growth temperature (B), and crystal growth time (C) were selected as the factors to be investigated. The L9 (3) model was adopted. 3The experiment was conducted, and the levels of the orthogonal experimental factors are shown in Table 1. The orthogonal experimental design and results are shown in Table 2.
[0069] Table 1 Table 2 The results of the orthogonal experiments show that the crystal growth time is the most significant factor affecting the yield of dewaxed *Vernicia fordii* oil in the dewaxing process. The order of influence of each factor on the yield is C>A>B, i.e., crystal growth time > perlite addition amount > crystal growth temperature. The crystal growth time is the most significant factor affecting the wax content of dewaxed *Vernicia fordii* oil. The order of influence of each factor on the wax content is B>C>A, i.e., crystal growth temperature > crystal growth time > perlite addition amount. The optimal process conditions for the yield of dewaxed *Vernicia fordii* oil are A1B1C1, i.e., perlite addition amount of 2 wt%, crystal growth temperature of -5 ℃, and crystal growth time of 18 h; the optimal process conditions for the wax content of dewaxed *Vernicia fordii* oil are A2B1C1. Verification experiments were conducted under the optimal combination of conditions (repeated three times, and the average result was taken). Under conditions A1B1C1, the yield of dewaxed *Vernicia fordii* oil and the wax content were 93.69% and 32.79 mg / kg, respectively. Under conditions A2B1C1, the yield of dewaxed *Vernicia fordii* oil and the wax content were 93.42% and 26.65 mg / kg, respectively. Considering factors such as oil yield, wax content, and cost, and from the perspective of equipment turnover, the optimal dewaxing process conditions can be determined to be A1B1C1, namely, perlite addition of 2 wt%, crystal growth temperature of -5 ℃, and crystal growth time of 18 h.
[0070] The physicochemical properties of the dewaxed *Vernicia fordii* oil obtained during the verification test under the optimal dewaxing process conditions A1B1C1 were determined and compared with those of the undewaxed oil (i.e., bleached *Vernicia fordii* oil). The results are shown in Table 3.
[0071] The following measurements were taken: color according to GB / T 22460-2008; moisture and volatile matter according to GB 5009.236-2016; insoluble impurities according to GB / T 15688-200; acid value according to GB 5009.229-2016; peroxide value according to GB 5009.227-201; saponification value according to GB / T 5534-2008; iodine value according to GB / T 5532-2022; phospholipid content according to GB / T 5537-2008; oxidation induction time according to GB / T 21121-2007; transparency according to GB / T 5525-2008; and freezing test according to Appendix A of GB / T 17756-1999.
[0072] Table 3 Note: The average of different values in the same row corresponds to P A significant difference of <0.05. Data are expressed as mean "±".
[0073] As shown in Table 3, under the optimal dewaxing conditions, there was no significant difference between the dewaxed and undewaxed *Vernicia fordii* oil. P <0.05), all indicators fully meet the industry standards for tung oil. The dewaxed tung oil has a color of Y6.5 and R1.1; an acid value of 0.09 mg / g, less than 3 mg / g; a peroxide value of 0.05 g / 100g, less than 0.25 g / 100g; an iodine value of 129.76 g / 100g, within the range of 125-146 g / 100g; a saponification value of 195.38 mg / g, within the range of 190-205 mg / g; a moisture and volatile matter content of 0.05%, less than 0.1%; an insoluble impurity content of 0.02%, less than 0.03%; and transparency and freezing test results meet the national standards for freezing tests of animal and vegetable oils.
[0074] The relative fatty acid content of dewaxed *Vernicia fordii* oil obtained during the verification test with the optimal dewaxing process conditions A1B1C1 was determined by gas chromatography, and the results are shown in Table 4.
[0075] Table 4 Note: Different letters in the same row indicate significant differences. p <0.05). C16:0. Palmitic acid; C16:1. Palmitoleic acid; C18:0. Stearic acid; C18:1. Oleic acid; C18:2. Linoleic acid; C18:3. Linolenic acid; C22:1. Erucic acid; UFA. Unsaturated fatty acids; SFA. Saturated fatty acids; MUFA. Monounsaturated fatty acids; PUFA. Polyunsaturated fatty acids.
[0076] As shown in Table 4, the fatty acids are mainly composed of linoleic acid, palmitic acid, oleic acid, palmitoleic acid, stearic acid, linolenic acid, and erucic acid. The saturated fatty acid in dewaxed tung oil is mainly palmitic acid, with a content of 16.01%; the unsaturated fatty acid is mainly linoleic acid, with a content of 68.69%. Dewaxed tung oil is an oilseed with a high linoleic acid content.
[0077] Comparative Example 1 A method for dewaxing tung oil, the steps of which are as follows: Weigh 100 g of crude tung oil and place it in a 250 mL beaker. Heat it to 90 °C to melt the wax, then cool it to room temperature. Add perlite (2.5 wt% of crude tung oil) and stir for 30 min. Place it in a 5 °C freezer for 24 h to grow crystals, then filter to obtain dewaxed tung oil.
[0078] Comparative Example 2 (1) Degumming pretreatment Weigh 25 g of crude tung oil, heat the oil to 60 ℃, add 0.4 mL of 0.16 g / mL citric acid solution, mix well, then add hot distilled water (70 ℃) at 8% of the mass of crude tung oil, stir evenly, and finally add 2 mL each of 0.14 mol / L EDTA-2Na solution and 0.06 mol / L SDS. React for 15 min, remove and let stand, then centrifuge at 5000 r / min for 20 min to obtain degummed tung oil.
[0079] (2) Dewaxing treatment Weigh 100 g of degummed tung oil into a 250 mL beaker, heat to 90 ℃ to melt the wax, cool to room temperature, add perlite (2.5 wt% of the degummed tung oil), stir for 30 min, place in a 5 ℃ freezer for 24 h to grow crystals, and then filter to obtain dewaxed tung oil.
[0080] Comparative Example 3 (1) Degumming pretreatment Weigh 25 g of crude tung oil, heat the oil to 60 ℃, add 0.4 mL of 0.16 g / mL citric acid solution, mix well, then add hot distilled water (70 ℃) at 8% of the mass of crude tung oil, stir evenly, and finally add 2 mL each of 0.14 mol / L EDTA-2Na solution and 0.06 mol / L SDS. React for 15 min, remove and let stand, then centrifuge at 5000 r / min for 20 min to obtain degummed tung oil.
[0081] (2) Deacidification pretreatment Weigh 25 g of degummed tung oil, keep the oil temperature at 35 ℃, add 2 mL of sodium hydroxide solution with a concentration of 0.15 g / mL, then add 0.25% of the oil weight of superalkali, continue stirring for 45 min, remove and let stand, centrifuge at 5000 r / min for 20 min, take out the supernatant oil and wash it with water (water temperature at 60 ℃, the amount added is 20 wt% of the degummed tung oil) and rotary evaporate (temperature at 70 ℃) to obtain deacidified tung oil.
[0082] (3) Dewaxing treatment Weigh 100 g of deacidified tung oil and place it in a 250 mL beaker. Heat it to 90 °C to melt the wax, then cool it to room temperature. Add perlite (2.5 wt% of the deacidified tung oil) and stir for 30 min. Place it in a 5 °C freezer for 24 h to grow crystals, then filter to obtain dewaxed tung oil.
[0083] Test Example 2 Effect of pretreatment process on dewaxing yield and wax content of tung oil The yield and wax content of dewaxed tung oil under different pretreatment processes in Example 1 (crystallization temperature of 5 ℃, perlite addition of 2.5 wt%, and crystallization time of 24 h) and Comparative Examples 1-3 are shown in Table 5 (each group of experiments was repeated three times under the corresponding conditions, and the results were averaged).
[0084] Table 5 Table 5 shows that the yield and wax content of dewaxed *Vernicia fordii* oil differed significantly depending on the pretreatment process before dewaxing. Example 1 showed a higher oil yield, while Comparative Examples 1-3 showed lower yields. This may be because the oils that were not degummed, deacidified, or decolorized contained more gum and impurities, and had higher viscosity at low temperatures, resulting in poor filtration and a slightly lower yield. Comparative Examples 1-2 had higher wax content, possibly because *Vernicia fordii* oil contains fatty acids with high melting points. These fatty acids easily crystallize and solidify at lower temperatures. During low-temperature dewaxing, the lower temperature of the untreated *Vernicia fordii* oil is unfavorable for wax crystallization and grain growth, and the higher oil viscosity reduces fluidity, thus significantly reducing the filtration speed and resulting in a higher final wax content. In Examples 1 and Comparative Example 3, the wax content was significantly reduced after degumming and deacidification pretreatment. To obtain a higher dewaxed oil yield and improve dewaxing efficiency, this invention arranges the dewaxing process after degumming and decolorization to reduce the impact of gums and other substances on the dewaxing effect.
[0085] Example 6 A method for refining tung oil and wax paste, the steps of which are as follows: (1) Degreasing treatment First, a certain amount of *Vernicia fordii* oil wax paste containing the filter aid perlite (a byproduct wax paste obtained during the verification test of the optimal dewaxing process conditions A1B1C1 in Example 5) was placed in a round-bottom flask. Hexane (the ratio of *Vernicia fordii* oil wax paste to hexane was 1:7 w / v) was added at 65 °C, and the mixture was refluxed for 90 min. The hot solution was filtered to remove insoluble particles or the filter aid. Then, the filtrate was cooled to 20 °C, and the insoluble matter was filtered out. This insoluble matter (50 g) was dissolved in isopropanol (350 mL) and refluxed at 80 °C for 30 min. The contents were cooled to room temperature, and the insoluble wax crystals were filtered out using a Buchner funnel. After drying, defatted *Vernicia fordii* wax was obtained.
[0086] (2) Decolorization treatment Accurately weigh a certain amount of defatted *Vernicia fordii* wax and place it in a round-bottom flask. Add petroleum ether (the ratio of defatted *Vernicia fordii* wax to petroleum ether is 1:20 w / v), then add 5% by weight of adsorbent (a mixture of activated carbon and diatomaceous earth in a mass ratio of 3:2). Heat at 80 °C for 60 min to obtain a first decolorization product. Add petroleum ether (the ratio of defatted *Vernicia fordii* wax to petroleum ether is 1:20 w / v) and 5% by weight of adsorbent (a mixture of activated carbon and diatomaceous earth in a mass ratio of 3:2) to the first decolorization product again, and heat at 80 °C for 60 min again (i.e., decolorization is performed twice) to obtain a second decolorization product. Filter the second decolorization product while keeping it at a constant temperature, concentrate the filtrate under vacuum, and pour the obtained wax into a transparent petri dish. Allow it to solidify completely to obtain the decolorized *Vernicia fordii* wax solid.
[0087] (3) Deodorization treatment The decolorized tung oil wax was washed with distilled water to remove the odor of petroleum ether. After drying, a tasteless, light yellow fine powder was obtained, which is the refined tung oil wax.
[0088] Test Example 3 I. Test Items and Test Methods 1. Determination of basic indicators of wax (1) Acid value: Weigh 2 g (accurate to 0.0001 g) of sample into a flask, add 25 mL of ethanol and heat for 2 h under normal stirring until clear and transparent. Use phenolphthalein as an indicator and titrate the mixture with standard KOH methanol solution (0.1 N) until pink color is observed. Stop titrating. Use the test group without any wax as a blank. The blank is also performed in the same way. Calculate the acid value based on the amount of KOH methanol solution used for the sample and blank titration. The calculation formula is shown in formula (2).
[0089] (2) In the formula: V - The volume of standard KOH methanol solution used for sample determination, in mL; V0 – The volume of standard KOH methanol solution used in the blank determination, in mL; C - The accurate concentration of the standard KOH methanol solution used, in mol / L; m - Mass of the sample, in g; 56.1 - Molar mass of potassium hydroxide, g / mol.
[0090] (2) Saponification value: Accurately weigh 2 g (accurate to 0.0001 g) of sample into a flask, add 40 mL of KOH ethanol solution (0.5 N), mix and reflux for 2 h to promote saponification, then use phenolphthalein as an indicator and titrate the solution with standard hydrochloric acid solution (0.5 N) until the pink color disappears. The blank is also done in the same way. Calculate the saponification value according to the amount of standard hydrochloric acid solution used for the sample and blank titration. The calculation formula is shown in formula (3).
[0091] (3) In the formula: I s -Saponification value, expressed as KOH, in milligrams per gram (mg / g). V0 - The volume of hydrochloric acid standard solution consumed in the blank determination, in milliliters (mL). V1 - The volume of hydrochloric acid standard solution consumed in the sample determination, in milliliters (mL). The actual concentration of c-hydrochloric acid standard solution is expressed in moles per liter (mol / L). m - the mass of the sample, expressed in grams (g).
[0092] (3) Purity: The purity was determined according to the method of Zhou Yuankai et al., and the purity of refined tung oil wax was calculated according to formula (4): (4) In the formula: P - Purity, % W0 - Mass of the sample weighed, in g; W1 - Mass of the sample dried to constant weight, in g.
[0093] (4) Whiteness detection A certain amount of solid wax sample was melted into a tin foil cup with a diameter of 8 cm. After natural cooling, a circular solid wax sample with a thickness of about 1.5 cm was obtained, and its whiteness was tested. After calibrating the colorimeter, the L*, a*, and b* values of the wax were measured, and the whiteness (WI) was calculated using formula (5): (5) In the formula: WI-whiteness; L* - Brightness index; a*, b* - chromaticity.
[0094] (5) Thermal stability The thermal properties of the wax were measured using differential scanning calorimetry (DSC). 7 mg of wax was accurately weighed and placed in an aluminum pan, with a blank aluminum pan serving as a control. The sample was heated from 20 °C to 150 °C at a rate of 10 °C / min and held at 150 °C for 5 minutes. The sample was then cooled to 20 °C at a rate of 10 °C / min, held for 5 minutes, and reheated to 150 °C. This cycle was repeated twice, and the thermal behavior of the wax was analyzed in the second cycle to eliminate the influence of thermal history. The melting point of the wax was expressed as an endothermic peak, and the enthalpy of melting and crystallization could be calculated from the heating curve of the endothermic plot, which could explain the integral of the heat flow curve.
[0095] II. Test Results 1. Basic Indicators Table 6 shows a comparison of the basic properties of the refined tung oil wax prepared in Example 6 with those of commercially available rice bran wax and commercially available beeswax.
[0096] Table 6 Note: The average of different values in the same row corresponds to P A significant difference of <0.05. Data are expressed as mean "±".
[0097] Table 6 shows that the acid value of refined *Vernicia fordii* wax is lower than that of plant-based rice bran wax but higher than that of animal-based beeswax. Acid value can be used as an indicator of free fatty acid (FFA) content, indicating that the FFA content of refined *Vernicia fordii* wax is lower than that of rice bran wax but higher than that of beeswax. The saponification value of wax can be used as an indicator of ester bonds in the sample and describes the average molecular weight and concentration of fatty acid methyl esters (FAMEs) in the sample. The saponification value of refined *Vernicia fordii* wax is lower than that of rice bran wax but higher than that of beeswax. The ester bonds in FAMEs are larger, and the average molecular weight of fatty acids is lower, indicating that the molecular weight of refined *Vernicia fordii* wax is lower than that of rice bran wax but higher than that of beeswax. The purity of refined *Vernicia fordii* wax is higher than that of rice bran wax and beeswax. Higher purity often means lower impurity content, and high-purity wax can better perform its functions. The whiteness of refined *Vernicia fordii* wax is similar to that of rice bran wax, while beeswax has the highest whiteness. Overall, the base color of refined *Vernicia fordii* wax is not significantly different from that of commercially available plant and animal waxes.
[0098] 2. Analysis of thermodynamic properties Figure 5 DCS melting and crystallization curves for refined tung oil wax (IPMW), rice bran wax (RBW), and beeswax (BW) are shown, where a is the crystallization curve and b is the melting curve. Their initial temperatures (T) are also shown. OCThe data for Tce, Tom, Tme, peak temperature (Tcp and Tmp), and enthalpy (ΔHc and ΔHm) are shown in Table 7.
[0099] Table 7 Note: Values are displayed as the mean ± standard deviation of three replicates. Values with different lowercase letters in the same column may differ significantly. p <0.05).
[0100] Phase transitions in waxes are a complex phenomenon, transforming them into different states with varying temperatures. The thermal properties of waxes, such as melting and crystallization transitions, can be precisely determined using DSC thermal analysis. The composition and molecular weight of a specific wax significantly influence its thermal stability. Studies have shown that waxes may contain shear and thermal histories, thus affecting the results obtained from DSC thermal analysis. The analysis uses two heating cycles and one cooling cycle. The second heating cycle is used to study the melting properties of waxes, obtaining the onset and peak temperatures of the melting and crystallization cycles. Due to differences in wax composition, the onset and peak temperatures of the crystallization or melting peaks also differ. Figure 5 As shown, the crystallization and melting curves of *Vernicia fordii* wax, rice bran wax, and beeswax are very similar in shape. The T-wave curves of *Vernicia fordii* wax and rice bran wax are... OC Tcp, ΔH C Tom, Tmp, and ΔHm are closer together; *Vernicia galbana* wax, rice bran wax, and beeswax all have two crystallization peaks: *Vernicia galbana* wax at 58.44 ℃ and 74.45 ℃; rice bran wax at 56.07 ℃ and 71.04 ℃; and beeswax at 33.24 ℃ and 48.66 ℃, indicating the presence of multiple crystalline phases or crystal form transformations. *Vernicia galbana* wax has the highest crystallization temperature, followed by rice bran wax. This may be because the n-alkanes in the waxes increase the crystallization temperature, while the formation of microlattices can reduce the crystallization transformation. During the melting process, the melting peak temperature of tung oil wax was 84.58 ℃, that of rice bran wax was 81.13 ℃, and that of beeswax was 59.23 ℃. Tung oil wax had the highest melting temperature, followed by rice bran wax, and then beeswax. The melting temperatures of tung oil wax and rice bran wax were both above 70 ℃, mainly due to their chemical composition, complex crystal lattice arrangement, and polydispersity. The higher melting temperature may be due to the higher number of carbon atoms in the molecules composed of rings or long branches in both waxes.
[0101] Example 7 An oleogel is prepared by the following steps: Using cold-pressed tung oil (prepared in the laboratory) as the base oil, a certain amount of refined tung wax (prepared in Example 6) and beeswax (added at 1, 3, 6, 9, 12, 15, 18, and 21 wt% of the base oil) were accurately weighed and dispersed in the base oil. The sample was stirred and heated until the wax was completely dissolved. The mixture was placed in a glass container, cooled to room temperature, and then placed in a refrigerator at 4±2 ℃ for 24 h. The prepared sample could be stored at 4±2 ℃ until analysis.
[0102] Test Example 4 Thermodynamic analysis of olegels The crystallization and melting thermodynamic behaviors of olegels have a significant impact on their processing properties, functional properties, and stability. Differential scanning calorimetry (DSC) was used to determine the thermal properties of the prepared olegels in the range of 0–100 °C, such as… Figure 6 As shown in the figure, a is the crystallization curve of the *Vernicia fordii* wax oil gel, b is the melting curve of the *Vernicia fordii* wax oil gel, c is the crystallization curve of the beeswax oil gel, and d is the melting curve of the beeswax oil gel. The initial temperature (Toc and Tom), peak temperature (Tc and Tm), and enthalpy (ΔHc and ΔHm) data of the oil gel are shown in Table 8.
[0103] Table 8 Note: Values are displayed as the mean ± standard deviation of three replicates. Values with different lowercase letters in the same column are significantly different. p <0.05).
[0104] Thermal behavior analysis results showed that the crystallization peaks of the *Vernicia fordii* wax oil gel were two peaks and one melting peak. The two crystallization peaks are likely due to the influence of *Vernicia fordii* wax; minor components (fatty alcohols) as impurities may reduce the crystallinity of the oil gel. Beeswax oil gel, on the other hand, showed only one crystallization peak and one melting peak. With increasing wax content, Toc, Tc, Tom, and Tm gradually increased. pThe value <0.05 indicates that the wax concentration has a significant impact on the thermal behavior of the oleogel. When the concentration of *Vernicia fordii* wax increased from 12% to 21%, the crystallization temperature, melting temperature, and enthalpy (ΔHc and ΔHc) of the *Vernicia fordii* wax oleogel were 45.68~48.31 ℃, 74.67~77.35 ℃, 15.41±0.11~27.42 J / g, and 15.33~26.70 J / g, respectively. The Tc, Tm, ΔHc, and ΔHm of the *Vernicia fordii* wax oleogel were all higher than those of beeswax. When the beeswax concentration increased from 9% to 21%, the crystallization temperature, melting temperature, and enthalpy (ΔHc and ΔHm) of the beeswax oleogloss were 45.51–49.38 °C, 47.48–54.15 °C, 5.58–5.36 J / g, and 11.06–8.13 J / g, respectively. With increasing beeswax concentration, Tc, Tm, ΔHc, and ΔHm of the beeswax oleogloss all increased because the beeswax base corresponds to the effect of free fatty alcohols and wax esters in the vegetable oil. Since all *Vernicia fordii* wax oleoglosses exhibited higher exothermic and endothermic enthalpies at higher *Vernicia fordii* wax concentrations, it indicates that *Vernicia fordii* wax oleoglosses can be used to prepare oleoglosses with similar thermal behavior to natural wax-based oleoglosses.
[0105] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims
1. A method for dewaxing and refining crude tung oil to obtain dewaxed tung oil and refined tung wax, characterized in that, Includes the following steps: Crude tung oil is subjected to degumming pretreatment, deacidification pretreatment and decolorization pretreatment in sequence to obtain decolorized tung oil; the decolorized tung oil is heated to melt wax and then cooled to 20-25°C, and then perlite is added to grow crystals; after the crystal growth is completed, it is filtered to obtain dewaxed tung oil and tung oil wax paste. The temperature for heating and melting the wax is 90°C; The amount of perlite added is 2 wt% of the decolorized tung oil; The crystal growth temperature is -5℃ and the time is 18h; The degumming pretreatment steps include: heating the crude tung oil to 60-90℃, adding a citric acid solution with a concentration of 0.16g / mL, mixing well, adding hot distilled water at a mass of 8% of the crude tung oil mass, stirring evenly, and finally adding an EDTA-2Na solution with a concentration of 0.14mol / L and an SDS solution with a concentration of 0.06mol / L, reacting for 15min, removing and allowing to stand, and centrifuging at 5000r / min for 20min to obtain degummed tung oil; The *Vernicia fordii* oil wax paste was mixed with hexane and refluxed at 65°C for 90 min. The mixture was then filtered while hot, and the insoluble matter was filtered out after the filtrate cooled to 20°C. The insoluble matter was dissolved in isopropanol and refluxed at 80°C for 30 min. The mixture was then cooled to 20-25°C, filtered, and dried to obtain defatted *Vernicia fordii* wax. Petroleum ether was added to the defatted *Vernicia fordii* wax, followed by an adsorbent. The mixture was heated at 80°C for 60 min to obtain a primary decolorizing product. Petroleum ether and an adsorbent were added again to the primary decolorizing product, and the mixture was heated again at 80°C for 60 min to obtain a secondary decolorizing product. The secondary decolorizing product was filtered and concentrated to obtain decolorized *Vernicia fordii* wax. The decolorized *Vernicia fordii* wax was washed and dried to obtain refined *Vernicia fordii* wax.
2. The method as described in claim 1, characterized in that, The ratio of the amount of *Vernicia fordii* oil wax paste to the amount of hexane is 1 g: 7 mL; And / or, the ratio of the insoluble matter to the isopropanol is 1 g: 7 mL; And / or, the ratio of the defatted tung oil wax to the amount of petroleum ether added each time is 1g:20mL; And / or, the adsorbent comprises activated carbon and diatomaceous earth in a mass ratio of 3:2; And / or, the amount of adsorbent added each time is 5 wt% of the defatted tung oil wax.
3. A dewaxed tung oil obtained by the method according to claim 1.
4. A refined tung oil wax obtained by the method according to any one of claims 1-2.
5. A method for preparing an oleogel, characterized in that, Includes the following steps: The refined tung oil wax as described in claim 4 is mixed with a base oil, heated until completely dissolved, cooled to 20-25°C, and then placed at 4±2°C for 24 hours to obtain the oil gel.
6. The method for preparing oleogel as described in claim 5, characterized in that, The amount of refined tung oil wax added is 12-21 wt% of the base oil.
7. An oleogel obtained by the method for preparing an oleogel according to any one of claims 5-6.
Citation Information
Patent Citations
Method for refining plant oil wax
CN106929160A
Peanut oil and preparation method thereof
CN107955703A
Method for preparing idesia oil Pickering emulsion
CN118766078A
The invention relates to a beta-apos-containing compound. Preparation method of crystalline woody oil-based oleogel
CN120753314A