Polyethylene glycol glycerol ricinoleate granules as well as preparation method and application thereof

Abstract

The invention relates to polyethylene glycol glycerol ricinoleate granules as well as a preparation method and application thereof. The granules comprise first polyethylene glycol glycerol ricinoleate with an HLB (Hydrophile-Lipophile Balance) value of 17-19, second polyethylene glycol glycerol ricinoleate with an HLB value of 12-14, a carrier and vitamin E acetate. According to the invention, fatty acid and / or hydrogenated vegetable oil are / is taken as a nutritional carrier, and polyethylene glycol glycerol ricinoleate with an HLB value of 12-14 is introduced, so that the dispersity of active ingredients with a high HLB value (17-19) in the carrier is effectively improved, and granulation is facilitated; meanwhile, the vitamin E acetate is added, so that the immunity of animals can be enhanced while the effects of resisting oxidation and prolonging the shelf life of the product are achieved. The granules solve the problems that pure products are not easy to mix, inconvenient to use and the like.

Description

Technical Field

[0001] This invention relates to the field of emulsifier technology, specifically to a polyethylene glycol glycerol ricinoleate granule, its preparation method, and its application. Background Technology

[0002] Polyethylene glycol glycerol ricinoleate is a nonionic surfactant with excellent emulsifying, dispersing, and solubilizing properties, and is widely used in the feed, pharmaceutical, cosmetic, and food industries. Its pure form is typically a white paste or pale yellow solid, exhibiting certain stability at room temperature. However, in practical applications, especially in the field of feed additives, pure polyethylene glycol glycerol ricinoleate has significant limitations, severely restricting its industrial promotion and application.

[0003] On the one hand, because the recommended addition amount of polyethylene glycol glycerol ricinoleate in feed is low, and its pure form is a paste or block solid with poor flowability, it easily adheres to the equipment walls during production, making it difficult to achieve uniform mixing with the feed matrix. Uneven distribution of active ingredients not only affects the stability and feeding effect of the final product, but may also lead to quality risks due to excessively high or low content in some areas, while also causing a decrease in additive utilization.

[0004] On the other hand, this substance is temperature-sensitive, with a melting point of approximately 45°C. In high-temperature environments (such as summer) or under the influence of production heat sources, the pure product is prone to softening, sticking together, or even agglomerating into spheres, leading to problems such as inconvenience in handling, poor weighing accuracy, and difficulties in process operation. Agglomeration further exacerbates uneven mixing, significantly impacting production efficiency and batch-to-batch consistency.

[0005] Currently, whey powder and soy protein are commonly used as carriers to pretreat polyethylene glycol glycerol ricinoleate to improve its processing characteristics. However, this method still has several significant shortcomings: First, the carrier and the active ingredient are prone to segregation during transportation and storage due to differences in physical properties, leading to decreased uniformity and unstable distribution of the active ingredient; second, the product generates a lot of dust during processing and use, which not only leads to material loss and reduced yield, but also poses occupational health hazards and challenges to the cleanliness of the production environment.

[0006] Therefore, there is an urgent need to develop a method that can significantly improve the flowability, dispersibility and thermal stability of polyethylene glycol glycerol ricinoleate, while ensuring ease of use and strong process adaptability to meet the application requirements of feed and other industrial fields.

[0007] The above background information is provided only to aid in understanding the concept and technical solution of this application. It does not necessarily belong to the prior art of this application, nor does it necessarily provide technical guidance. In the absence of clear evidence that the above information was disclosed before the filing date of this application, the above background information should not be used to evaluate the novelty and inventiveness of this application. Summary of the Invention

[0008] The purpose of this invention is to provide a polyethylene glycol glycerol ricinoleate granule, its preparation method and application, wherein the polyethylene glycol glycerol ricinoleate granule has good flowability, thermal stability and uniformity.

[0009] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0010] This invention provides a polyethylene glycol glycerol ricinoleate granule, which, based on 100% of the total mass of the polyethylene glycol glycerol ricinoleate granules, comprises:

[0011] First, polyethylene glycol glycerol ricinoleate 15%–65%, with an HLB value of 17–19;

[0012] The second polyethylene glycol glycerol ricinoleate is 1% to 5%, with an HLB value of 12 to 14;

[0013] The carrier comprises 30% to 80% fatty acids and / or hydrogenated vegetable oils, wherein the fatty acids are selected from one or more of C16 to C20 fatty acids;

[0014] Vitamin E acetate 0.01%–0.1%.

[0015] Polyethylene glycol glycerol ricinoleate (HLB value 17-19) is an excellent nutritional emulsifier suitable for monogastric animals. Compared with lecithin and bile acids, it exhibits superior stability, stronger hydrophilicity, and good biodegradability. This invention uses fatty acids and / or hydrogenated vegetable oils as carriers to prepare polyethylene glycol glycerol ricinoleate into granules to improve its application performance. This type of carrier not only has good carrying capacity and process adaptability, but also provides animals with essential energy and lipid nutrition, achieving an upgrade from a simple physical carrier to a functional nutritional carrier, significantly enhancing the added value of the product.

[0016] However, direct granulation of polyethylene glycol glycerol ricinoleate (PEG) with an HLB value of 17–19 presents certain difficulties due to its poor dispersibility in fatty acid or hydrogenated vegetable oil carriers. To overcome this problem, the applicant added PEG with an HLB value of 12–14, which forms a "molecular bridge" between the high-HLB PEG with glycerol ricinoleate and the carrier, enhancing the dispersion uniformity and compatibility of the high-HLB PEG with glycerol ricinoleate in the carrier. This lays an important foundation for improving the operability of subsequent granulation processes and the quality of the finished product.

[0017] Furthermore, this invention incorporates vitamin E acetate into the formulation. On one hand, it functions as an antioxidant, delaying product oxidation and extending shelf life; on the other hand, it can scavenge free radicals in animals, helping to maintain a healthy immune system and further enhancing the overall value of the product.

[0018] In some embodiments, based on the total mass of the polyethylene glycol glycerol ricinoleate granules as 100%, it comprises:

[0019] First, polyethylene glycol glycerol ricinoleate 15%–45%;

[0020] Second polyethylene glycol glycerol ricinoleate 1%–5%;

[0021] Carrier 50%–80%;

[0022] Vitamin E acetate 0.01%–0.1%.

[0023] In some preferred embodiments, the polyethylene glycol glycerol ricinoleate granules, based on a total mass of 100%, comprise:

[0024] First, polyethylene glycol glycerol ricinoleate 15%–25%;

[0025] Second polyethylene glycol glycerol ricinoleate 1%–5%;

[0026] Carrier 70%–80%;

[0027] Vitamin E acetate 0.01%–0.1%.

[0028] In some embodiments, the fatty acid is a saturated fatty acid, or a mixture of saturated and unsaturated fatty acids. When the fatty acid is a mixture of fatty acids and unsaturated fatty acids, the saturated fatty acid accounts for 75% or more of the total mass of the mixture. Further, the saturated fatty acid is selected from palmitic acid and stearic acid; the unsaturated fatty acid is an octadecanoic unsaturated fatty acid.

[0029] In some embodiments, the hydrogenated vegetable oil is a fully hydrogenated vegetable oil, i.e., a mixture of triglycerides composed of saturated fatty acids.

[0030] In some embodiments, the median particle size of the polyethylene glycol glycerol ricinoleate granules is 300 μm to 400 μm.

[0031] A second aspect of the present invention is to provide a method for preparing polyethylene glycol glycerol ricinoleate granules, comprising the following steps:

[0032] S1. Mix the first polyethylene glycol glycerol ricinoleate, the second polyethylene glycol glycerol ricinoleate and the carrier at 60-80°C, stir until uniform, add vitamin E acetate, continue stirring until uniform, obtain the mixture, and keep warm.

[0033] S2. The mixture is fed into a granulation tower for spray granulation, and the inlet air temperature is controlled to be no higher than 20°C to obtain polyethylene glycol glycerol ricinoleate granules.

[0034] In some embodiments, the preparation method further includes the steps of cooling, collecting, and sieving the obtained polyethylene glycol glycerol ricinoleate granules.

[0035] A third aspect of the present invention is to provide an application of the polyethylene glycol glycerol ricinoleate granules as described above, the application comprising adding the polyethylene glycol glycerol ricinoleate granules to feed.

[0036] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art:

[0037] This invention provides a polyethylene glycol glycerol ricinoleate granule formulation, using fatty acids and / or hydrogenated vegetable oil as a nutrient carrier. By introducing polyethylene glycol glycerol ricinoleate with an HLB value of 12-14, the dispersibility of high HLB value (17-19) active ingredients in the carrier is effectively improved, facilitating granulation. Simultaneously, the addition of vitamin E acetate not only provides antioxidant effects and extends product shelf life but also enhances animal immunity. This granule formulation solves the problems of difficulty in mixing and inconvenience in use associated with pure products. Attached Figure Description

[0038] Figure 1 The images show the actual effects of emulsification experiments conducted independently with oils using the granules, lysophosphatidylcholine, and bile acids in Example 1. Detailed Implementation

[0039] The present invention will be further described below with reference to embodiments. However, the present invention is not limited to the following embodiments. The implementation conditions used in the embodiments can be further adjusted according to different requirements of specific applications, and the implementation conditions not specified are conventional conditions in the industry. The technical features involved in the various embodiments of the present invention can be combined with each other as long as they do not conflict with each other.

[0040] Unless otherwise specified, the raw materials used in the following examples and comparative examples are all commercially available products.

[0041] Unless otherwise specified, “parts” in the following text refers to parts by weight.

[0042] Example 1: This example provides a polyethylene glycol glycerol ricinoleate granule, the preparation method of which includes the following steps:

[0043] (1) Weigh out 20 parts of polyethylene glycol glycerol ricinoleate (HLB value 18, purchased from Norinon, brand name Blido 688), 2 parts of polyethylene glycol glycerol ricinoleate (HLB value 13-14, purchased from Norinon, brand name Blido 694), 0.05 parts of vitamin E acetate and 77.95 parts of fatty acid (purchased from Dongma Oils, batch number 231220PK2D, main component is palmitic acid) for later use.

[0044] (2) Mix the two types of polyethylene glycol glycerol ricinoleate and fatty acid at 60°C, stir evenly, add vitamin E acetate, continue stirring to mix evenly, and then keep the mixture at 70°C±2°C.

[0045] (3) The mixture obtained in step (2) is transported to a granulation tower for spray granulation, and the air inlet temperature is controlled at 20°C.

[0046] (4) The granules obtained in step (3) are cooled, collected, passed through a 20-mesh sieve, and finally packaged to obtain polyethylene glycol glycerol ricinoleate granules.

[0047] Example 2: This example provides a polyethylene glycol glycerol ricinoleate granule, which is largely the same as Example 1, except that the amount of each material is different.

[0048] In this embodiment, there are 40 parts of polyethylene glycol glycerol ricinoleate (HLB value 18), 2 parts of polyethylene glycol glycerol ricinoleate (HLB value 13-14), 0.05 parts of vitamin E acetate, and 57.95 parts of fatty acids.

[0049] Example 3: This example provides a polyethylene glycol glycerol ricinoleate granule, which is largely the same as Example 1, except that the amount of each material is different.

[0050] In this embodiment, there are 60 parts of polyethylene glycol glycerol ricinoleate (HLB value 18), 2 parts of polyethylene glycol glycerol ricinoleate (HLB value 13-14), 0.05 parts of vitamin E acetate, and 37.95 parts of fatty acids.

[0051] Comparative Example 1: This comparative example provides a polyethylene glycol glycerol ricinoleate formulation, which is largely the same as that in Example 1, except that the amount of each material is different.

[0052] In this comparative example, there were 20 parts of polyethylene glycol glycerol ricinoleate (HLB value 18), 20 parts of polyethylene glycol glycerol ricinoleate (HLB value 13-14), 0.05 parts of vitamin E acetate, and 59.95 parts of fatty acids.

[0053] Comparative Example 2: This comparative example provides a polyethylene glycol glycerol ricinoleate formulation, which is substantially the same as that in Example 1, except that an equal amount of docosahexaenoic acid is used to replace the fatty acid.

[0054] Comparative Example 3: This comparative example provides a polyethylene glycol glycerol ricinoleate formulation, which is substantially the same as that in Example 1, except that an equal amount of caprylic acid is used to replace fatty acids.

[0055] Comparative Example 4: This comparative example provides a polyethylene glycol glycerol ricinoleate formulation, which is largely the same as that in Example 1, except that the amount of each material is different.

[0056] In this comparative example, there were 87.95 parts of polyethylene glycol glycerol ricinoleate (HLB value 18), 2 parts of polyethylene glycol glycerol ricinoleate (HLB value 13-14), 0.05 parts of vitamin E acetate, and 10 parts of fatty acids.

[0057] Performance testing:

[0058] 1. Physical properties of particles

[0059] Formation status: Randomly select a representative sample of 100g from the finished product and place it in an observation dish to observe the overall shape of the granules. When the granules are uniform and plump, with almost no dust or lumps, the granules are well-formed; when the granules are basically formed, with a small amount of fine powder or lumps, the granules are relatively well-formed; when the granules are basically formed, with a large amount of fine powder or lumps, the granules are generally well-formed; when the product is mainly a mixture of a large amount of fine powder or irregular lumps, it is difficult to form granules; when granules cannot be obtained, and the product is entirely in the form of paste, mud, or completely loose powder, it is difficult to form.

[0060] Color: Under a standard light source (such as a D65 daylight source), the sample is compared with a pre-determined color standard.

[0061] Median particle size: The particle size distribution of the particle population is measured using a laser particle size analyzer, and the average particle size is represented by D50.

[0062] 2. Specific surface area

[0063] The specific surface area is measured using the gas adsorption method; the specific testing method can be found in existing technologies.

[0064] 3. Differential scanning calorimetry (DSC), the test method is in accordance with the existing technology in this field.

[0065] The performance test results of the above embodiments and comparative examples are shown in Table 1 below.

[0066] Table 1

[0067]

[0068] 4. Thermal stability

[0069] The granules from Examples 1 to 3 were placed at 30°C, 40°C, and 50°C respectively, and stored for 48 hours. The physical properties of the granules were then observed.

[0070] Table 2

[0071] Ambient temperature 30℃ Ambient temperature 40℃ Ambient temperature 50℃ Example 1 No change No change Basically unchanged Example 2 No change soften Softened, slightly sticky Example 3 No change Softened, slightly sticky Softening, increased adhesion

[0072] 5. Emulsification performance testing:

[0073] The polyethylene glycol glycerol ricinoleate granules, lysophosphatidylcholine and bile acids from Example 1 were mixed with oil (purchased from a supermarket, brand name Fulinmen soybean oil) and purified water at a mass ratio of 1:50:50 to form an emulsion. The emulsion was poured into a transparent glass bottle or graduated cylinder, sealed, and left to stand at room temperature (25°C) for 1 minute. The phenomena were then observed and recorded.

[0074] The results are as follows Figure 1 As shown, the left, middle, and right images respectively used the polyethylene glycol glycerol ricinoleate granules, lysophosphatidylcholine, and bile acids from Example 1. It can be seen that the polyethylene glycol glycerol ricinoleate granules of the present invention have a superior in vitro emulsification effect on oils.

[0075] 6. Application Testing:

[0076] Six hundred 14-day-old yellow-feathered broiler chickens were randomly divided into three representative groups: a positive control group, a negative control group, and a test group. The chickens were housed in four-layer stacked cages with free access to water and feed throughout the experiment. The positive control group was fed a basal diet, the negative control group received a 30 kcal reduction per chicken per day on top of the basal diet, and the test group received the basal diet plus 250 g / t of polyethylene glycol glycerol ricinoleate granules (Example 1) on top of the basal diet. The experiment lasted 56 days. During the experiment, the feed troughs were emptied before each feeding to ensure the feed was completely used.

[0077] After the experiment, the indicators were measured. Among them:

[0078] Average weight at 56 days = (Total weight of chickens at the end of the period in the group - Initial total weight of chickens in the group) / Total number of chickens.

[0079] The test results are shown in Table 3 below.

[0080] Table 3

[0081] 56-day average weight / g Positive control group 1639.99 negative control group 1604.92 Test group 1641.15

[0082] As shown in Table 3, the polyethylene glycol glycerol ricinoleate granules of the present invention can make fuller use of the energy in the feed, reduce the feed conversion ratio, and save feed costs.

[0083] The present invention has been described in detail above, with the aim of enabling those skilled in the art to understand and implement the invention. However, this description should not be construed as limiting the scope of protection of the invention. All equivalent changes or modifications made in accordance with the spirit and essence of the invention should be included within the scope of protection of the invention.

Claims

1. A polyethylene glycol glycerol ricinoleate granule, characterized in that, Based on 100% of the total mass of polyethylene glycol glycerol ricinoleate granules, it comprises: First, polyethylene glycol glycerol ricinoleate 15%–65%, with an HLB value of 17–19; The second polyethylene glycol glycerol ricinoleate is 1% to 5%, with an HLB value of 12 to 14; The carrier comprises 30% to 80% fatty acids and / or hydrogenated vegetable oils, wherein the fatty acids are selected from one or more of C16 to C20 fatty acids; Vitamin E acetate 0.01%–0.1%.

2. The polyethylene glycol glycerol ricinoleate granules according to claim 1, characterized in that, Based on the total mass of the polyethylene glycol glycerol ricinoleate granules as 100%, it comprises: First, polyethylene glycol glycerol ricinoleate 15%–45%; Second polyethylene glycol glycerol ricinoleate 1%–5%; Carrier 50%–80%; Vitamin E acetate 0.01%–0.1%.

3. The polyethylene glycol glycerol ricinoleate granules according to claim 2, characterized in that, Based on the total mass of the polyethylene glycol glycerol ricinoleate granules as 100%, it comprises: First, polyethylene glycol glycerol ricinoleate 15%–25%; Second polyethylene glycol glycerol ricinoleate 1%–5%; Carrier 70%–80%; Vitamin E acetate 0.01%–0.1%.

4. The polyethylene glycol glycerol ricinoleate granules according to any one of claims 1 to 3, characterized in that, The fatty acid is a saturated fatty acid, or a mixture of saturated and unsaturated fatty acids. When the fatty acid is a mixture of fatty acids and unsaturated fatty acids, the saturated fatty acid accounts for 75% or more of the total mass of the mixture. The saturated fatty acid is selected from palmitic acid and stearic acid; The unsaturated fatty acid is an octadectocarbon unsaturated fatty acid.

5. The polyethylene glycol glycerol ricinoleate granules according to any one of claims 1 to 3, characterized in that, The hydrogenated vegetable oil is a fully hydrogenated vegetable oil.

6. The polyethylene glycol glycerol ricinoleate granules according to claim 1, characterized in that, The median particle size of the polyethylene glycol glycerol ricinoleate granules is 300 μm to 400 μm.

7. The method for preparing polyethylene glycol glycerol ricinoleate granules according to any one of claims 1 to 6, characterized in that, Includes the following steps: S1. Mix the first polyethylene glycol glycerol ricinoleate, the second polyethylene glycol glycerol ricinoleate and the carrier at 60-80°C, stir until uniform, add vitamin E acetate, continue stirring until uniform, obtain the mixture, and keep warm. S2. The mixture is fed into a granulation tower for spray granulation, and the inlet air temperature is controlled to be no higher than 20°C to obtain polyethylene glycol glycerol ricinoleate granules.

8. The preparation method according to claim 7, characterized in that, The preparation method further includes the steps of cooling, collecting and sieving the obtained polyethylene glycol glycerol ricinoleate particles.

9. The application of polyethylene glycol glycerol ricinoleate granules as described in any one of claims 1 to 6, characterized in that, The application includes adding the polyethylene glycol glycerol ricinoleate granules to feed.

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