A betaine phosphate-containing feed additive for improving net energy levels, its preparation method and application

Abstract

A betaine phosphate-containing feed additive for improving net energy levels, its preparation method, and its application belong to the field of feed additive technology. The preparation method includes: preparing compound betaine phosphate and compound methionine zinc, and mixing them; the preparation of compound betaine phosphate includes: preparing crude betaine phosphate, preparing a compound silica carrier, and crystallizing it; the preparation of compound methionine zinc includes: preparing an activated silica carrier, adsorbing starch, and adsorbing methionine zinc; the mixing involves mixing the compound betaine phosphate and compound methionine zinc, and stirring at room temperature to obtain the betaine phosphate-containing feed additive for improving net energy levels. The feed additive prepared by this invention has a strong effect on improving the net energy levels of broilers, is less prone to clumping, and has good storage resistance.

Description

Technical Field

[0001] This invention relates to the field of feed additive technology, specifically to a betaine phosphate-containing feed additive for improving net energy levels, its preparation method, and its application. Background Technology

[0002] Modern broiler production has entered a highly industrialized production model characterized by large-scale, automated, and intensive operations, creating an urgent need for precision nutrition technology systems. The dynamic and precise matching of feed nutritional value and requirements is the core of building such systems. Accurate alignment between energy requirements and feed energy nutritional value can fully unleash the production potential of livestock and poultry, achieving the goals of saving feed costs and reducing carbon and nitrogen emissions. It is also crucial for ensuring the sustainable and high-quality development of the livestock industry. Currently, animal energy nutrition systems still use the physical quantity "energy value" to describe the energy nutritional needs of animals and the energy nutritional value of feed, specifically divided into three levels: gross energy, metabolizable energy, and net energy. Net energy refers to the effective energy value remaining after subtracting the heat loss generated during metabolic utilization and feed intake and digestion from the metabolizable energy. It represents a more accurate "true" energy value for livestock and poultry to maintain and produce.

[0003] Studies have found that the net energy system, compared to the metabolizable energy system, considers the heat loss generated during animal feeding and digestion, and can more accurately reflect the animal's true energy requirements. Currently, net energy evaluation methods mainly include direct calorimetry and indirect calorimetry. Direct calorimetry uses calorimeters to directly measure the heat lost by the animal to the environment, and then combines this with metabolizable energy intake to calculate the net energy value. However, the operation of calorimeters is relatively cumbersome, and their application is limited in current research. Indirect calorimetry uses special methods to indirectly measure heat production and then calculate the net energy value, mainly divided into comparative slaughter methods and respiratory calorimetry. The comparative slaughter method calculates the energy deposition in the animal's body through comparative slaughter experiments, and then combines this with metabolizable energy intake to obtain the net energy value. However, the comparative slaughter method has the disadvantage of consuming a lot of manpower and resources. The respiratory calorimetry uses respiratory calorimeters to record the animal's carbon dioxide excretion and oxygen consumption over a certain period of time, and calculates the animal's total heat production based on respiratory entropy or carbon-nitrogen balance theory, and then calculates the net energy value. The respiratory calorimetry method is more convenient and faster, and is currently more widely used.

[0004] According to Xiong Taidi's "Research on Net Energy Requirements and Prediction Model of Medium-Growth Yellow-Feathered Broilers," a master's thesis from Foshan University of Science and Technology, published in 2024, the decrease in dietary net energy levels has varying degrees of impact on the production performance, tibia traits and organ indices, plasma biochemical indicators, and body component deposition rates of yellow-feathered broiler roosters and hens at different growth stages. According to Chen Simiao et al.'s "The Effect of Adding Exogenous Protease to Low-Protein Diets for Broilers on Net Energy Efficiency," a journal published in the *Journal of Animal Nutrition*, published in February 2025, dietary net energy parameters are consistent with broiler growth and slaughter performance indicators. The net energy system can be used as an evaluation index for the energy utilization effect of exogenous enzyme preparations in the diet. The thesis also discloses that adding exogenous protease to low-protein diets can improve net energy utilization efficiency and affect energy distribution, thereby increasing the average daily weight gain of broilers. According to Zhao Ying's master's thesis, "Net Energy Determination of Sorghum and Sunflower Seed Meal in Chicks Aged 2-4 and 5-8 Weeks," published in April 2023 at Shandong Agricultural University, net energy refers to the actual usable amount of feed energy used for body maintenance and production. In summary, improving net energy levels has a positive impact on broiler production performance, tibia traits and organ indices, plasma biochemical indicators, body component deposition rate, and the actual usable amount of feed energy for broilers.

[0005] Regarding how to improve the net energy level of broiler chickens, the existing technologies mainly disclose the following methods:

[0006] 1. According to the findings published by Ban Zhibin et al., "Comparative Study on Net Energy Efficiency and Standard Ileal Digestibility of Amino Acids between Conventional and Low-Protein Diets for Broilers," *Journal of Animal Nutrition*, January 2025, compared with conventional diets, low-protein diets significantly increased the metabolizable energy / total energy ratio of broilers aged 11–14 days; significantly reduced total heat production, heat loss, and protein deposition energy in broilers aged 21–24 days; significantly increased the net energy / metabolizable energy ratio; and significantly increased the net energy in broilers aged 35–38 days. Therefore, using low-protein diets can improve net energy levels.

[0007] 2. According to Chen Simiao's "The Effects of Dietary Treatment on Net Energy Utilization and Production Performance of Broilers," a master's thesis published in April 2023 at Jilin Agricultural University, a 1% and 2% reduction in crude protein levels will not affect broiler growth performance, but it will affect energy distribution. Fixed metabolizable energy, coupled with a decrease in crude protein levels, leads to excess energy being deposited as fat. Reducing crude protein also reduces heat gain and improves net energy efficiency. Therefore, adjusting the crude protein content in the diet can improve net energy levels.

[0008] 3. According to the findings of Chen Simiao et al., "The Effect of Adding Exogenous Protease to Low-Protein Diets for Broilers on Net Energy Efficiency," *Journal of Animal Nutrition*, February 2025, adding protease to low-protein diets can improve net energy utilization efficiency and affect energy distribution, thereby increasing average daily weight gain. Therefore, adding protease to low-protein diets can improve net energy levels.

[0009] 4. According to the information published by Yun Xianglong et al., "Evaluation of the Nutritional Value of Wheat in Poultry," *Feed Industry*, October 2022, there are significant differences in net energy values ​​among different wheat feed ingredients. Therefore, the type of feed affects the net energy level.

[0010] 5. According to the findings of Shen Jiajia et al., "Effects of Different Wheat Varieties and Xylanase Addition on Growth Performance, Nutrient Utilization, Net Energy, Physical Fitness, and Nutritional Utilization of Broilers of Different Ages," published in Guangdong Feed, January 2019, xylanase can improve net energy levels and fat deposition. Therefore, adding xylanase to wheat diets can improve net energy levels.

[0011] However, the above methods, such as using low-protein diets, adjusting the crude protein content in the diet, and adjusting the type of diet, all have the disadvantage of high requirements for the type and composition of the diet. Adding exogenous proteases is a method proposed for low-protein diets, and adding xylanase is a method proposed for wheat feed. The purpose is to improve the utilization efficiency of nutrients in the diet. However, the improvement effect is greatly affected by the type of diet, and the enzyme has poor stability, which makes the improvement effect greatly affected by the environment.

[0012] Feed additives refer to small or trace amounts of substances added to feed to ensure and improve feed quality and increase feed utilization. They have significant effects on improving animal production performance, maintaining intestinal health, saving breeding costs, and improving the quality of livestock products. Feed additives are widely used in production due to their diverse types and ease of use. According to He Weizhen's "Application of Guanidinylacetic Acid and Immobilized Intracellular Enzymes in Low-Energy Diets for Broilers," a master's thesis published by the Chinese Academy of Agricultural Sciences in June 2023, the amino acid derivative guanidinylacetic acid can improve arginine and glycine metabolism, increase amino acid utilization, and improve the net energy of broilers. Adding guanidinylacetic acid to low-energy diets can improve broiler production performance, achieving body weight, feed conversion ratio, breast muscle percentage, and leg muscle percentage comparable to or slightly better than conventional diets. Therefore, adding feed additives to diets can also improve net energy levels.

[0013] Betaine, also known as betaine glycoside, is an alkaline substance found in beet tubers. In its pure form, it is a colorless crystal. It can be used as an animal feed additive to supplement the methyl groups required for biological metabolism. According to Liu Lifu's article, "Application of Betaine as a Feed Additive in Livestock and Poultry Production," published in *New Agriculture* in October 2020, betaine is widely used in broiler farming. Adding betaine during broiler feeding significantly accelerates broiler growth and development and improves feed utilization. The applicant has experimented with adding betaine as a feed additive to broiler feed and found that it can improve the net energy level of broilers. However, according to the information published in January 2013 by Qingkong Yiyan, "Considering the Application of Betaine in Poultry Feed from a Cost Perspective," the addition of betaine to feed is limited due to its certain fluidity. Therefore, betaine hydrochloride, obtained by crystallizing betaine hydrochloride using the correct carrier, has emerged. It was also disclosed that different forms of betaine have the same metabolic components after passing through the stomach. Therefore, both betaine hydrochloride and anhydrous betaine can be used as effective feed additives in animal production.

[0014] According to the research published in November 2013 by Abudulajiang Nasir et al., "Study on Synthesis Method of Betaine Hydrochloride," *Chemical Reagents*, the preparation of betaine hydrochloride suffers from the difficulty in separating and removing byproducts such as sodium chloride or calcium chloride. This necessitates the use of desalination technology to remove these byproducts, further leading to disadvantages such as low product purity, complex separation processes, and high energy consumption. Considering that betaine phosphate precipitates almost quantitatively in 95% ethanol, has good crystal form, and is essentially non-hygroscopic, the applicant added betaine phosphate as a feed additive to broiler feed. They found that betaine phosphate, as one of the main forms of betaine, can also improve the net energy level of broilers.

[0015] However, when betaine phosphate is used directly as a feed additive to improve the net energy level of broilers, the following problems exist:

[0016] 1. According to Luo Xugang's article, "The Interrelationship between Methionine, Choline, Betaine, and Inorganic Sulfates in Poultry," published in the July 2000 issue of *China Poultry Industry Guide*, methionine and betaine play important roles in methyl transfer processes. During metabolism, betaine can only supply methyl groups and cannot "replace" or "save" the complete methionine molecules used for protein synthesis in the diet. Therefore, the effect of using betaine phosphate alone is limited, and it is necessary to use methionine and betaine phosphate in combination. However, methionine has a certain degree of hygroscopicity and is easily affected by moisture; therefore, feed additives prepared by mixing methionine and betaine phosphate have this moisture problem. Although zinc methionine can be used to replace methionine, according to the information published by Duan Jingna in "Preparation Method of Large-Particle Crystalline Zinc Methionine Complex and its Application in Laying Hen Premix" (Animal Husbandry and Veterinary Science, January 2021), the methionine chelates currently on the market have small particle size, high viscosity, low density, and poor flowability, making it difficult to mix thoroughly with feed. Furthermore, this will affect the effect of the prepared feed additive in improving net energy levels.

[0017] 2. When betaine phosphate is used as a feed additive to improve the net energy level of broilers, the addition amount is generally 0.1-0.2%. The addition amount is small, and it is difficult to achieve uniform mixing when directly added to broiler feed. According to the content published by Lü Yanchun in "Selection and Use of Carriers for Micro-feed Additives" in China Feed, June 2008, the effectiveness, uniformity and consistency of the active ingredients in the feed additive can be ensured by adding a carrier to the feed additive. However, this literature shows that different carriers have different properties and varying degrees of adhesion to betaine phosphate and methionine or methionine chelates. Inorganic carriers have low adhesion and are mostly used in the preparation of trace element premixes, while organic carriers have low adhesion and are mostly used in pharmaceutical additives. Considering the low adhesion of inorganic carriers, feed additives prepared from inorganic carriers are prone to powdering when stored at high temperatures. Therefore, in order to ensure adhesion to both betaine phosphate and methionine or methionine chelates, the most common method is to use organic carriers with strong adhesion. However, the stronger the adhesion, the easier it is for the carrier to clump together, which further leads to the problem of clumping in the prepared feed additives. Summary of the Invention

[0018] To address the shortcomings of existing technologies, this invention provides a betaine phosphate-containing feed additive for improving net energy levels, its preparation method, and its application. The prepared feed additive has a strong effect on improving the net energy levels of broilers, is less prone to clumping, and has good storage resistance.

[0019] To solve the above technical problems, the technical solution adopted by the present invention is as follows:

[0020] A method for preparing a betaine phosphate-containing feed additive to improve net energy levels includes: preparing compound betaine phosphate, preparing compound methionine zinc, and mixing them;

[0021] The preparation of the composite betaine phosphate includes: preparing crude betaine phosphate, preparing a composite silica carrier, and crystallizing;

[0022] To prepare crude betaine phosphate, trimethylamine aqueous solution was stirred at 100-300 rpm at room temperature, then chloroacetic acid and sodium hydroxide were added, the temperature was raised to 50-55°C and stirred for 120-150 min, the temperature was raised to 70-75°C and stirred for 120-150 min, the temperature was lowered to room temperature, some water was distilled off by vacuum concentration, the solution was cooled to room temperature, filtered, and the filtrate was collected. The filtrate was stirred at 100-300 rpm at room temperature, then phosphoric acid aqueous solution was added and stirred for 90-120 min, then ethanol aqueous solution was added, the temperature was raised to 70-75°C and stirred for 10-15 min, the temperature was lowered to 0-5°C, and the solution was allowed to stand for 25-30 h. The solution was filtered, the filter residue was collected, washed 2-3 times, and dried to obtain crude betaine phosphate.

[0023] In the preparation of crude betaine phosphate, the mass concentration of the trimethylamine aqueous solution is 30%.

[0024] The mass concentration of the phosphoric acid aqueous solution is 85%;

[0025] The volume concentration of the ethanol aqueous solution is 95%;

[0026] The mass ratio of trimethylamine aqueous solution, chloroacetic acid, sodium hydroxide, and phosphoric acid aqueous solution is 330–350: 159–168: 67.5–72: 200–220;

[0027] The mass ratio of trimethylamine aqueous solution to a portion of the water distilled off by vacuum concentration is 330–350:100–110;

[0028] The mass ratio of trimethylamine aqueous solution to ethanol aqueous solution is 330-350:150-170;

[0029] When washing the filter residue 2 to 3 times, use a 95% (v / v) ethanol aqueous solution for washing;

[0030] To prepare the composite silica carrier, rice starch and water are mixed and stirred at 50-100 rpm for 30-40 minutes at room temperature. The mixture is then heated to 85-90°C and stirred for 90-120 minutes. After cooling to room temperature, silica is added and stirred for 120-150 minutes. The mixture is then filtered, the filter residue is collected, and dried to obtain the composite silica carrier.

[0031] In the preparation of the composite silica carrier, the mass ratio of rice starch, water, and silica is 10-11:1000-1200:100-110;

[0032] The silica has a mesh size of 40 to 80 mesh;

[0033] The crystallization process involves mixing crude betaine phosphate with water, heating the mixture to 85–90°C, stirring at 50–100 rpm for 30–40 minutes, adding a composite silica carrier, stirring for another 30–40 minutes, concentrating under reduced pressure to remove some water, cooling to room temperature, adding an ethanol aqueous solution, cooling to 0–5°C, allowing the mixture to stand for 25–30 hours, filtering, collecting the filter residue, washing the residue 2–3 times, and drying it to obtain composite betaine phosphate.

[0034] In the crystallization, the volume concentration of the ethanol aqueous solution is 95%.

[0035] The mass ratio of crude betaine phosphate, water, and composite silica carrier is 50–55:5000–6000:500–600.

[0036] The mass ratio of crude betaine phosphate to a portion of the water extracted by vacuum concentration is 50–55:4800–5800.

[0037] The mass ratio of crude betaine phosphate to an aqueous ethanol solution is 50–55:200–300.

[0038] When washing the filter residue 2 to 3 times, use a 95% (v / v) ethanol aqueous solution for washing;

[0039] The preparation of the composite methionine zinc includes: preparing an activated silica carrier, adsorbing starch, and adsorbing methionine zinc;

[0040] The preparation of the activated silica support involves mixing silica, calcium chloride aqueous solution, and zinc sulfate aqueous solution, stirring at 50-100 rpm for 60-90 min at room temperature, adding sodium hydroxide aqueous solution to adjust the pH to 8.5-9, stirring for 30-60 min, filtering, taking the filter residue, washing the filter residue 2-3 times, and drying to obtain the activated silica support.

[0041] In the preparation of the activated silica support, the mass concentration of the calcium chloride aqueous solution is 1%;

[0042] The zinc sulfate aqueous solution has a mass concentration of 1%;

[0043] The mass concentration of the sodium hydroxide aqueous solution is 5%;

[0044] The mass ratio of silicon dioxide, calcium chloride aqueous solution, and zinc sulfate aqueous solution is 100-110:500-600:500-600;

[0045] The silica has a mesh size of 40 to 80 mesh;

[0046] Wash the filter residue 2-3 times with water;

[0047] The adsorbed starch is prepared by mixing rice starch and water, stirring at 50-100 rpm for 30-40 minutes at room temperature, heating to 85-90°C and stirring for 90-120 minutes, cooling to room temperature, adding activated silica carrier, stirring for 40-60 minutes, filtering, taking the filter residue, drying, and obtaining silica carrier after adsorbing starch.

[0048] In the adsorbed starch, the mass ratio of rice starch, water, and activated silica carrier is 5-5.5:1000-1200:100-110;

[0049] The adsorbed zinc methionine is prepared by mixing methionine and water, heating to 85-90°C, stirring at 50-100 rpm for 5-10 minutes, adding silica carrier after adsorbing starch, stirring for 10-20 minutes, adding anhydrous zinc sulfate, stirring for 60-90 minutes, filtering, taking the filter residue, drying, and obtaining composite zinc methionine.

[0050] In the zinc methionine adsorption process, the mass ratio of methionine, water, silica carrier after starch adsorption, and anhydrous zinc sulfate is 6–6.5:600–700:60–65:3.2–3.4.

[0051] The mixing process involves mixing compound betaine phosphate with compound methionine zinc and stirring at 20-40 rpm for 30-40 minutes at room temperature to obtain a betaine phosphate-containing feed additive that improves net energy levels.

[0052] In the mixture, the mass ratio of compound betaine phosphate to compound methionine zinc is 4-4.2:1.

[0053] A betaine phosphate-containing feed additive for improving net energy levels, prepared by the aforementioned method.

[0054] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0055] The feed additive prepared by this invention does not have the problem of clumping; after being stored for 42 days in an environment with a temperature of 30±2℃ and a relative humidity of 55±1%, it does not have the problem of powder shedding or clumping; and it can significantly improve the net energy level. Detailed Implementation

[0056] To provide a clearer understanding of the technical features, objectives, and effects of the present invention, specific embodiments of the present invention are now described.

[0057] The room temperature in Examples 1-2 and Comparative Examples 1-3 was 23±2℃.

[0058] Example 1

[0059] A method for preparing a betaine phosphate-containing feed additive to improve net energy levels is as follows:

[0060] 1. Preparation of compound betaine phosphate:

[0061] (1) Preparation of crude betaine phosphate: 330g of 30% trimethylamine aqueous solution was stirred at 100rpm at room temperature, then 159g of chloroacetic acid and 67.5g of sodium hydroxide were added, the temperature was raised to 50℃ and stirred for 120min, the temperature was raised to 70℃ and stirred for 120min, the temperature was lowered to room temperature, 100g of water was concentrated by vacuum distillation, the solution was cooled to room temperature, filtered, and the filtrate was collected. The filtrate was stirred at 100rpm at room temperature, then 200g of 85% phosphoric acid aqueous solution was added and stirred for 90min. 150g of 95% ethanol aqueous solution was added, the temperature was raised to 70℃ and stirred for 10min, the temperature was lowered to 0℃ and allowed to stand for 25h, filtered, and the filter residue was washed twice with 95% ethanol aqueous solution and dried to obtain crude betaine phosphate.

[0062] (2) Preparation of composite silica carrier: Mix 10g of rice starch and 1000g of water, stir at 50rpm for 30min at room temperature, heat to 85℃, stir for 90min, cool to room temperature, add 100g of silica, stir for 120min, filter, take the filter residue, dry, and obtain composite silica carrier.

[0063] The silica has a mesh size of 40.

[0064] (3) Crystallization: Mix 50g of crude betaine phosphate with 5000g of water, heat to 85℃, stir at 50rpm for 30min, add 500g of composite silica carrier, stir for 30min, concentrate under reduced pressure to remove 4800g of water, cool to room temperature, add 200g of 95% ethanol aqueous solution, cool to 0℃, stand for 25h, filter, take the filter residue, wash the filter residue twice with 95% ethanol aqueous solution, dry, and obtain composite betaine phosphate;

[0065] 2. Preparation of compound methionine zinc:

[0066] (1) Preparation of activated silica support: 100g silica, 500g calcium chloride aqueous solution with a mass concentration of 1% and 500g zinc sulfate aqueous solution with a mass concentration of 1% were mixed and stirred at 50rpm for 60min at room temperature. The pH was adjusted to 8.5 by adding sodium hydroxide aqueous solution with a mass concentration of 5%, and stirred for 30min. The mixture was filtered, the filter residue was washed twice with water, and dried to obtain activated silica support.

[0067] The silica has a mesh size of 40.

[0068] (2) Adsorption of starch: Mix 5g of rice starch and 1000g of water, stir at 50rpm for 30min at room temperature, heat to 85℃, stir for 90min, cool to room temperature, add 100g of activated silica carrier, stir for 40min, filter, take the filter residue, dry, and obtain silica carrier after adsorption of starch.

[0069] (3) Adsorption of zinc methionine: Mix 6g of methionine and 600g of water, heat to 85℃, stir at 50rpm for 5min, add 60g of silica carrier after adsorbing starch, stir for 10min, add 3.2g of anhydrous zinc sulfate, stir for 60min, filter, take the filter residue, dry, and obtain composite zinc methionine.

[0070] 3. Mixing: Mix compound betaine phosphate and compound methionine zinc at a mass ratio of 4:1, and stir at 20 rpm for 30 minutes at room temperature to obtain a betaine phosphate-containing feed additive that improves net energy level.

[0071] This embodiment also provides a betaine phosphate feed additive for improving net energy levels, prepared by the aforementioned preparation method.

[0072] Example 2

[0073] A method for preparing a betaine phosphate-containing feed additive to improve net energy levels is as follows:

[0074] 1. Preparation of compound betaine phosphate:

[0075] (1) Preparation of crude betaine phosphate: 350g of 30% trimethylamine aqueous solution was stirred at 300rpm at room temperature, then 168g of chloroacetic acid and 72g of sodium hydroxide were added, the temperature was raised to 55℃ and stirred for 150min, the temperature was raised to 75℃ and stirred for 150min, the temperature was lowered to room temperature, 110g of water was concentrated by vacuum distillation, the solution was cooled to room temperature, filtered, and the filtrate was collected. The filtrate was stirred at 300rpm at room temperature, then 220g of 85% phosphoric acid aqueous solution was added and stirred for 120min. Then 170g of 95% ethanol aqueous solution was added, the temperature was raised to 75℃ and stirred for 15min, the temperature was lowered to 5℃ and allowed to stand for 30h, filtered, and the filter residue was washed 3 times with 95% ethanol aqueous solution and dried to obtain crude betaine phosphate.

[0076] (2) Preparation of composite silica carrier: 11g of rice starch and 1200g of water were mixed and stirred at 100rpm for 40min at room temperature. The temperature was raised to 90℃ and stirred for 120min. The temperature was lowered to room temperature, 110g of silica was added, and stirred for 150min. The mixture was filtered, the filter residue was collected, and dried to obtain composite silica carrier.

[0077] The silica has a mesh size of 40.

[0078] (3) Crystallization: Mix 55g of crude betaine phosphate with 6000g of water, heat to 90℃, stir at 100rpm for 40min, add 600g of composite silica carrier, stir for 40min, concentrate and distill off 5800g of water under reduced pressure, cool to room temperature, add 300g of 95% ethanol aqueous solution, cool to 5℃, let stand for 30h, filter, take the filter residue, wash the filter residue 3 times with 95% ethanol aqueous solution, dry, and obtain composite betaine phosphate;

[0079] 2. Preparation of compound methionine zinc:

[0080] (1) Preparation of activated silica support: 110g silica, 600g calcium chloride aqueous solution with a mass concentration of 1% and 600g zinc sulfate aqueous solution with a mass concentration of 1% were mixed and stirred at 100rpm for 90min at room temperature. A sodium hydroxide aqueous solution with a mass concentration of 5% was added to adjust the pH to 9 and stirred for 60min. The mixture was filtered, and the filter residue was washed with water 3 times and dried to obtain activated silica support.

[0081] The silica has a mesh size of 40.

[0082] (2) Adsorption of starch: Mix 5.5g of rice starch and 1200g of water, stir at 100rpm for 40min at room temperature, heat to 90℃, stir for 120min, cool to room temperature, add 110g of activated silica carrier, stir for 60min, filter, take the filter residue, dry, and obtain silica carrier after adsorption of starch.

[0083] (3) Adsorption of zinc methionine: Mix 6.5g of methionine and 700g of water, heat to 90℃, stir at 100rpm for 10min, add 65g of silica carrier after adsorbing starch, stir for 20min, add 3.4g of anhydrous zinc sulfate, stir for 90min, filter, take the filter residue, dry, and obtain composite zinc methionine.

[0084] 3. Mixing: Mix compound betaine phosphate and compound methionine zinc at a mass ratio of 4.2:1, and stir at 40 rpm for 40 min at room temperature to obtain a betaine phosphate-containing feed additive that improves net energy level.

[0085] This embodiment also provides a betaine phosphate feed additive for improving net energy levels, prepared by the aforementioned preparation method.

[0086] Comparative Example 1

[0087] A method for preparing a betaine phosphate-containing feed additive to improve net energy levels is as follows:

[0088] 1. Preparation of betaine phosphate:

[0089] (1) Preparation of crude betaine phosphate: 330g of 30% trimethylamine aqueous solution was stirred at 100rpm at room temperature, then 159g of chloroacetic acid and 67.5g of sodium hydroxide were added, the temperature was raised to 50℃ and stirred for 120min, the temperature was raised to 70℃ and stirred for 120min, the temperature was lowered to room temperature, 100g of water was concentrated by vacuum distillation, the temperature was cooled to room temperature, filtered, and the filtrate was taken. The filtrate was stirred at 100rpm at room temperature, then 200g of 85% phosphoric acid aqueous solution was added and stirred for 90min. 150g of 95% ethanol aqueous solution was added, the temperature was raised to 70℃ and stirred for 10min, the temperature was lowered to 0℃, and the mixture was allowed to stand for 25h. The precipitate was centrifuged and the precipitate was taken. The precipitate was washed twice with 95% ethanol aqueous solution and dried to obtain crude betaine phosphate.

[0090] (2) Crystallization: Mix 50g of crude betaine phosphate with 25g of water, heat to 85℃, stir at 50rpm for 30min, cool to room temperature, add 25g of 95% ethanol aqueous solution, cool to 0℃, let stand for 25h, centrifuge, take the precipitate, wash the precipitate twice with 95% ethanol aqueous solution, dry, and obtain betaine phosphate;

[0091] 2. Preparation of zinc methionine: Mix 6g of methionine and 60g of water, heat to 85℃, stir at 50rpm for 5min, add 3.2g of anhydrous zinc sulfate, adjust the pH to 7 with 5% sodium hydroxide aqueous solution, stir for 60min, centrifuge, take the precipitate, dry, and obtain composite zinc methionine.

[0092] 3. Mixing: Mix betaine phosphate and zinc methionine at a mass ratio of 4:1, and stir at 20 rpm for 30 minutes at room temperature to obtain a betaine phosphate-containing feed additive that improves net energy level.

[0093] This comparative embodiment also provides a betaine phosphate-containing feed additive for improving net energy levels, prepared by the aforementioned preparation method.

[0094] Comparative Example 2

[0095] A method for preparing a betaine phosphate-containing feed additive to improve net energy levels is as follows:

[0096] 1. Preparation of compound betaine phosphate:

[0097] (1) Preparation of crude betaine phosphate: 330g of 30% trimethylamine aqueous solution was stirred at 100rpm at room temperature, then 159g of chloroacetic acid and 67.5g of sodium hydroxide were added, the temperature was raised to 50℃ and stirred for 120min, the temperature was raised to 70℃ and stirred for 120min, the temperature was lowered to room temperature, 100g of water was concentrated by vacuum distillation, the solution was cooled to room temperature, filtered, and the filtrate was collected. The filtrate was stirred at 100rpm at room temperature, then 200g of 85% phosphoric acid aqueous solution was added and stirred for 90min. 150g of 95% ethanol aqueous solution was added, the temperature was raised to 70℃ and stirred for 10min, the temperature was lowered to 0℃ and allowed to stand for 25h, filtered, and the filter residue was washed twice with 95% ethanol aqueous solution and dried to obtain crude betaine phosphate.

[0098] (2) Crystallization: Mix 50g of crude betaine phosphate with 5000g of water, heat to 85℃, stir at 50rpm for 30min, add 500g of silica, stir for 30min, concentrate under reduced pressure to remove 4800g of water, cool to room temperature, add 200g of 95% ethanol aqueous solution, cool to 0℃, let stand for 25h, filter, take the filter residue, wash the filter residue twice with 95% ethanol aqueous solution, dry, and obtain composite betaine phosphate;

[0099] The silica has a mesh size of 40.

[0100] 2. Preparation of compound methionine zinc: Mix 6g of methionine and 600g of water, heat to 85℃, stir at 50rpm for 5min, add 60g of silica, stir for 10min, add 3.2g of anhydrous zinc sulfate, stir for 60min, filter, take the filter residue, dry, and obtain compound methionine zinc;

[0101] The silica has a mesh size of 40.

[0102] 3. Mixing: Mix compound betaine phosphate and compound methionine zinc at a mass ratio of 4:1, and stir at 20 rpm for 30 minutes at room temperature to obtain a betaine phosphate-containing feed additive that improves net energy level.

[0103] This comparative embodiment also provides a betaine phosphate-containing feed additive for improving net energy levels, prepared by the aforementioned preparation method.

[0104] Comparative Example 3

[0105] A method for preparing a betaine phosphate-containing feed additive to improve net energy levels is as follows:

[0106] 1. Preparation of compound betaine phosphate:

[0107] (1) Preparation of crude betaine phosphate: 330g of 30% trimethylamine aqueous solution was stirred at 100rpm at room temperature, then 159g of chloroacetic acid and 67.5g of sodium hydroxide were added, the temperature was raised to 50℃ and stirred for 120min, the temperature was raised to 70℃ and stirred for 120min, the temperature was lowered to room temperature, 100g of water was concentrated by vacuum distillation, the solution was cooled to room temperature, filtered, and the filtrate was collected. The filtrate was stirred at 100rpm at room temperature, then 200g of 85% phosphoric acid aqueous solution was added and stirred for 90min. 150g of 95% ethanol aqueous solution was added, the temperature was raised to 70℃ and stirred for 10min, the temperature was lowered to 0℃ and allowed to stand for 25h, filtered, and the filter residue was washed twice with 95% ethanol aqueous solution and dried to obtain crude betaine phosphate.

[0108] (2) Preparation of composite silica carrier: Mix 10g of rice starch and 1000g of water, stir at 50rpm for 30min at room temperature, heat to 85℃, stir for 90min, cool to room temperature, add 100g of silica, stir for 120min, filter, take the filter residue, dry, and obtain composite silica carrier.

[0109] The silica has a mesh size of 40.

[0110] (3) Crystallization: Mix 50g of crude betaine phosphate with 5000g of water, heat to 85℃, stir at 50rpm for 30min, add 500g of composite silica carrier, stir for 30min, concentrate under reduced pressure to remove 4800g of water, cool to room temperature, add 200g of 95% ethanol aqueous solution, cool to 0℃, stand for 25h, filter, take the filter residue, wash the filter residue twice with 95% ethanol aqueous solution, dry, and obtain composite betaine phosphate;

[0111] 2. Preparation of compound methionine zinc:

[0112] (1) Adsorbing starch: Mix 5g of rice starch and 1000g of water, stir at 50rpm for 30min at room temperature, heat to 85℃, stir for 90min, cool to room temperature, add 100g of silica, stir for 40min, filter, take the filter residue, dry, and obtain silica carrier after adsorbing starch.

[0113] The silica has a mesh size of 40.

[0114] (2) Adsorption of zinc methionine: Mix 6g of methionine and 600g of water, heat to 85℃, stir at 50rpm for 5min, add 60g of silica carrier after adsorbing starch, stir for 10min, add 3.2g of anhydrous zinc sulfate, stir for 60min, filter, take the filter residue, dry, and obtain composite zinc methionine.

[0115] 3. Mixing: Mix compound betaine phosphate and compound methionine zinc at a mass ratio of 4:1, and stir at 20 rpm for 30 minutes at room temperature to obtain a betaine phosphate-containing feed additive that improves net energy level.

[0116] This comparative embodiment also provides a betaine phosphate-containing feed additive for improving net energy levels, prepared by the aforementioned preparation method.

[0117] Test Example 1

[0118] The feed additives prepared in Examples 1-2 and Comparative Examples 1-3 were observed to have the problem of clumping together. The results are as follows:

[0119]

[0120] The results of this test show that the feed additives prepared in Examples 1-2 and Comparative Examples 1-3 do not have the problem of clumping, indicating that using starch and silica as a composite carrier can avoid the clumping problem that exists when only starch-based organic carriers are used.

[0121] Test Example 2

[0122] The feed additives prepared in Examples 1-2 and Comparative Examples 1-3 were sealed in coated bags and stored for 42 days at a temperature of 30±2℃ and a relative humidity of 55±1%. The presence of powder shedding and clumping was then observed (since no carrier was used in the preparation of the feed additive in Example 1, it was not necessary to observe whether the feed additive prepared in Comparative Example 1 had powder shedding issues). The results are as follows:

[0123]

[0124] The results of this test show that the feed additives prepared in Examples 1 and 2 have good storage resistance.

[0125] Test Example 3

[0126] One hundred and eighty 20-day-old broiler chickens were randomly divided into six groups. Groups 1-5 were the experimental groups, and group 6 was the blank control group. The feed additives of Examples 1-2 and Comparative Examples 1-3 were added to the diets of the broiler chickens in groups 1-5, respectively. The amount of feed additives added to Examples 1-2 and Comparative Examples 2-3 was 2%, and the amount of feed additives added to Comparative Example 1 was 0.2%. No feed additives were added to the diets of the broiler chickens in the six groups. There were six replicates in each group, and five broiler chickens in each replicate.

[0127] During the test, groups 1 through 6 of broiler chickens used the same basal diet, the composition of which is as follows:

[0128]

[0129] The test was conducted at the Institute of Animal Nutrition and Feed, Jilin Academy of Agricultural Sciences. The feeding and management were carried out in accordance with the "AA Broiler Feeding and Management Manual 2019". Groups 1 to 6 were all cage-raised. During the experiment, white-feathered broilers in groups 1 to 6 were allowed free access to feed and water. The indoor environment was adjusted according to the age of the broilers.

[0130] After 5 consecutive days of feeding, the daily feed intake and daily weight gain of each broiler chicken in each group were tested. The average value of each group was calculated, and then the average value of the 6 replicates for each group was calculated. The feed conversion ratio of each group was also calculated. The results are as follows:

[0131]

[0132] After 5 consecutive days of feeding, the net energy level of broiler chickens in groups 1-6 was tested using respiratory calorimetry. Specifically, two broiler chickens were selected from each replicate of each group and transferred to the respiratory calorimetry device. After acclimatization for 1 day, the respiratory calorimetry test lasted for 3 days. During the test, the basal diet, feed additives, and feeding method of each group remained unchanged. The daily feed intake and daily weight gain of each broiler chicken in each group were tested during the test period. The average value of the 6 replicates for each group was calculated, and the feed conversion ratio of each group was also calculated. The results are as follows:

[0133]

[0134] At the same time, the average value of the energy data from the six repetitions in each group was calculated, and the results are as follows:

[0135]

[0136] The results of this test show that the feed additives prepared in Examples 1 and 2 have the lowest feed conversion ratio and the highest net energy level. Although the feed additives prepared in Comparative Examples 1-3 all used betaine phosphate and methionine as the main components compared to the feed additive prepared in Example 1, Comparative Example 1 did not use a carrier, which made it difficult for the feed additive prepared in Comparative Example 1 to be evenly dispersed in the basal diet. This resulted in uneven intake of betaine phosphate and methionine by broilers, affecting the net energy level of the three groups of broilers. Comparative Example 2 used an untreated carrier, which had limited adhesion to betaine phosphate and methionine and also had the problem of powder shedding. This resulted in uneven intake and reduced intake of betaine phosphate and methionine by broilers, affecting the net energy level of the four groups of broilers. In Comparative Example 3, the carrier used in the preparation of compound zinc methionine was not activated, which resulted in instability of zinc methionine in the compound zinc methionine and also had a certain impact on the adhesion of zinc methionine to the carrier. Furthermore, this had a certain impact on the net energy level of the five groups of broilers.

[0137] In summary, it is essential to formulate betaine phosphate into a complex betaine phosphate form and methionine zinc into a complex methionine zinc form in the preparation of feed additives. The principle utilized in preparing complex betaine phosphate is to first adsorb rice starch onto the surface of a silica carrier through intermolecular forces such as hydrogen bonds. Then, according to the content published by Wang Xiaoying in her master's thesis, "Betaine and its Hydrochloride Inhibit Indica Rice Retrogradation and Its Application in α-Indica Rice Convenience Rice," published in May 2013 at Central South University of Forestry and Technology, the betaine structure can encapsulate starch. Therefore, there is an intermolecular force between the betaine structure and starch, which uniformly disperses the betaine phosphate on the silica carrier surface. Furthermore, during crystallization, this promotes the uniform dispersion of betaine phosphate crystals on the silica carrier surface. Thus, starch can enhance the binding force between betaine phosphate crystals and the silica carrier and promote the uniform distribution of betaine phosphate crystals on the silica carrier surface. In the preparation of composite zinc methionine, the principle utilized is that calcium and zinc ions can be adsorbed onto the surface of a silica carrier, resulting in an activated silica carrier. Then, through the interaction between starch and calcium ions, starch is adsorbed onto the silica surface. Following the content published by Gao Binghui et al. in "Research on Dry Preparation Process of Amino Acid-Polysaccharide-Copper Organic Chelates" (Fujian Animal Husbandry and Veterinary Medicine, September 2025), based on the multiple complexation effects between starch polysaccharides and methionine with calcium and zinc ions, methionine is uniformly dispersed on the silica carrier surface. Calcium ions act as a link between starch polysaccharides and methionine, while zinc ions act as complexes to form zinc methionine crystals. The addition of zinc sulfate further complexes zinc ions uniformly onto the silica surface, achieving a uniform distribution of zinc methionine crystals. Furthermore, the interaction between starch polysaccharides and zinc methionine reduces the viscosity of the composite zinc methionine, improving its flowability. Simultaneously, the combination of an organic carrier (starch) and an inorganic carrier (silica) ensures both adhesion, flowability, and anti-caking properties.

Claims

1. A method for preparing a betaine phosphate-containing feed additive to improve net energy levels, characterized in that, include: Prepare compound betaine phosphate, prepare compound methionine zinc, and mix; The preparation of the composite betaine phosphate includes: preparing crude betaine phosphate, preparing a composite silica carrier, and crystallizing; To prepare the composite silica carrier, rice starch and water are mixed, stirred at room temperature, heated to 85-90°C, stirred, cooled to room temperature, silica is added, stirred, filtered, the filter residue is collected, and dried to obtain the composite silica carrier. The crystallization process involves mixing crude betaine phosphate with water, heating to 85-90°C, stirring, adding a composite silica carrier, stirring, concentrating under reduced pressure to remove some water, cooling to room temperature, adding an ethanol aqueous solution, cooling, allowing to stand, filtering, taking the filter residue, washing the filter residue, drying, and obtaining composite betaine phosphate. The preparation of the composite methionine zinc includes: preparing an activated silica carrier, adsorbing starch, and adsorbing methionine zinc; The preparation of the activated silica support involves mixing silica, calcium chloride aqueous solution, and zinc sulfate aqueous solution, stirring at room temperature, adjusting the pH to 8.5-9, stirring, filtering, collecting the filter residue, washing the filter residue, and drying to obtain the activated silica support. The adsorbed zinc methionine is prepared by mixing methionine and water, heating to 85-90°C, stirring, adding silica carrier after adsorbing starch, stirring, adding anhydrous zinc sulfate, stirring, filtering, taking the filter residue, drying, and obtaining composite zinc methionine. The mixing process involves uniformly mixing compound betaine phosphate and compound methionine zinc to obtain a feed additive containing betaine phosphate.

2. The method for preparing the betaine phosphate feed additive for improving net energy levels according to claim 1, characterized in that, To prepare crude betaine phosphate, a trimethylamine aqueous solution was stirred at room temperature, followed by the addition of chloroacetic acid and sodium hydroxide. The mixture was heated to 50–55°C and stirred, then heated to 70–75°C and stirred again. The mixture was cooled to room temperature, and some water was distilled off by vacuum concentration. The mixture was then cooled to room temperature, filtered, and the filtrate was collected. The filtrate was stirred at room temperature, and a phosphoric acid aqueous solution was added and stirred. An ethanol aqueous solution was added, and the mixture was heated to 70–75°C and stirred. The mixture was then cooled to 0–5°C, allowed to stand, filtered, and the filter residue was collected, washed, and dried to obtain crude betaine phosphate.

3. The method for preparing the betaine phosphate feed additive for improving net energy levels according to claim 2, characterized in that, In the preparation of crude betaine phosphate, the mass concentration of the trimethylamine aqueous solution is 30%. The mass concentration of the phosphoric acid aqueous solution is 85%; The volume concentration of the ethanol aqueous solution is 95%; The mass ratio of trimethylamine aqueous solution, chloroacetic acid, sodium hydroxide, and phosphoric acid aqueous solution is 330–350: 159–168: 67.5–72: 200–220; The mass ratio of trimethylamine aqueous solution to a portion of the water distilled off by vacuum concentration is 330–350:100–110; The mass ratio of trimethylamine aqueous solution to ethanol aqueous solution is 330-350:150-170.

4. The method for preparing the betaine phosphate feed additive for improving net energy levels according to claim 1, characterized in that, In the preparation of the composite silica carrier, the mass ratio of rice starch, water, and silica is 10-11:1000-1200:100-110; The silica has a mesh size of 40 to 80 mesh.

5. The method for preparing the betaine phosphate feed additive for improving net energy levels according to claim 1, characterized in that, In the crystallization, the volume concentration of the ethanol aqueous solution is 95%. The mass ratio of crude betaine phosphate, water, and composite silica carrier is 50–55:5000–6000:500–600. The mass ratio of crude betaine phosphate to a portion of the water extracted by vacuum concentration is 50–55:4800–5800. The mass ratio of crude betaine phosphate to an aqueous ethanol solution is 50–55:200–300.

6. The method for preparing the betaine phosphate feed additive for improving net energy levels according to claim 1, characterized in that, In the preparation of the activated silica support, the mass concentration of the calcium chloride aqueous solution is 1%; The zinc sulfate aqueous solution has a mass concentration of 1%; The mass ratio of silicon dioxide, calcium chloride aqueous solution, and zinc sulfate aqueous solution is 100-110:500-600:500-600; The silica has a mesh size of 40 to 80 mesh.

7. The method for preparing the betaine phosphate feed additive for improving net energy levels according to claim 1, characterized in that, The adsorbed starch is prepared by mixing rice starch and water, stirring at room temperature, heating to 85-90°C, stirring, cooling to room temperature, adding activated silica carrier, stirring, filtering, taking the filter residue, drying, and obtaining silica carrier after adsorbing starch. In the adsorbed starch, the mass ratio of rice starch, water, and activated silica carrier is 5-5.5:1000-1200:100-110.

8. The method for preparing the betaine phosphate feed additive for improving net energy levels according to claim 1, characterized in that, In the zinc methionine adsorption process, the mass ratio of methionine, water, silica carrier after starch adsorption, and anhydrous zinc sulfate is 6–6.5:600–700:60–65:3.2–3.

4. In the mixture, the mass ratio of compound betaine phosphate to compound methionine zinc is 4-4.2:

1.

9. A betaine phosphate-containing feed additive prepared by the preparation method according to any one of claims 1 to 8.

10. The use of the feed additive as described in claim 9 in the preparation of products that improve net energy levels.

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