Betaine-containing phosphate feed additive capable of improving net energy level and preparation method and application of betaine-containing phosphate feed additive

Abstract

The invention relates to a betaine phosphate-containing feed additive for improving net energy level and a preparation method and application thereof, and belongs to the technical field of feed additives, the preparation method comprises the following steps: preparing composite betaine phosphate, preparing composite zinc methionine, and mixing; the preparation of the composite betaine phosphate comprises the following steps: preparing a betaine phosphate crude product, preparing a composite silicon dioxide carrier, and crystallizing; the preparation of the compound zinc methionine comprises the following steps: preparing an activated silicon dioxide carrier, adsorbing starch and adsorbing the zinc methionine; in the step of mixing, the compound betaine phosphate and the compound zinc methionine are mixed and then stirred at room temperature, and the betaine phosphate-containing feed additive capable of improving the net energy level is obtained. The feed additive prepared by the invention has a strong effect of improving the net energy level of broiler chickens, is not easy to have the problems of bonding and clustering, and is good in storage resistance.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of feed additives, in particular to a betaine phosphate-containing feed additive for improving net energy level and a preparation method and application thereof. BACKGROUND

[0002] Modern broiler production has entered a highly industrialized production mode of scale, automation and high degree of intensification, and there is an urgent need for precise nutrition technology system. Dynamic accurate matching of feed nutritional value and requirement is the core of the construction of precise nutrition technology system. Accurate docking of energy requirement and feed energy nutritional value can fully develop the production potential of livestock and poultry, achieve the purpose of saving feed cost and reducing carbon and nitrogen emission, and is also the key to guarantee the sustainable and high-quality development of animal husbandry industry. At present, the physical quantity of "energy value" is still used in the animal energy nutrition system to describe the energy nutritional needs of animals and the energy nutritional value of feed, which is specifically divided into three levels of total energy, metabolic energy and net energy. Among them, net energy refers to the effective energy value left after the metabolic energy is reduced by the heat increment in the process of metabolic utilization and the heat increment in the process of feed intake and digestion, which is a more accurate "true" energy value for livestock and poultry to maintain and produce.

[0003] Studies have found that compared with the metabolic energy system, the net energy system takes into account the heat increment generated in the process of animal feeding and digestion, and can more accurately reflect the true energy requirement of animals. At present, the evaluation methods of net energy mainly include direct calorimetry and indirect calorimetry. Among them, direct calorimetry is to directly measure the heat dissipated to the outside world by a calorimetry device, and then calculate the net energy value combined with the metabolic energy intake. However, the operation of the calorimetry device is relatively cumbersome, and it is less used in current research. Indirect calorimetry is to indirectly calculate the heat production by special means, and then calculate the net energy value, which is mainly divided into comparative slaughter method and respiratory calorimetry. Among them, the comparative slaughter method calculates the energy deposition in the animal body by comparing the slaughter test, and then calculates the net energy value combined with the metabolic energy intake. However, the comparative slaughter method has the disadvantage of consuming a lot of manpower and material resources in the application process. Respiratory calorimetry is to record the carbon dioxide output and oxygen consumption of animals within a certain period of time by using a respiratory calorimetry device, and to calculate the total heat production of animals according to the respiratory entropy or carbon-nitrogen balance theory, and then to calculate the net energy value. Respiratory calorimetry is relatively convenient and fast, and is currently more commonly used.

[0004] According to the content disclosed in Xiong Taiji. Net energy requirement and prediction model of medium-speed yellow-feathered broilers. Foshan University Master Thesis. 2024, with the decrease of net energy level of diet, the production performance, tibia shape and organ index, plasma biochemical indicators and body composition deposition rate of yellow-feathered broiler cock and hen at different growth stages are affected to varying degrees. According to the content disclosed in Chen Simiao et al. Effect of adding exogenous protease to low-protein diet on net energy efficiency of broilers. Animal Nutrition. February 2025, the net energy parameters of diet are consistent with the growth performance and slaughter performance indicators of broilers, and the net energy system can be used as an evaluation index of the effect of exogenous enzyme preparation on diet energy utilization. It is also disclosed that adding exogenous protease to low-protein diet can improve net energy utilization efficiency and affect energy distribution, and improve the average daily gain of broilers. According to the content disclosed in Zhao Ying. Determination of net energy of egg chicks at 2-4 and 5-8 weeks of age with sorghum and sunflower meal. Shandong Agricultural University Master Thesis. April 2023, net energy refers to the actual available amount of feed energy, which is used for body maintenance and production. In summary, improving the net energy level has a positive significance for the production performance, tibia shape and organ index, plasma biochemical indicators, body composition deposition rate and actual available amount of feed energy of broilers.

[0005] To improve the net energy level of broilers, the existing technology mainly discloses the following methods: 1. According to the content disclosed in Ban Zhbin et al. Comparative study on net energy efficiency and ileal amino acid standard digestibility of conventional and low-protein diets for broilers. Animal Nutrition. January 2025, compared with conventional diet, low-protein diet can significantly increase the metabolic energy / total energy value of broilers at 11-14 days of age; significantly reduce the total heat production, heat increment and protein deposition energy of broilers at 21-24 days of age, significantly increase the net energy / metabolic energy value; significantly increase the net energy of broilers at 35-38 days of age. Therefore, using low-protein diet can improve the net energy level.

[0006] 2. According to the content disclosed in Chen Simiao. Effect of diet processing on net energy utilization and production performance of broilers. Jilin Agricultural University Master Thesis. April 2023, reducing the crude protein level by 1% and 2% will not affect the growth performance of broilers, but will affect their energy distribution. Reducing the crude protein level while keeping the maintenance energy constant will result in excess energy deposition as fat, and reducing the crude protein level will also reduce the heat increment and improve the net energy efficiency. Therefore, adjusting the crude protein content in the diet can improve the net energy level.

[0007] 3. According to the content disclosed in Chen Simiao et al. Effect of adding exogenous protease to low-protein diet on net energy efficiency of broilers. Animal Nutrition. February 2025, adding protease to low-protein diet can improve net energy utilization efficiency and affect energy distribution, and improve average daily gain. Therefore, adding protease to low-protein diet can improve the net energy level.

[0008] 4. According to the content disclosed by ZHANG, X. et al. Nutritive value of wheat for poultry. Feed industry. October 2022, the net energy values of different wheat raw materials are quite different. Therefore, the type of feed has an impact on the net energy level.

[0009] 5. According to the content disclosed by SHEN, J. et al. Effects of different wheat varieties and xylanase on growth performance, nutrient utilization, net energy for growth and body energy and nutrient utilization of broilers at different ages. Guangdong feed. January 2019, xylanase can improve the net energy level and fat deposition. Therefore, adding xylanase to wheat feed can improve the net energy level.

[0010] However, in the above methods, using low-protein feed, adjusting the crude protein content in the diet, and adjusting the type of feed all have the disadvantage of requiring high-quality feed types and ingredients. Adding exogenous protease is a method proposed for low-protein feed, and adding xylanase is a method proposed for wheat feed, aiming to improve the utilization efficiency of nutrients in the feed. However, the improvement effect is greatly influenced by the type of feed, and the stability of the enzyme is poor, resulting in a large influence of the environment on the improvement effect.

[0011] Feed additives are small or trace amounts of substances added to feed to ensure and improve feed quality and increase feed utilization. They have obvious effects on improving animal production performance, maintaining intestinal health, saving breeding costs, and improving the quality of livestock products. Feed additives have the advantages of diverse types and simple use, and are widely used in production. According to the content disclosed by HE, W. Z. Application of guanidino acetic acid and immobilized intracellular enzyme in low-energy feed for broilers. Master's thesis of Chinese Academy of Agricultural Sciences. June 2023, the amino acid derivative guanidino acetic acid can improve the metabolism of arginine and glycine, increase the utilization of amino acids, and improve the net energy production of broilers. Adding amino acid derivatives guanidino acetic acid to low-energy feed can improve the production performance of broilers, achieving body weight, feed conversion ratio, breast muscle rate, and leg muscle rate comparable to or slightly better than conventional feed. Therefore, adding feed additives to feed can also improve the net energy level.

[0012] Betaine is also known as betanin, which is an alkaline substance contained in sugar beet tubers. Pure product is colorless crystalline, which can be used as animal feed additives to supplement the methylation required by biological metabolism. According to Liu Lifu. Betaine as a feed additive in the application of livestock and poultry production. New agriculture. October 2020, betaine is widely used in broiler breeding industry. Adding betaine in the process of feeding broilers can significantly accelerate the growth and development of broilers and improve feed utilization. The applicant tried to add betaine as a feed additive to broiler feed and found that betaine can improve the net energy level of broilers. However, according to Qingkong Yanyan. Cost angle to consider the application of betaine in poultry feed. Feed wide angle. January 2013, betaine has certain liquidity, so its addition in feed is also limited. Therefore, betaine hydrochloride obtained by crystallizing hydrochloric acid betaine with correct application carrier is born, and it is also disclosed that different forms of betaine have the same metabolic composition when passing through the stomach, so whether betaine hydrochloride or anhydrous betaine can be used as an effective feed additive in animal production.

[0013] According to Abdurahman Jiang Nasr et al. Research on the synthesis method of betaine hydrochloride. Chemical reagents. November 2013, in the preparation of betaine hydrochloride, the by-product sodium chloride or calcium chloride in the product is difficult to separate and remove, which needs to use desalting technology to remove by-products, further leading to low product purity, complex separation process and high energy consumption. Considering that betaine phosphate almost quantitatively precipitates in 95% ethanol, and the crystal shape is good, it is basically not hygroscopic, so the applicant adds betaine phosphate as a feed additive to broiler feed and finds that betaine phosphate, as one of the main forms of betaine, can also improve the net energy level of broilers.

[0014] However, when betaine phosphate is directly used as a feed additive to improve the net energy level of broilers, the following problems exist: 1. According to the content disclosed in Luogang. Interrelationship between poultry egg methionine and choline, betaine, inorganic sulfate. China Poultry Guide. July 2000, egg methionine plays an important role in the methylation process together with betaine, in metabolism, betaine can only provide methyl groups, and cannot "replace" or "save" intact egg acid molecules for protein synthesis in the feed. Therefore, when betaine phosphate is used alone, the effect is limited, and egg methionine and betaine phosphate need to be mixed, but egg methionine has certain hygroscopicity and is easy to be damp, and the feed additive prepared by mixing egg methionine and betaine phosphate has the problem of being easy to be damp. Although egg methionine zinc can be used instead of egg methionine, according to the content disclosed in Duan Jingna. Preparation method of large particle size egg methionine zinc complex and application in laying hen premix. Animal Husbandry and Veterinary Science. January 2021, the particle size of the egg methionine chelate on the market is small, the viscosity is large, the density is small, the flowability is poor, and it is difficult to fully mix with the feed, and further, the effect of improving the net energy level of the prepared feed additive is affected.

[0015] 2. When betaine phosphate is used as a feed additive for improving 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 the broiler feed, according to the content disclosed in Lv Yanqun. Selection and use of trace feed additive carriers. China Feed. June 2008, the effectiveness, uniformity and consistency of active ingredients in the feed additive can be ensured by adding carriers to the feed additive. However, it can be seen from the document that different carriers have different performances, and the adhesion of betaine phosphate and egg methionine or egg methionine chelate is different. The adhesion of inorganic carriers is low, and they are mainly used for the preparation of trace element premixes. The adhesion of organic carriers is low, and they are mainly used for drug additives. Considering that the adhesion of inorganic carriers is low, the feed additive prepared from inorganic carriers is prone to powdering when stored at high temperature. Therefore, in order to ensure the adhesion of betaine phosphate and egg methionine or egg methionine chelate, the most commonly used method at present is to use organic carriers with strong adhesion. However, the stronger the adhesion, the more likely the carrier is to stick together, and further, the prepared feed additive is more likely to stick together. SUMMARY

[0016] In view of the deficiencies in the prior art, the present application provides a betaine phosphate-containing feed additive for improving the net energy level and a preparation method and application thereof. The prepared feed additive has a strong effect on improving the net energy level of broilers, is not prone to sticking together, and has good storage resistance.

[0017] To solve the above technical problems, the technical solutions adopted by the present application are as follows: The preparation method of the feed additive containing betaine phosphate for improving net energy level, comprising: preparing composite betaine phosphate, preparing composite zinc methionine, mixing; The preparation of the composite betaine phosphate comprises: preparing betaine phosphate crude product, preparing composite silicon dioxide carrier, and crystallizing; In the preparation of the betaine phosphate crude product, the aqueous solution of trimethylamine is stirred at a stirring speed of 100-300 rpm at room temperature, then the chloroacetic acid and sodium hydroxide are added, the temperature is raised to 50-55 DEG C, and the stirring is carried out for 120-150 min, the temperature is raised to 70-75 DEG C, and the stirring is carried out for 120-150 min, the temperature is lowered to room temperature, part of the water is evaporated by reduced pressure concentration, the temperature is lowered to room temperature, the filtration is carried out, the filtrate is taken, the filtrate is stirred at a stirring speed of 100-300 rpm at room temperature, then the aqueous solution of phosphoric acid is added, the stirring is carried out for 90-120 min, the aqueous solution of ethanol is added, the temperature is raised to 70-75 DEG C, the stirring is carried out for 10-15 min, the temperature is lowered to 0-5 DEG C, the standing is carried out for 25-30 h, the filtration is carried out, the filter residue is taken, the filter residue is washed for 2-3 times, and the drying is carried out to obtain the betaine phosphate crude product; In the preparation of the betaine phosphate crude product, the mass concentration of the aqueous solution of trimethylamine is 30%; The mass concentration of the aqueous solution of phosphoric acid is 85%; The volume concentration of the aqueous solution of ethanol is 95%; The mass ratio of the aqueous solution of trimethylamine, the chloroacetic acid, the sodium hydroxide, and the aqueous solution of phosphoric acid is 330-350:159-168:67.5-72:200-220; The mass ratio of the aqueous solution of trimethylamine and part of the water in the part of the water evaporated by reduced pressure concentration is 330-350:100-110; The mass ratio of the aqueous solution of trimethylamine and the aqueous solution of ethanol is 330-350:150-170; When the filter residue is washed for 2-3 times, the aqueous solution of ethanol with a volume concentration of 95% is used for washing; In the preparation of the composite silicon dioxide carrier, the rice starch and water are mixed, then the stirring is carried out at a stirring speed of 50-100 rpm at room temperature for 30-40 min, the temperature is raised to 85-90 DEG C, the stirring is carried out for 90-120 min, the temperature is lowered to room temperature, the silicon dioxide is added, the stirring is carried out for 120-150 min, the filtration is carried out, the filter residue is taken, and the drying is carried out to obtain the composite silicon dioxide carrier; In the preparation of the composite silicon dioxide carrier, the mass ratio of the rice starch, the water, and the silicon dioxide is 10-11:1000-1200:100-110; The mesh number of the silicon dioxide is 40-80; The crystallization, after mixing the betaine phosphate crude product and water, is heated to 85-90 DEG C, stirred at a stirring speed of 50-100 rpm for 30-40 min, the composite silicon dioxide carrier is added, stirred for 30-40 min, part of the water is evaporated by reduced pressure concentration, cooled to room temperature, the ethanol aqueous solution is added, cooled to 0-5 DEG C, and then placed for 25-30 h, filtered, the filter residue is taken, the filter residue is washed for 2-3 times, dried, and the composite betaine phosphate is obtained; In the crystallization, the volume concentration of the ethanol aqueous solution is 95%; The mass ratio of the betaine phosphate crude product, water and composite silicon dioxide carrier is 50-55:5000-6000:500-600; The mass ratio of the betaine phosphate crude product and part of the water in the part of the water evaporated by reduced pressure concentration is 50-55:4800-5800; The mass ratio of the betaine phosphate crude product and the ethanol aqueous solution is 50-55:200-300; When the filter residue is washed for 2-3 times, the ethanol aqueous solution with a volume concentration of 95% is used for washing; The preparation of the composite methionine zinc comprises: preparing an activated silicon dioxide carrier, adsorbing starch, and adsorbing methionine zinc; The preparation of the activated silicon dioxide carrier, after mixing the silicon dioxide, the calcium chloride aqueous solution and the zinc sulfate aqueous solution, is stirred at a stirring speed of 50-100 rpm for 60-90 min at room temperature, the sodium hydroxide aqueous solution is added to adjust the pH to 8.5-9, stirred for 30-60 min, filtered, the filter residue is taken, the filter residue is washed for 2-3 times, dried, and the activated silicon dioxide carrier is obtained; In the preparation of the activated silicon dioxide carrier, the mass concentration of the calcium chloride aqueous solution is 1%; The mass concentration of the zinc sulfate aqueous solution is 1%; The mass concentration of the sodium hydroxide aqueous solution is 5%; The mass ratio of the silicon dioxide, the calcium chloride aqueous solution and the zinc sulfate aqueous solution is 100-110:500-600:500-600; The mesh number of the silicon dioxide is 40-80 mesh; When the filter residue is washed for 2-3 times, water is used for washing; The adsorption of starch, after mixing the rice starch and water, is stirred at a stirring speed of 50-100 rpm for 30-40 min at room temperature, heated to 85-90 DEG C, and stirred for 90-120 min, cooled to room temperature, the activated silicon dioxide carrier is added, stirred for 40-60 min, filtered, the filter residue is taken, and dried, and the silicon dioxide carrier after adsorption of starch is obtained; The mass ratio of rice starch, water and activated silicon dioxide carrier in the adsorbed starch is 5-5.5:1000-1200:100-110; In the adsorbed zinc methionine, the mass ratio of methionine, water, adsorbed starch silicon dioxide carrier and anhydrous zinc sulfate is 6-6.5:600-700:60-65:3.2-3.4. In the adsorbed zinc methionine, the mass ratio of methionine, water, adsorbed starch silicon dioxide carrier and anhydrous zinc sulfate is 6-6.5:600-700:60-65:3.2-3.4. In the mixing, the mass ratio of the compound betaine phosphate and the compound zinc methionine is 4-4.2:1. In the mixing, the mass ratio of the compound betaine phosphate and the compound zinc methionine is 4-4.2:1.

[0018] A betaine phosphate-containing feed additive with improved net energy level prepared by the preparation method.

[0019] Compared with the prior art, the betaine phosphate-containing feed additive with improved net energy level has the following beneficial effects: The feed additive prepared by the method does not have the problem of sticking together, does not have the problem of powder loss and sticking together after being stored in an environment with a temperature of 30±2℃ and a relative humidity of 55±1% for 42 days, and can significantly improve the net energy level. DETAILED DESCRIPTION

[0020] In order to have a clearer understanding of the technical features, objectives and effects of the present application, the specific embodiments of the present application will be described.

[0021] The room temperature in examples 1-2 and comparative examples 1-3 is 23±2℃.

[0022] Example 1 A preparation method of a betaine phosphate-containing feed additive with improved net energy level, specifically as follows: 1. Preparation of compound betaine phosphate: (1) Preparation of betaine phosphate crude product: 330 g of 30% trimethylamine aqueous solution was stirred at room temperature at a stirring speed of 100 rpm, then 159 g of chloroacetic acid and 67.5 g of sodium hydroxide were added, the temperature was raised to 50 °C, stirred for 120 min, the temperature was raised to 70 °C, stirred for 120 min, the temperature was lowered to room temperature, 100 g of water was distilled off by reduced pressure concentration, cooled to room temperature, filtered, and the filtrate was stirred at room temperature at a stirring speed of 100 rpm, then 200 g of 85% phosphoric acid aqueous solution was added, stirred for 90 min, 150 g of 95% ethanol aqueous solution was added, the temperature was raised to 70 °C, stirred for 10 min, the temperature was lowered to 0 °C, and stood for 25 h, filtered, and the filter residue was washed with 95% ethanol aqueous solution twice, dried, and the betaine phosphate crude product was obtained; (2) Preparation of composite silica carrier: 10 g of rice starch and 1000 g of water were mixed, stirred at room temperature at a stirring speed of 50 rpm for 30 min, the temperature was raised to 85 °C, stirred for 90 min, the temperature was lowered to room temperature, 100 g of silica was added, stirred for 120 min, filtered, and the filter residue was dried to obtain the composite silica carrier; The mesh number of the silica is 40 mesh; (3) Crystallization: 50 g of betaine phosphate crude product and 5000 g of water were mixed, the temperature was raised to 85 °C, stirred at a stirring speed of 50 rpm for 30 min, 500 g of composite silica carrier was added, stirred for 30 min, 4800 g of water was distilled off by reduced pressure concentration, the temperature was lowered to room temperature, 200 g of 95% ethanol aqueous solution was added, the temperature was lowered to 0 °C, and stood for 25 h, filtered, the filter residue was washed with 95% ethanol aqueous solution twice, dried, and the composite betaine phosphate was obtained; 2. Preparation of composite methionine zinc: (1) Preparation of activated silica carrier: 100 g of silica, 500 g of 1% calcium chloride aqueous solution, and 500 g of 1% zinc sulfate aqueous solution were mixed, stirred at room temperature at a stirring speed of 50 rpm for 60 min, 5% sodium hydroxide aqueous solution was added to adjust the pH to 8.5, stirred for 30 min, filtered, the filter residue was washed with water twice, and dried to obtain the activated silica carrier; The mesh number of the silica is 40 mesh; (2) Adsorption of starch: 5 g of rice starch and 1000 g of water were mixed, stirred at room temperature at a stirring speed of 50 rpm for 30 min, the temperature was raised to 85 °C, stirred for 90 min, the temperature was lowered to room temperature, 100 g of activated silica carrier was added, stirred for 40 min, filtered, and the filter residue was dried to obtain the silica carrier after adsorption of starch; (3) adsorbing zinc methionine: 6 g of methionine and 600 g of water were mixed, and then heated to 85°C, stirred at a stirring speed of 50 rpm for 5 min, 60 g of the silica carrier after adsorbing starch was added, stirred for 10 min, 3.2 g of anhydrous zinc sulfate was added, stirred for 60 min, filtered, and the residue was obtained and dried to obtain the composite zinc methionine; 3. mixing: the composite betaine phosphate and the composite zinc methionine were mixed at a mass ratio of 4:1, stirred at a stirring speed of 20 rpm for 30 min at room temperature, and a betaine phosphate-containing feed additive for improving net energy level was obtained.

[0023] The embodiment also provides a betaine phosphate-containing feed additive for improving net energy level prepared by the preparation method.

[0024] Example 2 A preparation method of a betaine phosphate-containing feed additive for improving net energy level, specifically as follows: 1. preparing the composite betaine phosphate: (1) preparing the crude betaine phosphate: 350 g of a 30% mass concentration of trimethylamine aqueous solution was stirred at a stirring speed of 300 rpm at room temperature, then 168 g of chloroacetic acid and 72 g of sodium hydroxide were added, heated to 55°C, stirred for 150 min, heated to 75°C, stirred for 150 min, cooled to room temperature, 110 g of water was distilled out by reduced pressure concentration, cooled to room temperature, filtered, and the filtrate was stirred at a stirring speed of 300 rpm at room temperature, then 220 g of an 85% mass concentration of phosphoric acid aqueous solution was added, stirred for 120 min, 170 g of a 95% volume concentration of ethanol aqueous solution was added, heated to 75°C, stirred for 15 min, cooled to 5°C, and stood for 30 h, filtered, the residue was obtained and washed with a 95% volume concentration of ethanol aqueous solution for 3 times, and dried to obtain the crude betaine phosphate; (2) preparing the composite silica carrier: 11 g of rice starch and 1200 g of water were mixed, stirred at a stirring speed of 100 rpm at room temperature for 40 min, heated to 90°C, stirred for 120 min, cooled to room temperature, 110 g of silica was added, stirred for 150 min, filtered, and the residue was obtained and dried to obtain the composite silica carrier; The mesh number of the silica is 40 mesh; (3) Crystallization: 55 g of the crude betaine phosphate and 6000 g of water were mixed, heated to 90°C, stirred at a stirring speed of 100 rpm for 40 min, 600 g of the composite silicon dioxide carrier was added, stirred for 40 min, 5800 g of water was evaporated by reduced pressure concentration, cooled to room temperature, 300 g of ethanol aqueous solution with a volume concentration of 95% was added, cooled to 5°C, and stood for 30 h, filtered, and the filter residue was taken and washed with 95% ethanol aqueous solution for 3 times, and dried to obtain the composite betaine phosphate; 2. Preparation of the composite zinc methionine: (1) Preparation of the activated silicon dioxide carrier: 110 g of silicon dioxide, 600 g of 1% calcium chloride aqueous solution, and 600 g of 1% zinc sulfate aqueous solution were mixed, stirred at a stirring speed of 100 rpm for 90 min at room temperature, 5% sodium hydroxide aqueous solution was added to adjust the pH to 9, stirred for 60 min, filtered, the filter residue was taken and washed with water for 3 times, and dried to obtain the activated silicon dioxide carrier; The mesh number of the silicon dioxide is 40 mesh; (2) Adsorption of starch: 5.5 g of rice starch and 1200 g of water were mixed, stirred at a stirring speed of 100 rpm for 40 min at room temperature, heated to 90°C, stirred for 120 min, cooled to room temperature, 110 g of the activated silicon dioxide carrier was added, stirred for 60 min, filtered, the filter residue was taken and dried to obtain the silicon dioxide carrier after adsorption of starch; (3) Adsorption of zinc methionine: 6.5 g of methionine and 700 g of water were mixed, heated to 90°C, stirred at a stirring speed of 100 rpm for 10 min, 65 g of the silicon dioxide carrier after adsorption of starch was added, stirred for 20 min, 3.4 g of anhydrous zinc sulfate was added, stirred for 90 min, filtered, the filter residue was taken and dried to obtain the composite zinc methionine; 3. Mixing: the composite betaine phosphate and the composite zinc methionine were mixed according to a mass ratio of 4.2:1, stirred at a stirring speed of 40 rpm for 40 min at room temperature to obtain the betaine phosphate-containing feed additive with improved net energy level.

[0025] The embodiment also provides a betaine phosphate-containing feed additive with improved net energy level prepared by the preparation method.

[0026] Comparative Example 1 A preparation method of a betaine phosphate-containing feed additive with improved net energy level is as follows: 1. Preparation of betaine phosphate: (1) Preparation of betaine phosphate crude product: 330 g of a 30% mass concentration trimethylamine aqueous solution was stirred at room temperature at a stirring speed of 100 rpm, then 159 g of chloroacetic acid and 67.5 g of sodium hydroxide were added, the temperature was raised to 50℃, and stirring was performed for 120 min, the temperature was raised to 70℃, and stirring was performed for 120 min, the temperature was lowered to room temperature, 100 g of water was distilled off by reduced pressure concentration, the temperature was lowered to room temperature, and the filtrate was obtained, the filtrate was stirred at room temperature at a stirring speed of 100 rpm, then 200 g of a 85% mass concentration phosphoric acid aqueous solution was added, stirring was performed for 90 min, 150 g of a 95% volume concentration ethanol aqueous solution was added, the temperature was raised to 70℃, and stirring was performed for 10 min, the temperature was lowered to 0℃, and standing was performed for 25 h, centrifugation was performed, the precipitate was obtained, the precipitate was washed twice with a 95% volume concentration ethanol aqueous solution, and drying was performed, to obtain a betaine phosphate crude product; (2) Crystallization: 50 g of the betaine phosphate crude product and 25 g of water were mixed, the temperature was raised to 85℃, and stirring was performed at a stirring speed of 50 rpm for 30 min, the temperature was lowered to room temperature, 25 g of a 95% volume concentration ethanol aqueous solution was added, the temperature was lowered to 0℃, and standing was performed for 25 h, centrifugation was performed, the precipitate was obtained, the precipitate was washed twice with a 95% volume concentration ethanol aqueous solution, and drying was performed, to obtain a betaine phosphate; 2. Preparation of zinc methionine: 6 g of methionine and 60 g of water were mixed, the temperature was raised to 85℃, and stirring was performed at a stirring speed of 50 rpm for 5 min, 3.2 g of anhydrous zinc sulfate was added, a 5% mass concentration sodium hydroxide aqueous solution was used to adjust the pH to 7, and stirring was performed for 60 min, centrifugation was performed, the precipitate was obtained, and drying was performed, to obtain a complex zinc methionine; 3. Mixing: the betaine phosphate and the zinc methionine were mixed according to a mass ratio of 4:1, and stirring was performed at a stirring speed of 20 rpm at room temperature for 30 min, to obtain a betaine phosphate-containing feed additive for improving net energy level.

[0027] The comparative example also provides a betaine phosphate-containing feed additive for improving net energy level, which is prepared by the preparation method.

[0028] Comparative Example 2 A preparation method of a betaine phosphate-containing feed additive for improving net energy level is as follows: 1. Preparation of complex betaine phosphate: (1) Preparation of betaine phosphate crude product: 330 g of 30% trimethylamine aqueous solution was stirred at room temperature at a stirring speed of 100 rpm, then 159 g of chloroacetic acid and 67.5 g of sodium hydroxide were added, the temperature was raised to 50℃, and stirred for 120 min, the temperature was raised to 70℃, and stirred for 120 min, the temperature was lowered to room temperature, 100 g of water was distilled off by reduced pressure concentration, and cooled to room temperature, then filtered, the filtrate was stirred at room temperature at a stirring speed of 100 rpm, then 200 g of 85% phosphoric acid aqueous solution was added, stirred for 90 min, 150 g of 95% ethanol aqueous solution was added, the temperature was raised to 70℃, and stirred for 10 min, the temperature was lowered to 0℃, and stood for 25 h, then filtered, the filter residue was washed with 95% ethanol aqueous solution twice, and dried to obtain the betaine phosphate crude product; (2) Crystallization: 50 g of betaine phosphate crude product and 5000 g of water were mixed, the temperature was raised to 85℃, and stirred at a stirring speed of 50 rpm for 30 min, 500 g of silicon dioxide was added, and stirred for 30 min, 4800 g of water was distilled off by reduced pressure concentration, the temperature was lowered to room temperature, 200 g of 95% ethanol aqueous solution was added, the temperature was lowered to 0℃, and stood for 25 h, then filtered, the filter residue was washed with 95% ethanol aqueous solution twice, and dried to obtain the composite betaine phosphate; The mesh number of the silicon dioxide is 40 mesh; 2. Preparation of composite zinc methionine: 6 g of methionine and 600 g of water were mixed, the temperature was raised to 85℃, and stirred at a stirring speed of 50 rpm for 5 min, 60 g of silicon dioxide was added, and stirred for 10 min, 3.2 g of anhydrous zinc sulfate was added, and stirred for 60 min, then filtered, and the filter residue was dried to obtain the composite zinc methionine; The mesh number of the silicon dioxide is 40 mesh; 3. Mixing: the composite betaine phosphate and the composite zinc methionine were mixed according to a mass ratio of 4:1, and stirred at a stirring speed of 20 rpm at room temperature for 30 min to obtain the betaine phosphate-containing feed additive for improving net energy level.

[0029] The comparative example also provides a betaine phosphate-containing feed additive for improving net energy level prepared by the preparation method.

[0030] Comparative Example 3 A preparation method of a betaine phosphate-containing feed additive for improving net energy level is provided, and specifically as follows: 1. Preparation of composite betaine phosphate: (1) Preparation of betaine phosphate crude product: 330 g of 30% trimethylamine aqueous solution was stirred at room temperature at a stirring speed of 100 rpm, then 159 g of chloroacetic acid and 67.5 g of sodium hydroxide were added, the temperature was raised to 50 °C, and stirred for 120 min, the temperature was raised to 70 °C, and stirred for 120 min, the temperature was lowered to room temperature, 100 g of water was distilled out by reduced pressure concentration, and cooled to room temperature, and filtered, the filtrate was stirred at room temperature at a stirring speed of 100 rpm, then 200 g of 85% phosphoric acid aqueous solution was added, stirred for 90 min, 150 g of 95% ethanol aqueous solution was added, the temperature was raised to 70 °C, and stirred for 10 min, the temperature was lowered to 0 °C, and stood for 25 h, and filtered, the filter residue was washed with 95% ethanol aqueous solution twice, and dried to obtain the betaine phosphate crude product; (2) Preparation of composite silica carrier: 10 g of rice starch and 1000 g of water were mixed, and stirred at room temperature at a stirring speed of 50 rpm for 30 min, the temperature was raised to 85 °C, and stirred for 90 min, the temperature was lowered to room temperature, 100 g of silica was added, and stirred for 120 min, and filtered, the filter residue was dried to obtain the composite silica carrier; The mesh number of the silica is 40 mesh; (3) Crystallization: 50 g of betaine phosphate crude product and 5000 g of water were mixed, the temperature was raised to 85 °C, and stirred at a stirring speed of 50 rpm for 30 min, 500 g of composite silica carrier was added, and stirred for 30 min, 4800 g of water was distilled out by reduced pressure concentration, the temperature was lowered to room temperature, 200 g of 95% ethanol aqueous solution was added, the temperature was lowered to 0 °C, and stood for 25 h, and filtered, the filter residue was washed with 95% ethanol aqueous solution twice, and dried to obtain the composite betaine phosphate; 2. Preparation of composite methionine zinc: (1) Adsorption of starch: 5 g of rice starch and 1000 g of water were mixed, and stirred at room temperature at a stirring speed of 50 rpm for 30 min, the temperature was raised to 85 °C, and stirred for 90 min, the temperature was lowered to room temperature, 100 g of silica was added, and stirred for 40 min, and filtered, the filter residue was dried to obtain the silica carrier after adsorption of starch; The mesh number of the silica is 40 mesh; (2) Adsorption of methionine zinc: 6 g of methionine and 600 g of water were mixed, the temperature was raised to 85 °C, and stirred at a stirring speed of 50 rpm for 5 min, 60 g of silica carrier after adsorption of starch was added, and stirred for 10 min, 3.2 g of anhydrous zinc sulfate was added, and stirred for 60 min, and filtered, the filter residue was dried to obtain the composite methionine zinc; 3. Mixing: mixing the complex betaine phosphate and the complex methionine zinc according to the mass ratio of 4:1, stirring at the stirring speed of 20 rpm for 30 min at room temperature to obtain the betaine phosphate-containing feed additive with improved net energy level.

[0031] The comparative example also provides the betaine phosphate-containing feed additive with improved net energy level prepared by the preparation method.

[0032] Test Example 1 Whether the feed additives prepared in Examples 1-2 and Comparative Examples 1-3 have the problem of sticking together is observed, and the observation results are as follows:

[0033] It can be seen from the results of the test example that the feed additives prepared in Examples 1-2 and Comparative Examples 1-3 do not have the problem of sticking together, which shows that the complex carrier prepared by compounding starch and silicon dioxide can avoid the problem of sticking together when only using starch organic carrier.

[0034] Test Example 2 The feed additives prepared in Examples 1-2 and Comparative Examples 1-3 are respectively sealed in film bags, and then stored in an environment with a temperature of 30±2℃ and a relative humidity of 55±1% for 42 days, and then whether there is the problem of powder dropping and sticking together is observed (since Example 1 does not use carrier in the preparation of the feed additive, therefore, whether the feed additive prepared in Comparative Example 1 has the problem of powder dropping does not need to be observed), and the observation results are as follows:

[0035] It can be seen from the results of the test example that the storage resistance of the feed additives prepared in Examples 1-2 is good.

[0036] Test Example 3 180 20-day-old white-feathered broilers are selected and randomly divided into 6 groups, wherein 1-5 groups are used as test groups, and 6 group is used as a blank control group. The feed additives of Examples 1-2 and Comparative Examples 1-3 are respectively added to the daily diet of the white-feathered broilers in 1-5 groups, the addition amount of the feed additives of Examples 1-2 and Comparative Examples 2-3 is 2%, the addition amount of the feed additive of Comparative Example 1 is 0.2%, and the daily diet of the white-feathered broilers in 6 group does not add any feed additive, each group has 6 replicates, and each replicate has 5 white-feathered broilers.

[0037] In the test, the white-feathered broilers in 1-6 groups use the same basic daily diet, and the composition of the basic daily diet is as follows:

[0038] The test was carried out in the Animal Nutrition and Feed Research Institute of Jilin Provincial Academy of Agricultural Sciences. The feeding and management referred to the "AA Chicken Raising and Management Manual 2019". Groups 1-6 all used cage feeding. During the test, groups 1-6 white feather chickens all used free feeding and drinking water. The environment in the house was adjusted according to the age of the chickens.

[0039] After continuous feeding for 5 days, the daily feed intake and daily weight gain of each white feather chicken in each group were tested, the average value of each group was calculated, then the average value of 6 replicates of each group was calculated, and the feed-meat ratio of each group was calculated. The results are as follows:

[0040] After continuous feeding for 5 days, the net energy level of groups 1-6 white feather chickens was tested by respiratory calorimetry. Specifically, 2 white feather chickens were selected from each replicate of each group and transferred into the respiratory calorimetry device for adaptation for 1 day, and respiratory calorimetry test for 3 days. During the test, the basic diet, feed additive and feeding method of each group were kept unchanged. The daily feed intake and daily weight gain of each white feather chicken in each group during the test were tested, the average value of 6 replicates of each group was calculated, and the feed-meat ratio of each group was calculated. The results are as follows:

[0041] At the same time, the average value of the energy data of 6 replicates of each group was calculated, and the results are as follows:

[0042] From the results of this test example, it can be seen that the feed-meat ratio of the feed additive prepared in examples 1-2 is the lowest, and the net energy level is the highest. Although the feed additives prepared in comparative examples 1-3 and example 1 all use betaine phosphate and methionine as the main component, comparative example 1 does not use a carrier, which makes it difficult for the feed additive prepared in comparative example 1 to disperse uniformly in the basic diet, resulting in uneven intake of betaine phosphate and methionine by white feather chickens, which affects the net energy level of group 3 white feather chickens; the carrier used in comparative example 2 is not treated, which has limited adhesion to betaine phosphate and methionine, and also has the problem of powder loss, resulting in uneven intake and reduced intake of betaine phosphate and methionine by white feather chickens, which affects the net energy level of group 4 white feather chickens; the carrier used in the preparation of compound methionine zinc in comparative example 3 is not activated, which causes the instability of methionine zinc in the compound methionine zinc, and also affects the adhesion of methionine zinc to the carrier. Further, it has a certain influence on the net energy level of group 5 white feather chickens.

[0043] In summary, in the preparation of feed additives, it is necessary to prepare betaine phosphate into a compound betaine phosphate and prepare zinc methionine into a compound zinc methionine. In the preparation of compound betaine phosphate, the principle used is that rice starch is first adsorbed on the surface of the silica carrier by intermolecular forces such as hydrogen bonds, and then according to the content disclosed by Wang Xiaoying in "Betaine and its hydrochloride inhibit indica rice retrogradation and its application in alpha-indica rice instant rice." Master's thesis, Central South University of Forestry and Technology. May 2013, the betaine structure can wrap starch, so there is intermolecular force between the betaine structure and the starch, which uniformly disperses the betaine phosphate on the surface of the silica carrier. Further, in crystallization, it promotes the uniform dispersion of betaine phosphate crystals on the surface of the silica carrier, so the starch can improve the bonding force of betaine phosphate crystals to the silica carrier and promote the uniform distribution of betaine phosphate crystals on the surface of the silica carrier. In the preparation of compound zinc methionine, the principle used is that calcium ions and zinc ions can be adsorbed on the surface of the silica carrier to obtain activated silica carrier, then starch is adsorbed on the surface of the silica by the interaction force between starch and calcium ions, and then according to the content disclosed by Gao Binghui et al. in "Dry process for preparing amino acid-polysaccharide-copper organic chelate." Fujian Journal of Animal Husbandry and Veterinary Medicine. September 2025, according to the multiple complexation between starch polysaccharide and methionine and calcium ions and zinc ions, methionine is uniformly dispersed on the surface of the silica carrier, wherein calcium ions play a role in connecting starch polysaccharide and methionine, and zinc ions play a role in complexing methionine to form zinc methionine crystal seeds, then zinc sulfate is added to uniformly complex zinc ions on the surface of the silica, achieving uniform distribution of zinc methionine crystals, and using the interaction between starch polysaccharide and zinc methionine to reduce the stickiness of compound zinc methionine and improve the flowability of compound zinc methionine. At the same time, the organic carrier (starch) and inorganic carrier (silica) are compounded, while ensuring adhesion, flowability and anti-caking properties.

Claims

1. A method for the preparation of a betaine phosphate containing feed additive with improved net energy level, characterized in that, The application relates to a preparation method of a betaine phosphate feed additive. The preparation method comprises the following steps: preparing a betaine phosphate compound, preparing a methionine zinc compound, and mixing. The preparation method of the betaine phosphate compound comprises the following steps: preparing a betaine phosphate crude product, preparing a compound silicon dioxide carrier, and crystallizing. The preparation method of the compound silicon dioxide carrier comprises the following steps: mixing rice starch and water, stirring at room temperature, heating to 85-90 DEG C, stirring, cooling to room temperature, adding silicon dioxide, stirring, filtering, taking the filter residue, and drying to obtain the compound silicon dioxide carrier. The crystallizing step comprises the following steps: mixing the betaine phosphate crude product and water, heating to 85-90 DEG C, stirring, adding the compound silicon dioxide carrier, stirring, evaporating part of water through vacuum concentration, cooling to room temperature, adding an ethanol aqueous solution, cooling, standing, filtering, washing the filter residue, drying, and obtaining the betaine phosphate compound. The preparation method of the methionine zinc compound comprises the following steps: preparing an activated silicon dioxide carrier, adsorbing starch, and adsorbing methionine zinc. The adsorbing methionine zinc step comprises the following steps: mixing methionine and water, heating to 85-90 DEG C, stirring, adding the silicon dioxide carrier after adsorbing starch, stirring, adding anhydrous zinc sulfate, stirring, filtering, taking the filter residue, and drying to obtain the methionine zinc compound. The mixing step comprises the following step: uniformly mixing the betaine phosphate compound and the methionine zinc compound to obtain the betaine phosphate feed additive.

2. The method of preparing a betaine phosphate containing feed additive for improved net energy level according to claim 1, characterized in that, The preparation method of the betaine phosphate crude product comprises the following steps: stirring a trimethylamine aqueous solution at room temperature, then adding chloroacetic acid and sodium hydroxide, heating to 50-55 DEG C, stirring, heating to 70-75 DEG C, stirring, cooling to room temperature, evaporating part of water through vacuum concentration, cooling to room temperature, filtering, stirring the filtrate at room temperature, adding a phosphoric acid aqueous solution, stirring, adding an ethanol aqueous solution, heating to 70-75 DEG C, stirring, cooling to 0-5 DEG C, standing, filtering, washing the filter residue, drying, and obtaining the betaine phosphate crude product.

3. The method of preparing a betaine phosphate containing feed additive for improved net energy level according to claim 2, characterized in that, In the preparation method of the betaine phosphate crude product, 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 the trimethylamine aqueous solution, the chloroacetic acid, the sodium hydroxide, and the phosphoric acid aqueous solution is 330-350:159-168:67.5-72:200-220. The mass ratio of the trimethylamine aqueous solution and part of water evaporated through vacuum concentration is 330-350:100-110. The mass ratio of the trimethylamine aqueous solution and the ethanol aqueous solution is 330-350:150-170.

4. The method of preparing a betaine phosphate containing feed additive for improved net energy level according to claim 1, characterized in that, In the preparation method of the compound silicon dioxide carrier, the mass ratio of the rice starch, the water, and the silicon dioxide is 10-11:1000-1200:100-110. The mesh number of the silicon dioxide is 40-80.

5. The method of preparing a betaine phosphate containing feed additive for improved net energy level according to claim 1, characterized in that, In the crystallizing step, the volume concentration of the ethanol aqueous solution is 95%. The mass ratio of the betaine phosphate crude product, the water, and the compound silicon dioxide carrier is 50-55:5000-6000:500-600. The mass ratio of the betaine phosphate crude product and part of water evaporated through vacuum concentration is 50-55:4800-5800. The mass ratio of the crude betaine phosphate to the ethanol aqueous solution is 50-55:200-300.

6. The method of preparing a betaine phosphate containing feed additive for improved net energy level according to claim 1, characterized in that, The activated silica carrier is prepared by mixing silica, calcium chloride aqueous solution and zinc sulfate aqueous solution, stirring at room temperature, adjusting pH to 8.5-9, stirring, filtering, taking the filter residue, washing the filter residue, and drying to obtain the activated silica carrier; In the preparation of the activated silica carrier, the mass concentration of the calcium chloride aqueous solution is 1%. The mass concentration of the zinc sulfate aqueous solution is 1%. The mass ratio of silica, calcium chloride aqueous solution, zinc sulfate aqueous solution is 100-110:500-600:500-600. The mesh number of the silica is 40-80.

7. The method of preparing a betaine phosphate containing feed additive for improved net energy level 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℃, stirring, cooling to room temperature, adding the activated silica carrier, stirring, filtering, taking the filter residue, and drying to obtain the silica carrier after adsorbing starch. In the adsorption of starch, the mass ratio of rice starch, water, and activated silica carrier is 5-5.5:1000-1200:100-110.

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

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

1.

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

10. Use of the feed additive of claim 9 in the preparation of a net energy level improving product.

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