Study on Preparation Process of Composite Amino Acid Chelate with Feed

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Summary is obtained by hydrolysis of feed grade sulfuric acid to obtain a composite amino acid, and a composite amino acid chelad zinc is prepared to the zinc sulfate, which is used as a new generation of feed additives. The effects of different factors on composite amino acid chelate zinc synthesis were studied by pH titled curves. When it was determined at the pH 7.1, the total amount of free amino acid and the zinc molar ratio were 2: 1, the chelation rate can reach 92% or more. Key words composite amino acids; chelation; zinc map Class S816.34 Metal trace eleme Amino acid chelate has been more than 10 years in my country. The amino acid chelate is absorbed to the metabolism superior to other general inorganic salts microefficie, and the main advantage of it is generally reported that the production of various enzy is promoted, enhances the immunity and resistance energy of the animal body. 2 trace eleme enter blood circulation with amino acid absorption pathway, and high absorption rate. 3 can alleviate antagonism competition between minerals, and various trace eleme are more thoroughly absorbed by livestock. 4 amino acid chelate is easily dissolved than inorganic salts, and the solubility is high [1]. Zinc is one of the necessary trace eleme of animals. As the third generation of feed additives, zinc amino acid zinc in the aquatic product, the application of the livestock farm industry has achieved significant results. The production of amino acid chelate salts is also mature. It can achieve good results with a single amino acid and trace element chelation, but in the application of a aquaculture industry, its cost is higher. There have been a few manufacturers to apply different protein sources to prepare composite amino acids, such as feather powder, blood powder and animal internal organs, etc., th raw materials have higher cost, some decomposition requireme are high, and some have a serious environmental pollution, not very ideal. In this paper, soybean meal is used as an amino acid source, and a composite amino acid is obtained by acid hydrolysis method, and then the composite amino acid is chelated with inorganic zinc to obtain a composite amino acid chelate zinc product. This method is simple, no pollution, and the cost is low, which is a ideal method. 1 Materials and Method 1.1 Test material soybean meal (feed grade, CP 43%), zinc sulfate (feed stage, 98%), sulfuric acid (analytical pure, 98%), lime pulp (commercially available), sodium hydroxide (analysis Pure), acetone (analyzing pure). 1.2 Test Equipment Atomic Absorption Spectrometry (SP2900), precise acidity gauge PHS-3C, filter, centrifugal precipitate. 1.3 Test Method 1.3.1 Soybean Water Water Solutions: Soybean Meal Crushed 16 h Sieve ¡ú Hydrogen Hydrogen Solution ¡ú Pumping Filter ¡ú Lime Terminal and ¡ú Soyfiltration ¡ú Composite Amino Acid Test Feed Grade Soybean Meal (Sense), first measure its crude protein After the content, after crushing, 4 mol / L sulfuric acid hydrolyzate is used in a certain amount of liquid. A certain amount of time was hydrolyzed at a certain temperature, and the free amino acid content was measured. 1.3.2 Chelating reaction chelation flow: Composite amino acid fluid ¡ú detect free amino acid quantity ¡ú zinc sulfate ¡ú adjust pH ¡ú insulation chelation ¡ú concentrated drying ¡ú Crushing moisture to prevent the composite amino acid solution to detect free amino acid content, after a certain The coordination ratio is added to zinc sulfate, and is adjusted to the best.The pH of the chelation, after the insulation is chelated, the material is concentrated. 1.4 Detection method 1.4.1 Determination of crude protein Kemifergic nitrogen. 1.4.2 Determination of free amino acids Improve formaldehyde method [2, 3]. 1.4.3 Determination of the chelation rate Principle Since the solubility of the composite amino acid chelate in the organic solvent such as acetone is extremely small, the free zinc can be dissolved in acetone solution [4]. With this characteristic, this paper uses acetone to precipitate the amino acid chelate zinc, filter out precipitate, and determine the soluble zinc in the filtrate. Methods are weighing 0.1 g of sample, adding 10 ml of distilled water, and after dissolving, the evaporation is concentrated to about 5 ml. Turn it into a 50 ml capacity bottle with acetone. Filtered with a quantitative slow filter paper, the suction filtrate diluted a certain number of ti to detect the zinc content. [NextPage] 2 Results and Discussion 2.1 The determination of soybean meal hydrolysis process parameters has more reports on soybean meal hydrolysis, which is more mature, and its conditional parameters are basically consistent. This paper uses 4 mol / L of sulfuric acid as a hydrolyzate, for easy control, normal pressure, boiling reflux [5]. The soybean meal was smashed over 16 h sieve. The soybean meal and the sulfuric acid solution were 1 g / 2.5 ml. The hydrolysis time is the most important parameter in normal pressure hydrolysis. In this paper, the best hydrolysis time is judged in the hydrolysis time – the amount of the alkaliogram curve, see Figure 1.

At different ti , a small amount of hydrolyzing was drawn, and the supernatant was clarified by the centrifuge, quantitatively sucking a certain volume, referring to the formaldehyde method for titration with the same concentration of sodium hydroxide solution. As can be seen from Figure 1, the hydrolysis time is more than 12 h, the curve is flat, and the total amount of free amino acid has been stabilized. Therefore, it is possible to determine whether the hydrolysis time is slightly greater than 12 h. 2.2 Determination of chelate parameters 2.2.1 Effect of the pH of the important parameter medium of the composite amino acid and zinc chelation, the molar ratio, chelation time, chelation temperature, etc. are important parameters that affect the composite amino acid and zinc chelation. The pH of the medium is the most affected by the chelation reaction. The pH is too large, and the hydroxyl group is easily formed to form a zinc hydroxide precipitate with zinc ions. The pH is too small, and the H + will replace the metal ions and the power supply group to reduce the chelate rate. Therefore, the precision control of the pH is critical to the chelation reaction. In this paper, the chelation reaction of zinc ions and composite amino acids is described herein by pH value, see Figure 2.
In FIG. 2, the AA curve is to titrate the composite amino acid curve with a sodium hydroxide solution of about 0.1 mol / L, and the AA + Zn curve is a composite of the same concentration of sodium hydroxide solution. Curve of amino acid solution. The curve C is the difference curve of the above two curves. As can be seen from Figure 2, when the pH of the AA + Zn line is about 4.5 or so, the C curve begins to rise rapidly, and H + is started in the system. This is in line with the theory of amino acid and metal ion chelation, ie each 2 molecular amino acids and 1 molecular zinc chelation,2 molecules of H + will be released. As the alkali is continuously added, when the pH is 6.3 to 7.1, when the pH is 6.3 to 7.1, the difference curve ebits a flat line, indicating that the added base is fully neutralized, resulting in no change in pH. PH u003d 7.1 can be considered as a completion point of the reaction, and therefore, it is determined herein to determine the optimum pH of 7.1. 2.2.2 Molar ratio of the probe ratio of the molar ratio means that the molar ratio of the free amino acid and zinc ion in the solution. The molar ratio is high, which is conducive to the zinc ion chelation, but the zinc concentration in the product is low, the utilization of amino acid is not high. This is unfavorable to reduce the cost of the product. The molar ratio is too low, then the chelation is incomplete, the product quality is low. In this paper, the total amount of free amino acid is 1: 1, 2: 1, 3: 1, 4: 1, respectively, in Table 1, respectively, in the same free amino acid.
The test results show that when the molar ratio is 2: 1 or more, the zinc ion can be compared to the composite amino acid chelation, so the determined molar ratio is 2: 1. 2.2.3 The effect of chelation temperature on the chelate rate has different reports on the temperature of the composite amino acid to the metal ion. This may be related to the different sources of composite amino acids. In this paper, chelation is carried out at a ratio of 2: 1, at 10 ¡ã C, 30 ¡ã C, 60 ¡ã C, 100 ¡ã C, and the test data is shown in Table 2.
The test results show that the temperature on the chelation reaction is not large. It can chelate better at room temperature. 2.2.4 Chelating time affects the chelation rate Chelating reaction is a rapid reaction, as long as the zinc salt is dissolved, the chelation reaction is basically completed [6]. The chelating reaction is characterized in that H + is generated in the solution, so the chelate reaction will be carried out, and the pH of the solution will be reduced. In this paper, the precise acidity coupling has been observed for a solution that has been adjusted to pH u003d 7.10, and the observation record is shown in Table 3.
It can be seen from Table 3 that the chelate reaction is fast, which is consistent with the literature report. 3 Conclusions 3.1 Synthesizing the composite amino acid chelate zinc synthesis process conditions, the mature parameter is 2: 1, the pH is 7.1, the temperature is room temperature, and the chelation ratio can reach more than 92%. The test method proposed in this paper has a certain reference value for the study of other metal ions and composite amino acid chelations. 3.2 On the basis of the test, the production process flow is initially determined as follows: soybean meal ¡ú broken ¡ú hydrolysis ¡ú medium sum ¡ú filtration ¡ú orthose amino acid ¡ú add zinc salt ¡ú adjust pH ¡ú chelation ¡ú concentrate dry ¡ú smash mix ¡ú finished packaging According to this article The composite amino acid chelate laboratory sample made by the determined parameters was tested for 32% of crude protein and 9% total zinc, which can meet the production needs of feed additives. There is a certain reference value for industrial production.

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