Study on Preparation Process of Composite Amino Acid Chelate with Feed

LIMA Fish Feed Machine,Chicken Feed Machine

Abstract To obtain a composite amino acid by hydrolysis by feed grade sulfuric acid, a composite amino acid chelate zinc is prepared from zinc sulfate, 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
Classification number S816.34
Research and development of metal trace elements 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 microefficients, and the main advantage of it is generally reported that the production of various enzymes is promoted, enhances the immunity and resistance energy of the animal body. 2 trace elements enter blood circulation with amino acid absorption pathway, and high absorption rate. 3 can alleviate antagonism competition between minerals, and various trace elements 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 elements 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., these raw materials have higher cost, some decomposition requirements 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 Material and Method
1. Test material
soybean meal (feed grade, CP 43%), zinc sulfate (feed stage, 98%), sulfuric acid (purified, 98%), lime pulp ( Commercially available), sodium hydroxide (purified), acetone (analytical pure).
1.2 Test equipment
Atomic absorption spectrophotometer (SP2900), precise acidity gauge PHS-3C, centrifuge, centrifugal precipitate.
1.3 Test method
1.3.1 Soybean meal hydrolysis
hydrolysis process:
soybean meal crushed 16 mesh sieve ¡ú hydrolysis ¡ú filtration ¡ú ʯ »Ò ¡ú ¡ú ¡ú filter ¡ú composite amino acid solution
The test feed grade soybean meal (released), first measured its crude protein content, and then hydrolyzed with 4 mol / L sulfuric acid according to 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
Chelating process:
Composite amino acid solution ¡ú detect free amino acid quantity ¡ú zinc sulfate ¡ú regulate pH ¡ú insulation chelation ¡ú concentrated drying ¡ú Crushing moisturizing preservation
After the composite amino acid fluid detects free amino acid content, after a certain The coordination ratio is added to zinc sulfate, adjusted to the optimum chelation pH, and after the insulation is chelated, the material fluid is concentrated.
1. Determination of the detection method
1.4.1 Determination of crude protein
Kemahi nitrogenic method.
1.4.2 Determination of free amino acid
Improve formaldehyde method [2, 3].
Determination of the chelate 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. Method
Tested 0.1 g of sample, dissolved 10 ml of distilled water, after dissolving, evaporated to the solution volume of 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 times to detect the zinc content.
2 Results and Discussion
2. Determination of Water Hydrolysis Process Parameters
About the information report on soybean meal hydrolyzed, it 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 mesh sieve. The soybean meal and the sulfuric acid solution were 1 g / 2.5 ml.
The hydrolysis time is the most important parameter in the hydrolysis of normal pressure. In this paper, the best hydrolysis time is judged in the hydrolysis time – the amount of the alkaliogram curve, see Figure 1.

At different times, a small amount of hydrolyzed liquid was drawn, and the supernatant was clarified by the centrifuge, and the quantitative suction volume was quantified, referred 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 grown. Therefore, it is possible to determine whether the hydrolysis time is slightly greater than 12 h.
2. Determination of chelate parameters
2.2.1 Effect of important parameters of composite amino acid and zinc chelation
medium, molar ratio, chelation time, chelation temperature, etc., affect composite amino acids An important parameter with 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 liquid curve with a sodium hydroxide solution of about 0.1 mol / L, and the AA + Zn curve is a curve of a composite amino acid liquid after zinc hydroxide 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, the C curve begins to rise rapidly, and H + is started in the system. This is the theory of the amino acid and the metal ion chelation, i.e., each 2 molecular amino acids and 1 molecular zinc chelation will release 2 molecules of H +. 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 exhibits 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 The effect of molar ratio on the chelation ratio
molar ratio means 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, the resulting results in Table 1, respectively.

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 chelation rate
There is a different temperature of 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 The effect of chelation time on the chelate rate
The chelation reaction is a rapid reaction, and as long as the zinc salt is dissolved, the chelate 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.

As can be seen from Table 3, 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 determined that the mature parameter is 2: 1, the pH is 7.1, the temperature is room temperature, the chelation rate can reach 92 %above. Test methods proposed in this article for other metalsThe study of ions and composite amino acid chelation has a certain reference value.
On the basis of the test, it is initially determined that the production process is as follows:
Soybean meal ¡ú Broken ¡ú hydrolysis ¡ú neutralization ¡ú filter ¡ú orthopedic acid ¡ú zinc salt ¡ú adjust pH ¡ú chelation ¡ú concentrate dry ¡ú Crush mix¡ú Finished packaging
Composite amino acid chelate zinc laboratory samples made in this paper, 32% of crude proteins, 9% total zinc, and can meet the production needs of feed additives.There is a certain reference value for industrial production.

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