Preparation method of L-valine nitrate

Abstract

The invention discloses a preparation method of L-valine nitrate, comprising the following steps of: adding L-valine into purified water under the normal temperature, evenly stirring and then adding nitric acid, wherein the mol ratio of the L-valine to the nitric acid is 1:1-1.1, and the weight ratio of the L-valine to the water of 1:0.4; gradually clarifying the solution at the reaction temperature of 40 to 70 DEG C and regulating the pH value of the solution to be 1 to 2 by using the nitric acid; cooling the clarified solution to 10 to 25 DEG C; carrying out solid-liquid separation on precipitated crystals; flushing the crystals and then drying at 60 to 85 DEG C to obtain an L-valine nitrate finished product; taking liquid subjected to the solid-liquid separation as a mother solution, and continuously recycling. In the preparation method of the L-valine nitrate, the food-grade L-valine and chemical reagent-grade-nitric acid are adopted to react, therefore, the reaction conditions are mild, the process is reasonable, simple and convenient, and the product has good quality and high purity up to more than 99 percent; in addition, the crystallized mother solution can be continuouslyrecycled in the production, therefore, the invention has the yield coefficient up to more than 98 percent and is suitable for industrial large production.

Description

technical field

[0001] The invention belongs to a method for preparing amino acid nitrate, in particular to a method for preparing L-valine nitrate with good product quality, high yield and low cost. Background technique

[0002] Amino acids are the basic substances that make up the protein needed for animal nutrition. Generally, people can produce various amino acids to meet the body's needs through their own production or through food. However, in special cases such as illness, injury or heavy exercise, in order to restore the balance of various metabolisms in the body, enhance immunity and athletes recover as soon as possible to increase muscle strength, it is necessary to supplement various amino acids.

[0003] L-Valine is one of the twenty protein amino acids. The chemical name is: L-2-amino-3-methylbutanoic acid. From a nutritional point of view, L-valine is one of the eight essential amino acids for human nutrition.

[0004] L-valine acts on the corpus luteum, br...

Examples

Embodiment 1

[0022] Add 100 kg of L-valine to 40 kg of purified water at room temperature, stir evenly, then add 81 kg of 68% nitric acid while stirring, and gradually heat to 55°C±5°C after adding the nitric acid. As the temperature rises, the solution is gradually clarified, and the pH is detected before the end of the reaction, and the pH of the solution is adjusted to 2 with nitric acid. After the solution is completely clarified, it is cooled to 20°C to produce crystals, and the crystals and mother liquor are separated by centrifugation. The crystals are dried, washed with absolute ethanol with 10-20% of the weight of the crystals, dried, and dried at 80°C. The finished product of L-valine nitrate was obtained with a yield of 30%. After centrifugation, the mother liquor continues to be recycled repeatedly.

Embodiment 2

[0024] At room temperature, add 100 kg of L-valine to about 40 kg of mother liquor produced in Example 1, stir well, then add 81 kg of 68% nitric acid, and gradually heat to 45°C ± 5°C after adding nitric acid. As the temperature increased, the solution was gradually clarified, and the pH was detected before the end of the reaction, and the pH of the solution was adjusted to 2 with nitric acid. After the solution is completely clarified, it is cooled to 15°C to produce crystals, and the crystals and mother liquor are separated by centrifugation. The crystals are dried, washed with absolute ethanol with a weight of 10-20% of the crystals, dried, and dried at 80°C. The finished product of L-valine nitrate is obtained, and the yield is nearly 100%. The mother liquor continues to be recycled repeatedly

Embodiment 3

[0026] At room temperature, 100 kilograms of L-valine is added in about 40 kilograms of mother liquors that embodiment 2 produces, after stirring, add 81 kilograms of 68% nitric acid, stir while adding nitric acid, make it mix homogeneously. Control the nitric acid addition rate so that the solution temperature gradually reaches 40°C without external heating. As the stirring solution was gradually clarified, the pH was checked before the end of the reaction, and the pH of the solution was adjusted to 2 with nitric acid. After the solution is completely clarified, it is cooled to 10°C to produce crystals, the crystals and mother liquor are separated by centrifugation, the crystals are dried, and the crystals are rinsed with absolute ethanol with 10-20% of the weight of the crystals, and then dried at 80°C to obtain the product. L-valine nitrate finished product, the yield is nearly 100%. The mother liquor continues to be recycled repeatedly.

technical field

[0001] The invention belongs to a method for preparing amino acid nitrate, in particular to a method for preparing L-valine nitrate with good product quality, high yield and low cost. Background technique

[0002] Amino acids are the basic substances that make up the protein needed for animal nutrition. Generally, people can produce various amino acids to meet the body's needs through their own production or through food. However, in special cases such as illness, injury or heavy exercise, in order to restore the balance of various metabolisms in the body, enhance immunity and athletes recover as soon as possible to increase muscle strength, it is necessary to supplement various amino acids.

[0003] L-Valine is one of the twenty protein amino acids. The chemical name is: L-2-amino-3-methylbutanoic acid. From a nutritional point of view, L-valine is one of the eight essential amino acids for human nutrition.

[0004] L-valine acts on the corpus luteum, br...

Examples

Embodiment 1

[0022] Add 100 kg of L-valine to 40 kg of purified water at room temperature, stir evenly, then add 81 kg of 68% nitric acid while stirring, and gradually heat to 55°C±5°C after adding the nitric acid. As the temperature rises, the solution is gradually clarified, and the pH is detected before the end of the reaction, and the pH of the solution is adjusted to 2 with nitric acid. After the solution is completely clarified, it is cooled to 20°C to produce crystals, and the crystals and mother liquor are separated by centrifugation. The crystals are dried, washed with absolute ethanol with 10-20% of the weight of the crystals, dried, and dried at 80°C. The finished product of L-valine nitrate was obtained with a yield of 30%. After centrifugation, the mother liquor continues to be recycled repeatedly.

Embodiment 2

[0024] At room temperature, add 100 kg of L-valine to about 40 kg of mother liquor produced in Example 1, stir well, then add 81 kg of 68% nitric acid, and gradually heat to 45°C ± 5°C after adding nitric acid. As the temperature increased, the solution was gradually clarified, and the pH was detected before the end of the reaction, and the pH of the solution was adjusted to 2 with nitric acid. After the solution is completely clarified, it is cooled to 15°C to produce crystals, and the crystals and mother liquor are separated by centrifugation. The crystals are dried, washed with absolute ethanol with a weight of 10-20% of the crystals, dried, and dried at 80°C. The finished product of L-valine nitrate is obtained, and the yield is nearly 100%. The mother liquor continues to be recycled repeatedly

Embodiment 3

[0026] At room temperature, 100 kilograms of L-valine is added in about 40 kilograms of mother liquors that embodiment 2 produces, after stirring, add 81 kilograms of 68% nitric acid, stir while adding nitric acid, make it mix homogeneously. Control the nitric acid addition rate so that the solution temperature gradually reaches 40°C without external heating. As the stirring solution was gradually clarified, the pH was checked before the end of the reaction, and the pH of the solution was adjusted to 2 with nitric acid. After the solution is completely clarified, it is cooled to 10°C to produce crystals, the crystals and mother liquor are separated by centrifugation, the crystals are dried, and the crystals are rinsed with absolute ethanol with 10-20% of the weight of the crystals, and then dried at 80°C to obtain the product. L-valine nitrate finished product, the yield is nearly 100%. The mother liquor continues to be recycled repeatedly.