Clean preparation method of high-purity methionine hydroxyl analogue calcium salt

A technology of high-purity methionine hydroxyl and methionine hydroxyl, which is applied in the field of clean preparation of high-purity methionine hydroxyl analog calcium salt, can solve the problems of ammonium sulfate unpleasant smell, loss of organic solvent, large investment in equipment, etc., to avoid by-product inorganic The effect of ammonium salt generation, reduction of solid waste generation, and high monomer content

A technology of high-purity methionine hydroxyl and methionine hydroxyl, which is applied in the field of clean preparation of high-purity methionine hydroxyl analog calcium salt, can solve the problems of ammonium sulfate unpleasant smell, loss of organic solvent, large investment in equipment, etc., to avoid by-product inorganic The effect of ammonium salt generation, reduction of solid waste generation, and high monomer content

CN113105376APending Publication Date: 2021-07-13山西铁峰化工有限公司

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  • Clean preparation method of high-purity methionine hydroxyl analogue calcium salt
  • Clean preparation method of high-purity methionine hydroxyl analogue calcium salt

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preparation example Construction

[0026] The clean preparation method of a kind of high-purity methionine hydroxyl analogue calcium salt of the present invention comprises the following steps:

[0027]1) Use 2-hydroxy-4-methylthiobutyronitrile as raw material, add water, and carry out hydration reaction under the catalysis of solid acid or solid base to obtain 2-hydroxy-4-methylthiobutyroamide salt solution;

[0028] 2) adding strong acid or strong base to the 2-hydroxy-4-methylthiobutyramide saline solution for hydrolysis to obtain 2-hydroxy-4-methylthiobutyric acid;

[0029] 3) Add CaO or Ca(OH) to the 2-hydroxy-4-methylthiobutyric acid 2 , through a salt-forming reaction, the aqueous solution of the mixture and ammonia are obtained, and the ammonia is absorbed by water to obtain ammonia water.

[0030] 4) The aqueous solution of the mixture is subjected to chromatographic desalination treatment to obtain an aqueous solution of methionine hydroxyl analogs and an aqueous solution of inorganic ammonium salt; ...

Embodiment 1

[0048] 30g ZrOCl 2 · 8H 2 O, add 45 mL H 2 SiO 3 dissolve, add NH 3 ·H 2 O to adjust pH=8, add 10g of powdered activated carbon, fully stir at 100°C for 1 hour, age, and wash with suction until no Cl - , Dry at 80°C for 10h. h 2 SO 4 Soak in water for 3 hours, filter, wash, and dry, and then roast at 300°C for 2 hours to obtain activated carbon-loaded SO 4 2- / SiO 2 -ZrO 2 New solid superacid catalyst.

Embodiment 2

[0050] 30g ZrOCl 2 · 8H 2 O, add 45 mL H 2 SiO 3 dissolve, add NH 3 .H 2 O to adjust pH=8, add 15g of powdered activated carbon, fully stir at 100°C for 1 hour, age, filter and wash until no Cl - , Dry at 80°C for 10h. h 2 SO 4 Soak in water for 3h, filter and wash, dry and roast at 300°C for 2h to obtain SO 4 2- / SiO 2 -ZrO 2 Solid superacid catalyst.

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Abstract

The invention discloses a clean preparation method of high-purity methionine hydroxyl analogue calcium salt. The clean preparation method comprises the following specific steps: adding water into 2-hydroxy-4-methylthiobutyronitrile serving as a raw material, carrying out a hydration reaction under the catalytic action of solid acid / solid alkali, adding strong acid or strong alkali for hydrolysis to obtain 2-hydroxy-4-methylthiobutyric acid, then adding CaO or Ca(OH)2, carrying out a salt forming reaction to obtain an aqueous solution of a mixture, carrying out chromatographic desalination treatment on the aqueous solution of the mixture to obtain an aqueous solution of a methionine hydroxyl analogue, and finally carrying out spray drying on the aqueous solution of the methionine hydroxyl analogue to obtain a target product. Compared with a traditional method, the method disclosed by the invention has the advantages that the step of neutralizing and alkali washing after the reaction is finished is avoided, the generation of a byproduct, namely inorganic ammonium salt is avoided, reaction is simple, conditions are mild, and the method is safe and environment-friendly; and in addition, a catalyst, namely the solid acid or solid alkali adopted in the method can be recycled, so production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a clean preparation method of high-purity methionine hydroxyl analogue calcium salt. Background technique [0002] The traditional method for preparing methionine is to use acrolein and methyl mercaptan as raw materials to produce methionine, and then to obtain methionine product through cyanamide reaction. [0003] J.Am used 3,6-bis-(β-chloroethyl)-2,5-diketopiperazine as raw material to react with thiourea and then dimethyl sulfate to obtain a methylthio-substituted intermediate, followed by hydrolysis Get methionine. However, the intermediates of this synthetic route need to use butyrolactone derivatives as raw materials, which can be obtained through multi-step synthetic reactions. The synthetic route is long and the yield is low, and the raw material cost is high and has no industrial value. [0004] Methionine Hydroxy Analogue (MHA) is a highly acid...

Claims

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Application Information

Patent Timeline
13 Jul 2021
Publication
CN113105376A
IPC
C07C319/20; C07C319/28; C07C323/52; B01J27/053; B01J27/135; B01J35/02
CPC
C07C319/20; C07C319/28; B01J27/053; B01J27/135; B01J35/00; B01J35/30; C07C323/52
Inventors
朱远斌; 樊保敏