Method for continuous preparation of high bulk density methionine crystal

Patent metadata

Field	Value
Publication number	US-10293273-B2
Application number	US-201515549833-A
Country	US
Kind code	B2
Filing date	Dec 23, 2015
Priority date	Feb 12, 2015
Publication date	May 21, 2019
Grant date	May 21, 2019

Abstract

The present disclosure relates to a method for continuous preparation of high bulk density methionine crystals. The process of the method is as follows: a hydrolysate solution, which is obtained from a reaction of 5-(β-methylmercaptoethyl) hydantoin and a potassium carbonate solution, is mixed with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section; after being cooled, the mixture enters a liquid distributor of a neutralization region in the upper part of the crystallizer and is sprayed in the form of liquid droplet or trickle into carbon dioxide gas for neutralization reaction, and then naturally falls into a crystallization region in the lower part to be mixed with a material in the region; the obtained mixture grows on fine crystals in a system to form crystals having larger particle diameters, and meanwhile new crystal nucleuses are formed; in a deposition area in the middle part of the crystallization region, the crystals having larger particle diameters deposits into an elutriation leg, while the fine crystals circulate with the external circulation material, and a part of the external circulation material is used to elutriate the crystals in the elutriation leg, while another part of the same is used to be mixed with the hydrolysate solution; and the crystals in the elutriation leg are separated, washed and dried to obtain the high bulk density methionine product.

First claim

What is claimed is:

1. A method for continuous preparation of high bulk density methionine crystals, comprising the following steps:
(1) mixing a hydrolysate solution containing potassium methionine obtained from a reaction of 5-(β-methylmercaptoethyl)hydantoin and a potassium carbonate solution with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section to form a mixture material; the mixture material entering a liquid distributor of a neutralization region in an upper part of the crystallizer after being cooled and being sprayed in the form of liquid droplet or trickle to gas-liquid contact area to carry out a neutralization reaction with carbon dioxide gas so that obtaining a neutralization solution containing methionine;
(2) making the neutralization solution naturally fall into a crystallization region in the lower part of the crystallizer to form crystals in the crystallization region, and then making the crystals having larger particle diameters deposited into a elutriation leg in a deposition area in the middle part of the crystallization region;
(3) feeding the methionine crystals in the elutriation leg through a crystal mush pump into a rotary drum filter to be subjected to separation, washing and drying to obtain methionine products;
wherein the external circulation material is initially a saturated methionine solution and the bulk density of the high bulk density methionine crystals is at least 800 kg/m 3 .

2. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein the crystallization process comprises growing on fine crystals already formed in the crystallization region to form crystals having larger particle diameters, while controlling the oversaturation to form new crystal nucleuses.

3. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein in the deposition area in the middle part of the crystallization region, fine crystals and a part of the methionine solution enter an external circulation pipe for cooling and circulation; and a part of the external circulation materials is used to elutriate the crystals in the elutriation leg, while another part of the external circulation materials is used to be mixed with the hydrolyzate solution containing potassium methionine.

4. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein the DTB neutralization crystallizer having a gas phase neutralization section has a gas phase space at an upper part, and a liquid distributor and a gas distributor are provided so that the liquid as a dispersed phase is subjected to a gas-liquid neutralization reaction in a carbon dioxide gas as a continuous phase.

5. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein a volume ratio of the hydrolyzate solution containing potassium methionine in the outer circulation pipe of the DTB neutralization crystallizer having a gas phase neutralization section to the outer circulation material is 1:5-50, and the temperature of the material after being mixed is reduced by a cooler by 0.5-5° C.

6. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein a volume ratio of the outer circulation material in the elutriation leg at the lower part of the DTB neutralization crystallizer having a gas phase neutralization section to the output volume of crystal mush is (1-5):1.

7. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein an agitation rate in the crystallization region of the DTB neutralization crystallizer having a gas phase neutralization section is 50-500 rpm.

8. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein the temperature of the crystallization region of the DTB neutralization crystallizer having a gas phase neutralization section is 10-40° C.

9. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein the hydrolyzate solution containing potassium methionine stays in the neutralization crystallizer for 0.3-3 hours.

10. The method for continuous preparation of high bulk density methionine crystals according to claim 1 , wherein a pressure of the gas-phase carbon dioxide in the DTB neutralization crystallizer having a gas phase neutralization section is 0.3-1.2 Mpa.

11. A DTB neutralization crystallizer having a gas phase neutralization section for continuous preparation of high bulk density methionine crystals, comprising:
(1) a liquid distributor for forming the liquid droplets or trickles of mixed liquor containing potassium methionine and a gas distributor for supplying carbon dioxide gas that are provided in a neutralization region at an upper part,
(2) a liquid guide shell and a stirrer provided in the middle part,
(3) a crystal deposition area provided at a lower part, which includes an elutriation leg for depositing crystals,
(4) an external circulation system for recycling potassium methionine solution in a crystallization region, and a part of the solution being supplied to the elutriation leg while another part of the same being mixed with the hydrolyzate solution containing potassium methionine and then circulating supply to a material inlet of the neutralization crystallizer,
and wherein the bulk density of the high bulk density methionine crystals is at least 800 kg/m 3 .

12. The DTB neutralization crystallizer having a gas phase neutralization section according to claim 11 , further comprising a rotary drum filter for separating and washing crystal mush from the elutriation leg.

Assignees

• Shandong Nhu Amino Acid Co Ltd
• Univ Zhejiang
• Zhejiang Nhu Co Ltd

Inventors

• Chen Zhirong
• Wang Zhixuan
• Chen Cong
• Wang Zhengjiang
• Wang Cunchao
• Li Yin
• Zhang Zhixiang

Classifications

• B01D9/0054

  Use of anti-solvent · CPC title

• C07C323/58 Primary

  with amino groups bound to the carbon skeleton · CPC title

• B01D9/0013

  by indirect heat exchange · CPC title

• B01D9/0027

  by means of conveying fluid, e.g. spray-crystallisation (spray-drying F26B) · CPC title

• B01D2009/0086

  Processes or apparatus therefor · CPC title