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Method for producing IMP and GMP through anti-solvent cooling crystallization based on solvent spray oscillation

A cooling crystallization and anti-solvent technology, which is applied in the field of food seasoning, can solve the problems of cumbersome operation, energy consumption, anti-solvent waste, and limited effect, and achieve the effect of short time consumption, small temperature fluctuation, and good dissolution strength

Pending Publication Date: 2022-02-08
肇东星湖生物科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, anti-solvent was continuously added for crystallization at the beginning, and no crystal seeds were added to control the supersaturation in the initial stage of crystallization, which was very easy to nucleate and produce fine particles; in the later stage, vacuum evaporation of anti-solvent was used to increase the solubility to dissolve crystal particles, but it did not affect the particle size. Distinguishing large particles and small particles at the same time consumes undersaturation, and the amount of anti-solvent evaporated each time is small to increase the solubility. cost

Method used

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  • Method for producing IMP and GMP through anti-solvent cooling crystallization based on solvent spray oscillation
  • Method for producing IMP and GMP through anti-solvent cooling crystallization based on solvent spray oscillation
  • Method for producing IMP and GMP through anti-solvent cooling crystallization based on solvent spray oscillation

Examples

Experimental program
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Effect test

Embodiment 1

[0039] A method for producing IMP+GMP based on solvent spray vibration and anti-solvent cooling crystallization, comprising the steps of:

[0040] Step 1: Weigh 30g each of IMP and GMP with an analytical balance, and measure 200mL of water with a graduated cylinder. The two are added to a 500mL crystallization kettle 1, and the water bath is heated to 65°C by controlling the high and low temperature constant temperature tank 10. Stirring at a stirring speed of 180rpm makes The solute is fully dissolved and the pH is adjusted to 7.9. Then keep 80mL of water in the jacketed thermos cup 11 connected in series with the crystallizer water bath. Add 100 mL of anti-solvent 90% ethanol at a rate of 4 mL / min, add 2.8 g of IMP+GMP seed crystals (the mass ratio of IMP and GMP seed crystals is 1:1), and the seed crystals are prepared by mixing and recrystallizing IMP and GMP. After growing the crystal for 20 minutes, start the program to cool down at 5°C / h, 8°C / h, 12°C / h, 14°C / h, 16°C / h,...

Embodiment 2

[0045] Step 1: Weigh 30g each of IMP and GMP with an analytical balance, and measure 200mL of water with a graduated cylinder. The two are added to a 500mL crystallization kettle 1, and the water bath is heated to 65°C by controlling the high and low temperature constant temperature tank 10. Stirring at a stirring speed of 180rpm makes The solute is fully dissolved and the pH is adjusted to 7.8. Then 105mL of water is kept warm in the jacketed thermos cup 11 connected in series with the crystallizer water bath. Add 100 mL of anti-solvent 90% ethanol at a rate of 6 mL / min, add 3.0 g of IMP+GMP seed crystals (the mass ratio of IMP and GMP seed crystals is 1:2), and the seed crystals are prepared by mixing and recrystallizing IMP and GMP, After growing the crystal for 20 minutes, start the program to cool down at 4°C / h, 6°C / h, 8°C / h, 10°C / h, 12°C / h, 14°C / h, and drop to the end in 6 hours.

[0046] Step 2: When the temperature is lowered to 55°C, adjust the stirring speed of the ...

Embodiment 3

[0050] Step 1: Weigh 30g each of IMP and GMP with an analytical balance, and measure 220mL of water with a graduated cylinder. The two are added to the crystallization kettle 1, and the temperature of the high and low temperature constant temperature bath 10 is raised to 63°C and stirred at a stirring speed of 200rpm to make the solute Dissolve fully and adjust the pH to 7.6. Then keep 100mL of water in the jacketed thermos cup 11 connected in series with the crystallizer water bath. Add 110 mL of anti-solvent 90% ethanol at an addition rate of 6 mL / min, add 4.0 g of IMP+GMP seed crystals (the mass ratio of IMP and GMP seed crystals is 2:1), and the seed crystals are prepared by mixing and recrystallizing IMP and GMP. After 20 minutes, start the program to cool down at 5°C / h, 7°C / h, 10°C / h, 14°C / h, 15°C / h, and drop to the end in 5 hours.

[0051] Step 2: When the temperature drops to 53°C, adjust the stirring speed of the agitator 2 to 60rpm, the particles will naturally sett...

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Abstract

The invention discloses a method for producing IMP and GMP through anti-solvent cooling crystallization based on solvent spray oscillation, wherein the method comprises the steps: adding raw materials IMP and GMP into water in a crystallization kettle, heating and stirring until the raw materials are completely dissolved, and adjusting the pH value; dropwise adding an anti-solvent, adding a crystal growth crystal, and cooling; enabling the solvent water to form fan-shaped water mist through a spray head, spraying the fan-shaped water mist onto a raw material liquid level of the crystallization kettle, enabling the use amount of the solvent water for primary solvent spray oscillation to be 25%-50% of the total amount of the solvent, controlling the primary spray time to be 1-2 min, recovering stirring to the heating stirring speed, cooling, and forming primary solvent spray oscillation; repeating the solvent spray oscillation for 2-4 times; and cooling, filtering, washing and drying to obtain a crystal product. The product provided by the invention has the advantages of narrow particle size distribution, large particle size, good crystal form, high yield, easy control of operation conditions, improvement according to a factory process, and high operability.

Description

technical field [0001] The invention claims a preparation method of 5'-taste nucleotide disodium, which belongs to the field of food seasonings, and specifically relates to a method for preparing 5'-taste nuclei with narrow particle size distribution and large particle size by introducing solvent spray and vibration Disodium glucoside method. Background technique [0002] 5'-Inosinate Disodium (5'-Inosinate Monophosphate Disodium, or, Disodium 5 '-inosinat, referred to as IMP) and 5'-Guanosine Monophosphate Disodium (5'-Guanosine Monophosphate Disodium, or, Disodium 5'-guanyLate, referred to as GMP), has a taste effect, mixed with MSG (sodium glutamate) Synergistic effect can be produced at the same time, which can increase the freshness several times to dozens of times; at the same time, 5'-flavored nucleotide disodium can improve the quality of food, and it has a synergistic effect on sweet and salty tastes, and has a synergistic effect on sour and bitter tastes. And fis...

Claims

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Application Information

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IPC IPC(8): A23L27/23A23L27/00B01D9/02B01D9/00
CPCA23L27/23A23L27/88A23L27/86A23L27/84B01D9/0081B01D9/00
Inventor 江燕斌赵望黄励坚任洪发郑明英严盟
Owner 肇东星湖生物科技有限公司
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