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Method for regulating and controlling disodium guanylate crystallization process through oil separation and transformation

A technology of disodium guanylate and hydrochloric acid, applied in organic chemistry methods, chemical instruments and methods, organic chemistry and other directions, can solve the problems of ethanol residue, methanol toxicity, high solubility, etc., and achieve low residual amount, uniform particle size, high Yield effect

Active Publication Date: 2017-07-07
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solubility of disodium guanylate in methanol is greater than that of ethanol and methanol is toxic. Therefore, ethanol is usually used as a dissolving agent for food-grade disodium guanylate, but there will still be ethanol residues in the final product, which is Undesirable in some industry testing

Method used

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  • Method for regulating and controlling disodium guanylate crystallization process through oil separation and transformation
  • Method for regulating and controlling disodium guanylate crystallization process through oil separation and transformation
  • Method for regulating and controlling disodium guanylate crystallization process through oil separation and transformation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step 1: Pour 1.1 times isopropanol into 100ml of 5'-guanylate disodium solution with a stirring intensity of 300rpm, pH=9.8, and a concentration of 150g / L, and the system is in an oily state;

[0035] Step 2: Add 0.45g I-type 5'-guanylate disodium crystals to the mixed solution obtained in Step 1 as a seed crystal, and the crystal status in the system is as follows: figure 1 As shown, start to add pH=7.5 dropwise at a rate of 5% per hour of the volume of the disodium guanylate aqueous solution of pH=9.8, and the concentration is 30ml of 5’-disodium guanylate solution of 150g / L;

[0036] Step 3: Add 25ml isopropanol and 20ml 0.5mol / L hydrochloric acid mixed solution ( figure 2 shown), while slowly cooling down to 10°C ( Figure 4 Shown), suction filtration, drying to obtain type I 5 '- disodium guanylate crystal product.

[0037] The product purity is: 99.4%, the yield is: 99.0%, and the light transmittance is 99.3%. According to the method, the final product obtained...

Embodiment 2

[0039] Step 1: Pour 0.9 times isopropanol into 100ml of 5'-guanylate disodium solution with a stirring intensity of 200rpm, pH=10.0, and a concentration of 150g / L, and the system is in an oily state;

[0040] Step 2: Add 0.45 g of I-type 5'-disodium guanylate crystals to the mixed solution obtained in step 1 as a seed crystal, and start to add dropwise at a rate of 6% per hour of the volume of the disodium guanylate aqueous solution at pH=10.0 25ml of 5'-guanylate disodium solution with pH=7.5 and a concentration of 150g / L;

[0041] Step 3: After step 2, add 45ml of isopropanol and 30ml of 0.5mol / L hydrochloric acid mixed solution dropwise at a rate of 7% per hour of the volume of the disodium guanylate aqueous solution with pH=9.8, while slowly cooling down to 5°C for suction filtration, Dry to obtain type I 5'-guanylate disodium crystal product.

[0042] Product purity: 99.2%, yield: 99.1%, light transmittance: 99.2%.

Embodiment 3

[0044] Step 1: Pour 1.1 times of isopropanol into 100ml of 5'-guanylate disodium solution with a stirring intensity of 150rpm, pH=9.8, and a concentration of 200g / L, and the system is in an oily state;

[0045] Step 2: Add 0.35 g of type I 5'-disodium guanylate crystals to the mixed solution obtained in step 1 as a seed crystal, and start to add dropwise at a rate of 6% per hour of the volume of the disodium guanylate aqueous solution with pH=9.8 pH=7.7, 40ml 5'-guanylate disodium solution with a concentration of 200g / L;

[0046] Step 3: After step 2 is completed, add 30ml of isopropanol and 23ml of 0.6mol / L hydrochloric acid mixed solution dropwise at a rate of 7% per hour of the volume of the disodium guanylate aqueous solution with pH = 9.8, while slowly cooling down to 10°C for suction filtration, Dry to obtain type I 5'-guanylate disodium crystal product.

[0047] The product purity is: 99.0%, the yield is: 98.3%, and the light transmittance is 99.1%.

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Abstract

The invention discloses a method for regulating and controlling a disodium guanylate crystallization process through oil separation and transformation. The method comprises the following steps: step 1: adding isopropyl alcohol into a disodium guanylate water solution with the pH (Potential of Hydrogen) value of 9.5 to 10.0 as a counter solvent and enabling a mixed solution to be at an oil state; step 2: adding a disodium guanylate I type crystal into the mixed solution obtained by the step 1 as a seed crystal; slowly dropwise adding a disodium guanylate water solution with the pH value of 7.0 to 7.7 and carrying out crystal transformation, wherein the temperature of a system is controlled to be 20 DEG C to 40 DEG C and stirring strength is 150rpm to 400rpm; step 3: dropwise adding a mixed solution of the isopropyl alcohol and hydrochloric acid into the solution obtained by the step 2 and carrying out cooling treatment to improve the yield of a product; filtering and drying to obtain the product. The method disclosed by the invention has the advantage that the crystallization process is simple to operate and has good repeatability; the disodium guanylate I type crystal product with uniform granularity can be obtained and the problems of difficult crystal transformation, low yield and the like, caused by the fact that the isopropyl alcohol is used as a solvating-out agent, can be effectively improved.

Description

technical field [0001] The invention relates to a dissolution and crystallization method for preparing high-purity disodium guanylate crystals, belonging to the technical field of separation and crystallization. Background technique [0002] Disodium 5'-guanylate (also known as disodium 5'-triphosphate, disodium guanylate, guanosine-5'-sodium phosphate, etc.), English name: Disodium5'-guanylate (referred to as GMP or GMPNa 2 ), molecular formula C 10 h 12 N 5 Na 2 o 8 P, relative molecular mass 407.12, disodium guanylate type I crystal with 7 crystal water molecular formula C 10 h 12 N 5 Na 2 o 8 P·7H 2 O, the relative molecular mass is 533.26, and the structural formula is shown in the figure: [0003] [0004] Disodium 5'-guanylate belongs to the second-generation umami agent, which has a mushroom-like aroma, and is often mixed with glutamic acid or inosinic acid to significantly enhance the umami effect. In addition to being used as a food additive, disodiu...

Claims

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Application Information

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IPC IPC(8): C07H19/20C07H1/06
CPCC07H1/06C07H19/20C07B2200/13
Inventor 应汉杰陈俏邹逢霞庄伟杨朋朋吴菁岚周精卫
Owner NANJING UNIV OF TECH
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