Ammonia-catalyst fytic hydrodizing process to prepare inositol in near critical water medium

A technology for catalyzing phytin and near-critical water with medium ammonia, applied in hydrolysis preparation, organic chemistry, etc., can solve the problems of not being widely used, and achieve the effect of simple reaction process and high product yield

Inactive Publication Date: 2007-09-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Utilizing this method to produce inositol can improve yield and product quality, and reduce production cost, which is a new trend in the development of inositol production, but it is not widely used at present

Method used

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  • Ammonia-catalyst fytic hydrodizing process to prepare inositol in near critical water medium
  • Ammonia-catalyst fytic hydrodizing process to prepare inositol in near critical water medium

Examples

Experimental program
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Effect test

Embodiment 1

[0041]Add 300g of deionized water and 50g of phytin into a 500mL batch autoclave, start stirring, raise the temperature to 100°C, open the exhaust valve for 2 minutes, and use water vapor to remove the air in the kettle. Add 22mL of 25% ammonia water into the kettle with a high-pressure metering pump, so that the concentration of ammonia water in the reaction solution reaches 15g / L, and continue to heat up to 200°C for 120 minutes for hydrolysis. After the hydrolysis is completed, turn off the heating device, cool down to 90°C, open the exhaust valve, and empty the ammonia in the kettle. The hydrolyzed product was filtered, concentrated, crystallized, decolorized, secondary crystallized, and vacuum dried to obtain 5.9 g of refined inositol, and the product was analyzed by HPLC with a purity of 81%.

Embodiment 2

[0043] Add 300g of deionized water and 60g of phytin into a 500mL batch autoclave, start stirring, raise the temperature to 100°C, open the exhaust valve for 3 minutes, and use water vapor to remove the air in the kettle. Use a high-pressure metering pump to add 30 mL of 25% ammonia water into the kettle to make the concentration of ammonia water in the reaction solution reach 20 g / L, and continue to heat up to 220 ° C for 100 min for hydrolysis. After the hydrolysis is completed, turn off the heating device, cool down to 90°C, open the exhaust valve, and empty the ammonia in the kettle. The hydrolyzed product was filtered, concentrated, crystallized, decolorized, secondary crystallized, and vacuum dried to obtain 8.6 g of refined inositol. The purity of the product was 84% ​​through HPLC analysis.

Embodiment 3

[0045] Add 300g of deionized water and 75g of phytin into a 500mL batch autoclave, start stirring, raise the temperature to 100°C, open the exhaust valve for 4 minutes, and use water vapor to remove the air in the kettle. Add 5.5mL of 25% ammonia water into the kettle with a high-pressure metering pump to make the concentration of ammonia water in the reaction solution reach 4g / L, and continue to heat up to 240°C for 70 minutes for hydrolysis. After the hydrolysis is completed, turn off the heating device, cool down to 90°C, open the exhaust valve, and empty the ammonia in the kettle. The hydrolyzed product was filtered, concentrated, crystallized, decolorized, secondary crystallized, and vacuum dried to obtain 14.2 g of refined inositol, and the purity of the product was 87% through HPLC analysis.

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Abstract

The invention discloses a method for preparing inosite by means of catalyzing fytic acid hydrolyze in a near-critical aqueous medium, including the steps as follows: 1) adding de-ionized water and fytic acid in the high-pressure reaction vessel with a mass rate of 1:1 - 6:1, blending, heating to 100 DEG C, opening the air outlet valve for 2-5 minutes, taking away the oxygen in the vessel by vapor; 2) adding 25% ammonia into vessel by high pressure measuring pump to make the ammonia concentration up to 0.5-20g/L, keeping on heating to 200-350 DEG C for hydrolyzing 10-120 min; 3) after hydrolyzation, cooling, and opening the air outlet valve to empty the ammonia gas in the vessel when the temperature declines to the 90 DEG C, then the ammonia gas to be recycle and prepared to the ammonia which is back to step 2 for a repetition; 4) hydrolysate being filtering, concentrating, crystallizing to get coarse inosite, the crystallized mother liquid back to the concentration step; 5) coarse inosite being decoloring, secondary crystallizing, drying in vacuum to obtain pure inosite, the crystallized mother liquid back to the concentration step in 4. The invention can reuse the ammonia as catalyzer in the reaction, is simple, green, high-yield.

Description

technical field [0001] The invention relates to a method for preparing inositol by ammonia-catalyzed hydrolysis of phytin in a near-critical water medium. Background technique [0002] Inositol (inositol, CAS No.: 87-89-8), that is, hexahydroxycyclohexane. Inositol in a broad sense refers to the general term of 9 known stereoisomers, but usually refers to myo-inositol (1,2,3,5 / 4,6-hexahydroxycyclohexane), which has been found The names of the eight isomers are shown in Table 1. [0003] Stereostructure name 1, 2, 3, 4, 5, 6-cis 1, 2, 3, 4, 5-cis 1,2,3,4-cis 1,2,4,5-cis 1, 2, 4, 6-cis 1,2,3-cis 1,2,4-cis 1,3,5-cis all-cis-inositol epi-inositol allo-inositol muco-inositol myo-inositol neo-inositol chiro-D, L-inositol bcyllo-inositol [0004] myo-inositol is a cyclic alcohol widely present in animals and plants, and exists in the form of free alcohol or various compounds. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/135C07C29/12
Inventor 吕秀阳傅杰
Owner ZHEJIANG UNIV
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