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Stable propyl gallate crystal form and preparation method thereof

A technology of propyl gallate and stability, which is applied in the field of preparation of propyl gallate crystal form G, can solve the problems of easy moisture absorption, poor high temperature resistance and the like, and achieves the effects of good stability and no chemical change.

Inactive Publication Date: 2016-04-27
GUIYANG JILONG TANNIN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the physical and chemical properties of propyl gallate such as poor high temperature resistance, easy moisture absorption, and light can promote its decomposition are unfavorable factors for its storage and safe use.

Method used

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  • Stable propyl gallate crystal form and preparation method thereof
  • Stable propyl gallate crystal form and preparation method thereof
  • Stable propyl gallate crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of propyl gallate crystal form G:

[0029] Mix and dissolve 1.0 g of propyl gallate and 1 mL of DMF (N,N-dimethylformamide), add it dropwise to 100 mL of reverse osmosis water under stirring, keep stirring at room temperature (25°C), slowly precipitate crystals, and collect them by filtration. Dry at 70°C for 12 hours to obtain 0.91 g of propyl gallate crystal form G crystal product.

Embodiment 2

[0031] Preparation of propyl gallate crystal form G:

[0032] Mix and dissolve 1.0 g of propyl gallate and 1 mL of methanol, add it dropwise to 100 mL of reverse osmosis water under stirring, keep stirring at room temperature (25°C), slowly precipitate crystals, and collect them by filtration. Dry at 70°C for 12 hours to obtain 0.78 g of propyl gallate crystal form G crystal product.

Embodiment 3

[0034] Preparation of propyl gallate crystal form G:

[0035] Mix and dissolve 1.0 g of propyl gallate and 1 mL of ethanol, add dropwise to 100 mL of reverse osmosis water under stirring, keep stirring at room temperature (25°C), slowly precipitate crystals, and collect by filtration. Dry at 70°C for 12 hours to obtain 0.82 g of propyl gallate crystal form G crystal product.

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Abstract

The invention discloses a stable propyl gallate crystal form. The stable propyl gallate crystal form is characterized in that the stable propyl gallate crystal form is a propylgallate crystal G, under test conditions of an X-ray tube utilizing Cu-K target radiation, X-ray wavelength of 1.5406 angstroms, tube voltage of 40KV, tube current of 40mA, a step size of 0.02 degrees, a scanning scope of 4-100 degrees and a scanning rate of 6 degrees per minute, the stable propyl gallate crystal is subjected to X-ray powder diffraction and the result of scanning at the reflection angle shown in the description shows that the stable propyl gallate crystal has characteristic peaks of 2.31+ / -0.2, 3.28+ / -0.2, 3.36+ / -0.2, 3.84+ / -0.2, 5.94+ / -0.2, 7.00+ / -0.2, 7.67+ / -0.2 and 9.65+ / -0.2, and in the infrared spectrogram, the stable propyl gallate crystal has characteristic absorption peaks at wavelength of 3501.9, 3328.9, 1690.6, 1616.6, 1540.4, 1467.61, 1407.4, 1340.4, 1313.7, 1248.3, 1197.9 and 1037.7 cm<-1>.

Description

technical field [0001] The invention belongs to the field of fine chemical products of organic chemical products, and relates to a preparation method of crystal form G of propyl gallate. Background technique [0002] In the early 1940s, F.Bohm and Th.Salotischka discovered the protective effect of propyl gallate on oil. Oils and fats contain a large amount of unsaturated fatty acids, which inevitably undergo oxidative deterioration in varying degrees during production, processing and storage, resulting in odor, discoloration, reduction of food quality, and destruction of nutritional value. Most of these oil oxides are harmful to the human body and can cause various diseases. Now, propyl gallate has become one of several kinds of oil inhibitors widely used in various countries. Our country started to produce it in the 1950s and used it to preserve the quality of biscuits and other snacks. The US Food and Drug Administration (FDA) approved it to have GRAS (Notarized Safe) qu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/84C07C67/52
CPCC07C69/84C07B2200/13C07C67/52
Inventor 罗波罗志军
Owner GUIYANG JILONG TANNIN CHEM
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