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Eutectic structure of vanillin and amide compound and preparation method thereof

An amide compound, vanillin technology, applied in the separation/purification of carbonyl compounds, chemical instruments and methods, crystal growth and other directions, can solve the problems of easy crystal transformation, poor solubility of vanillin, unstable solid phase, etc. To achieve the effect of good crystal morphology, good solubility and strong stability

Active Publication Date: 2022-07-29
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] To sum up, vanillin has the problems of poor solubility, unstable solid phase and prone to crystal transformation. Therefore, it is urgent to study co-crystallization, develop new preparation methods, and design vanillin co-crystal products with good solubility and strong stability. Through single crystal cultivation, analyze the eutectic structure, so that it has good solubility

Method used

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  • Eutectic structure of vanillin and amide compound and preparation method thereof
  • Eutectic structure of vanillin and amide compound and preparation method thereof
  • Eutectic structure of vanillin and amide compound and preparation method thereof

Examples

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Effect test

Embodiment 1

[0036] 1. Preparation of co-crystal powder products of vanillin and nicotinamide or vanillin and isonicotinamide

[0037] 1) Under stirring conditions, the vanillin raw material was added to dioxane at a temperature of 60° C. to obtain vanillin, and then 1 g of vanillin (7 mmol) was added to a crystallizer containing 7 mL of dioxane solvent, so that Its concentration is 1mol / L; constant temperature stirring for 30 minutes makes the vanillin solid completely dissolve to obtain vanillin solution, and the stirring speed is 400rpm;

[0038] 2) Under the temperature condition of 60°C, add nicotinamide or isonicotinamide in an equimolar (7mmol) with vanillin to the vanillin solution obtained in the above step 1), and keep stirring until the solution is completely dissolved and becomes a clear solution. , the stirring speed is 400rpm;

[0039] 3) Under the temperature condition of 60 ℃, add 0.01 g of mesoporous silica nanoparticles to the clear solution obtained in the above step 2), ...

Embodiment 2

[0049] 1. Preparation of co-crystal powder products of vanillin and nicotinamide or vanillin and isonicotinamide

[0050] 1) Under stirring conditions, the vanillin raw material was added to acetone at a temperature of 50° C. to obtain vanillin, and then 0.5 g of vanillin (3.5 mmol) was added to a crystallizer filled with 7 mL of ethanol solvent to make its concentration 0.5 mol / L; constant temperature stirring for 30 minutes makes the vanillin solid completely dissolve to obtain a vanillin solution, and the stirring speed is 300rpm;

[0051] 2) Under the temperature condition of 50°C, add nicotinamide or isonicotinamide in an equimolar (3.5mmol) with vanillin to the vanillin solution obtained in the above step 1), and keep stirring until the dissolution completely becomes clear. solution, stirring at a rate of 400 rpm;

[0052] 3) Under the temperature condition of 50 ℃, add 0.0025g of mesoporous silica nanoparticles to the clear solution obtained in the above step 2), the m...

Embodiment 3

[0062] 1. Preparation of co-crystal powder products of vanillin and nicotinamide or vanillin and isonicotinamide

[0063] 1) Under stirring conditions, the vanillin raw material was added to ethyl acetate at a temperature of 40° C. to obtain vanillin, and then 0.8 g of vanillin (4.5 mmol) was added to a crystallizer filled with 7 mL of ethanol solvent to make its concentration is 0.8mol / L; constant temperature stirring for 30 minutes makes the vanillin solid completely dissolve to obtain vanillin solution, and the stirring speed is 200rpm;

[0064] 2) Under the temperature condition of 40°C, add nicotinamide or isonicotinamide in an equimolar (4.5 mmol) with vanillin to the vanillin solution obtained in the above step 1), and keep stirring until the dissolution completely becomes clear. solution, stirring at a rate of 200 rpm;

[0065] 3) Under the temperature condition of 40°C, add 0.0008g of mesoporous silica nanoparticles to the clear solution obtained in the above step 2)...

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Abstract

The preparation method of the eutectic structure of the vanillin and the amide compound comprises the following steps: firstly, preparing a vanillin solution under a stirring condition, then adding nicotinamide or isonicotinamide which is equal to the vanillin in mole into the obtained vanillin solution, and keeping the stirring process until the nicotinamide or isonicotinamide is completely dissolved and becomes a clear solution; adding the silicon dioxide nanoparticles into the clear solution according to the mass ratio to adsorb vanillin, nicotinamide or isonicotinamide, and then separating, freeze-drying, heating, melting and drying to finally obtain a eutectic powder product of vanillin and nicotinamide or vanillin and isonicotinamide; at normal temperature, the eutectic powder product of vanillin and nicotinamide and the eutectic powder product of vanillin and isonicotinamide are dissolved in an organic solvent, after saturation is achieved, the mixture is placed in a constant-temperature and constant-humidity box to be slowly volatilized, the single crystal structure is determined, the yield is very high and can reach 90% or above, the purity reaches 98% or above, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical engineering crystallization, in particular to a co-crystal structure of vanillin and an amide compound and a preparation method thereof. Background technique [0002] Vanillin (C 8 H 8 O 3 , 152.11g / mol, CAS NO:121-33-5), also known as vanillin, the English name is vanillin, the chemical name is 3-methoxy-4-hydroxybenzaldehyde, is from the rut plant vanilla An organic compound extracted from beans, usually white or similar white crystalline powder, slightly sweet, slightly soluble in hot water and ethanol, not easily soluble in cold water and vegetable oil. Vanillin has the aroma of vanilla bean and strong milky aroma, which can enhance and fix the aroma. It is widely used in cosmetics, tobacco, cakes, candy and baked food industries. It is one of the world's largest synthetic spice varieties. First, the industrial production of vanillin has a history of more than 100 years. Vanillin can als...

Claims

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Application Information

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IPC IPC(8): C07C47/58C07C45/78C07C45/79C07C45/81C07D213/81C07D213/82C30B7/06C30B29/54
CPCC07C47/58C07C45/78C07C45/79C07C45/81C07D213/81C07D213/82C30B29/54C30B7/06C07B2200/13
Inventor 欧阳金波周利民邢晓红徐丽刘峙嵘
Owner EAST CHINA UNIV OF TECH
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