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Crystallization method for improving crystal habit of ethyl vanillin by adding polyvinylpyrrolidone

A technology of polyvinylpyrrolidone and ethyl vanillin, which is applied in the separation/purification of carbonyl compounds, organic chemistry, etc., and can solve the problems that there is no patent for the recrystallization and refining process of ethyl vanillin

Active Publication Date: 2019-03-29
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] At present, the technologies related to ethyl vanillin are all patents on the synthesis process of ethyl vanillin, and there is no patent on the recrystallization and refining process of ethyl vanillin products

Method used

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  • Crystallization method for improving crystal habit of ethyl vanillin by adding polyvinylpyrrolidone
  • Crystallization method for improving crystal habit of ethyl vanillin by adding polyvinylpyrrolidone
  • Crystallization method for improving crystal habit of ethyl vanillin by adding polyvinylpyrrolidone

Examples

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Embodiment 1

[0027] Add 65g of distilled water to 35g of absolute ethanol, then add 15g of ethyl vanillin and 0.05g of polyvinylpyrrolidone K60, heat up to 50°C under stirring, and cool down to 21°C at a rate of 12°C / h after all solids are dissolved . Subsequently, 2% ethyl vanillin by mass of ethyl vanillin was added as a seed crystal, and the crystal was grown for 30 minutes. After the crystal growth, the temperature was lowered to 0°C at a rate of 12°C / h. The product was obtained after filtration and drying. The product is a thick flaky colorless transparent crystal with a crystal habit like figure 2 As shown, the aspect ratio is 0.22, the tap density is 0.433g / ml, the angle of repose is 47°, and the particle size distribution is as follows Figure 4 As shown, the main particle size d(0.5) is 275 μm.

Embodiment 2

[0029] Add 55g of distilled water to 45g of absolute ethanol, then add 22.5g of ethyl vanillin and 0.50g of polyvinylpyrrolidone K60, heat up to 50°C under stirring, and cool down to 21.5°C at a rate of 12°C / h after all solids are dissolved. ℃. Subsequently, ethyl vanillin with 1% mass of ethyl vanillin was added as a seed crystal, and the crystal was grown for 20 minutes. After the crystal growth, the temperature was lowered to 5°C at a rate of 12°C / h. The product was obtained after filtration and drying. Its aspect ratio is 0.12, the tap density of the product is 0.469g / ml, the angle of repose is 37°, and the main particle size d(0.5) is 508μm.

Embodiment 3

[0031] Add 70g of distilled water to 30g of absolute ethanol, then add 10g of ethyl vanillin and 0.1g of polyvinylpyrrolidone K90, heat up to 35°C under stirring, and cool down to 15°C at a rate of 2.5°C / h after all solids are dissolved . Subsequently, 0.01% ethyl vanillin by mass of ethyl vanillin was added as a seed crystal, and the crystal was grown for 40 minutes. After the crystal growth, the temperature was lowered to 0°C at a rate of 2.5°C / h. The product was obtained after filtration and drying. Its aspect ratio is 0.27, the tap density of the product is 0.451g / ml, and the angle of repose is 45°. The main particle size d(0.5) is 382 μm.

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Abstract

The invention relates to a crystallization method for improving the crystal habit of ethyl vanillin by adding polyvinylpyrrolidone. The method includes: adding an ethyl vanillin crude product and polyvinylpyrrolidone into a mixed solvent, performing stirring and heating to 35DEG C-50DEG C for dissolution, after the solid is completely dissolved, performing cooling to 15DEG C-25DEG C, adding ethylvanillin seed crystal, conducting grain growing for 10-40min, then performing cooling to 0DEG C-10DEG C, filtering the magma and conducting drying to obtain a ethyl vanillin crystal. The ethyl vanillin product prepared by the method provided by the invention has nonbreakable crystal, is thick flake shaped, has a height-to-width ratio of 0.11-0.25, large particle size, a main particle size of 275-508microm, a tap density up to 0.31-0.47g / mL, good fluidity and a repose angle of 37-47DEG C. The product obtained by the method is easy for filtration and drying, and is beneficial to storage and transportation, thus greatly improving the market competitiveness of the product.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, and specifically relates to a crystallization method for improving the crystal habit of ethyl vanillin by adding polyvinylpyrrolidone Background technique [0002] Ethyl vanillin, also known as ethyl vanillin, 3-ethoxy-4-hydroxybenzaldehyde, English name ethyl vanillin, CAS registration number: 121~32~4, white to slightly yellow scale crystalline powder, Has a strong vanilla bean aroma; melting point 77 ~ 78 ℃. Soluble in ethanol, ether, glycerin, propylene glycol, slightly soluble in water. Its formula C 9 h 10 o 3 , the structural formula is as follows: [0003] [0004] Ethyl vanillin is a synthetic spice that has not been found in nature. It has a strong milky aroma, and its aroma is 3 to 4 times that of vanillin. [0005] Ethyl vanillin is mainly used in the field of food additives, often used as sweeteners and fixatives in beverages, cigarettes, food an...

Claims

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Application Information

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IPC IPC(8): C07C45/81C07C47/575
CPCC07C45/81C07C47/575
Inventor 尹秋响张世豪周玲郝红勋侯宝红张美景龚俊波鲍颖谢闯王静康
Owner TIANJIN UNIV
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