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Continuous purification method of thymol

A technology of thymol and purification method, applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve the problems of unfavorable industrial large-scale application, high cost of crystallization solvent and temperature control, large recovery loss and the like

Inactive Publication Date: 2021-05-18
ANHUI HAIHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, organic solvents are mainly used for the purification of thymol, but the crystallization temperature of organic solvents is low, the crystallization solvent and temperature control costs are high, and the recovery loss is large, and all products are separated after crystallization to obtain finished products, but For large-scale industrial production, due to the large amount of processing at one time, the load of corresponding supporting equipment is serious, which is not conducive to large-scale industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Prepare 2 kg of a crude product with a mass content of 80% thymol, 2 kg of finished thymol (content greater than 98%), 5 kg of pure water, and 320 g of thymol seed crystals.

[0026] (2) According to the mass ratio of 80% thymol crude product and pure water 2:1, each weigh 2 kg of 80% thymol crude product and 1 kg of pure water and put them into the crystallization kettle;

[0027] (3) After the crude thymol and pure water were mixed evenly without delamination, a small amount of material was taken to measure its crystallization point T, and the crystallization point T was 27.7°C.

[0028] (4) Stir continuously at a rotation speed of 95r / min, cool the crystallization kettle to T+5°C, that is, start adding seed crystals at 32.7°C, add 320g of thymol seed crystals, and keep warm for 1h at a cooling rate of 2°C / h down to 20°C;

[0029] (5) Part of the material in the crystallization kettle is discharged and centrifugally filtered, and the water phase and the oil phase...

Embodiment 2

[0034] (1) Prepare 2 kg of crude product with a mass content of 85% thymol, 2 kg of finished thymol (content greater than 98%), 5 kg of pure water, and 320 g of thymol seed crystals.

[0035] (2) According to the mass ratio of 85% thymol crude product and pure water 1.5:1, each weigh 1.5 kg of 85% thymol crude product and 1 kg of pure water and put them into the crystallization kettle;

[0036] (3) After the crude thymol and pure water were mixed evenly without delamination, a small amount of material was taken to measure its crystallization point T, and the crystallization point T was 31.5°C.

[0037] (4) Stir continuously at a rotation speed of 95r / min, cool the crystallization kettle to T+3°C, that is, start adding seed crystals at 34.5°C, add 320g of thymol seed crystals, and keep warm for 1h at a cooling rate of 2°C / h down to 15°C;

[0038](5) Part of the material in the crystallization kettle is discharged and centrifugally filtered, and the water phase and the oil phas...

Embodiment 3

[0043] (1) Prepare 1 kg of crude product with a mass content of 95% thymol, 2 kg of finished thymol (content greater than 98%), 5 kg of pure water, and 135 g of thymol seed crystals.

[0044] (2) According to the mass ratio of 95% thymol crude product and pure water 1:1, each weigh 1 kg of 95% thymol crude product and 1 kg of pure water and put them into the crystallization kettle;

[0045] (3) After the crude thymol and pure water were mixed evenly without stratification, a small amount of material was taken to measure its crystallization point T, and the crystallization point T was 26.4°C.

[0046] (4) Stir continuously at a rotation speed of 120r / min, cool the crystallization kettle to T+2°C, that is, start adding seed crystals at 28.4°C, add 135g of thymol seed crystals, and keep warm for 30min at a cooling rate of 5°C / h down to 20°C;

[0047] (5) Part of the material in the crystallization kettle is discharged and centrifugally filtered, and the water phase and the oil p...

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Abstract

The invention relates to a continuous purification method of thymol. The method comprises the following steps: putting a certain amount of a thymol crude product and water into a crystallization kettle, uniformly mixing without layering, measuring the crystallization point T of the material, continuously stirring the obtained mixed material, adding thymol seed crystal when the crystallization kettle is cooled to be slightly higher than T, then cooling to 15-20 DEG C, discharging and centrifugally filtering part of the material in the crystallization kettle, discharging the water phase and the oil phase together to obtain a thymol finished product, and discharging to realize continuous water crystallization and purification of the thymol crude product. The method is especially suitable for industrial mass production, the quality of the purified thymol finished product reaches 98% or above, the thymol content in the oil phase mother liquor is 62% or below, the quality of the continuously purified thymol finished product is kept stable, and the oil phase and the water phase after discharging and centrifuging can be continuously used.

Description

technical field [0001] The invention belongs to the field of thymol, in particular to a continuous purification method of thymol. Background technique [0002] Thymol, also known as thymol, thymol, chemical name is 5-methyl-2-isopropylphenol, English name: thymol, white to light yellow crystalline powder at room temperature, it has the characteristics of thyme or thyme Its special aroma and sweet spicy flavor are often used in the preparation of various food flavors such as gummies, peppermint, citrus and mushroom flavors; and it has strong antiseptic and bactericidal properties, and is a widely used chemical. The bactericidal ability is stronger than phenol, but the toxicity is lower than phenol. It can be used as medical medicine and oral hygiene product; it also has antifungal and parasitic functions, and can be used to treat wounds and store anatomical specimens. An important raw material of the brain, it can be used as an insect repellant; it can also be used as an ant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/68C07C37/84C07C39/06
CPCC07C37/685C07C37/84C07C39/06
Inventor 张其忠郝宗贤欧加思韩辉
Owner ANHUI HAIHUA CHEM
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