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Crystallization and purification method of 1-hydroxyl-3,5-dimethyl-4-chlorobenzene

A purification method, the technology of dimethyl phenol, applied in the field of industrial purification of organic matter, can solve the problems of high solvent cost, environmental pollution, etc., and achieve the effect of high purity

Active Publication Date: 2014-03-05
湖南瑞冠生物化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a crystallization and purification method of 1-hydroxy-3,5-dimethyl-4-chlorobenzene, which uses water as a solvent and does not produce waste gas or waste liquid during the purification process. emission, which solves the technical problems of serious environmental pollution and high cost of solvents in existing purification methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 1000kg of 3,5-dimethylphenol (MX) chlorination product and 1000kg of water into the 3000L cold analysis kettle to form a mixture. The composition of 1000kg 3,5-dimethylphenol chlorination products added to the cold analysis tank was detected by gas chromatography (GC): 3,5-dimethylphenol (MX) 0.7%; 1-hydroxy- 3,5-Dimethyl-4-chlorobenzene (PCMX) 86.7%; o-chlorinated product (OCMX) 10.5%; dichlorinated product (DCMX) 2.1%.

[0025] While stirring, heat the mixture with steam to melt above 92°C, close the steam inlet and outlet, keep it warm for 5-10 minutes, then turn on circulating cooling water for cooling, cool the mixture to below 35°C to crystallize within 4 hours, and then process the obtained Crystals were centrifuged. The product is white crystal with coarse crystal form. GC analysis results are: MX: 0.20%; PCMX: 99.23%; OCMX (ortho-chlorinated product): 0.15%; DCMX (di-chlorinated product): 0.42%.

Embodiment 2

[0027] Add 1000kg of crude 1-hydroxy-3,5-dimethyl-4-chlorobenzene (PCMX) and 1000kg of water into a 3000L cold analysis kettle to form a mixture. The content of 1000kg 1-hydroxyl-3,5-dimethyl-4-chlorobenzene (PCMX) crude product added to the cold analysis tank is detected by gas chromatography (GC) and consists of: 3,5-dimethylphenol ( MX) 0.3%; 1-hydroxy-3,5-dimethyl-4-chlorobenzene (PCMX) 94.7%; ortho-chlorinated product (OCMX) 3.5%; di-chlorinated product (DCMX) 1.5%.

[0028] While stirring, heat the mixture with steam until it melts at 98°C, close the steam inlet and outlet, keep it warm for 5 to 10 minutes, then turn on the circulating cooling water for cooling, cool the mixture to below 30°C within 4 hours, and then process the mixture Centrifuge. The product is white crystal with coarse crystal form. GC analysis results are: MX: 0.10%; PCMX: 99.47%; OCMX (ortho-chlorinated product): 0.11%; DCMX (di-chlorinated product): 0.32%.

Embodiment 3

[0030] Add 1000kg of 1-hydroxyl-3,5-dimethyl-4-chlorobenzene substandard products and 1000kg of water in the production process to the 3000L cold analysis kettle to form a mixture. The content of unqualified products in the production process of 1000kg 1-hydroxyl-3,5-dimethyl-4-chlorobenzene added to the cold analysis tank was detected by gas chromatography (GC), and the composition was: 1-hydroxyl-3, 5-Dimethyl-4-chlorobenzene (PCMX) 98.7%; Alcohol dissolved with visible impurities.

[0031] While stirring, heat the mixture with steam until it melts at 95°C, filter it with a bag filter to remove insoluble impurities, close the steam inlet and outlet, keep it warm for 5-10 minutes, and then turn on the circulating cooling water for cooling, within 4 hours The mixture was cooled to below 35°C, and then the mixture was centrifuged. The product is white crystal with coarse crystal form. The result of GC analysis is: PCMX: 99.75%; the product sample is dissolved in alcohol, and ...

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Abstract

The invention relates to the technical field of industrial purification of organic matters and discloses a crystallization and purification method of 1-hydroxyl-3,5-dimethyl-4-chlorobenzene. The crystallization and purification method comprises the following step of taking water as a crystallization solvent to purify a 1-hydroxyl-3,5-dimethyl-4-chlorobenzene crude product. In the crystallization and purification method of the 1-hydroxyl-3,5-dimethyl-4-chlorobenzene, an organic mater is prevented from being taken as the solvent, so that the crystallization and purification method is environmentally-friendly and green. Meanwhile, after purification, an obtained product has high purity, and the purity of the product can achieve above 99 percent through gas chromatographic analysis. The crystallization and purification method is suitable for the purification of a 1-hydroxyl-3,5-dimethyl-4-chlorobenzene product in the industry and the cosmetic industry.

Description

technical field [0001] The invention relates to the technical field of industrial purification of organic matter, in particular to a method for crystallization and purification of 1-hydroxyl-3,5-dimethyl-4-chlorobenzene. Background technique [0002] 1-Hydroxy-3,5-dimethyl-4-chlorobenzene, also known as 4-chloro-3,5-dimethylphenol, has a CAS number of 88-04-0 and its English abbreviation is PCMX. 1-Hydroxy-3,5-dimethyl-4-chlorobenzene has a wide range of uses. It is not only an intermediate for synthetic dyes and pigments, but also an important raw material for medicine, pesticides and organic synthesis. It is also an important microorganism Killer. In addition, 1-hydroxy-3,5-dimethyl-4-chlorobenzene has an excellent inhibitory effect on bacteria, molds and most fungi, and can be used as an antibacterial agent, antifungal agent, and disinfectant, and is widely used in industry and cosmetics . [0003] Since Dubois reacted with equimolar sulfuryl chloride and molten phenol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/28C07C37/84
Inventor 吴飞胡汉忠
Owner 湖南瑞冠生物化工科技有限公司