Method of purifying macrocyclic ester compound of musk

A purification method and compound technology, applied in the direction of organic chemistry, can solve the problems of difficult to guarantee product quality, slow speed of activated carbon, easy to appear turbidity, etc., to achieve the effect of short cycle, pure aroma, and avoid turbidity

Inactive Publication Date: 2003-07-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problems that this method exists mainly are: (1) carry out successively because of three treatment steps, and operation period is long, and expense height; , cold filtration is very difficult; (3) Activated carbon decolorization and filtration is the last process of product refinement, some soluble substances in activated carbon will di

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 300 parts of cycloethylene tridecanedioic acid crude product and 10 parts of powdery activated carbon into the distillation bottle, heat to 100° C. under stirring, and the stirring speed is 60 r / min. Then feed steam to carry out steam distillation, stop passing steam after about 0.8h. The ratio of the amount of water vapor introduced to the weight of the crude product is about 0.4:1, filtered while it is hot, and the activated carbon is separated and removed. The colorless crude product filtrate is distilled and dehydrated under a vacuum of 350mmHg. Carry out rectification and purification, and keep the vacuum at 1-2mmHg. When the product is distilled out, collect the first distilled light component in the front fraction receiver, when the temperature of the distillate reaches 130°C and remains constant, start to collect the product, and collect the fraction at 130-135°C As a refined product, the yield was 88.1%. The appearance of the product is transparent, the a...

Embodiment 2

[0024] Add 260 parts of dodecanedioic acid cycloethylene ester and 8 parts of powdered activated carbon into the distillation flask, stir and mix at a speed of 80r / min, start to heat up, when heated to 110°C, pass in water vapor for steam distillation , and carry out decolorization adsorption at the same time. The weight ratio of the amount of water vapor introduced to the amount of crude product is 0.8:1, and it takes about 2 hours. Then the system is evacuated and dehydrated under a vacuum of 350mmHg, so that the moisture in the crude product can be removed as much as possible. Filtrate while hot, filter out the activated carbon, the filtrate is the crude product of decolorization and deodorization treatment, and then carry out rectification and purification, the vacuum degree of rectification is less than 1.5mmHg, cut off the front light fraction, and collect the fraction at 125-132°C. It is the finished cycloethylene dodecanedioate. The appearance of the product is trans...

Embodiment 3

[0026]350 parts of mixed cycloethylene dicarboxylate crude products and 15 parts of powdered activated carbon were added to a distillation flask, and decolorization, adsorption and steam distillation were carried out according to the method of Example 1. The temperature of the material is 110°C, the stirring speed is 60r / min, the time for feeding water vapor is about 1.5h, and the ratio of the amount of water vapor to the amount of crude product is 0.25:1. It takes about 2.5 hours to dehydrate under normal pressure. Then filter while hot to remove activated carbon, the filtrate is purified by vacuum distillation, the vacuum degree ≯ 1.5mmHg, after cutting off the front fraction, collect the middle fraction at 124-148°C as the refined product. Through gas chromatography analysis, the content of cycloethylene undecanedioate is 2.3%, the content of cycloethylene dodecanedioate is 14.8%, the content of cycloethylene tridecanedioate is 48.7%, and the content of cycloethylene tetrad...

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Abstract

The present invention discloses the purification process of macrolides musk compounds. The vapor distillation step and decoloring adsorption step are coupled so that the adsorption decoloring and bad smell elimination of coarse product are completed simultaneously in the same process. The product is finally purified. The whole purification process is simple, and the product is colorless, transparent, smell-less and stable, and has color, fragrance and purity reaching the requirement of high quality perfume.

Description

technical field [0001] The invention belongs to a method for purifying macrocyclic ester musk compounds, in particular to a method for purifying macrocyclic diester musk compounds. Background technique [0002] Macrocyclic ester musk compounds are a very important class of musk compounds. They are known as the "king of fragrances" in the field of fragrances. Fragrance effect, widely used in the deployment of fragrances for personal products such as various detergents, soaps, shampoos and hair care products. [0003] At present, macrocyclic diester musk compounds at home and abroad all use α, ω-long-chain dicarboxylic acids and diols as the main raw materials to obtain high-molecular-weight linear polyesters through alkyd condensation reactions, and the linear polyesters are then heated at high temperature In the presence of a catalyst, the depolymerization and cyclization produces a crude musk compound product, which is then purified by rectification to obtain a high-purity...

Claims

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Application Information

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IPC IPC(8): C07D321/00
Inventor 王崇辉方向晨佟明友宋喜军
Owner CHINA PETROLEUM & CHEM CORP
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