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Method for treating free hydrogen chloride in tonalid crude product intermediate

A technology of musk tona and an intermediate is applied in the field of processing crude musk tona, and can solve the problems of affecting color and luster, acidity of cymene, affecting aroma and the like.

Inactive Publication Date: 2018-03-06
YUNNAN YUXI YUNXI ESSENCE & SPICERY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there will be a problem in the actual processing process: a small amount of hydrogen chloride is still left in the crude product of the intermediate, which causes acidity when the intermediate recycles cymene, and corrodes the recovery tower
In the purification of crude products, a small amount of hydrogen chloride is still brought into the product to make the product have a slightly acidic smell, affecting the aroma and color

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] principle:

[0015] Choose to use low-concentration ammonia water to stir and wash at a certain temperature. The washed material is then washed twice with clear liquid until the pH is 7. Sour, the effect is obvious. Utilize ammonia water to dissociate NH3 gas at a certain temperature to allow it to permeate into the product containing hydrogen chloride. produce NH 3 Gas neutralization reaction with HCL to become water-soluble NH 4 CL, and then washed with water to remove the generated NH 4 cl.

[0016] Among them, the reaction basis: NH 3 +HCL→NH 4 CL (gas phase reaction)

[0017] The musk intermediate containing 40% cymene, which is the material after washing with hydrochloric acid and clear water, weighs 1000g by heating to a temperature of 40°C, and mixes 100g of 7% concentration (0.4molNH 3 ) Ammonia water is slowly added dropwise to the material. At this time, there are obvious white crystals adsorbed on the tube wall on the condenser tube. This phenomenon ...

Embodiment 2

[0021] The musk intermediate containing 40% cymene, which is the material after washing with hydrochloric acid and clear water, weighs 1000g by heating to a temperature of 50°C, and mixes 100g of 10% concentration (0.5molNH 3 ) Ammonia water is slowly added dropwise to the material. At this time, there are obvious white crystals adsorbed on the tube wall on the condenser tube. This phenomenon proves that there are free ions of hydrogen chloride in the material. , to generate ammonium chloride NH4CL. When the product encounters condensation, it becomes white crystals of ammonium chloride and adsorbs on the wall of the condenser tube. The crystals are washed away with clear water, and then 50 grams of 8% ammonia water are weighed and added dropwise to the condenser pipe wall during the second dropwise addition, and crystals are rarely separated out. At this time, we raised the liquid temperature to 55°C, and there was a large amount of ammonia smell overflowing from the top of t...

Embodiment 3

[0023] The musk intermediate containing 40% cymene, which is the material after washing with hydrochloric acid and clear water, weighs 1000g by heating to a temperature of 52°C, and mixes 100g of 8% concentration (0.43molNH 3 ) Ammonia water is slowly added dropwise to the material. At this time, there are obvious white crystals adsorbed on the tube wall on the condenser tube. This phenomenon proves that there are free ions of hydrogen chloride in the material. , to generate ammonium chloride NH4CL. When the product encounters condensation, it becomes white crystals of ammonium chloride and adsorbs on the wall of the condenser tube. The crystals are washed away with clear water, and then 50 grams of 8% ammonia water are weighed and added dropwise to the condenser pipe wall during the second dropwise addition, and crystals are rarely separated out. At this time, we raised the liquid temperature to 52°C, and there was a large amount of ammonia smell overflowing from the top of t...

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PUM

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Abstract

The invention provides a method for treating free hydrogen chloride in a tonalid crude product intermediate. The method comprises the steps of utilizing ammonium hydroxide for freeing out NH3 gas at acertain temperature, and permeating the NH3 gas into a product containing hydrogen chloride; carrying out neutralization reaction on the NH3 gas and HCL gas to become water-soluble NH4CL, and then washing with clear water to remove the generated NH4CL; washing the washed material with a clear liquid for twice until ph is 7, so that a washed intermediate semi-finished product cannot be acidized during a fractionation and purification process, and an obvious effect is achieved.

Description

technical field [0001] The invention belongs to the field of perfume chemical reaction, especially for the treatment of the intermediate crude product of musk musk containing free HCL ions, and the effect is obvious. Background technique [0002] Spice is a pleasant substance that can emit fragrance, and it is the most important component of essence. The blending of various spices enriches people's olfactory world. Today, the fragrance and fragrance industry has become an important industry in the country. The participation of fragrances in the industries of cigarettes, alcohol, beverages, cosmetics, and perfumes is inseparable. It is closely related to people's basic necessities of life and indispensable. [0003] Tuna musk (Tonalide) is the trade name of pFw company in the Netherlands, and its chemical name is 7-acetyl-1.1,3,4,4,6-hexamethyltetrahydronaphthalene. It is a white crystal with a melting point of 55-56°C. It is a higher-grade artificial musk than Jiale musk. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/148C07C13/48C07C15/02C07C45/85C07C49/792
CPCC07C7/14858C07C45/85C07C49/792C07C13/48C07C15/02
Inventor 陈永斌谭桂生李发扬代丽珍
Owner YUNNAN YUXI YUNXI ESSENCE & SPICERY