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Preparation method of galaxolide

A technology of Jiale musk and catalyst, which is applied in the directions of essential oil/fragrance, fat production, organic chemistry, etc., can solve the problems of complex and cumbersome process, cumbersome process, serious equipment corrosion, etc., achieve simple process route, and promote condensation and cyclization reaction Effect

Active Publication Date: 2021-02-05
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the reaction between hexamethylindanol and paraformaldehyde needs to be catalyzed by HCl gas first, and then NaOH solution is added to complete the condensation cyclization. Produces highly toxic by-product chloromethyl ether, which is less safe and more harmful to operators
[0005] In view of the deficiencies in the above-mentioned processes, it is urgent to develop a new method for the preparation of musk carole, which can replace the methyleneation reagent paraformaldehyde, and overcome the complicated and cumbersome process, serious equipment corrosion, low safety, and adverse effects on the present production. Unfriendly environment and other issues

Method used

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  • Preparation method of galaxolide

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Experimental program
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Effect test

Embodiment 1

[0038] Mix 89.7g of palladium acetate and 113.4g of tricyclohexylphosphine in 500g of distilled water, raise the temperature to 60°C and stir for 3 hours. After the end, add 127.5g of 4A molecular sieves under stirring to obtain slurry A;

[0039] Using 20wt% sodium bicarbonate solution as alkaline precipitating agent B, respectively heating slurry A and alkaline precipitating agent B to 30°C, and slowly adding alkaline precipitating agent B to slurry A until the pH of the system is 9, Control the reaction temperature of the precipitation process to 30°C; then age at 80°C for 2 hours to obtain the slurry;

[0040] The slurry was filtered, washed with deionized water to obtain a filter cake, and the filter cake was dried at 100°C for 7 hours, then calcined at 300°C for 12 hours, crushed and pressed into tablets to obtain Catalyst 1. After ICP analysis, it is determined that in Catalyst 1, by mass (if there is no special mark, the crystal water of the above-mentioned metal salt ...

Embodiment 2

[0042] Mix 84.0g of palladium chloride and 148.2g of 1,2-bisdiphenylphosphineethane in 500g of distilled water, raise the temperature to 50°C and stir for 6h, after the end, add 97.8g of neutral alumina under stirring and mix to obtain slurry A;

[0043] Use 20wt% ammonium carbonate solution as alkaline precipitant B, heat slurry A and alkaline precipitant B to 40°C respectively, and slowly add alkaline precipitant B to slurry A until the pH of the system is 8.0, Control the reaction temperature of the precipitation process to 40°C; then age at 90°C for 1.5h to obtain the slurry;

[0044] The slurry was filtered and washed with deionized water to obtain a filter cake, and the filter cake was dried at 110°C for 9 hours, then calcined at 450°C for 7 hours, crushed and pressed into tablets to obtain Catalyst 2. After ICP analysis, it was determined that in catalyst 2, the percentages of the following components in the total mass of catalyst 2 were: 17% of Pd, 50% of 1,2-bisdiphe...

Embodiment 3

[0046] Mix 431.3g of tetrakistriphenylphosphine palladium and 83.4g of tributylphosphine in 1000g of distilled water, raise the temperature to 70°C and stir for 4 hours. After the end, add 75.5g of silicon dioxide and mix under stirring to obtain slurry A;

[0047] Use 15wt% ammonia solution as alkaline precipitant B, heat slurry A and alkaline precipitant B to 40°C respectively, and slowly add alkaline precipitant B to slurry A until the pH of the system is 10.0, and control The reaction temperature of the precipitation process is 40°C; then the slurry is obtained after aging at 70°C for 3 hours;

[0048] The slurry was filtered and washed with deionized water to obtain a filter cake. The filter cake was dried at 90° C. for 10 h, then calcined at 400° C. for 10 h, crushed and pressed into tablets to obtain Catalyst 3 . After ICP analysis, it was determined that in the catalyst 3, the percentages of the following components in the total mass of the catalyst 3 by mass were: 20% o...

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Abstract

The invention discloses a preparation method of galaxolide, which comprises the following steps: carrying out methylene etherification reaction on hexamethyl indanol and a TEBBE reagent (CAS: 67719-69-1) under the action of a supported Pd catalyst, carrying out condensation cyclization to generate galaxolide, and carrying out continuous rectification to separate the product. The supported Pd catalyst is represented as Pd-X / Y, X is selected from triphenylphosphine, tributylphosphine, tricyclohexylphosphine, bis(diphenylphosphine) methane, 1, 2-bis(diphenylphosphine) ethane and 4, 5-bis(diphenylphosphin)-9,9-dimethyl xanthene, and Y is selected from carbon nanotubes, ordered mesoporous carbon, neutral alumina, silica, a molecular sieve and kaolin. The process provided by the invention avoidsthe problems of complex process, serious equipment corrosion, low safety, environmental friendliness and the like in the prior art, and the raw material conversion rate and the product selectivity can reach 93% or above.

Description

technical field [0001] The invention relates to a production method of musk musk, in particular to a method for producing musk musk through methylene etherification reaction with TEBBE reagent and condensation and cyclization, and belongs to the technical field of chemical industry. [0002] technical background [0003] Galaxolide is a widely used musk-type synthetic fragrance. The product has a strong aroma, good stability, is safe and non-toxic to the human body, and is cheap compared to natural fragrances. It is very popular among perfumers. At present, there are generally problems such as low reaction yield, high production cost, serious equipment corrosion, and difficulties in the treatment of three wastes in the process of synthesizing Jiale musk in my country. Therefore, it is important to study a new, efficient, and environmentally friendly method for synthesizing Jiale musk. significance. [0004] The current production process of Jiale musk mostly adopts a three-st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/94C11B9/00
CPCC07D311/94C11B9/008
Inventor 朱梦瑶刘杰张静任一臻陈来中张永振
Owner WANHUA CHEM GRP CO LTD
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