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Preparation method of galaxolide

A technology of Jiale musk and catalyst, which is applied in the chemical industry, can solve the problems of high production cost, cumbersome and complex process, and complicated and cumbersome process, and achieve the effects of inhibiting the formation of by-products, simple process route, and avoiding environmental pollution

Active Publication Date: 2021-08-10
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The current technology in my country mostly uses 1,1,2,3,3-pentamethylindan to obtain the intermediate hexamethylindanol through alkylation reaction, and then forms ether cyclization with paraformaldehyde to obtain Jiale musk. The process is cumbersome and complicated, and excessive pentamethylindane or toxic chlorobenzene is used as the reaction solvent in the process, which has high cost, high energy consumption, and low yield; the etherification reaction of paraformaldehyde needs to be catalyzed by HCl gas, which may Chloromethyl ether is produced as a highly toxic by-product, which poses a great safety hazard and also seriously corrodes equipment.
[0005] In view of the deficiencies in the above-mentioned processes, it is urgent to develop a new preparation method for musk carole, which overcomes the complicated and cumbersome process, low reaction yield, high production cost, serious equipment corrosion, low safety, and environmental impact. Unfriendly etc.

Method used

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  • Preparation method of galaxolide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Mix 7.6g of cerium chloride and 25.8g of 5-methylbenzotriazole in 500g of distilled water, add 97.8g of aluminum chloride and 36.1g of 4A molecular sieve under stirring, raise the temperature to 80°C and stir for 8 hours to obtain a slurry;

[0038] The slurry was filtered and washed with deionized water to obtain a filter cake, and the filter cake was dried at 90°C for 8 hours, then calcined at 500°C for 2 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 raw material is not counted, and there is no loss of organic matter and carrier, the same below), the percentage of the following components accounting for the total mass of Catalyst 1 is: Ce 5% , Al 23%, 5-methylbenzotriazole 30%, 4A molecular sieve 42%.

Embodiment 2

[0040] Mix 9.9g of cerium chloride and 32.7g of 1-benzoylpiperazine in 300g of distilled water, and add 61.7g of manganese acetate (CH 3 COO) 2 Mn, 35.5g of neutral alumina, heated up to 85°C and stirred for 6h to obtain a slurry;

[0041] The slurry was filtered, washed with deionized water to obtain a filter cake, and the filter cake was dried at 100°C for 10 hours, then calcined at 450°C for 3 hours, crushed and pressed into tablets to obtain Catalyst 2. After ICP analysis, it was determined that in the catalyst 2, the following components accounted for the percentages of the total mass of the catalyst 2 by mass: 6% Ce, 21% Mn, 35% 1-benzoylpiperazine, and 38% neutral alumina.

Embodiment 3

[0043] Mix 22.8g of cerium nitrate and 46.55g of 5-methylbenzotriazole in 500g of distilled water, add 68.3g of nickel nitrate and 44.1g of silicon dioxide under stirring, raise the temperature to 90°C and stir for 4 hours to obtain a slurry;

[0044] The slurry was filtered and washed with deionized water to obtain a filter cake, which was dried at 120° C. for 10 h, then calcined at 400° C. for 4 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 were: Ce 8%, Ni 18%, 5-methylbenzotriazole 38%, and silicon dioxide 36%.

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Abstract

The invention discloses a preparation method of galaxolide, which comprises the following steps: under the action of a supported cerium catalyst, carrying out alkylation reaction on 1, 1, 2, 3, 3, 5-hexamethylindane and epoxypropane, then carrying out dehydration condensation cyclization to generate galaxolide, and carrying out continuous rectification to separate the product. The problems of complex process, low raw material utilization rate, low safety and the like in the prior art are solved, the process is simple, the raw material conversion rate is greater than 95%, and the product selectivity is greater than 92%.

Description

technical field [0001] The invention relates to a production method of Jiale musk, in particular to a production method of 1,1,2,3,3,5-hexamethylindane and propylene oxide through the alkylation reaction followed by dehydration condensation and cyclization to form musk The method of music musk belongs to the technical field of chemical industry. [0002] technical background [0003] Galaxolide is a synthetic tricyclic heterochromatic musk. As a substitute for natural musk, it is widely used in flavors, fragrances and daily chemicals. Jiale musk has good light stability and high aroma quality, and it is a product with the most development potential among polycyclic musks. [0004] The current technology in my country mostly uses 1,1,2,3,3-pentamethylindan to obtain the intermediate hexamethylindanol through alkylation reaction, and then forms ether cyclization with paraformaldehyde to obtain Jiale musk. The process is cumbersome and complicated, and excessive pentamethylinda...

Claims

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Application Information

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IPC IPC(8): C07D311/94B01J31/22
CPCC07D311/94B01J31/1815Y02P20/52
Inventor 朱梦瑶张静李建锋张永振
Owner WANHUA CHEM GRP CO LTD
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