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Treatment method of recycled pentamethyl indane

A technology of pentamethylindene and treatment methods, applied in chemical instruments and methods, purification/separation of hydrocarbons, hydrocarbons, etc., can solve the problem of low reaction conversion rate and yield, low yield, and low yield of main reaction and other issues to achieve the effect of improving conversion rate, reducing production cost and improving production efficiency

Active Publication Date: 2020-11-13
安徽金轩科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the industrialized production of Jiale musk, the Friedel-Crafts alkylation reaction between pentamethylindane and propylene oxide has always had problems such as low reaction conversion and yield, and nearly 40% of pentamethylindane does not participate in the reaction, so Jiale Pentamethylindane must be recovered during the distillation and purification of musk (the pentamethylindane is evaporated out of the rectification tower, and alcohols with a boiling point close to the pentamethylindane will be brought out together), but the recovered pentamethylindane The yield of methylindane and propylene oxide Friedel-Crafts alkylation reaction is even lower, because there are a lot of organic alcohols in the pentamethylindane of recovery, and the catalyst is aluminum trichloride in the main reaction material, and this catalyst and alcohols Dehydration reaction occurs, the generated water will be hydrolyzed with aluminum trichloride to obtain hydrochloric acid, hydrochloric acid and propylene oxide react to generate chloropropanol, and the generated alcohols undergo a cyclic reaction, and the final main reaction yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 2

[0024] 1. Pump 3000kg of pentamethylindane solution with a pentamethylindane content of about 80% recovered from the Jiale Musk Rectification Tower into a 5000L indane recovery kettle, turn on the stirring, turn on the vacuum pump, and turn on the Feed the cut-off door, use a stainless steel hose to pump in 15kg of ferrous sulfate. After the ferrous sulfate is pumped out, turn off the vacuum pump and open the emptying cut-off door of the kettle.

[0025] 2. Slowly add 300kg of 98% sulfuric acid dropwise, the temperature will rise slowly for about 1-2 hours. After the dropwise addition, open the steam inlet valve of the kettle and slowly raise the temperature to 50-60 degrees. After the temperature stabilizes, slowly drop Add 200kg of 34% hydrogen peroxide, and drip it for about 1 hour. After the temperature is stable, open the steam cut-off door of the kettle, slowly raise the temperature to 80 degrees, and keep it at 80 degrees for 5 hours. About 700kg goes into the acid wate...

example 3

[0029] 1. Pump 3000kg of pentamethylindane solution with a pentamethylindane content of about 80% recovered from the Jiale Musk Rectification Tower into a 5000L indane recovery kettle, turn on the stirring, turn on the vacuum pump, and turn on the Feed the cut-off door, use a stainless steel hose to pump in 13kg of ferrous sulfate. After the ferrous sulfate is pumped out, turn off the vacuum pump and open the emptying cut-off door of the kettle.

[0030] 2. Slowly add 200kg of 98% sulfuric acid dropwise, the temperature will rise slowly for about 1-2 hours. After the dropwise addition, open the steam inlet valve of the kettle and slowly raise the temperature to 50-60 degrees. After the temperature stabilizes, slowly drop Add 300kg of 34% hydrogen peroxide, and drip it in about 1 hour. After the temperature is stable, open the steam cut-off door of the kettle, slowly raise the temperature to 80 degrees, and keep it at 80 degrees for 5 hours. About 700kg goes into the acid water...

example 4

[0034] 1. Pump 3000kg of pentamethylindane solution with a pentamethylindane content of about 80% recovered from the Jiale Musk Rectification Tower into a 5000L indane recovery kettle, turn on the stirring, turn on the vacuum pump, and turn on the Feed the cut-off door, use a stainless steel hose to pump in 13kg of ferrous sulfate. After the ferrous sulfate is pumped out, turn off the vacuum pump and open the emptying cut-off door of the kettle.

[0035] 2. Slowly add 300kg of 98% sulfuric acid dropwise, the temperature will rise slowly for about 1-2 hours. After the dropwise addition, open the steam inlet valve of the kettle and slowly raise the temperature to 50-60 degrees. After the temperature stabilizes, slowly drop Add 300kg of 34% hydrogen peroxide, and drip it in about 1 hour. After the temperature is stable, open the steam cut-off door of the kettle, slowly raise the temperature to 80 degrees, and keep it at 80 degrees for 5 hours. About 800kg is put into the acid wat...

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Abstract

The invention relates to a treatment method for recovering pentamethyl indane in galaxolide production. The treatment method comprises the following steps: adding a certain amount of ferrous sulfate into a recovered pentamethyl indane solution, and slowly and dropwise adding a certain amount of concentrated sulfuric acid to provide an acidic environment; after the concentrated sulfuric acid is dropwise added, controlling a certain temperature, dropwise adding hydrogen peroxide and carrying out Fenton oxidation reaction; after dropwise adding is completed, carrying out heating to a certain temperature to continue the reaction, and after the reaction is completed, conducting standing for layering and separating out lower-layer acid water; adding excessive alkaline water into an upper-layer pentamethyl indane phase for neutralization; and after neutralization is completed, separating out lower-layer alkaline water to obtain treated pentamethyl indane. According to the method, the conversion rate of pentamethyl indane is increased, production cost is reduced, production efficiency is greatly improved, the reaction efficiency and the material utilization rate of the whole production process are optimized, and the economic benefits of enterprises are increased.

Description

Technical field: [0001] The invention belongs to the technical field of chemical production, and relates to a method for treating pentamethylindane recovered in the production of musk musk. Background technique: [0002] Jiale musk (English name: Galaxolide) is the first synthetic musk successfully developed by the International Fragrance and Fragrance Company (IFF) in the 1960s. Molecular weight 258.4, boiling point 129°C (107Pa), chemical name is 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta-γ-2- Benzopyran has a strong and long-lasting musky aroma, accompanied by woody aroma, and is widely used in cosmetics, soap essence and other industries. [0003] Pentamethylindane is an intermediate product of Carol musk. At present, the main industrial route is to react α-methylstyrene and isopentene with phosphoric acid as a catalyst to generate pentamethylindane, and then pentamethylindane and Propylene oxide undergoes Friedel-Crafts alkylation reaction to obtain hexame...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/45C07C7/00C07C7/148C07D311/94
CPCC07C7/005C07C7/14858C07D311/94C07C2602/08C07C13/45
Inventor 易建康常业坤吕祖鹏何基达
Owner 安徽金轩科技有限公司
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