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Method for synthesizing 4-terpineol by catalyzing 1,4-cineole through supported acid catalyst

A catalyst and acid-loaded technology, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of complex and cumbersome post-processing, expensive metal lithium, and no application seen, so as to broaden the source and process. Simple, easy-to-operate effect

Active Publication Date: 2017-05-10
云南森美达生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The conversion rate of the second method raw material 1, 4-cineole and the selectivity of 4-terpineol are all higher, but there are many places to be improved
If alkaline reaction is used in the 1,3-propylenediamine / lithium system, the required temperature is high, the reaction time is long, the amount of 1,3-propylenediamine or other amine solvents is large, and the metal lithium is expensive and the utilization rate is low. Not high, the post-processing is complicated and cumbersome, so the production cost is high
The only report about the mixed acid system at present is that the mixed acid composed of phosphoric acid and acetic acid is used. The conversion rate of 1, 4-cineole and the selectivity of 4-terpineol can reach up to 75%, but its acid consumption is large. , and requires a large amount of solvent extraction and separation before it can be reused. The biggest problem is that it has not yet seen its industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Mix 10 grams of mordenite with 30 grams of concentrated sulfuric acid solution with a mass fraction of 98%, heat to 50° C. and stir for 1 hour;

[0028] Step 2: Place the stirred mixed solution naturally to cool to room temperature, separate the remaining concentrated sulfuric acid, filter, rinse the attached acid on the surface of mordenite with distilled water, and dry the obtained mordenite at 50°C for 2 hours under reduced pressure to obtain Mordenite supported acid catalyst;

[0029] Step 3: Add 100g of raw material oil (containing 77.8% of 1,4-cineole) and 6g of mordenite-supported acid catalyst into the reaction flask, and stir and react at 50°C for 8 hours; the reaction liquid contains 1,4-cineole by gas chromatography -Cineole 4.2%, 4-terpineol 59.6%, α-terpinene 7.3%, γ-terpinene 5.2%;

[0030] Step 4: The reaction solution was filtered to recover the mordenite-supported acid catalyst, and the oil phase was distilled under reduced pressure to obtain a...

Embodiment 2

[0032] Step 1: Mix 10 grams of mordenite with 50 grams of concentrated sulfuric acid solution with a mass fraction of 85%, heat to 45° C. and stir for 2 hours;

[0033] Step 2: Place the stirred mixed solution naturally to cool to room temperature, separate the remaining concentrated sulfuric acid, filter, rinse the attached acid on the surface of mordenite with distilled water, and dry the obtained mordenite at 50°C for 2 hours under reduced pressure to obtain Mordenite supported acid catalyst;

[0034] Step 3: Add 100g of raw material oil (containing 86% of 1,4-cineole) and 5g of mordenite-supported acid catalyst into the reaction bottle, stir and react at 60°C for 5h; the reaction solution contains 1,4-cineole by gas chromatography -Cineole 3.7%, 4-terpineol 67.5%, α-terpinene 6.4%, γ-terpinene 5.6%.

[0035] Step 4: The reaction solution was filtered to recover the mordenite-supported acid catalyst, and the oil phase was distilled under reduced pressure to obtain a chroma...

Embodiment 3

[0037] Step 1: Mix 10 grams of mordenite with 40 grams of concentrated sulfuric acid solution with a mass fraction of 90%, heat to 50° C. and stir for 1.5 hours;

[0038] Step 2: Place the stirred mixed solution naturally to cool to room temperature, separate the remaining concentrated sulfuric acid, filter, rinse the attached acid on the surface of mordenite with distilled water, and dry the obtained mordenite at 50°C for 2 hours under reduced pressure to obtain Mordenite supported acid catalyst;

[0039] Step 3: Add 100g of raw material oil (containing 47.2% of 1,4-cineole) and 3g of mordenite-supported acid catalyst into the reaction flask, stir and react at 60°C for 7h; -Cineole 4.8%, 4-Terpineol 34%, α-Terpinene 4.1%, γ-Terpinene 3.5%.

[0040] Step 4: The reaction solution was filtered to recover the mordenite-supported acid catalyst, and the oil phase was distilled under reduced pressure to obtain a chromatographic content of 98.7% for 4-terpineol.

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PUM

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Abstract

The invention discloses a method for synthesizing 4-terpineol by catalyzing 1,4-cineole through a supported acid catalyst. The method comprises the following steps: preparing a catalyst, preparing 4-terpineol and the like. According to the method for synthesizing 4-terpineol by catalyzing 1,4-cineole through the supported acid catalyst disclosed by the invention, the chromatogram content can be 5% or lower after the 1,4-cineole in the raw oil is completely reacted, while the selectivity of the 4-terpineol reaches 80% or higher. Meanwhile, in addition to the 4-terpineol produced in the reaction, alpha-terpinene, gamma-terpinene and the like with high additional value can be produced, and the used mordenite supported acid catalyst can be recycled. The method disclosed by the invention has the advantages of small catalyst dosage, high selectivity, short reaction time, simple and convenient process, simplicity in operation and the like.

Description

technical field [0001] The invention relates to a method for synthesizing 4-terpineol, in particular to a method for synthesizing 4-terpineol from 1,4-cineole catalyzed by a loaded acid catalyst. Background technique [0002] 4-Terpineol is a monocyclic monoterpene alcohol, also known as terpineol-4, terpinen-4-ol, 1-p-menten-4-ol, 1-methyl-4-isopropyl- 1-cyclohexen-4-ol, 4-terpineol, naturally occurs in natural plant essential oils such as tea tree oil. 4-Terpineol has spicy, woody, earthy and lily aromas, and is an important fine chemical product. 4-Terpineol is a strong disinfectant, antiseptic and ideal spice, widely used in cosmetics, soap, shampoo, toothpaste and other products, and has been widely used in biological pesticides. [0003] 4-Terpineol has obvious killing and inhibiting effects on bacteria, fungi and viruses. In the antibacterial experiment, it is effective against all bacteria and has special biological activity. 4-Terpineol extracted from Japanese cyp...

Claims

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Application Information

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IPC IPC(8): C07C35/18C07C29/10B01J29/18
CPCB01J29/18C07C29/103C07C35/18Y02P20/584
Inventor 黄金龙邱安彬汪锦航刘学东翁国荣崔军涛李强
Owner 云南森美达生物科技股份有限公司
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