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Preparation method of lyral

A new lily of the valley aldehyde and mixture technology, applied in the field of the preparation of new lily of the valley aldehyde, can solve the problems of increased treatment costs, increased raw material costs, hazardous wastes, etc., and achieves prevention of dehydration and polymerization, easy dehydration and polymerization, and reduced contact. effect of time

Inactive Publication Date: 2019-05-10
WUHAN GEYUAN FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are also reports of other synthetic processes, but the yield is lower and has no industrial significance
[0004] In the above-mentioned first approach, during the desulfurization process of myrcene sulfone, myrcenyl alcohol is easy to dehydrate and polymerize, causing the yield of myrcenyl alcohol to be difficult to exceed 70%, thus greatly affecting the yield of lyral
In the above-mentioned second way, when myrcenyl alcohol and acrolein carry out Diels-Alder reaction, usually need to add catalyst, feed amount reaches 3~5% (calculated by myrcenyl alcohol), raw material cost has increased, and needs to dissolve catalyst first It is easy to reinvest, which increases the complexity of the operation; 3) The catalyst cannot be recycled and becomes a dangerous waste, which increases the processing cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of lyral, comprising the following steps successively:

[0027] 1) Add 1500kg myrcenyl sulfone (94.3% by weight), 4.5kg alkaline substance and 1.5kg polymerization inhibitor in the batching kettle; the alkaline substance is triethanolamine and sodium hydroxide according to the molar ratio of 1 : a mixture formed by mixing 1; the polymerization inhibitor is a mixture formed by mixing hydroquinone and 2,6-di-tert-butyl-4-methylphenol according to a molar ratio of 1:1;

[0028] 2) Put the mixed material into the preheating tube at 42kg / h, control the temperature at 120°C, pressure -0.078Mpa, and preheat for 3 seconds;

[0029] 3) Put the preheated material into the cracking device, control the temperature at 125° C., pressure -0.081 Mp, and crack for 3 seconds to obtain a cracked product containing myrcenol; the yield of cracked myrcenol is 90%;

[0030] 4) Put the lysate into the rectification tank for rectification treatment. The temperature of the ...

example 2

[0036] A preparation method of lyral, comprising the following steps successively:

[0037] 1) Add 1500kg myrcenyl sulfone (95.1% by weight), 7.5kg mixed alkali and 4.5kg polymerization inhibitor in the batching kettle; the basic substance is triethanolamine and sodium hydroxide according to the molar ratio of 1: 1.2 The mixture formed by mixing; the polymerization inhibitor is a mixture formed by mixing hydroquinone and 2,6-di-tert-butyl-4-methylphenol according to the molar ratio of 1:1.2;

[0038]2) Put the mixed material into the preheating tube at 42kg / h, control the temperature at 122°C, pressure -0.079Mpa, and preheat treatment time for 5 seconds;

[0039] 3) Put the preheated material into the cracking device, control the temperature to 128°C, the pressure to -0.081Mp, and the cracking treatment time for 5 seconds to obtain a cracked product containing myrcenol; the yield of cracked myrcenol is 90.8%;

[0040] 4) Put the lysate into the rectification tank for rectific...

example 3

[0046] A preparation method of lyral, comprising the following steps successively:

[0047] 1) Add 1500kg of myrcenyl sulfone (94.7% by weight), 5kg of mixed alkali and 3kg of polymerization inhibitor into the batching kettle; the basic substance is formed by mixing triethanolamine and sodium hydroxide according to the molar ratio of 1:0.8 The mixture; The polymerization inhibitor is the mixture formed by mixing hydroquinone and 2,6-di-tert-butyl-4-methylphenol according to the molar ratio of 1:0.8;

[0048] 2) Put the mixed material into the preheating tube at 42kg / h, control the temperature at 124°C, pressure -0.078Mpa, and preheat treatment time for 4 seconds;

[0049] 3) Put the preheated material into the cracking device, control the temperature at 132°C, the pressure at -0.081Mp, and the cracking treatment time for 4 seconds to obtain a cracked product containing myrcenol; the yield of cracked myrcenol is 89.9%;

[0050] 4) Put the lysate into the rectification tank for...

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Abstract

The invention provides a preparation method of lyral. The preparation method sequentially includes the steps of mixing myrcenol sulfone, alkali and a polymerization inhibitor according to a weight ratio of 1000: (3-5): (1-3), and preheating the mixture at 120-125 DEG C and under minus 0.03Mpa to minus 0.09Mpa for 1-10 seconds; performing pyrolysis at 125-135 DEG C and under minus 0.03Mpa to minus0.09Mpa for 1-10 seconds to obtain a lysate containing myrcenol; performing rectification at the kettle temperature of 135-150 DEG C and the top temperature of 70-100 DEG C as well as under the kettlepressure of minus 0.03Mpa to minus 0.09Mpa and the top pressure of minus 0.03Mpa to minus 0.09Mpa, and collecting materials discharged from the tower top, wherein the materials contain the myrcenol and myrcene; subjecting the materials and acraldehyde to addition reaction without a catalyst, and carrying out rectification under reduced pressure to obtain the lyral. The preparation method has theadvantages that the conversion-per-pass yield of the myrcenol is increased through pyrolysis of the myrcenol sulfone, so that the total yield is increased, and by-products are reduced.

Description

technical field [0001] The invention relates to a synthesis method of fine chemicals, in particular to a preparation method of lyral. Background technique [0002] Liral (Lyral) usually contains 4-(4-hydroxy-4-methylpentyl)-3-cyclohexene-1-carbaldehyde and 3-(4-hydroxy-4-methylpentyl)- 3-Cyclohexene-1-carbaldehyde is a mixture of two isomers. Neoliral is an important fine chemical, which is a colorless viscous liquid with a light and sweet fragrance of rabbit ear grass and a good fragrance of lily of the valley. The fragrance is stable and long-lasting. Lilial is widely used in daily chemical flavors, and can be used to prepare the flavors of high-end perfumes, soaps, detergents, cosmetics and other daily chemical products. [0003] There are two main routes for the synthesis of lyral: one: myrcene is hydrated to generate myrcenol, and during hydration, myrcene and sulfur dioxide are first reacted to generate cyclic myrcene sulfone to protect the myrcene molecular structur...

Claims

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Application Information

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IPC IPC(8): C07C45/69C07C47/46C07C29/00C07C33/02C07C29/80
Inventor 林齐伦
Owner WUHAN GEYUAN FINE CHEM CO LTD
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