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Methyl decyl lactone synthetic perfume normal pressure production method

A technology of methyl decolactone and synthesizing perfume, applied in directions such as organic chemistry, to achieve the effects of high reaction conversion rate, mild reaction conditions, and relatively easy process to implement

Inactive Publication Date: 2015-08-26
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses the natural raw material heptanal as a raw material, and has certain development prospects, but an organozinc reagent is used in the synthesis process, and must be reacted in an inert solvent, and further research is required to realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] a) Put 100kg of acrylic acid, 270kg of sec-octanol, 15kg of initiator di-tert-butyl peroxide, and 2kg of catalyst boric acid into a 630L stirring pot, stir and mix evenly, and control the batching temperature at 20-25°C.

[0034] In this step, the batching amount of secondary octanol and the mol ratio of acrylic acid are 1.49:1; the batching amount of di-tert-butyl peroxide and the mol ratio of acrylic acid are 0.07:1; the batching amount of boric acid is 2% of the weight of acrylic acid %.

[0035] b) Measure 550kg of sec-octanol into the enamel reaction kettle through the head tank, and raise the temperature of the reaction kettle to 155°C-160°C. In this step, the molar ratio of the amount of secondary octanol to acrylic acid is 3.04:1.

[0036] In steps a) and b), the molar ratio of the total amount of secondary octanol to acrylic acid is 4.53:1.

[0037] c) Add the ingredient mixture in step a) dropwise into the reaction kettle in step b) through the dropping pump...

Embodiment 2

[0045] a) Put 400kg of acrylic acid, 1590kg of sec-octanol, 80kg of initiator di-tert-butyl peroxide, and 16kg of catalyst boric acid into the stirring pot, stir and mix evenly, and control the batching temperature at 20-25°C.

[0046] In this step, the batching amount of secondary octanol and the mol ratio of acrylic acid are 2.2:1; the batching amount of di-tert-butyl peroxide and the mol ratio of acrylic acid are 0.2:1; the batching amount of boric acid is 4% of the weight of acrylic acid %.

[0047] b) Add 3976kg of sec-octanol into the stainless steel reaction kettle through the overhead tank, and raise the temperature of the reaction kettle to 160°C-165°C. In this step, the molar ratio of the amount of secondary octanol to acrylic acid is 5.5:1.

[0048] In steps a) and b), the molar ratio of the total amount of secondary octanol to acrylic acid is 7.7:1.

[0049] c) Add the ingredient mixture in step a) dropwise into the reaction kettle in step b) through the dropping...

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PUM

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Abstract

The present invention provides a methyl decyl lactone synthetic perfume normal pressure production method, raw materials are easy to obtain, product yield is high, process conditions are mild, production cost is low, the process of production is free of environmental pollution, and the raw materials cause no production equipment corrosion. The method includes the following steps: a) stirring and mixing evenly acrylic acid, sec-octyl alcohol, initiator di-tertiary butyl peroxide and catalyst boric acid; b) adding the sec-octyl alcohol into a reaction kettle according to the dosage; c) dropwise adding the mixture obtained by the step a) into the reaction kettle for atmospheric pressure reaction; d) stirring at 100-200 DEG C for reaction for 2-5 hours; e) transferring reaction products into a water washing pot, adding clear water for layering, and separating the lower layer water phase; f) transferring upper layer organic phase reaction products to a kettle type distillation tower, heating, recycling the sec-octyl alcohol under vacuum; and g) transferring surplus reaction products into a kettle type rectification tower for fractionation to obtain methyl decyl lactone with the content of 99%.

Description

technical field [0001] The invention relates to the technical field of fine chemical production, in particular to a method for producing methyl decanolactone synthetic perfume. Background technique [0002] The chemical name of methyl decalactone is 5-methyl-5-hexyl-2(3H)furanone, CAS number 7011-83-8, also known as γ-methyl-decalactone, dihydrojasmonolactone, γ- Methyl-γ-decalactone has a gardenia-like floral aroma, accompanied by fruity, coconut and green notes. Methyldecalactone is a colorless to light yellow liquid with a boiling point of 160 °C / 18mmHg, a flash point of >110 °C, a relative density of 0.930~0.950 (25 / 25 °C), and a refractive index of 1.440~1.460 (20 °C). In daily chemical essence, it is widely used in all kinds of jasmine fragrance and fruity fragrance, and has a good fragrance-fixing effect. [0003] Methyldecalactone can also be used as a food additive. It has been identified as GRAS by FEMA, FEMA No. 3786, and has been approved by the US Food an...

Claims

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Application Information

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IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 董金龙王天义汪民富徐基龙汪洋
Owner ANHUI HYEA AROMAS
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