Constant-pressure production device for methyl decalactone synthesized spice and production method
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A technology for synthesizing methyl decolactone and fragrance, which is applied in directions such as organic chemistry, and achieves the effects of mild reaction conditions, relatively easy process and simple operation.
Active Publication Date: 2015-07-29
ANHUI HYEA AROMAS
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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
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Embodiment 1
[0041] In this embodiment, secondary octanol and acrylic acid are used as main raw materials, and the by-products are tert-butanol and water.
[0042] a) Put the materials sec-octanol, di-tert-butyl peroxide and acrylic acid into sec-octanol high tank 1, di-tert-butyl peroxide high tank 2, acrylic acid or methyl acrylate high tank 3 respectively , acrylic acid or methyl acrylate head tank 3 maintains a temperature of 20 ± 5 ° C; from the above three head tanks, 100 kg of acrylic acid, 270 kg of sec-octanol, and 15 kg of initiator di-tert-butyl peroxide are put into the batching pot 4, Stir and mix evenly, and control the batching temperature at 20-25°C.
[0043] In this step, the molar ratio of the amount of secondary octanol to acrylic acid is 1.49:1; the molar ratio of the amount of di-tert-butyl peroxide to acrylic acid is 0.07:1.
[0044] b) Metering 550 kg of sec-octanol from the sec-octanol header tank 1 into the reactor 6 as a base material through a direct connection ...
Embodiment 2
[0057] The process of this embodiment is the same as that of Embodiment 1, the difference is that in this embodiment, methyl acrylate is used instead of acrylic acid; by-products are tert-butanol and methanol; the ratio of each raw material is different from that of Embodiment 1.
[0058] Specific steps include:
[0059] a) Put the materials sec-octanol, di-tert-butyl peroxide and methyl acrylate into sec-octanol head tank 1, di-tert-butyl peroxide head tank 2, acrylic acid or methyl acrylate head tank 3 Standby in the middle, the No. 3 high-level tank maintains a temperature of 20±5°C;
[0060] Put 120kg of methyl acrylate, 270kg of sec-octanol, and 20kg of initiator di-tert-butyl peroxide into the batching pot from the above three high-level tanks, stir and mix evenly, and control the batching temperature at 20-25°C.
[0061] In this step, the molar ratio of the batching amount of secondary octanol to methyl acrylate is 1.5:1; the molar ratio of the batching amount of di-te...
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Abstract
The invention provides a constant-pressure production device for methyl decalactone synthesized spice. The constant-pressure production device comprises a DL-2-Octanol high-level tank, a di-tert-butyl peroxide high-level tank, and an acrylic or methyl acrylate high-level tank and further comprises a kettle type rectifying tower, wherein the DL-2-Octanol high-level tank, the di-tert-butyl peroxide high-level tank and the acrylic or methyl acrylate high-level tank are in pipeline connection with an ingredient pan; the ingredient pan is in pipeline connection with a dropwise adding pump, one or more dropwise adding pipes are arranged in a reaction kettle, and the dropwise adding pump is connected with the dropwise adding pipes; the bottom of the reaction kettle is in pipeline connection with a rinsing pan, the bottom of the rinsing pan is in pipeline connection with a standing high-level tank through a pump A, the standing high-level tank is in pipeline connection with a kettle type distillation tower, and the bottom of the kettle type distillation tower is in pipeline connection with a material high-level temporary storage groove through a pump C; the material high-level temporary storage groove is in pipeline connection with the kettle type rectifying tower, and the kettle type rectifying tower is connected with a product vacuum holding tank through a first-class condenser and a second-class condenser. According to the constant-pressure production device disclosed by the invention, the methyl decalactone synthesized spice can be synthesized in a constant-pressure manner, the product yield is high, the technological conditions are mild, the production cost is relatively low, and environmental pollution is avoided in a production process.
Description
technical field [0001] The invention relates to the technical field of fine chemical production, in particular to an atmospheric pressure production device for synthesizing fragrances from methyldecalactone. 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 ...
Claims
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