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A kind of preparation method of acetate compound and adopted catalyst

An esterification catalyst and compound technology, applied in the preparation of organic compounds, organic compounds/hydrides/coordination complex catalysts, preparation of carboxylic acid esters, etc. Production costs and other issues, to achieve high acid and alkali resistance, solve environmental pollution, reduce comprehensive costs

Active Publication Date: 2022-05-31
SHANDONG NHU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the acetates prepared by this method, take linalyl acetate as an example: the content of linalyl acetate in the product is 97%, containing 1.49% of dihydrolinalyl acetate impurities, resulting in low product purity
In addition, the use of zinc acetate as a catalyst is not easy to recycle and apply mechanically, causing it to remain in the kettle liquid for a long time, which may easily cause catalyst deactivation
In addition, the esterification reagents in the above reports are enones or enol esters, which are more expensive and increase production costs.
[0010] In addition, some esterification reactions are carried out directly at high temperature without adding a catalyst
Although the preparation process is simplified, the reaction rate will be greatly reduced, and the high temperature will also lead to an increase in side reactions, which is not conducive to the smooth progress of the esterification reaction.
[0011] In summary, in the existing methods for synthesizing acetates, there are obvious shortcomings, such as low conversion rate, poor selectivity, high requirements for equipment, waste salt and waste water, poor product aroma, and unstable chromaticity And other issues

Method used

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  • A kind of preparation method of acetate compound and adopted catalyst
  • A kind of preparation method of acetate compound and adopted catalyst
  • A kind of preparation method of acetate compound and adopted catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] At 45 °C, 20 g of MCM-248 molecular sieve and 200 g of polyvinylpyrrolidone (PVP) (CAS: 9003-39-8, K30) were dispersed in 200 mL of deionized water, and the stirring was started to make it evenly dispersed. After 8 hours, filter The solid was taken out, and placed in a vacuum drying oven at 80° C. and dried to obtain a modified carrier, which was recorded as MCM-248-PVP. At 25 °C, 4.83 g of FeCl 3 ·6H 2 O was dissolved in 10 mL of deionized water, then the modified carrier MCM-248-PVP was added, and stirring was started. The temperature was raised to 45°C, kept for 6 hours, filtered, and the obtained solid was dried in a vacuum drying oven at 80°C to obtain a catalyst of 5.0wt.% FeCl 3 / MCM-248-PVP.

[0070] Loading amount = (metal relative atomic mass / metal salt relative molecular weight * metal salt mass) / carrier mass * 100%

Embodiment 2~54

[0072] By changing the types and proportions of surfactants, carriers and metal salts, following the method of Example 1, the following catalysts were obtained respectively (as shown in Table 1).

[0073] Table 1 Catalyst and preparation parameters

[0074]

[0075]

[0076]

[0077]

[0078] acac stands for acetylacetone; OAc stands for acetate.

Embodiment 55

[0080] At 20 °C, 20 g of MCM-248 molecular sieve and 200 g of polyvinylpyrrolidone (PVP) (CAS: 9003-39-8, K30) were dispersed in 200 mL of deionized water. The solid was taken out, and placed in a vacuum drying oven at 80° C. and dried to obtain a modified carrier, which was recorded as MCM-248-PVP. At 25 °C, 4.83 g of FeCl 3 ·6H 2 O was dissolved in 10 mL of deionized water, then the modified carrier MCM-248-PVP was added, and stirring was started. The temperature was raised to 45°C, kept for 6 hours, filtered, and the obtained solid was dried in a vacuum drying oven at 80°C to obtain a catalyst of 5.0wt.% FeCl 3 / MCM-248-PVP 1 .

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Abstract

The invention discloses a preparation method of acetate compounds and the catalyst used. The preparation method comprises: under the catalysis of the esterification catalyst, alcohol and acetic anhydride undergo esterification reaction, and after the reaction is completed, after-treatment is carried out to obtain the For acetate compounds, the esterification catalyst used is firstly modified with a modifier on the carrier, and then loaded with a metal salt. When the obtained catalyst is used for the esterification reaction, the active site on the substrate and the catalyst can be combined , the obtained acetic acid ester compounds are quickly detached from the catalyst, which not only improves the reaction rate but also reduces the occurrence of side reactions.

Description

technical field [0001] The invention belongs to the fields of fine chemicals and flavors and fragrances, and particularly relates to a preparation method of an acetate compound and a catalyst used. Background technique [0002] Acetate compounds are a very common class of fragrances, widely used in the flavor and fragrance industry, such as linalyl acetate, which is fragrant and elegant, similar to natural bergamot, and has a wide range of uses in perfumery. Lemon oil, lavender oil and other precious spices and essences have high economic value. Geranyl acetate, naturally present in citronella oil, geranium oil, and lavender oil, has the aroma of a mixture of rose oil and lavender oil, and presents an apple fragrance after dilution, and is widely used in the preparation of edible and daily fragrances. Menthyl acetate has a soft mint fragrance, cool and fresh, and is an edible spice allowed by the national standard for the preparation of mint, fruit and other flavors. Other...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/145C07C69/16C07C69/14B01J31/06B01J31/02B01J31/04
CPCB01J31/069B01J31/0204B01J31/0254B01J31/0239B01J31/0244B01J31/0271B01J31/0225B01J31/0229B01J31/0215B01J31/04C07C67/08C07C2601/14B01J2231/49C07C69/145C07C69/16C07C69/14Y02P20/584
Inventor 周剑平马慧娟马啸于明王云龙贺洪峰张传波黄军
Owner SHANDONG NHU PHARMA
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