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Method for preparing beta-naphthyl methyl ether

A technology of naphthalene methyl ether and methanol, which is applied in the field of preparation of chemical products, can solve problems such as product separation and safety difficulties, achieve better color and aroma, high yield, and easy to obtain

Pending Publication Date: 2022-03-08
杭州可菲克化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In CN 106831360 B, the organic acid SO 4 2- / Hβ is the catalyst, through the tubular gas phase catalytic reaction, the pressure and high temperature reaction is adopted, the material is easy to coke and carbonize in the reaction, which makes the separation and safety of the product difficult, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for preparing β-naphthyl methyl ether is characterized in that comprising the following steps:

[0022] (1) With a certain proportion of methyl alcohol and 2-naphthol as raw materials, the mass ratio of methyl alcohol and 2-naphthol is 1.0:1 and puts into the reactor; Catalyst, the reaction temperature is controlled at 70-150°C; in order to promote the reaction, methanol is used to distill out methanol and entrain water at the same time during the reaction. After the reaction at a certain temperature, methanol is gradually added at the same time; (2) After the reaction is completed, excess methanol is put into the reactant to filter, and the dissolved and filtered catalyst is reused; (3) After the methanol is recovered from the material, it is decolorized by high vacuum distillation , You can get β-naphthyl methyl ether. The whole reaction ends without producing secondary pollutants.

[0023] Through product detection, the purity of β-naphthyl methyl ether re...

Embodiment 2

[0025] A method for preparing β-naphthyl methyl ether is characterized in that comprising the following steps:

[0026] (1) With a certain proportion of methyl alcohol and 2-naphthol as raw materials, the mass ratio of methyl alcohol and 2-naphthol is 1.5: 1 and puts into the reaction kettle. When feeding materials, the mass ratio of methyl alcohol and 2-naphthol is 1.0:1 input; high-temperature cationic acidic resin polyperfluorosulfonic acid resin is used as a catalyst, and the reaction temperature is controlled at 70-150°C; when the reaction reaches a certain level, the remaining methanol is added to the reactor.

[0027] (2) After the reaction finishes, drop into ethanol to filter in the reactant, and reuse the catalyst after dissolving and filtering; (3) After the material reclaims ethanol, adopt high vacuum distillation to decolorize to obtain β-naphthyl methyl ether. The whole reaction ends without producing secondary pollutants.

[0028] Through the detection of the p...

Embodiment 3

[0030] With the same raw material ratio of embodiment 2, and the same operating conditions, the solvent dropped into in step (2) is dimethylbenzene, and the catalyst adopts alkyl-substituted naphthalene sulfonic acid type resin, through the recovery and decolorization of step (3) Finally, high-quality β-naphthyl methyl ether can also be obtained. The whole reaction ends without producing secondary pollutants.

[0031] Through the detection of the product, the purity of β-naphthyl methyl ether reaches 99.6%, the conversion rate of 2-naphthol reaches more than 97.92%, and the selectivity reaches 98.5%. The recovered catalyst has been reused many times, and the reaction speed has no obvious change. There is no expansion and breakage at high temperature and during stirring.

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Abstract

The invention discloses a preparation process of a chemical product, and particularly relates to a production method for preparing beta-naphthyl methyl ether. According to the method, methanol and 2-naphthol in a certain proportion are used as raw materials, high-temperature-resistant cationic acidic resin is used as a catalyst for reaction, and after the reaction is finished, the catalyst can be recycled through filtration and can be reused; and after recovering the solvent from the material, carrying out high-vacuum distillation decoloration to obtain the high-content beta-naphthyl methyl ether. The method has the advantages that the catalyst can be conveniently recycled, the yield is high, no secondary wastewater is generated after reaction, the method is more environment-friendly, and the product is better in color and aroma through high-vacuum decoloration; and the high-temperature cation acidic resin is also very easy to obtain.

Description

technical field [0001] The invention discloses a preparation process of chemical products, specifically a production method for preparing β-naphthyl methyl ether. Background technique [0002] β-Naphthyl methyl ether is an important raw material for synthetic fragrances, widely used in blending fragrances of floral flavors, and also used as fragrances for soaps. In recent years, with the development of the pharmaceutical industry, β-naphthyl methyl ether is used to prepare various pharmaceutical intermediates. At present, there are two main methods for preparing β-naphthyl methyl ether. One is to use β-naphthol and dimethyl sulfate as raw materials, carry out methylation reaction in aqueous sodium hydroxide solution, and then obtain it through neutralization, washing and distillation. The second is to use concentrated sulfuric acid as a catalyst, add 2-naphthol and methanol in proportion to the reactor, then drop concentrated sulfuric acid for reflux reaction for 6-8 hours,...

Claims

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Application Information

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IPC IPC(8): C07C41/09C07C41/42C07C43/20
CPCC07C41/09C07C41/42C07C43/202Y02P20/584
Inventor 朱旭光黄桂钟
Owner 杭州可菲克化学有限公司
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