Preparation method of dimethyl ethyl aminobenzoate midbody nitrobenzoic acid ethyl ester

A technology of ethyl dimethylaminobenzoate and ethyl nitrobenzoate, which is applied in the field of preparation of ethyl dimethylaminobenzoate intermediate p-nitrobenzoate, to reduce the amount of three wastes and reduce the cost Effect

Inactive Publication Date: 2016-02-24
浙江优创材料科技股份有限公司
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  • Application Information

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Problems solved by technology

[0003] For the above-mentioned technical problem of prior art, the purpose of this invention is to provide a kind of preparation method of ethyl dimethylaminobenzoate intermediate p-nitrobenzoate, adopt super strong solid acid as catalyzer, use fixed bed reactor The preparation method of continuous esterification obtains the target product, which solves the problem of producing a large amount of waste acid and high-salt wastewater in the existing industrial production, and greatly reduces the discharge of wastewater

Method used

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  • Preparation method of dimethyl ethyl aminobenzoate midbody nitrobenzoic acid ethyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The reaction equation of preparing ethyl dimethylaminobenzoate intermediate p-nitrobenzoate of the present invention is as follows:

[0022] .

[0023] Concrete preparation steps are:

[0024] Add 15kg of p-nitrobenzoic acid and 60kg of ethanol into a 100L reactor, stir and dissolve, pump the metering pump into the first-stage fixed bed (temperature: 50-80°C) pre-installed with HY type solid acid catalyst, and the material coming out The content is controlled at more than 80%, and then pumped into the second-stage fixed-bed reactor (temperature 80-150°C) with a metering pump, and the content of the material coming out is more than 98%.

[0025] Put the material into the desolventizer, separate the excess ethanol and water, add 5% sodium carbonate solution to wash, wash off the excess raw material at 70-80°C, add water to disperse, centrifuge, and dry to obtain the finished product with a yield of more than 96%. .

Embodiment 2-5

[0027] The proportioning ratio of p-nitrobenzoic acid and ethanol in Examples 2-5 is shown in Table 1 below, and the other steps are the same as in Example 1, and the yields are all above 96%.

[0028]

[0029] The present invention adopts a super strong solid acid as a catalyst, and obtains the target product through the preparation method of continuous esterification in a fixed-bed reactor, which solves the problem of producing a large amount of waste acid and high-salt waste water in the existing industrial production, and greatly reduces waste water production. emission.

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Abstract

The invention relates to a preparation method of dimethyl ethyl aminobenzoate midbody nitrobenzoic acid ethyl ester. The preparation method includes the following steps that 1, nitrobenzoic acid and ethyl alcohol are added to a dissolution kettle, and the mixture obtained after dissolution is pumped into a fixed-bed reactor through a metering pump, wherein the fixed-bed reactor is pre-filled with an HY type solid acid catalyst, and the temperature of the fixed-bed reactor is controlled; 2, after the content of the material obtained after a fixed-bed reaction reaches the index, the material is pumped into a desolvation kettle, after desolvation, alkali washing and washing, cooling and dispersing, centrifuging and drying are conducted, and the product is obtained. The target product is obtained through the preparation method in which ultra-high solid acid serves as the catalyst and the fixed-bed reactor is used for continuous esterification, the problem that a large amount of waste acid and high-salinity wastewater is generated in existing industrial production is solved, and the emission of wastewater is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, in particular to a preparation method of ethyl dimethylaminobenzoate intermediate p-nitrobenzoate. Background technique [0002] Ethyl p-nitrobenzoate is an important chemical product intermediate, an important raw material for making benzocaine, tetracaine hydrochloride, and ultraviolet absorbers. The current industrial production method is p-nitrobenzoic acid and Ethanol is dehydrated and esterified to obtain the target product. The key is the choice of catalyst for the reaction. Concentrated sulfuric acid, methanesulfonic acid, etc. are used. The main problem with such a catalyst is the production of a large amount of waste acid and waste water, and the pressure on environmental protection is high. Contents of the invention [0003] For the above-mentioned technical problem of prior art, the purpose of this invention is to provide a kind of preparation method of ethyl dimethylaminoben...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/57C07C201/12B01J29/08
CPCC07C201/12B01J29/084C07C205/57
Inventor 任志龙朱晓东施根祥
Owner 浙江优创材料科技股份有限公司
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