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Process for preparing ethyl p-dimethylaminobenzoate

A technology of ethyl dimethylaminobenzoate and ethyl nitrobenzoate is applied in the field of preparation of ethyl p-dimethylaminobenzoate, and can solve the problems of high preparation cost, environmental protection, safety, many three wastes, low yield and the like, Achieve the effect of enhancing market competitiveness, high environmental protection benefits, and high yield

Inactive Publication Date: 2007-08-01
吴建龙
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the perspective of industrial production, the above two synthetic processes have disadvantages such as low yield and many wastes, which lead to problems such as high preparation cost, environmental protection and safety.

Method used

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  • Process for preparing ethyl p-dimethylaminobenzoate
  • Process for preparing ethyl p-dimethylaminobenzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Taking a reactor with a volume of 50L as a container, follow the steps below:

[0023] Premixing: put 7kg of ethyl p-nitrobenzoate and 25kg of methanol (99% content) into a 50L reaction kettle at one time, stir at room temperature until completely dissolved.

[0024] The reaction kettle needs to be replaced with nitrogen, the specific method: vacuumize to -0.07~-0.09Mpa, fill with nitrogen 0.05~0.07Mpa, then vacuumize to -0.07~-0.09Mpa, fill with nitrogen 0.05~0.07Mpa, repeat this twice .

[0025] One-step hydrogenation: add 0.2kg skeleton nickel catalyst under the protection of nitrogen, carry out a one-step hydrogenation reaction at a temperature of 70°C and a hydrogenation pressure of 1.0Mpa, and the reaction time is 10 hours; during the hydrogenation reaction, the reaction is exothermic and cooled by adjusting the reactor jacket The flow rate of water is used to control the reaction temperature.

[0026] Then still need to carry out nitrogen replacement again to r...

Embodiment 2

[0033] Taking a reactor with a volume of 50L as a container, follow the steps below:

[0034] Premixing: put 7kg of ethyl p-nitrobenzoate and 30kg of methanol (95% content) into a 50L reaction kettle at one time, stir at room temperature until completely dissolved.

[0035] The reaction kettle needs to be replaced with nitrogen, the specific method: vacuumize to -0.07~-0.09Mpa, fill with nitrogen 0.05~0.07Mpa, then vacuumize to -0.07~-0.09Mpa, fill with nitrogen 0.05~0.07Mpa, repeat this twice .

[0036] One-step hydrogenation: add 0.1kg skeleton nickel catalyst under the protection of nitrogen, carry out a one-step hydrogenation reaction at a temperature of 80°C and a hydrogenation pressure of 0.8Mpa, and the reaction time is 12 hours; during the hydrogenation reaction, the reaction is exothermic and cooled by adjusting the reactor jacket The flow rate of water is used to control the reaction temperature.

[0037] Then still need to carry out nitrogen replacement again to r...

Embodiment 3

[0044] In the one-step hydrogenation, the catalyst is replaced by a 0.02kg palladium-carbon catalyst, and in the two-step hydrogenation, the catalyst is replaced by a 0.05kg palladium-carbon catalyst. The obtained product content is 99.5%, and the reaction yield is 96%.

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PUM

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Abstract

The invention discloses a making method of p-dimethyl ethyl benzoate, which comprises the following steps: preblending ethyl benzoate and carbinol; adding cavaform to do catalytic hydrogenation; filtering; distilling; condensing; crystallizing; drying; obtaining the product.

Description

technical field [0001] The invention relates to a preparation method of ethyl p-dimethylaminobenzoate. Background technique [0002] Ethyl p-dimethylaminobenzoate is a white crystal, which is an amine synergist, and is usually used together with a photoinitiator in coatings polymerized by ultraviolet radiation. In addition, ethyl p-dimethylaminobenzoate It can also be used in printing inks, photoresists, wood varnishes, and metal coatings. [0003] The synthesis route of ethyl p-dimethylaminobenzoate publicly reported in the literature at present mainly contains following two: 1, take p-dimethylaminobenzoic acid, ethanol as raw material, and protonic acid is the synthetic ethyl p-dimethylaminobenzoate as catalyst; 2. For example, the patent number is 00112515.X, and the name is "Preparation Method of Ethyl p-Dimethylaminobenzoate". This method uses ethyl p-aminobenzoate, methanol, and 37% formaldehyde solution as raw materials, and undergoes catalytic hydrogenation Synthes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/04C07C227/14C07C229/54
Inventor 吴建龙
Owner 吴建龙
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