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Catalyst for synthesizing p-dimethylaminobenzoate and its preparation method and application

A technology of dimethylaminobenzoate and nitrobenzoate, which is applied in the field of catalysts and preparations for the synthesis of p-dimethylaminobenzoate, and can solve the problems of high toxicity, low production efficiency and low product yield and other problems, to achieve the effect of strong acidity, cost-effectiveness improvement, and high molar yield

Active Publication Date: 2022-03-01
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These three methods all have defects such as low production efficiency, high toxicity, and low product yield, and cannot meet the requirements of current domestic environmental protection. Phase catalysts are gradually updated and replaced by new catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. a catalyst for synthesizing p-dimethylaminobenzoate, comprising metal Ni, Pd and carrier aluminum oxide, the mass percentage composition of Ni is 0.8% in the described catalyst, and the mass percentage composition of Pd is 0.3%, The rest is alumina; wherein, the alumina is a hollow bar-shaped γ-alumina with a length of 3-6mm, an outer diameter of 1.5mm, and an inner diameter of the middle cavity of 0.8mm.

[0028] 2. a preparation method of a catalyst for synthesizing p-dimethylaminobenzoate, comprising the following steps:

[0029] (1) Carrier pretreatment: Soak alumina in a hydrochloric acid solution with a volume concentration of 10% for 2 hours, take it out and dry it at 120°C for 12 hours, then soak it in ethanol until the adsorption is saturated, take it out and dry it at 120°C 12h, and then roasted at 800°C for 1.5h in a muffle furnace to obtain a pretreated alumina carrier;

[0030] (2) Preparation of Ni-loaded catalyst precursor by equal-volume impregnation...

Embodiment 2

[0035] 1. a catalyst for synthesizing p-dimethylaminobenzoate, comprising metal Ni, Pd and carrier alumina, the mass percentage composition of Ni is 1% in the described catalyst, and the mass percentage composition of Pd is 0.2%, The rest is alumina; wherein, the alumina is a hollow bar-shaped γ-alumina with a length of 3-6mm, an outer diameter of 1.5mm, and an inner diameter of the middle cavity of 0.8mm.

[0036] 2. a preparation method of a catalyst for synthesizing p-dimethylaminobenzoate, comprising the following steps:

[0037] (1) Carrier pretreatment: Soak alumina in a hydrochloric acid solution with a volume concentration of 9% for 2 hours, take it out and dry it at 120°C for 12 hours, then soak it in ethanol until the adsorption is saturated, take it out and dry it at 120°C 12h, and then roasted in a muffle furnace at 900°C for 0.5h to obtain a pretreated alumina carrier;

[0038] (2) Preparation of Ni-loaded catalyst precursor by equal-volume impregnation method: D...

Embodiment 3

[0043] 1. a catalyst for synthesizing p-dimethylaminobenzoate, comprising metal Ni, Pd and carrier aluminum oxide, the mass percentage composition of Ni is 1% in the described catalyst, and the mass percentage composition of Pd is 0.3%, The rest is alumina; wherein, the alumina is a hollow bar-shaped γ-alumina with a length of 3-6mm, an outer diameter of 1.5mm, and an inner diameter of the middle cavity of 0.8mm.

[0044] 2. a preparation method of a catalyst for synthesizing p-dimethylaminobenzoate, comprising the following steps:

[0045] (1) Carrier pretreatment: Soak alumina in a hydrochloric acid solution with a volume concentration of 6% for 2 hours, take it out and dry it at 120°C for 12 hours, then soak it in ethanol until the adsorption is saturated, take it out and dry it at 120°C 12h, and then roasted in a muffle furnace at 900°C for 1h to obtain a pretreated alumina carrier;

[0046] (2) Preparation of Ni-loaded catalyst precursor by equal-volume impregnation meth...

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Abstract

The invention discloses a catalyst for synthesizing p-dimethylaminobenzoate and its preparation method and application, comprising metal Ni, Pd and carrier alumina, the mass percentage of Ni in the catalyst is 0.8-1.1%, Pd The mass percentage content of aluminum oxide is 0.2‑0.5%, and the rest is alumina. The invention also discloses the preparation method and application of the catalyst. The prepared catalyst uses p-nitrobenzoate and formaldehyde as raw materials to complete the nitro hydrogenation and methylation reaction in one step to generate the target product with high molar yield; the method of staged loading and staged feeding is adopted during preparation , at the upper end of the reaction tube, the catalyst mainly carries out the nitro hydrogenation reaction, which is an exothermic reaction and the reaction is violent. The material after the reaction at the upper end enters the catalyst at the lower end with the reaction heat. The material is mainly amino compounds, and methylation occurs with formaldehyde. The remaining small amount of unreacted nitro compounds are rapidly converted to amino compounds on the undiluted catalyst.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for synthesizing p-dimethylaminobenzoate, its preparation method and application. Background technique [0002] P-dimethylaminobenzoate compounds, commonly used mainly include methyl p-dimethylaminobenzoate, ethyl p-dimethylaminobenzoate, n-butyl p-dimethylaminobenzoate, isoamyl p-dimethylaminobenzoate Esters and isooctyl p-dimethylaminobenzoate, these p-dimethylaminobenzoic acid compounds have good anti-ultraviolet properties, so they are widely used in anti-ultraviolet additives, and can play a better role in cosmetics and sunscreens. Good sunscreen effect, especially isooctyl p-dimethylaminobenzoate is recommended by the US Food and Drug Administration as a first-class sunscreen agent. p-Dimethylaminobenzoate compounds, as ultraviolet photoinitiators, are also a class of highly efficient amine accelerators. They are usually used in combination with ph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C07C227/04C07C229/60
CPCC07C227/04B01J23/892C07C229/60
Inventor 林涛张力程杰张炳亮万克柔张之翔曾永康曾利辉高武
Owner XIAN CATALYST NEW MATERIALS CO LTD
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