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Method for preparing 2-ethylhexyl 4-(dimethylamino)benzoate through hydrogenation by taking water as solvent

A technology of dimethylaminobenzoic acid and p-nitrobenzoic acid, which can be used in the preparation of cyanide reaction, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as toxicity, achieve simple process, less use of species, and lightening The effects of dealing with stress

Active Publication Date: 2020-09-01
浙江优创材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the existing review process of isooctyl p-dimethylaminobenzoate, some organic solvents need to be used, which has certain toxicity. For example, the patent with application number "CN201010209076.7" discloses a kind of The synthetic method of octyl ester (EHA), but the reaction solvent A that this patent uses can be benzene, toluene, xylene, chlorobenzene and dichlorobenzene, preferably xylene, and xylene just has certain toxicity

Method used

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  • Method for preparing 2-ethylhexyl 4-(dimethylamino)benzoate through hydrogenation by taking water as solvent
  • Method for preparing 2-ethylhexyl 4-(dimethylamino)benzoate through hydrogenation by taking water as solvent
  • Method for preparing 2-ethylhexyl 4-(dimethylamino)benzoate through hydrogenation by taking water as solvent

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Use water as solvent hydrogenation to prepare the method for isooctyl p-dimethylaminobenzoate, comprising the steps:

[0032] (1) water, isooctyl p-nitrobenzoate and active nickel catalyst are added in proportion to the reactor;

[0033] (2) Heating until hydrogen gas is introduced, heat preservation and pressure keeping and reaction until no hydrogen is absorbed (heating temperature is 85°C, and hydrogen pressure control is 0.5-0.7MPa);

[0034] (3) cooling, adding paraformaldehyde to the reactor, and then adding the catalyst of active nickel in proportion;

[0035] (4) Heating until hydrogen gas is introduced, heat preservation and pressure keeping, until no hydrogen is absorbed (the heating temperature is 85°C, and the hydrogen pressure control is 0.5-0.7MPa);

[0036] (5) Continue heat preservation and pressure holding for 4 hours, terminate the reaction, and take samples for analysis;

[0037] (6) After the catalyst is filtered, the catalyst is recycled, activate...

Embodiment 2-5

[0042] Embodiment 2-5 (following embodiment is used for researching the impact of catalyst usage times on product)

[0043] With the nickel catalyst of Example 1, through reactivation, the specific method of activation is: after adding a certain amount of recovered catalyst into the catalyst washing tank, add an appropriate amount of methanol, stir for 10 minutes at 50-55 ° C, keep the temperature for 20 minutes, put The supernatant is hydraulically fed into the washing liquid temporary storage tank. After washing with methanol for 5 times according to the above method, add an appropriate amount of deionized water, stir at 60-65°C for 10 minutes, let it stand for 20 minutes, pour the supernatant into the washing liquid temporary storage tank, and wash it with water three times according to the above method. After washing, operate according to the catalyst activation procedure. The following table shows the specific practical times and results:

[0044] Table 1 The impact of c...

Embodiment 6

[0046] Embodiment 6 (for researching the impact of one-time hydrogenation on product)

[0047] The preparation method of the nickel catalyst is the same as that of Comparative Document 1.

[0048] Use water as solvent hydrogenation to prepare the method for isooctyl p-dimethylaminobenzoate, comprising the steps:

[0049] (1) Water, isooctyl p-nitrobenzoate, paraformaldehyde and active nickel catalyst are added in proportion to the reactor;

[0050] (2) Heating until hydrogen gas is introduced, heat preservation and pressure keeping and reaction until no hydrogen is absorbed (heating temperature is 80-90°C, hydrogen pressure control is 0.5-0.7MPa);

[0051] (3) Continue to keep warm and pressurized for 4 hours, terminate the reaction, and take samples for analysis;

[0052] (4) After the catalyst is filtered, the catalyst is reclaimed, activated and reused, the stratification is allowed to stand, the water layer is discharged into the sewage system, and the oil layer enters t...

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Abstract

The invention relates to the field of fine chemical engineering, in particular to a method for preparing 2-ethylhexyl 4-(dimethylamino)benzoate through hydrogenation by taking water as a solvent. Themethod for preparing 2-ethylhexyl 4-(dimethylamino)benzoate through hydrogenation by taking water as a solvent is characterized by comprising the following steps: (1) adding water, 4-nitro-benzoic acid 2-ethyl-hexyl ester and an active nickel catalyst into a reactor in proportion; (2) performing heating, introducing hydrogen, and carrying out heat preservation and pressure maintaining reaction until no hydrogen is absorbed; (3) cooling, namely adding paraformaldehyde into the reactor, and supplementing the active nickel catalyst in proportion; (4) heating, introducing hydrogen, and carrying out heat preservation and pressure maintaining reaction until hydrogen is not absorbed; (5) continuing to preserve heat and pressure for several hours, terminating the reaction, and sampling and analyzing; (6) after the catalyst is filtered, recycling, activating and reusing the catalyst, standing for layering, discharging a water layer into a sewage system, and feeding an oil layer into a distillation tower; and (7) heating, rectifying and purifying by the distillation tower until the product specification is met, and barreling and packaging.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a method for preparing isooctyl p-dimethylaminobenzoate through hydrogenation using water as a solvent. Background technique [0002] P-dimethylaminobenzoate series compounds are a kind of high-efficiency amine accelerators, used together with free radical (II) type photoinitiators, mainly used for UV curing of varnish coating systems on paper, wood, metal and plastic surfaces , can also be used for the ultraviolet radiation polymerization reaction of single or multiple monomers, and is also a sensitizer with excellent performance. Initiation can effectively eliminate the interference of oxygen on photoinitiated polymerization. [0003] P-dimethylaminobenzoate series compounds can be used as excellent anti-ultraviolet additives and are widely used in water-resistant sunscreen cosmetics, including isoamyl p-dimethylaminobenzoate (IADB) and isooctyl p-dimethylaminobenzoate E...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C227/04C07C229/60
CPCB01J23/755C07C227/04C07C227/18C07C229/60Y02P20/584
Inventor 茅月成施根祥吴建龙
Owner 浙江优创材料科技股份有限公司
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