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 k

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
Comparison scheme
Effect test

Example Embodiment

[0030] Example 1

[0031] The method for preparing isooctyl p-dimethylaminobenzoate by hydrogenating water as a solvent includes the following steps:

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

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

[0034] (3) Cool down, add paraformaldehyde to the reactor, and then add active nickel catalyst in proportion;

[0035] (4) Heat to, pass in hydrogen, keep heat preservation and pressure reaction until no hydrogen is absorbed (heating temperature is 85°C, hydrogen pressure control is 0.5-0.7MPa);

[0036] (5) Continue to keep heat preservation and pressure for 4 hours, terminate the reaction, and sample and analyze;

[0037] (6) After filtering the catalyst, the catalyst is recovered and activated for reuse, standing for stratification, and the wat...

Example Embodiment

[0042] Example 2-5 (The following examples are used to study the effect of the number of times the catalyst is used on the product)

[0043] After reactivating the nickel catalyst of Example 1, the specific method of activation is as follows: after adding a certain amount of recovered catalyst to the catalyst washing pot, adding an appropriate amount of methanol, stirring at 50-55°C for 10 minutes, keeping the temperature at rest for 20 minutes, 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, and let stand for 20 minutes. The supernatant is hydraulically put into the washing liquid temporary storage tank and washed with water three times as described above. After washing, operate according to the catalyst activation procedure. The following table shows the specific practical times and results:

[0...

Example Embodiment

[0046] Example 6 (used to study the effect of one-time hydrogenation on the product)

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

[0048] The method for preparing isooctyl p-dimethylaminobenzoate by hydrogenating water as a solvent includes the following steps:

[0049] (1) Add water, isooctyl p-nitrobenzoate, paraformaldehyde and active nickel catalyst into the reactor in proportion;

[0050] (2) Heated to, pass in hydrogen gas, keep heat preservation and pressure reaction until no hydrogen is absorbed (heating temperature is 80~90℃, hydrogen pressure control is 0.5-0.7MPa);

[0051] (3) Continue to keep heat preservation and pressure for 4 hours, terminate the reaction, and sample and analyze;

[0052] (4) After filtering the catalyst, the catalyst is recovered and activated for reuse, standing for stratification, the water layer is discharged into the sewage system, and the oil layer is entered into the distillation tower;

[00...

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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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