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Environment-friendly preparation process of N-(4-ethoxy carbonyl phenyl)-N'-methyl-N'-phenyl formamidine

A kind of technology of ethoxycarbonyl phenyl, phenylformamidine

Active Publication Date: 2016-02-10
CHANGZHOU YONGHE FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the concentrated sulfuric acid used in the prior art is commercially available pure concentrated sulfuric acid, so that the cost is relatively high, and the concentrated sulfuric acid directly enters the acid-base neutralization process after the esterification reaction, which will not only produce a large amount of high-salt wastewater, but also cause environmental damage. Larger pollution, but also cause the hydrolysis of ethyl p-nitrobenzoate, resulting in a reduction in the yield of esterification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1）

[0027] This example is the ethanol recovery treatment method that collects in step 3. and step 4. of comparative example 1:

[0028] First, carry out rectification on the collected ethanol to obtain preliminary recovered ethanol with a purity of 96% to 97%; then add sodium hydroxide (the addition amount is about 1% of the weight of ethanol) to the preliminary recovered ethanol, heat to reflux, Insulate for 2 hours; finally start atmospheric distillation, collect fractions, stop heating when the internal temperature reaches 85°C, and obtain recycled ethanol with a purity ≥ 99.5%.

Embodiment 1）

[0030] The green preparation process of N-(4-ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine of the present embodiment is as follows:

[0031] 1. Put 80kg of recycled ethanol (1.74kmol) obtained according to the recycling method of Example 1 into the reactor, then drop into 50kg of p-nitrobenzoic acid (0.30kmol) and 10kg of commercially available concentrated sulfuric acid (0.10kmol) under stirring ), after the addition, the temperature was raised to 80±2°C with stirring, and the reaction was refluxed for 6h.

[0032] After the reaction is finished, ethanol is distilled out at normal pressure first, and when it is steamed to 95-98°C, the ethanol is distilled out under reduced pressure.

[0033] Move the upper catalyst layer (that is, the concentrated sulfuric acid layer) to the still, and distill under reduced pressure (vacuum degree <-0.09MPa). After steaming to 120-122°C, control the temperature to distill until anhydrous distills out to obtain Recycling concentrated s...

Embodiment 2）

[0043] All the other of this embodiment are identical with embodiment 1, and difference is: the concentrated sulfuric acid that adopts in the step 1. is the recovery treatment concentrated sulfuric acid that obtains according to the recovery treatment method in the step 1. of embodiment 1, and reaction result is shown in Table 1.

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Abstract

The invention discloses an environment-friendly preparation process of N-(4-ethoxy carbonyl phenyl)-N'-methyl-N'-phenyl formamidine. The process comprises the steps of firstly, making p-nitrobenzoic acid be subjected to an esterification reaction and catalytic hydrogenation, obtaining ethyl p-aminobenzoate, then making ethyl p-aminobenzoate be subjected to two steps of condensation reactions, and obtaining N-(4-ethoxy carbonyl phenyl)-N'-methyl-N'-phenyl formamidine, wherein ethanol adopted in the esterification reaction is recycled and processed ethanol, and the recycled and processed ethanol is obtained by collecting, recycling and processing ethanol generated in the condensation reactions. According to the process, the ethanol generated in the condensation reactions are recycled and processed and then applied to the esterification reaction, production cost is lowered, environmental pollution is reduced, the process is an environment-friendly preparation process, and in particular, compared with absolute ethyl alcohol on the market, the ethanol recycled and processed through the process hardly has influence on the esterification effect.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a green preparation process of N-(4-ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine. Background technique [0002] N-(4-ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine is a highly efficient anti-ultraviolet additive, which can efficiently absorb ultraviolet light in the 240-340nm band. N-(4-ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine has good compatibility with organic macromolecules, and has good light and heat stability, and is widely used in polyurethane, Adhesives, foams and other polymer materials. N-(4-ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine is liquid at room temperature, has good processability, and is compatible with ultraviolet light of benzophenone or benzotriazole Compared with absorbents, N-(4-ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine has better anti-ultraviolet performance, so it has a broad market prosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C257/12C07C229/60C07C227/04
Inventor 栾永勤陆海峰姜友林许晓春
Owner CHANGZHOU YONGHE FINE CHEM
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