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Method for preparing N,N'-bis (4-ethoxycarbonylphenyl)-N'-benzylformamidine from waste residues for preparing UV-1

A technology of ethoxycarbonyl phenyl and UV-1 is applied in the field of preparing N,N'-bis(4-ethoxycarbonylphenyl)-N'-benzylformamidine, which can solve the problem of undisclosed recycling and use methods, etc.

Pending Publication Date: 2018-09-04
CHANGZHOU YONGHE FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this document does not disclose the specific recycling method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1）

[0028] First pump 272kg of triethyl orthoformate (1.84kmol) into the reaction kettle, then put in 45.4kg of ethyl p-aminobenzoate (0.275kmol), and raise the temperature to 90±2°C, at this time, distillate appears. Put the distillate into the receiving tank to recover ethanol, then raise the temperature of the material to 140±2°C, and keep it warm for 1 hour. After the reaction, distill under reduced pressure to recover triethyl orthoformate to obtain 57.5kg of NE and 4.3kg of NE respectively Waste residue (containing about 20wt% NE and 80wt% NET).

（ example 2）

[0030] First pump 272kg of triethyl orthoformate (1.84kmol) into the reaction kettle, then put in 45.4kg of ethyl p-aminobenzoate (0.275kmol), and raise the temperature to 90±2°C, at this time, distillate appears. Put the distillate into the receiving tank to recover ethanol, then raise the temperature of the material to 140±2°C, and keep it warm for 4 hours. After the reaction, distill under reduced pressure to recover triethyl orthoformate to obtain 59.6kg of NE and 1.6kg of NE respectively Waste residue (containing about 10wt% NE and 90wt% NET).

Embodiment 1）

[0032] The method for preparing N,N'-bis(4-ethoxycarbonylphenyl)-N'-benzylformamidine from the waste residue of UV-1 production in this example is a separation method, which has the following steps:

[0033] ① Add 1 kg of the NE waste residue obtained in Example 1 to 3 kg of toluene, stir for 2-3 hours, filter with suction, and dry to obtain 796 g of crude NET as a pale yellow solid with a purity of 98.2%.

[0034] ②Add 796g of NET crude product obtained in step ① into 2kg of DMF, then add 25g of activated carbon, heat up to 60-65°C, keep warm for 2h, filter with suction, rinse the filter cake with 150g of DMF, and combine the eluent and filtrate to obtain a DMF solution containing NET.

[0035] ③ Control the temperature of the DMF solution containing NET obtained in step ② at 40-45°C, add 480g of benzyl chloride and 610g of potassium carbonate, keep warm at 40-45°C for 24h after adding, suction filter, and filter the cake with 150g of DMF rinse.

[0036] Add the filtrate an...

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Abstract

The invention discloses a method for preparing N,N'-bis (4-ethoxycarbonylphenyl)-N'-benzylformamidine from waste residues for preparing UV-1. According to the method, after reaction treatment or separation treatment is carried out on the NE waste residues generated by production of N-(4-ethoxycarbonylphenyl)-N'-methyl-N'-benzylformamidine, the product and benzyl chloride are subjected to N-alkylation reaction, and N,N'-bis (4-ethoxycarbonylphenyl)-N'-benzylformamidine is obtained. The reaction treatment includes the steps that the NE waste residues are dissolved in a polar aprotic solvent, activated carbon treatment is carried out, then ethyl p-aminobenzoate is added for condensation reaction, and finally, the product and benzyl chloride are subjected to the N-alkylation reaction. The separation treatment includes the steps that the NE waste residues are dissolved in a methylbenzene solvent, after NE is separated, the product is dissolved in the polar aprotic solvent, and after activated carbon treatment, the product and benzyl chloride are subjected to N-alkylation reaction. By means of the reaction method, more NEPA can be obtained, and by means of the separation method, NEPA higher in purity can be obtained.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for preparing N,N'-bis(4-ethoxycarbonylphenyl)-N'-benzylformamidine from waste residue produced from UV-1. Background technique [0002] N,N'-bis(4-ethoxycarbonylphenyl)-N'-benzylformamidine [hereinafter referred to as NEPA] is an important ultraviolet absorber, which is used in many organic materials such as plastic products, resins Adding the UV absorber to the synthesis process of products, cosmetics, fuels, textiles, etc., can avoid the damage of the physical properties of the synthetic products caused by the photodegradation of ultraviolet rays (such as product discoloration, decolorization or fragility and cracking), and has a wide range of applications. market prospects. [0003] At present, the method of preparing NEPA is divided into two-step access method and one-step access method according to the difference of access to 4-ethoxycarbonylphe...

Claims

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Application Information

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IPC IPC(8): C07C257/12C07C257/06
CPCC07C257/12
Inventor 许晓春姜友林栾永勤陆海峰孙成和
Owner CHANGZHOU YONGHE FINE CHEM
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