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A method of reclaiming 4-hydroxybenzophenone laurate

A technology of hydroxybenzophenone and laurate, applied in the separation/purification of carboxylate, preparation of carboxylate, chemical instruments and methods, etc., can solve problems such as process influence, achieve high recovery efficiency and good color Effect

Active Publication Date: 2019-02-01
SICHUAN LUTIANHUA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, affected by the process, this will cause another problem, that is, more 4-HPL (39% ~ 75.6%, wt) will be included in the hydrochloride filter cake, so it is necessary to check the hydrochloride filter cake 4-HPL product in filter cake for recovery

Method used

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  • A method of reclaiming 4-hydroxybenzophenone laurate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 145.71g of triethylamine hydrochloride filter cake (the mass content of hydrochloride is 28.9%), add 252.66g of desalted water, heat and stir at 60-65°C, filter to remove impurities after completely melting, let stand, the water phase and the organic phase The layers were separated quickly, the organic phase was at the bottom, and 110.34g of the organic phase was discharged from the bottom, and 7.26g of the organic phase was dehydrated by distillation to obtain 103.08g of 4-HPL recovered product (the mass content of hydrochloride was 1.2%). The remaining aqueous phase was cooled to 40°C and filtered to obtain 2.30g White solidified lumps, this part is not counted for reuse, and the aqueous phase was concentrated by distillation at 110°C to obtain 41.63g of triethylamine hydrochloride (purity 98.3%), and the distillation condensate was recycled. The reaction results are shown in Table 1.

[0028] Table 1 Recovery data in case of large 4-HPL mass content (71.1%) in t...

Embodiment 2

[0033] Take 200.03g of triethylamine hydrochloride filter cake (the mass content of hydrochloride is 59.8%), add 717.83g of desalted water, heat and stir at 60-65°C, filter and remove impurities after completely melting, let it stand, the water phase and the organic phase The layers were separated rapidly, the organic phase was at the bottom, and 85.19 g of the organic phase was discharged from the bottom, and 5.72 g of the organic phase was dehydrated by distillation to obtain 79.47 g of 4-HPL recovered product (hydrochloride salt mass content 1.3%), and the remaining aqueous phase was cooled to 40 ° C and filtered to obtain 2.43 g White solidified lumps, this part is not counted for reuse, and the aqueous phase is concentrated by distillation at 110°C to obtain 119.00 g of triethylamine hydrochloride (purity 98.6%), and the distillation condensate is recycled. The reaction results are shown in Table 2.

[0034] Table 2 The recovery data in the case of small 4-HPL mass conten...

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Abstract

The invention discloses a method for recovering 4-HPL (4-benzoylphenyl laureate). The method comprises steps as follows: 1) hydrochloride filter cakes and desalted water are placed in a reaction kettle, heated and stirred to be dissolved, and a solution is obtained; 2) the solution is filtered for impurity removal, and filtrate A is obtained; 3) the filtrate is left to stand for layering, and a lower-layer substance is discharged after the filtrate is divided into upper and lower layers; 4) the discharged lower-layer substance is subjected to distillation dehydration, and a 4-HPL recovered product is obtained; 5) an upper-layer substance is cooled and filtered, residual product coagula are filtered out, and filtrate B is obtained; 6) the filtrate B is subjected to distillation concentration at 110 DEG C, and a hydrochloride product is obtained. 4-HPL with the purity higher than 98.0% and a triethylamine hydrochloride product can be directly obtained, the recovery efficiency is high (the recovery rate of 4-HPL is higher than 97.6% and the recovery rate of triethylamine hydrochloride is higher than 97.0%), and the color of recovered products is good.

Description

technical field [0001] The invention relates to a method for recovering 4-hydroxybenzophenone laurate, in particular to a method for recovering 4-hydroxybenzophenone laurate from a hydrochloride filter cake. Background technique [0002] 4-Benzoylphenyl laureate (4-HPL for short) is a widely used UV photoinitiator. Its synthesis reaction equation is as follows: [0003] [0004] Remaining HCl in the system will cause the reaction to be incomplete. In order to eliminate HCl, the patent CN91111465.3 uses an excessive amount of anhydrous pyridine, which is used as a solvent to dissolve the raw material of 4-hydroxybenzophenone, so as to facilitate the reaction with the dripping lauroyl chloride. At the same time, it is also used as an absorbent, and pyridine reacts with HCl to generate pyridine hydrochloride, so that the acylation reaction can be carried out thoroughly. However, due to the use of excessive organic solvents, subsequent separation and treatment are cumbersome...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/48C07C67/54C07C69/24C07C209/86C07C211/05
CPCC07C67/48C07C67/54C07C209/86C07C69/24C07C211/05
Inventor 李勇傅挺进涂勇戴志谦蒋弟勇罗光碧
Owner SICHUAN LUTIANHUA