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Preparation method of bisbenzoxazinone ultraviolet absorber

A technology of benzoxazinone and ultraviolet rays, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems that do not meet safety production requirements, complicated operations, high production costs

Active Publication Date: 2021-11-09
JIANGSU KAITENG PHARMA RAW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process avoids the use of alkali and eliminates the residue of alkali metal ions from the source, hydrogen chloride gas is highly toxic, and high-temperature purging is not only complicated to operate, but also does not meet the safety production requirements
[0005] In a word, the existing bisbenzoxazinone ultraviolet absorbers all have defects such as high production cost, high residual alkali metal ions, and poor safety to varying degrees, which need to be improved urgently.

Method used

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  • Preparation method of bisbenzoxazinone ultraviolet absorber
  • Preparation method of bisbenzoxazinone ultraviolet absorber
  • Preparation method of bisbenzoxazinone ultraviolet absorber

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Add 166 g (1 mole) terephthalic acid, 302 g (2 moles) methyl anthranilate, 5 g (0.05 mole) trimethyl borate to a 5 liter flask equipped with mechanical stirring and reflux trap , 2 liters of toluene, started stirring, heated to reflux to separate water. After the water in the water separator no longer increases, recover 1 liter of toluene, cool down to room temperature, and obtain a suspension. Filtrate, recover the filtrate for mechanical use, wash the filter cake with toluene, wash with deionized water, and dry to obtain the intermediate of dimethyl bisamidobenzoate;

[0023] Add the dimethyl bisamide benzoate intermediate obtained in the previous step into a 3-liter flask equipped with mechanical stirring, add 2 liters of thionyl chloride, heat and reflux for 8 hours, then drop to room temperature, filter, and recover dichloromethane from the filtrate The sulfoxide, the filter cake was washed with deionized water until neutral, and dried in vacuum at 100° C. to obta...

Embodiment 2-13

[0027] The operation steps are the same as in Example 1, with 1 part of terephthalic acid 166 grams (1 mole) feeding basis, other feeding and results are listed in Table 1, when metal ions are not detected, the content is recorded as <5ppm.

[0028] Table 1

[0029]

[0030]

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Abstract

The invention discloses a preparation method of a bisbenzoxazinone ultraviolet absorber, which comprises: (1) reacting terephthalic acid and anthranilate as raw materials in the presence of a catalyst and an inert solvent to obtain a bisamide Methyl ester intermediate; (2) Heating the bisamide methyl ester intermediate in thionyl chloride to reflux and close the ring, namely. The preparation method of the present invention adopts boric acid ester as a catalyst, removes inorganic alkali reagents through dehydration amidation, and eliminates metal ion residues from the source, and analysis of metal ion residues shows that common metal ions such as sodium, potassium, iron, chromium and aluminum remain Both are below 50ppm, which significantly reduces the use of post-treatment water, eliminates by-product inorganic salts and salty wastewater, and reduces the generation and discharge of three wastes.

Description

technical field [0001] The invention relates to a preparation method of an ultraviolet absorber, in particular to a method for preparing a bisbenzoxazinone ultraviolet absorber with low metal residue, and belongs to the synthesis field of the bisbenzoxazinone field. Background technique [0002] Dibenzoxazinone UV absorber UV3638 is a kind of high-performance UV absorber with good heat resistance and little influence on the performance of polymer materials such as plastics. Its chemical structure is as follows: figure 1 shown. [0003] In 2002, Takemoto Oil Co., Ltd. disclosed (CN1420137) that UV3638 can be used as an ultraviolet absorber for the anti-ultraviolet protection of polymer materials such as plastics and the preparation method of UV3638. Use terephthaloyl chloride and anthranilic acid in inorganic bases, especially alkali metal salts, such as sodium carbonate, sodium hydroxide, etc. or organic bases, such as pyridine, alkyl ammonium hydroxide, etc. as acid-bindin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D265/22B01J31/14
CPCB01J31/146C07D265/22
Inventor 孙国平刘文煜张月宝李斌
Owner JIANGSU KAITENG PHARMA RAW MATERIALS CO LTD