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Method for removing metal residues in dibenzoxazinone ultraviolet light absorber

A technology of bisbenzoxazinone and benzoxazinone, which is applied in the field of removing metal residues in bisbenzoxazinone ultraviolet absorbers, can solve the problems of not being able to use inorganic alkalis and increasing production costs

Active Publication Date: 2021-05-04
JIANGSU KAITENG PHARMA RAW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to obtain UV3638 products with low metal residues, not only should inorganic bases not be used in the production process, but also metal equipment should be avoided, raw materials and solvents also need to be specially purified, and the production cost is significantly increased

Method used

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  • Method for removing metal residues in dibenzoxazinone ultraviolet light absorber
  • Method for removing metal residues in dibenzoxazinone ultraviolet light absorber
  • Method for removing metal residues in dibenzoxazinone ultraviolet light absorber

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Removal of metal residues in embodiment 1 bisbenzoxazinone ultraviolet absorber

[0019] Take 100 grams of ordinary quality UV3638 product, the metal residue analysis shows that the sodium content is 760ppm, iron is 35ppm, (chromium, nickel and aluminum are less than 1ppm, recorded as undetected), added to the deionized water, washed clean, dried and filled with Mechanical stirring (tetrafluoro stir bar), reflux condenser and thermometer in a 3-liter four-necked flask. Then, 500 g of o-dichlorobenzene, 100 g of acetic anhydride and 10 g of acetic acid were added in sequence. Start stirring, heat to reflux (internal temperature 150°C), and part of the solid dissolves. After stirring for 2 hours, the heating was stopped and cooled to room temperature. Filtration, the filter cake was slurried with methanol, filtered again, the filter cake was rinsed with methanol, dried by suction and dried at 100° C. to obtain 98.7 g of UV3638 product. Metal analysis showed sodium 13pp...

Embodiment 2

[0021] Removal of metal residue in embodiment 2 bisbenzoxazinone ultraviolet absorber

[0022] The operation is the same as in Example 1, but the amount of o-dichlorobenzene, acetic anhydride and acetic acid is doubled, and only one extraction is performed, namely 100 grams of UV3638 products of ordinary quality, 1000 grams of o-dichlorobenzene, 200 grams of acetic anhydride and 20 grams of acetic acid . 98.1 g of purified UV3638 product were obtained. Metal analysis showed that both sodium and iron were less than 5 ppm and were recorded as not detected.

Embodiment 3-16

[0023] Removal of metal residues in embodiment 3-16 bisbenzoxazinone ultraviolet absorber

[0024] The operation steps are the same as in Example 1, and the consumption of each raw material is the same as in Example 2, that is, the above-mentioned 100 grams of UV3638 products of ordinary quality are used as the charging benchmark, 1000 grams of aromatic hydrocarbon solvent, the type, consumption and sodium and iron residual analysis of auxiliary solvent and carboxylic acid. The results are listed in Table 1, and when it is less than 5ppm, it is recorded as not detected. Since nickel, chromium and aluminum metal residues were not detected in UV3638 ordinary products, they were not detected again.

[0025] The removal result of metal residues in table 1 embodiment 4-17 bisbenzoxazinone ultraviolet absorber

[0026]

[0027]

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PUM

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Abstract

The invention discloses a method for removing metal residues in a dibenzoxazinone ultraviolet light absorber. The method comprises the following step: separating the metal residues in the dibenzoxazinone ultraviolet light absorber from the dibenzoxazinone ultraviolet light absorber by adopting a thermal extraction method by taking a high-boiling-point aromatic hydrocarbon solvent and a polar auxiliary solvent as a mixed extraction solvent. A mixed extraction system composed of two solvents is adopted, one solvent is a high-boiling-point aromatic hydrocarbon solvent, and the other solvent is a polar coordination auxiliary solvent with a complexing effect on metal ions. The residual value of the metals such as sodium, iron and the like in the dibenzoxazinone ultraviolet light absorber produced by using the existing process can be reduced from the common product with the residual value of hundreds of ppm to the high-quality product with the residual value of less than 5 ppm, and the cost is not significantly increased. And when a small amount of carboxylic acid is added during mixed extraction, the removal efficiency is higher. In addition, the extraction solvent in the method can be recycled through distillation, and emission of three wastes is not increased.

Description

technical field [0001] The invention relates to a method for removing metal residues in ultraviolet absorbers, in particular to a method for removing metal residues in bisbenzoxazinone ultraviolet absorbers, and belongs to the field of removing metal residues in bisbenzoxazinone ultraviolet absorbers. Background technique [0002] Dibenzoxazinone UV absorber (UV3638) is a kind of UV absorber with excellent performance. Industrially, the current mature production process of UV3638 is to react with terephthaloyl chloride and anthranilic acid under the condition of inorganic bases, such as sodium carbonate, sodium hydroxide, etc. as acid binding agents, to form bisamides, and then use acetic anhydride to bind them. The ring gets ( figure 1 ). [0003] In general, the production process of UV3638 is not complicated, but due to the poor solubility of bisamide intermediates and products UV3638 in almost all common organic solvents, the inorganic bases used in the current product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D265/22
CPCC07D265/22
Inventor 潘守浩陈新宜肖淑华刘中华
Owner JIANGSU KAITENG PHARMA RAW MATERIALS CO LTD