Novel synthetic method of bis-benzoxazine ketone ultraviolet absorbent

Abstract

The invention provides a novel synthetic method of a bis-benzoxazine ketone ultraviolet absorbent, and belongs to the technical field of fine chemical engineering. The method comprises the following steps: A, stirring, anhydrides, used as raw materials, of o-aminobenzoic acid and (o-, m-, p-) phthaloyl dichloride or (o-, m-, p-)phthalic acid for a certain time in a non-polar solvent; B, adding chemical dehydrating agent or physical dehydrating agent in a reaction system without separating, slowly heating and refluxing for a certain time to obtain (o-, m-, p-)substituted bis-benzoxazine ketone ultraviolet absorbent; wherein the stirring time in the step A is not less than 1 hour, the refluxing time is 5-10 hours in the step B, the chemical dehydrating agent used in the step B is various dehydrating agents reacted with the water, including but not limited to alkaline calcium oxide, soda lime, acidic concentrated sulfuric acid, concentrated phosphoric acid, polyphosphoric acid, phosphorus pentoxide, thionyl chloride, acetic anhydride and the like, neutral molecular sieve, water-absorbent, anhydrous cupric sulfate and the like; the physical dehydrating agent comprises but not limited to non-protonic solvent such as benzene, methylbenzene, xylene and the like. The method provided by the invention has the advantages of being simple in operation flow, low in cost, simple in equipment, and suitable for the scale industrial production.

Description

Technical field: [0001] The invention belongs to the field of fine chemicals and relates to a synthesis method of bisbenzoxazinone ultraviolet absorbers. Background technique: [0002] UV absorbers are widely used and are important additives to prevent UV damage. There are many types of commonly used UV absorbers, but they can be roughly divided into two categories: inorganic compounds and organic compounds. Among them, inorganic compounds (such as kaolin, calcium carbonate, talc, some metal oxides, etc.) have strong reflective ability, are environmentally friendly, and have no obvious toxic effects, so they have been widely used in cosmetics, glass, construction and other fields. However, this type of compound has poor light transmittance, poor compatibility with organic materials, and is easy to agglomerate, so it is difficult to be applied in the ultraviolet protection application field of organic materials such as organic glass and polymer film. Organic compounds (such...

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Problems solved by technology

[0008] This method can obtain products, but the solvent consumption in the experiment is too large, and repeated operations of adding and removing solvents are required, the cost is high and the operation is complicated

It is also reported in the literature that isatoic anhydride is used as a raw material for one-step preparation, but the raw material price of isatoic anhydride is relatively high, and it needs to be purified and decolorized before use, the reaction yield is not high, and the cost is difficult to control

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