Patent application CN10525317A discloses a preparation process of octyltriazinone and its tautomer, which adopts a mixed solution of methanol or ethanol and water for solidification; the method can obtain solidified agglomerated products, and the operation is simple, The yield is high, but the crystals cannot be formed;
Patent Application No. 639134 discloses a tautomeric form of 2,4,6-triphenylamino-p-((carbonyl-2-ethylhexyl-1-oxy)-1,3,5-triazine ( 1) preparation method, this method focuses on the solvent that recrystallization uses; Take isooctyl p-aminobenzoate and cyanuric chloride as starting materials,
Patent application CN10525317A discloses a preparation process of octyltriazinone and its tautomer, which adopts a mixed solution of methanol or ethanol and water for solidification; the method can obtain solidified agglomerated products, and the operation is simple, The yield is high, but the crystals cannot be formed;
Patent Application No. 639134 discloses a tautomeric form of 2,4,6-triphenylamino-p-((carbonyl-2-Ethylhexyl Triazinone-1-oxy)-1,3,5-triazine ( 1) preparation method, this method focuses on the solvent that recrystallization uses; Take isooctyl p-aminobenzoate and cyanuric chloride as starting materials,respond in xylene solvent to obtain 2,4,6-triphenylamine tautomeric blend of base-p-( carbonyl-2/- ethylhexyl-1/- oxy) -1,3,5- triazine; then in one or more solvents picked from the team containing Formation in the existence of: aliphatic alcohols having 2-8 carbon atoms, aliphatic carboxylic acid alkyl esters having an overall of 3-10 carbon atoms, aromatic carboxylic acid alkyl esters having a total amount of 8-12 carbon atoms, aliphatic carbonates having an overall of 3-9 carbon atoms, nitriles having a total of 2-8 carbon atoms, dialkyl ketones having a total of 3-6 carbon atoms, and Aliphatic sulfones, wherein the solvent or combination might furthermore contain approximately 30% by weight of hydrocarbons; this method can achieve a crystalline product, however the formation procedure is complicated, lengthy, and product yields are reduced; Above two technical options, all do not connect to the preparation method of target item octyl triazinone, and the technique of its formation (solidification) has issues. SUMMARY OF THE DEVELOPMENT
The function of this creation is to aim at above issue, supply the artificial technique of ultraviolet absorber Ethylhexyl Triazinone (hereinafter referred to as: UVT-150), its resources is easy to obtain, mild response problems, three wastes are couple of, and also product pureness is high. In order to fix the above-mentioned technical troubles, the technological plan adopted in the present innovation is: an artificial method of ultraviolet absorber ethylhexyl triazinone, which takes melamine, p-chlorobenzoic acid and isooctyl alcohol as beginning resources, as well as passes through two actions. Synthesis, one-step formation to obtain the target product, It is additionally called 2,4,6-tri-anilino-( p-carbonyl-2-ethylhexyl-1-oxygen) -1,3,5- triazine, 4,4′,4″-( 1, 3,5-triazine-2,4,6- triimino) Ethylhexyl Triazinone tris( 2-ethylhexyl) ester, or UV absorber UVT-150. The synthesis consists of the complying with actions:
Action 1) Synthesis of H3TATAB
The specific action in action 1) are: very first add a solvent, a catalyst, 7K, and also melamine, mix, and also dropwise right into the p-chlorobenzoic acid liquified in the exact same solvent at area temperature level; Complete the insulation reaction 4-6h; then add water for dilution, after cooling down, suction filtration, cleaning with water to nonpartisanship, draining pipes, drying out to get white strong HJATAB. Wherein, add water to dilute after the product response as well as be cooled to suction filtration after 5 ~ 10 ℃, due to the fact that the solubility of the response product in the solvent is huge, by adding water, the solubility is lowered, and also the item is separated out. Even more, the solvent symphonious 1) is a dialkyl ketone having 3-6 carbon atoms; for example: acetone, butanone, 2-pentanone, 3-pentanone, 2-hexanone, cyclohexanone or 1, 4-dioxane. This sort of solvent is needed to have solid solubility, which can much better liquify the reaction raw materials as well as the created products, and can alter the solubility by including water to separate out the produced products, as well as can also recognize the recuperation and reuse of the solvent. Better, action 1) water consumption in the response system is: 3 ～ 5 times of melamine weight; The molar intake ratio of melamine and p-chlorobenzoic acid is 1:3.1 ～ 3.3, 3 The mol proportion of polycyanamide and catalyst is 1:1.6 ～ 2. According to the theoretical proportioning quantity of material response, embrace the proportioning that p-chlorobenzoic acid is somewhat excessive, and also the usage of driver is reasonably adjusted via the examination result, and the optimum proportioning amount is figured out. The enhancement of a standard driver can efficiently promote the formation of the reaction.
