- Preparation method of hindered amine light stabilizer 119
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The invention provides a preparation method of a hindered amine light stabilizer 119, and particularly relates to the field of chemical processes. The preparation method comprises the following steps: preparation of an intermediate (I): adding a reactant, namely cyanuric chloride and a reaction solvent, then adding N-n-butyl-N-2,2,6,6-tetramethyl piperidylamine, then adding alkali, continuing reacting for 12 hours, and splitting phases after the reaction is finished so as to finally obtain the intermediate (I); preparation of an intermediate II: adding a catalyst Pd/C, a reaction solvent, and reactants, namely paraformaldehyde and the intermediate I in a molar ratio of 1: (2.1-2.9), then introducing hydrogen with a pressure of 0.5-2 MPa, and performing reacting for 6-9 hours at a temperature of 40-90 DEG C so as to finally obtain the intermediate II; and preparation of a target product, namely a compond (III): firstly, adding a reaction solvent, reactants consisting of the intermediate II and N,N'-bis(3-aminopropyl)ethylenediamine in a molar ratio of (4.1-4.9): 1 and alkali into a reaction container, then replacing air in a reaction system with nitrogen, and carrying out a reflux reaction at 90-120 DEG C for 5-8 hours so as to obtain the target product, namely the compound (III) after the reaction is finished. The preparation method has the advantages of simplicity, high preparation efficiency, high yield, small pollution and the like.
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Paragraph 0036; 0047-0051; 0062-0066; 0077-0081; 0092-0095
(2021/08/28)
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- Hindered amine light stabilizer intermediate and preparation method of hindered amine light stabilizer
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The invention provides a hindered amine light stabilizer intermediate and a preparation method of a hindered amine light stabilizer. The hindered amine light stabilizer intermediate is 2-chloro-4,6-di(N-butyl-N-1,2,2,6,6-pentamethyl-4-piperidyl amino)-1,3,5-triazine, and the preparation method comprises the following steps: in the presence of hydrogen, carrying out hydrogenation substitution reaction on 1,2,2,6,6-pentamethyl-4-piperidone and n-butyl amine, carrying out substitution reaction on the obtained intermediate 1 and cyanuric chloride to obtain 2-chloro-4,6-di(N-butyl-N-1,2,2,6,6-pentamethyl-4-piperidyl amino)-1,3,5-triazine. Formaldehyde or formic acid does not need to be adopted in the preparation process, the method has the advantages of being small in environmental pollution and equipment corrosion, and after the method is used for reaction preparation of the hindered amine light stabilizer, the target product is high in purity, good in color and luster and short in meltingrange.
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Page/Page column 11-14
(2021/01/29)
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- Preparation method of hindered amine light stabilizer
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The invention relates to a preparation method of a hindered amine light stabilizer. The method comprises the following steps: reacting cyanuric chloride with N,N'-bis(3-aminopropyl)ethylenediamine toobtain an intermediate I; reacting the intermediate I with N-butyl-2,2,6,6-tetramethyl-4-piperidylamine to obtain an intermediate II; and adding paraformaldehyde or formaldehyde and formic acid, and carrying out a methylation reaction to obtain the target product. The method adopting the above new synthetic route has the advantages of avoiding of high-temperature or high-pressure reaction conditions in preparation, improvement of the density of hindered amine functional groups of the product, high purity, avoiding of the step of possibly generating hydrolysis byproducts, and great reduction ofthe industrial production cost of the product.
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Paragraph 0048-0056
(2020/04/06)
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- Method for preparing hindered amine light stabilizer 119 and derivatives of hindered amine light stabilizer 119
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The invention provides a method for preparing a hindered amine light stabilizer 119 and derivatives of the hindered amine light stabilizer 119. The preparation method comprises the steps: performing areaction on N-n-butyl-N-2,2,6,6-tetramethyl piperidyl amine and cyanuric chloride so as to obtain an intermediate I, performing a reaction on the intermediate I and N,N'-bis(3-aminopropyl)ethylenediamine under the catalysis action of alkaline and the protection action of N2 so as to obtain an intermediate II, then performing a N-alkylation reaction on the intermediate II and aldehyde under the catalysis action of Reney nickel in a hydrogen atmosphere, and synthesizing the hindered amine light stabilizer 119 or derivatives of the hindered amine light stabilizer 119, wherein xylene is preferably selected as a solvent, sodium hydroxide is preferably selected as alkaline, paraformaldehyde is preferably selected as the aldehyde, and the total yield of the obtained product hindered light stabilizer 119 reaches 93.5%. The Raney nickel is adopted as a catalyst, paraformaldehyde and other aldehyde compounds are adopted as reagents for alkylation with hydrogen, and the preparation method has the advantages of simple post-treatment, a recyclable catalyst, little corrosion to equipment and the like.
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Paragraph 0025; 0028-0029; 0032
(2019/11/21)
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