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A kind of preparation method of hindered amine light stabilizer and intermediate

The technology of an intermediate and an alkali agent is applied in the preparation field of hindered amine light stabilizers, which can solve the problems of low product yield, product loss and the like, and achieve high product yield, convenient post-processing, and cheap and easy-to-obtain catalysts and solvents. Effect

Active Publication Date: 2020-07-10
ZHONGBEI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalysts mentioned in this invention must be acetic acid and boric acid, and they coexist in the reaction system, both of which are indispensable, resulting in many conditions. After the reaction, a large amount of water is used, which easily causes the loss of the product, resulting in a low product yield.

Method used

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  • A kind of preparation method of hindered amine light stabilizer and intermediate
  • A kind of preparation method of hindered amine light stabilizer and intermediate
  • A kind of preparation method of hindered amine light stabilizer and intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 31.2g of 2,2,6,6-tetramethylpiperidinamine, 9.4g of formamide, 2.03g of boric acid and 17.1g of acetic acid into a 250mL three-necked flask, and then add 100mL of xylene into it, under nitrogen Under protected conditions, the temperature was raised to 180°C and stirred for 1 h. Then the mixed solution was cooled to 100° C., at this temperature, 70 mL of aqueous sodium hydroxide solution was added for alkali washing, kept stirring for 2 h, then lowered to room temperature and filtered under reduced pressure, and the obtained solid was washed twice with water to obtain the intermediate product (I). The rate is 91.6%.

Embodiment 2

[0040] 31.2g of 2,2,6,6-tetramethylpiperidinamine, 9.4g of formamide, 0.2g of boric acid and 24.9g of formic acid were added to a 250mL three-necked flask, and then 90mL of xylene was added to it. Under the condition of protection, the temperature was raised to 130°C and stirred for 12h. Then the mixed solution was cooled to 80°C, 70mL of sodium hydroxide aqueous solution was added at this temperature, kept stirring for 1.5h, then lowered to room temperature and filtered under reduced pressure, and the obtained solid was washed 3 times with water to obtain the intermediate product (I). 92.3%.

Embodiment 3

[0042] According to Example 1, 31.2g 2,2,6,6-tetramethylpiperidinamine, 18.8g formamide, 2.5g boric acid and 25.2g propionic acid were added to a 250mL three-necked flask, and then 100mL of dimethicone was taken Chlorobenzene was added thereto, and under the condition of nitrogen protection, the temperature was raised to 180° C., and stirred for 10 h. Then the mixed solution was cooled to 120°C, 80mL of sodium hydroxide aqueous solution was added at this temperature, kept stirring for 1h, then lowered to room temperature and filtered under reduced pressure, and the obtained solid was washed 3 times with water to obtain the intermediate product (I), with a yield of 91.9 %.

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Abstract

A method for preparing a hindered amine light stabilizer N,N'-bis(2,2,6,6-tetramethyl-4-piperidyl)-N,N'-dialdehydo alkyl diamine comprises the steps of causing 4-formamido-2,2,6,6-tetramethyl-piperidine, dibromo alkane and a catalyst to be subjected to backflow stirring reaction for 1-24 h, instantly slowly adding water, cooling while stirring, performing washing, filtration and drying, and obtaining the product. A method for preparing an intermediate 4-formamido-2,2,6,6-tetramethyl-piperidine comprises the steps of causing 2,2,6,6-tetramethyl-piperidine, formamide, Lewis acid catalyst and an alkali-binding agent to undergo heating reaction for 1-24 h at normal pressure, performing cooling, alkaline wash, filtration, wash and drying. A synthesis process is simple and easy to operate, and aftertreatment is convenient; the required raw material, catalyst and solvent are easy to obtain, and the methods conform to the economy principle and is safe, environmentally friendly and high in product yield.

Description

technical field [0001] The invention relates to a preparation method of 4-formamido-2,2,6,6-tetramethylpiperidine, and further relates to a hindered amine light stabilizer N,N'-bis(2,2,6, The invention discloses a preparation method of 6-tetramethyl-4-piperidinyl)-N, N'-dialdehyde alkyldiamine, which belongs to the field of preparation of hindered amine light stabilizers. Background technique [0002] At present, in agricultural plastic films, military equipment, plexiglass, lighting materials, light-resistant coatings, industrial packaging materials and many other polymer products that are exposed to outdoors or light for a long time, light stabilizers are essential additive components. Mainly include light shielding agents (carbon black, zinc oxide and some inorganic pigments), ultraviolet absorbers (salicylates, benzophenones, benzotriazoles, etc.), quenchers (organic compounds of nickel) And free radical scavengers (hindered amine derivatives). In the past two decades,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/58C08K5/3435
CPCC07D211/58C08K5/3435
Inventor 武海花李迎春蔡智奇宫青海
Owner ZHONGBEI UNIV