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Preparation method of hindered amine light stabilizer

A hindered amine light stabilizer and solvent technology, which is applied in the field of preparation of hindered amine light stabilizers, can solve the problems of complex operation, high cost, and high price, and achieve the effects of simple operation, lower price, and low cost

Inactive Publication Date: 2013-09-25
启东金美化学有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The need of the present invention is to provide a preparation method of a hindered amine light stabilizer, which mainly solves the problems in the prior art that the price of using dicarboxylic acid ester as a raw material is relatively high, the reaction process is relatively mild, the operation is relatively complicated, and the cost is relatively high. Higher, lower yield and other technical issues

Method used

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  • Preparation method of hindered amine light stabilizer
  • Preparation method of hindered amine light stabilizer
  • Preparation method of hindered amine light stabilizer

Examples

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Effect test

Embodiment 1

[0026] Example 1: The preparation method of a hindered amine light stabilizer in this example, add 200ml of solvent naphtha to a 500ml flask, then add the raw materials sebacic acid (20.2g 0.1mol) and 2,2,6,6-tetra Methylpiperidinol (34.6g 0.22mol) and catalyst, warmed to reflux. After 10-15 hours, the reaction ends. The temperature is lowered to precipitate, and the separated solvent is reused. Washed with water and further refined to obtain pure bis(2,2,6,6-tetramethyl-4-piperidinyl) sebacate with a melting point of 81-83°C, with a yield of 80.5%

Embodiment 2

[0027] Example 2: The preparation method of a hindered amine light stabilizer of this example, add 200ml of the recovered solvent oil of Example 1 in a 500ml flask, and then add the raw materials sebacic acid (20.2g 0.1mol) and 2,2, 6,6-tetramethylpiperidinol (0.22mol) and catalyst, heated to reflux for reaction. After 10-15 hours, the reaction ends. The temperature is lowered to precipitate, and the separated solvent is reused. Wash with water, put the crude product into solvent oil and add activated carbon for decolorization and recrystallization to obtain bis(2,2,6,6-tetramethyl-4-piperidinyl) sebacate with a main content>98%, and the yield is 94.0 %.

Embodiment 3

[0028] Example 3: The preparation method of a hindered amine light stabilizer in this example, add 200ml of solvent naphtha to a 500ml flask, then add the raw material sebacic acid (20.2g 0.1mol) and 1, 2, 2, 6, 6 -Pentamethylpiperidinol (0.22mol) and catalyst, heated to reflux reaction. After 10-15 hours of reaction, the color is washed with water, and the solvent is distilled off for reuse. Bis(1,2,2,6,6-pentamethyl-4-piperidinyl) sebacate was obtained with a yield of 90.0%.

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Abstract

The invention relates to a light stabilizer, and especially relates to a preparation method of a hindered amine light stabilizer. The method is mainly used for solving the technical problems of high cost, non-mild reaction process, complicated operation, high cost, and low yield of prior art adopting dicarboxylate as a raw material. According to the invention, alkyl-substituted-4-hydroxyl piperidine and dicarboxylic acid are added into solvent oil; nitrogen is delivered for protection; heating and dissolving are carried out, and temperature maintaining is carried out; and a reflux reaction is carried out, wherein a molar ratio of alkyl-substituted-4-hydroxyl piperidine to dicarboxylic acid is 2.0:1 to 2.6:1; cooling precipitation is carried out after the reaction is completed; the solvent is separated, and water washing is carried out, such that a crude product is obtained. The crude product is added into fresh solvent oil, and active carbon is added for discoloring; and re-crystallization is carried out, such that a pure hindered amine light stabilizer is obtained.

Description

technical field [0001] The invention relates to a light stabilizer, in particular to a preparation method of a hindered amine light stabilizer. Background technique [0002] Due to its superior performance, hindered amine light stabilizers (HALS) have become the mainstream of the light stabilizer consumption market in synthetic material additives, and occupy a dominant position in the consumption structure of the light stabilizer market in the world. With the continuous deepening of basic research and applied research on light stabilizers, the application range of HALS is constantly expanding. At present, the application of HALS has covered many fields such as agricultural film, engineering plastics, fibers, polymer coatings, artificial carpets and various outdoor plastic products. [0003] People have known and can use various methods to prepare bis(substituted piperidine) esters. Among the existing synthetic methods reported in domestic and foreign literature, there are m...

Claims

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Application Information

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IPC IPC(8): C07D211/46
Inventor 潘永凯周兴旺
Owner 启东金美化学有限公司
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