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Synthesis method of light stabilizer HS-112

A technology of HS-112 and light stabilizer, which is applied in the direction of organic chemistry, can solve the problems of few research reports on synthetic methods, achieve good industrial application prospects, reduce side reactions, and simplify reaction steps

Inactive Publication Date: 2017-05-24
GANSU RES INSTION OF CHEM IND GRICI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The domestic market is completely dependent on imports, and there are few research reports on synthetic methods

Method used

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  • Synthesis method of light stabilizer HS-112

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 60g of UV-770 dry product, 300mL of 95% ethanol, 2.0g of catalyst magnesium hydroxide, add them to a three-necked flask, stir and heat to 75℃, add hydrogen peroxide (30%H 2 O 2 , 56g), keep the reaction for 10h, the color of the reaction liquid gradually changes from colorless to red. After the reaction is over, filter out the catalyst while it is hot, and add appropriate amount of MnO 2 Remove excess hydrogen peroxide and filter out MnO 2 . Distill under reduced pressure at 50°C. Stop the distillation when no liquid flows out. At this time, the product in the flask is a viscous red substance—bis(2,2,6,6-tetramethylpiperidinyl)sebacate nitroxide Free radicals.

[0024] Add n-octane to the bis(2,2,6,6-tetramethylpiperidinyl) sebacate nitroxide radical to dissolve by heating, add molybdenum trioxide, heat up to 125°C, and add dropwise under reflux Tert-butyl hydroperoxide (TBHP, 60g), heat preservation and reaction for 3h, the reaction liquid gradually changes from re...

Embodiment 2

[0026] Weigh 60 g of UV-770 dry product, 300 mL of 95% ethanol, 2.0 g of magnesium chloride hexahydrate as a catalyst, add them to a three-necked flask, stir and heat to 75°C, add hydrogen peroxide (30% H 2 O 2 , 56g), keep the reaction for 10h, the color of the reaction liquid gradually changes from colorless to red. After the reaction is over, filter out the catalyst while it is hot, and add appropriate amount of MnO 2 Remove hydrogen peroxide, filter out MnO 2 . Distill under reduced pressure at 50°C. Stop the distillation when no liquid flows out. At this time, the product in the flask is a viscous red substance-bis(2,2,6,6-tetramethylpiperidinyl)sebacate nitroxide Free radicals.

[0027] Add n-octane to the bis(2,2,6,6-tetramethylpiperidinyl) sebacate nitroxide radical to dissolve by heating, add the catalyst molybdenum trioxide, heat up to 125℃, and add dropwise under reflux Tert-butyl hydroperoxide (TBHP, 60g), heat preservation and reaction for 3h, the reaction liquid gr...

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Abstract

The invention discloses a synthesis method the a light stabilizer bis(1-octyoxy-2,2,6,6-tetramethyl-4-piperidyl) sebacate, belongs to the field of organic chemical synthesis. The bis(1-octyoxy-2,2,6,6-tetramethyl-4-piperidyl) sebacate is the material, ethanol solution is the solvent, and magnesium hydrate or magnesium chloride hexahydrate is the catalyst. Oxidation reaction is conducted with the action of aquae hydrogenii dioxidi which is used as the oxidant to generate bis(2,2,6,6-tetramethyl-1-piperidinyloxy-4-yl)sebacate free radicals. Then molybdenum trioxide is used as the catalyst, normal octane is used as the material and solvent to react with the bis(2,2,6,6-tetramethyl-1-piperidinyloxy-4-yl)sebacate free radicals to obtain the light stabilizer HS-112. The method uses two steps to synthesize the HS-112. The process is simple, the reaction time is short the side effects are few, the pollution is minimal, the production cost is low, the reaction yield rate is high, and therefore the industrial application prospect is good.

Description

Technical field [0001] The invention relates to a method for synthesizing a light stabilizer HS-112, which belongs to the field of organic chemistry synthesis. Background technique [0002] Bis(1-octyloxy-2,2,6,6-tetramethyl-4-piperidinyl) sebacate is a hindered amine light stabilizer, trade name: light stabilizer HS-112 . The molecular formula of bis(1-octyloxy-2,2,6,6-tetramethyl-4-piperidinyl) sebacate is: C 44 H 84 N 2 O 6 , The structural formula is as follows: [0003] [0004] Traditional hindered amine light stabilizers generally have high alkalinity, and high alkalinity limits the synergistic stabilizing effect of hindered amine light stabilizers in halogen-containing resins, acidic resins, and stable systems that may breed acidic substances. In the late 1980s, the research on the hypoalkalinity of hindered amines attracted widespread attention at home and abroad. HS-112 uses -OC8H17 to replace the hydrogen atom on the nitrogen of UV-770 (bis(2,2,6,6-tetramethyl-4-piper...

Claims

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Application Information

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IPC IPC(8): C07D211/94
CPCC07D211/94
Inventor 耿来红高玉清刘云利潘炳庆
Owner GANSU RES INSTION OF CHEM IND GRICI
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