Method for preparing hindered phenolic antioxidant by using composite catalyst

A composite catalyst, technology of hindered phenols, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve elimination, human and environmental hazards, and low reaction rate. and other problems to achieve the effect of reducing the reaction time, ensuring product quality and high product quality

Active Publication Date: 2019-03-29
LIAONING DINGJIDE PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this type of catalyst is not suitable for the reaction with polyols, such as the reaction of methyl β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate with pentaerythritol to generate tetrakis[β-(3, 5-Di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester (Antioxidant 1010) reacts poorly
U.S. Patent No. 4,594,444 proposes the use of tin-containing compounds, such as dibutyltin oxide catalysts, for the transesterification of sterically hindered hydroxyphenyl carboxylic acid esters and higher aliphatic alcohols. The resulting products have high yield, high purity, and good appearance and color. However, the antioxidants produced by tin-containing catalysts will cause harm to human body and the environment when used in polyol

Method used

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  • Method for preparing hindered phenolic antioxidant by using composite catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) In a reactor equipped with a stirrer, condenser, vacuum gauge, and thermometer, put 145kg (1.07kmol) of pentaerythritol, 1620kg (5.54kmol, excess 30mol%) of 35 methyl ester melted at 80°C, and evenly After mixing, add 0.49kg (0.021kmol) of lithium amide and 0.35kg (0.0053kmol) of lithium acetate under nitrogen protection; when the mixture is heated to 130-135°C at 10,000pa, the internal pressure of the reaction begins to change, about 11,000pa, It shows that the materials in the kettle start to react, and when the temperature in the kettle reaches 140°C, a large number of bubbles are generated on the surface of the kettle, and the pressure of the kettle also changes to about 13000-15000pa, indicating that the reaction in the kettle is violent, and the temperature of the kettle must be controlled at about 140℃, otherwise it will A large amount of reactant is taken out of the kettle by the by-product methanol. When the kettle temperature reaches 140°C, keep it at this...

Embodiment 2

[0038] Reaction process is with embodiment 1, and the pentaerythritol of 145kg (1.07kmol) is loaded into reactor, the 35 methyl esters of 1995kg (6.82kmol, excessive 60mol%), the amide lithium of 0.61kg (0.027kmol) and 0.35kg (0.0053kmol) lithium acetate. After the distillation of 3,5-methyl ester, about 4-6 hours later, the degree of vacuum is about 100 Pa, the temperature is 195-200°C, and the value of distilled methyl ester is 732kg.

[0039] Yield: 1204kg (96.0% of theoretical amount) of crystal 1010, melting point 118°C-119°C. Product light transmittance: 425nm: 98.2%, 500nm: 99.4%.

Embodiment 3

[0041] Reaction process and other materials add-on are the same as embodiment 1, just, 35 methyl esters 1370kg (4.69kmol, excessive 10mol%). After the distillation of 3,5-methyl ester, about 2-3 hours later, the degree of vacuum is about 100 Pa, the temperature is 195-200°C, and the value of distilled methyl ester is 116kg.

[0042] Yield: 1141kg (91.0% of theoretical amount) of crystal 1010, melting point 116°C-118°C. Product light transmittance: 425nm: 97.7%, 500nm: 99.1%.

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Abstract

The invention discloses a method for preparing a hindered phenolic antioxidant by using a composite catalyst, belonging to the field of preparation of antioxidants. The method comprises the followingsteps: evenly mixing 3-(3, 5-di-tert-butyl-4-hydroxyphenyl) methyl propionate with pentaerythritol, and then adding the lithium amide/lithium acetate composite catalyst for catalyzing, distilling, crystallizing, filtering and drying to obtain the hindered phenolic antioxidant 1010. The hindered phenolic antioxidant prepared by the method effectively avoids the influence, caused by adopting an organotin catalyst, on a human body and the environment; compared with single use of lithium amide or lithium acetate as a catalyst, the method is rapider in reaction speed, and guarantees the color of reaction liquid, thus guaranteeing the product quality.

Description

technical field [0001] The invention relates to the field of preparation of antioxidants, in particular to a method for preparing hindered phenolic antioxidants with a composite catalyst. Background technique [0002] Hydroxy-phenylpropionate undergoes transesterification reaction with aliphatic alcohols in the presence of a catalyst. After the by-product alcohol is removed during the reaction, the resulting reaction solution is purified to obtain a product that is a sterically hindered phenolic antioxidant. , which is effective in preventing oxidation and thermal degradation of various organic materials. Steric hindered phenolic antioxidants are usually used in combination with phosphite auxiliary antioxidants or ultraviolet absorbers, which have a good synergistic effect. [0003] Basic catalysts are usually used to prepare hindered phenolic antioxidants, such as β-(3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate in sodium tert-butoxide, potassium tert-butoxide, In ...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C69/732B01J31/26
CPCB01J31/26C07C67/03C07C69/732
Inventor 玄永强吴春叶王爱民王恒赵金豹
Owner LIAONING DINGJIDE PETROCHEM
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