Preparation method of bis(2,4-dicumylphenyl)pentaerythritol diphosphite antioxidant

A technology of pentaerythritol diphosphite and cumyl phenyl, which is applied in the field of preparation of phosphite antioxidants, can solve problems such as unsatisfactory yield levels, and achieves simple and easy operability, high selectivity, low The effect of raw material consumption

Active Publication Date: 2017-04-26
RIANLON +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the synthetic preparation methods of published synthetic patents and literatures, the yield of the obtained product is not higher than 85%, which is not ideal

Method used

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  • Preparation method of bis(2,4-dicumylphenyl)pentaerythritol diphosphite antioxidant
  • Preparation method of bis(2,4-dicumylphenyl)pentaerythritol diphosphite antioxidant

Examples

Experimental program
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Embodiment 1

[0022] 1) Add 41.0 grams of pentaerythritol, 2.05 grams of N, N-dimethylhexadecylamine, and 190 grams of xylene into a four-neck flask equipped with a stirrer, a thermometer, a condenser, and a nitrogen conduit in a 1000 ml bottle, and feed nitrogen to install hydrogen chloride Absorption device, dropping funnel; add 94.9 grams of phosphorus trichloride weighed dropwise at 10-15 ° C, dropwise in 1.5 hours, and slowly heat up to 25-30 ° C within 2-3 hours, the hydrogen chloride gas generated through the absorption The device absorbs treatment; after 2-3 hours, the temperature is raised to 38-40°C, and after 2-3 hours, the temperature is raised to 80-85°C and kept for 0.5 hours, and the nitrogen gas is stopped, and the vacuum gauge pressure is - (0.05-0.06MPa) Reaction under reduced pressure and reflux for 1 hour, remove hydrogen chloride and excess phosphorus trichloride, stop decompression at 70-80°C and fill with nitrogen for protection, to obtain dichloropentaerythritol dipho...

Embodiment 2

[0026] 1) Add 41.0 grams of pentaerythritol, 1.7 grams of N,N-dimethylhexadecylamine, 165 grams of toluene, and feed nitrogen into a four-neck flask equipped with a stirrer, thermometer, condenser, and nitrogen conduit in a 1000ml device, and the device absorbs hydrogen chloride Device, dropping funnel; add 96.0 grams of phosphorous trichloride weighed dropwise at 10-15°C, drop it in 1 hour, then slowly heat up to 20-25°C in 2 hours, and the hydrogen chloride gas generated is absorbed and treated by the absorption device; After another 3 hours, the temperature was raised to 30-35 ° C, and after 2 hours, the temperature was raised to 80-82 ° C, and the temperature was kept for 0.5 hours, and the nitrogen gas was stopped, and the vacuum gauge pressure was - (0.06-0.07 MPa) under reduced pressure and reflux for 1 hour. Remove hydrogen chloride and excess phosphorus trichloride, stop decompression at 70-80°C and fill with nitrogen for protection, to obtain dichloropentaerythritol d...

Embodiment 3

[0029]1) Add 41.0 grams of pentaerythritol, 1.8 grams of N,N-dimethyltetradecamine, 123 grams of xylene, and feed nitrogen into a four-neck flask equipped with a stirrer, a thermometer, a condenser, and a nitrogen conduit in 1000 ml, and install hydrogen chloride Absorption device, dropping funnel; dropwise add 92.9 grams of phosphorus trichloride weighed at 10-15 °C, dropwise addition is completed in 1.5 hours, and slowly heat up to 25-30 °C in 3 hours, and the hydrogen chloride gas generated is absorbed and treated by the absorption device ; After 2.0 hours, the temperature was raised to 35-40°C, and after 3 hours, the temperature was raised to 80-85°C, and kept for 0.5 hours, and the nitrogen gas was stopped, and the vacuum gauge pressure was - (0.06-0.07MPa) decompression and reflux reaction for 1 hour , remove hydrogen chloride and excess phosphorus trichloride, stop depressurization at 70-80°C and fill with nitrogen for protection, to obtain dichloropentaerythritol diphos...

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Abstract

The invention relates to a preparation method of a bis(2,4-dicumylphenyl)pentaerythritol diphosphite antioxidant. The preparation method comprises the steps of dropwise adding phosphorus trichloride at a nitrogen environment in an existing system of pentaerythritol, a catalyst and a solvent so as to obtain dichlone pentaerythritol diphosphite reaction liquid, adding 2,4-dicumylphenol, heating to 130-140 DEG C in the presence of nitrogen to react, carrying out reduced pressure backflow reaction to obtain a reactant, adding organic amine to neutralize and regulate the reactant to be alkaline, continuing to carry out esterification reaction until reaction mediums are still alkaline, cooling, and filtering, so as to obtain bis(2,4-dicumylphenyl)pentaerythritol diphosphite. By controlling the reaction process, high-selectivity and high-yield bis(2,4-dicumylphenyl)pentaerythritol diphosphite with a spiral structure is obtained, the yield of the product is higher than 92%, the recovery rates of generated side effects and an unreacted raw material, namely 2,4-dicumylphenol are higher than 90%, the consumption of the raw materials is reduced, and the simple and feasible operability is realized.

Description

technical field [0001] The invention relates to a preparation method of bis(2,4-dicumylphenyl)pentaerythritol diphosphite antioxidant, which belongs to the preparation technology of phosphite antioxidant. Background technique [0002] Bis(2,4-dicumylphenyl)pentaerythritol diphosphite is used as an antioxidant. Compared with other commonly used phosphite antioxidants, it has excellent high temperature stability and low volatility at high temperatures. Excellent resistance to hydrolysis, stability in air and within the polymer, excellent protection against yellowing and high temperature degradation during processing. [0003] The preparation method of two (2,4-dicumylphenyl) pentaerythritol diphosphite has the following several modes: (1) first generates dichloropentaerythritol diphosphite by pentaerythritol and phosphorus trichloride reaction, then adds 2 , 4-dicumylphenol continues the esterification reaction to obtain the product; (2) 2,4-dicumylphenol reacts with phosphor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/65746
Inventor 李克国孙春光汤翠祥范小鹏
Owner RIANLON
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