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Preparation method of environment-friendly antioxidant triphosphite

A technology of triphosphite and antioxidant, which is applied in the field of preparation of triphosphite, and can solve the problems of recycling, regeneration and large pollution

Inactive Publication Date: 2015-03-04
MAOMING KEDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the disadvantages that the liquid alkaline catalyst for the synthesis of tris(2,4-di-tert-butylphenyl)phosphite is not easy to recycle and regenerate and cause great pollution, the invention provides an environment-friendly antioxidant tris(2,4-di-tert- The preparation method of butylphenyl) phosphite

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] a. Add 100 g of 2,4-di-tert-butylphenol, 350 g of toluene and 2.0 g of activated 717 strong basic anion resin into the reaction kettle; Add 25 g of phosphorus into the reactor; c, heat to 110° C., react for 1.5 h, stop nitrogen flow, and evaporate toluene under reduced pressure to obtain crystals; d, then add a small amount of isopropanol to filter and wash the crystals to obtain crude tri(2 , 4-di-tert-butylphenyl) phosphite; e, recrystallized with cyclohexane, filtered, washed and dried to obtain refined tris (2,4-di-tert-butylphenyl) phosphite. Wherein, step b and step d are all carried out under the situation of stirring. The obtained compound is a white crystalline powder product, and the calculated yield is 83%.

Embodiment 2

[0022] a. Add 100 g of 2,4-di-tert-butylphenol, 200 g of toluene and 6.0 g of activated 717 strong basic anion resin into the reaction kettle; Add 15g of phosphorus into the reaction kettle; c, heat to 110°C, react for 1.5h, stop nitrogen flow, and evaporate toluene under reduced pressure to obtain crystals; d, then add a small amount of isopropanol to filter and wash the crystals to obtain crude tri(2 , 4-di-tert-butylphenyl) phosphite; e, recrystallized with cyclohexane, filtered, washed and dried to obtain refined tris (2,4-di-tert-butylphenyl) phosphite. Wherein, step b and step d are all carried out under the situation of stirring. The obtained compound is a white crystalline powder product, and the calculated yield is 95%.

Embodiment 3

[0024] a. Add 100g of 2,4-di-tert-butylphenol, 200g of toluene and 10g of activated 717 strong basic anion resin into the reaction kettle; 20g was added to the reaction kettle; c, heated to 110°C, reacted for 1.5h, stopped nitrogen, and evaporated toluene under reduced pressure to obtain crystals; d, then added a small amount of isopropanol to filter and wash the crystals to obtain crude tri(2, 4-di-tert-butylphenyl)phosphite; e, recrystallized with cyclohexane, filtered, washed and dried to obtain refined tris(2,4-di-tert-butylphenyl)phosphite. Wherein, step b and step d are all carried out under the situation of stirring. The obtained compound is a white crystalline powder product, and the calculated yield is 89%.

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Abstract

The invention discloses a preparation method of an environment-friendly antioxidant triphosphite. The method comprises the following steps: a. adding 2,4-di-tert-butyl phenol, a solvent and a catalyst into a reaction kettle, wherein the mass ratio of the 2,4-di-tert-butyl phenol to the catalyst is 1:(0.02-0.4), and the solvent is 1.0-3.5 times by mass of the 2,4-di-tert-butyl phenol; b. in a nitrogen protective atmosphere, heating to 40-60 DEG C, and adding phosphorus trichloride into the reaction kettle, wherein the mass ratio of the phosphorus trichloride to the 2,4-di-tert-butyl phenol is (0.1-0.25):1; c. heating to 70-150 DEG C, reacting for 1-5 hours, stopping introducing nitrogen, and distilling off the solvent under reduced pressure to obtain a crystal; and d. adding a small amount of isopropanol, filtering, and washing the crystal to obtain crude tri(2,4-di-tert-butyl-phenyl)phosphite, wherein the catalyst is a strongly alkaline anion resin. Compared with the traditional preparation method, the preparation method disclosed by the invention uses the solid catalyst which is convenient for operation and recovery, thereby avoiding environment pollution.

Description

[0001] technical field [0002] The invention relates to a preparation method of triphosphite, in particular to a preparation method of environment-friendly antioxidant triphosphite. Background technique [0003] Phosphites are the main auxiliary antioxidants for polyolefin processing. Compared with other types of auxiliary antioxidants, phosphite antioxidants have little effect as polyolefin antioxidants alone, but they can be combined with various auxiliary antioxidants. Synergistic use of additives, especially phenolic antioxidants, can endow the polymer with excellent processing stability, heat resistance stability, color improvement and long-lasting weather resistance, and can adapt to the high temperature trend of plastic processing in the world today. [0004] At present, the synthesis of tris(2,4-di-tert-butylphenyl)phosphite adopts the method of esterification of 2,4-di-tert-butylphenol and phosphorus trichloride under the action of a catalyst. The catalysts for sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/145
CPCY02P20/584
Inventor 吴亚郡杨春洪陈小平陈东庆王世琴
Owner MAOMING KEDA CHEM
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