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Preparation method of phosphite antioxidant 168

A phosphite and antioxidant technology, applied in the field of antioxidant preparation, can solve the problems of long process operation time, environmental pollution, low batch output, etc., and achieves reduction of reaction solvent, shortened reaction time, and by-product generation amount. less effect

Inactive Publication Date: 2019-04-09
LIAONING DINGJIDE PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The disadvantages of the above-mentioned preparation process are mainly: due to the addition of reacting benzene and neutralizing benzene, the process operation time is long and the batch output is low, and, because the catalyst and anti-hydrolysis agent used are all amine compounds, there are many varieties, and the filtered Catalysts and anti-hydrolysis agents are mixtures of amine hydrochlorides, which can only be treated as waste residues, causing pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 1-liter four-neck flask equipped with a thermometer, electric stirring, reflux condenser and gas outlet, add 300 g of 2,4-di-tert-butylphenol and 2 g of di-n-butylamine, and put the Raise to a temperature of 55°C, under the surface of 2,4-di-tert-butylphenol, evenly add 57.2g of phosphorus trichloride dropwise, the dropping time is controlled at about 3.5h, and the reaction temperature gradually rises to 160°C during the dropping process ℃, keep this temperature until the evolution of HCl gas stops, time 4h. Add 2 g of anti-hydrolysis agent, stir for 0.5 h, and filter to remove the white crystals of di-n-butylamine hydrochloride formed by the catalyst and anti-hydrolysis agent. Then it is heated to about 195°C for more than 1 hour under negative pressure, and the excess 2,4-di-tert-butylphenol is removed by distillation under the pressure of 0.1kpa and the temperature in the bottle at 200°C to obtain tri(2,4-di-tert-butylphenol tert-butyl) phosphite antioxidant 16...

Embodiment 2

[0028] In a 1-liter four-neck flask equipped with a thermometer, electric stirring, reflux condenser and gas outlet, add 300 g of 2,4-di-tert-butylphenol and 2.5 g of di-n-butylamine, and put the bottle under nitrogen protection. Internally rise to a temperature of 85°C, under the surface of 2,4-di-tert-butylphenol, evenly add 55.6g of phosphorus trichloride dropwise, the dropping time is controlled at about 4h, and the reaction temperature gradually rises to 140°C during the dropping process °C, keep this temperature until the evolution of HCl gas stops, the time is 5h. Add 2.2 g of an anti-hydrolysis agent, stir for 0.5 h, and filter to remove the white crystals of di-n-butylamine hydrochloride formed by the catalyst and the anti-hydrolysis agent. Then heated to about 210°C under negative pressure and over 1h, and the excess 2,4-di-tert-butylphenol was distilled off under the pressure of 0.1kpa and the temperature in the bottle was 220°C to obtain tri(2,4- Di-tert-butyl) ph...

Embodiment 3

[0030] In a 1-liter four-neck flask equipped with a thermometer, electric stirring, reflux condenser and gas outlet, add 300 g of 2,4-di-tert-butylphenol and 1.8 g of di-n-butylamine, and put the bottle under nitrogen protection. Internally rise to a temperature of 90°C, under the surface of 2,4-di-tert-butylphenol, evenly add 52.7g of phosphorus trichloride dropwise, the dropping time is controlled at about 5h, and the reaction temperature gradually rises to 150°C during the dropping process ℃, keep this temperature until the evolution of HCl gas stops, time 4h. Add 1.85 g of an anti-hydrolysis agent, stir for 0.5 h, and filter to remove the white crystals of di-n-butylamine hydrochloride formed by the catalyst and the anti-hydrolysis agent. Then it is heated to about 200°C under negative pressure and over 1 hour, and the excess 2,4-di-tert-butylphenol is distilled off under the pressure of 0.1kpa and the temperature in the bottle is 200°C to obtain tri(2,4- Di-tert-butyl) p...

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Abstract

The invention discloses a preparation method of a phosphite antioxidant 168 and belongs to the technical field of antioxidant preparation. The preparation method is as follows: adding excessive 2,4-di-tert-butylphenol and a catalyst into a reaction kettle, adding phosphorus trichloride, and carrying out a synthetic reaction to generate tri(2,4-di-tert-butyl)phosphite; then, adding an anti-hydrolytic agent, then, carrying out filtration, and evaporating the excessive 2,4-di-tert-butylphenol in filtrate to obtain a crude product of tri(2,4-di-tert-butyl)phosphite; and then, crystallizing the crude product, and carrying out centrifuging, washing and drying to obtain a final finished product. By using the preparation method of the phosphite antioxidant 168, the consumption of raw materials isreduced, a reaction solvent is reduced, the reaction time is shortened, and the generation amount of byproducts is low; and a phosphite antioxidant 168 product prepared by using the preparation methodhas the characteristics of high purity (larger than or equal to 99%, low acid value (smaller than or equal to 0.3 mgKOH / g) and good hydrolysis resistance (PH is larger than or equal to 7).

Description

technical field [0001] The invention relates to the field of preparation of antioxidants, in particular to a preparation method of phosphite antioxidants. Background technique [0002] Antioxidant 168, chemical name tris(2,4-di-tert-butyl) phosphite, is a widely used phosphite solid auxiliary antioxidant, it does not mainly act according to the mechanism of free radical capture . Such compounds do not exhibit significant activity when they are used alone as stabilizers in resins. When it is combined with primary antioxidants such as phenolic antioxidants, it has a strong synergistic effect. In the application of polyolefins, phosphite antioxidant 168 has the dual functions of decomposing hydroperoxides and terminating free radical chains. Function, by decomposing the peroxide produced in the oxidation process to generate stable inactive products, thereby delaying the oxidation process of polymer materials and prolonging the service life of the product. Resistive phenol / ph...

Claims

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Application Information

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IPC IPC(8): C07F9/145
CPCC07F9/145
Inventor 玄永强吴春叶王爱民王恒赵金豹
Owner LIAONING DINGJIDE PETROCHEM
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