Preparation method of antioxidant product with stable performance

A technology of stable performance and antioxidant, applied in the field of preparation of antioxidant products with stable performance, can solve the quality and stability defects of antioxidant 168 products, unable to obtain high-purity antioxidant 168 products, and the occurrence of 168 products. Hydrolysis reaction and other problems, to achieve the effect of long-term anti-hydrolysis performance, good anti-oxidation performance, and easy industrial production

Active Publication Date: 2010-08-11
溧阳常大技术转移中心有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chlorine atoms in phosphorus trichloride are all replaced by hydroxyl groups, and will be converted into phosphorous acid, which cannot continue to undergo esterification reaction with 2,4 phenol; if part of the chlorine atoms are replaced by hydroxyl groups, the intermediate product will continue to undergo esterification with 2,4 phenol reaction, the result will undoubtedly generate irreversible by-products of phosphite monoester dihydroxylate and phosphite diester monohydroxylate, which will be mixed into the product, making it impossible to obtain high-purity antioxidant 168 products
[0014] One of the disadvantages of the above method is that in the process of preparing the antioxidant 168 product, substances such as 2,4-di-tert-butylphenol and organic solvents are added or other natural conditions bring a small amount of water into the reactor, which is not removed in the process. Trace Water Measures
[0015] The second disadvantage of the above method is that in the process of preparing the antioxidant 168 product, there is no measure to remove a certain amount of impurities such as HCl and organic amine catalyst hydrochloride wrapped in the crystallized product, which leads to the hydrolysis reaction of the 168 product
The fatal weakness of antioxidant 168 is the hydrolysis reaction. Once hydrolyzed, it will not only cause unnecessary loss of antioxidants, but also make the polymer aging without effective protection, and its hydrolyzed acid substances will corrode during the polymer processing process. equipment
[0016] Two reasons cause the quality and stability of the obtained antioxidant 168 product to be defective

Method used

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  • Preparation method of antioxidant product with stable performance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Put 558Kg (2.709mol) of 2,4-di-tert-butylphenol and 120Kg of xylene solvent into a 2000-liter esterification reaction kettle, raise the temperature to 80-85°C, reduce the pressure to -0.055--0.085MPa, and reflux dehydration for 50-60 Minutes, pass cooling water to cool down to 45-50°C, add catalyst pyridine 2.0Kg, add dropwise 126.0Kg (0.918mol) 2.95 / 1 phosphorus trichloride, dropwise time is 60-70 minutes. After adding phosphorus trichloride dropwise, keep warm at 50-52°C for 50-60 minutes. Raise the temperature to 130-135°C, and keep the temperature for 80-90 minutes. Adjust the reaction temperature to 125-130°C, reduce the pressure to -0.045--0.065MPa, reflux for 110-120 minutes, and the reaction ends. After the reaction, add 850Kg of xylene to the reaction kettle to completely dissolve the crude antioxidant 168 crystalline product, add 3Kg of triethylamine at 50-60°C, keep warm at 50-60°C, and stir for 30 minutes. Add 7.0Kg of filter aid diatomite, keep warm at 50...

Embodiment 2

[0035] Put 558Kg (2.709mol) of 2,4-di-tert-butylphenol and 120Kg of xylene solvent into a 2000-liter esterification reaction kettle, raise the temperature to 80-85°C, reduce the pressure to -0.055--0.085MPa, and reflux dehydration for 50-60 Minutes, pass cooling water to cool down to 45-50°C, add catalyst pyridine 2.5Kg, add dropwise 124.0Kg (0.903mol) 3 / 1 phosphorus trichloride, dropwise time is 60-70 minutes. After adding phosphorus trichloride dropwise, keep warm at 50-52°C for 50-60 minutes. Raise the temperature to 130-135°C, and keep the temperature for 60-65 minutes. Adjust the reaction temperature to 125-130° C., reduce the pressure to -0.045--0.065 MPa, reflux for 140-150 minutes, and the reaction ends. After the reaction, add 850Kg of xylene to the reaction kettle to completely dissolve the crude antioxidant 168 crystal, add 2.5Kg of triethylamine at 50-60°C, keep warm at 50-60°C, and stir for 30 minutes. Add 6.0Kg of filter aid diatomite, keep warm at 50-60°C, sti...

Embodiment 3

[0037] Put 558Kg (2.709mol) of 2,4-di-tert-butylphenol and 150Kg of xylene solvent into a 2000-liter esterification reaction kettle, raise the temperature to 80-85°C, depressurize to -0.055--0.085MPa, and reflux dehydration for 50-60 Minutes, pass cooling water to cool down to 45-50°C, add catalyst pyridine 2.2Kg, add dropwise 120.0Kg (0.874mol) 3.1 / 1 phosphorus trichloride, dropwise time is 60-70 minutes. After adding phosphorus trichloride dropwise, keep warm at 50-52°C for 50-60 minutes. Raise the temperature to 130-135°C, and keep the temperature for 140-150 minutes. Adjust the reaction temperature to 125-130° C., reduce the pressure to -0.045--0.065 MPa, reflux for 90-95 minutes, and the reaction ends. After the reaction is over, add 800Kg of xylene to the reaction kettle to completely dissolve the crude antioxidant 168 crystallization product, add 3.5Kg of triethylamine at 50-60°C, keep warm at 50-60°C, and stir for 30 minutes. Add 8.0Kg of filter aid diatomite, keep w...

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PUM

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Abstract

The invention provides a preparation method of antioxidant product with stable performance. 2, 4-di-tert-butylphenol and phosphorus trichloride are taken as raw materials, organic amino compound is taken as catalyst, organic solvent is taken as reaction solvent, esterification is carried out to prepare tri(2,4-ditertrabutyl phenyl) phosphite ester crystal product, namely antioxidant crude product; after reaction is completed, the organic solvent is added into a kettle, so that the antioxidant crystal product is completely dissolved into the organic solvent, an amount of triethylamine is added to react with HCl remained in product mixture, so as to generate triethylamine hydrochloride crystal, filter aid is added to remove solids triethylamine hydrochloride and organic amine catalyst hydrochloride by heat filtering, reduced pressure distillation is carried out to remove the organic solvent, and crystal is washed by low carbon fatty alcohol, thus obtaining the antioxidant product with stable performance. The invention has the advantages of simple production technology, high product yield and good quality; and the obtained product has long time hydrolytic resistance, pyrolysis resistance and good oxidation resistance.

Description

technical field [0001] The invention relates to a process for preparing an antioxidant product with stable performance, in particular to a process for preparing tris(2,4-di-tert-butylphenyl)phosphite. Background technique [0002] Antioxidant 168 product belongs to phosphorous acid antioxidant, chemical name: tris(2,4-di-tert-butylphenyl) phosphite, specifically refers to the following formula (I): [0003] [0004] Antioxidant 168 is an excellent phosphite antioxidant product, which is widely used in polymer materials such as synthetic rubber, polyolefin plastics, and engineering plastics. When it is used in conjunction with hindered phenolic primary antioxidants, it has a good synergistic effect and can effectively improve the processing stability, heat resistance stability, color improvement and weather resistance of polymer materials. It is a phosphite secondary antioxidant Mainstream varieties of agents. [0005] The preparation process of antioxidant 168, in the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/145
Inventor 杜飞范延超秦永胡建伟
Owner 溧阳常大技术转移中心有限公司
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