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Preparation method for 2,2'-thiobis(4-tert-octylphenolato)-n-butylamine nickel(ii)

A technology of tert-octylphenol and n-butylamine nickel is applied in the field of preparation of 2,2'-thiobis-n-butylamine nickel, and can solve the problems of unstable product quality, large reaction fluctuation, large numerical value change, etc. To achieve the effect of improving reaction stability, avoiding by-products, and low toxicity

Active Publication Date: 2018-10-09
乐凯化学材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The system is a heterogeneous reaction, the reaction fluctuates greatly, resulting in unstable product quality, the actual product content is low, and the value changes greatly
N-butylamine is used as a reaction reagent, and at the same time, it is used as an acid-binding agent to undergo a complex reaction with the added nickel salt, producing a large number of by-products and polluting the environment
In addition, the excess n-butylamine is mixed with the by-product acetic acid, which dissolves in water and is difficult to recycle, resulting in a large amount of waste water and polluting the environment.

Method used

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  • Preparation method for 2,2'-thiobis(4-tert-octylphenolato)-n-butylamine nickel(ii)
  • Preparation method for 2,2'-thiobis(4-tert-octylphenolato)-n-butylamine nickel(ii)

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Pour 900L of toluene, 450L of N,N-dimethylformamide, and 400L of water into a 5000L reactor, turn on the stirring, add 360kg of 2,2′-thiobis-p-tert-octylphenol, 193.6kg of hexahydrate and chloride nickel. Heat to 70°C, dissolve 32.5kg of sodium hydroxide in 200kg of water, add it from the high-level tank at an even speed within 3 hours, and keep it for 5 hours after the addition. At that time, stop stirring and let stand for 20 minutes, then divide and remove the lower aqueous phase. Add 59.5kg of n-butylamine to the organic phase, and stir at 50-80°C for 2 hours. The reaction solution was distilled to remove the solvent, dried and pulverized to obtain a light green powder product with a yield of 95.4% and a purity of 99.3%.

Embodiment 2

[0035] Pour 900L of petroleum ether, 450L of propanol, and 400L of water into the reactor, turn on the stirring, and add 630kg of 2,2′-thiobis-p-tert-octylphenol, 508.2kg of hexahydrate and nickel chloride. Heat to 70°C, dissolve 125 kg of sodium hydroxide in 200 kg of water, add it from the elevated tank at an even speed within 3 hours, and keep it for 5 hours after adding. At that time, stop stirring and let stand for 20 minutes, then divide and remove the lower aqueous phase. Add 104 kg of n-butylamine to the organic phase, and stir for 2 hours at 50-80°C. The reaction solution was distilled to remove the solvent, dried and pulverized to obtain a light green powder product with a yield of 95.6% and a purity of 99.2%.

Embodiment 3

[0037] Pour 900L of toluene, 300L of N-methylpyrrolidone, and 300L of water into the reactor, turn on the stirring, and add 495 kg of 2,2′-thiobis-p-tert-octylphenol, 332 kg of hexahydrate and nickel chloride. Heat to 70°C, dissolve 89.6kg of sodium hydroxide in 200kg of water, add it from the elevated tank at an even speed within 3 hours, and keep it for 5 hours after adding. At that time, stop stirring and let stand for 20 minutes, then divide and remove the lower aqueous phase. Add 84.2kg of n-butylamine to the organic phase, and stir at 50-80°C for 2 hours. The reaction solution was distilled to remove the solvent, dried and pulverized to obtain a light green powder product with a yield of 96.1% and a purity of 99.3%.

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Abstract

The invention discloses a preparation method for 2,2'-thiobis(4-tert-octylphenolato)-n-butylamine nickel(ii). The preparation method comprises the following steps: (1) adding hydrocarbon solvent, solvent which mutually dissolves with water, and water into a kettle, adding 2,2'-thio p-(tert-octyl) phenol and nickelous salt under stirring, heating to 40-90 DEG C, evenly dripping inorganic base solution from an elevated tank within 1-3 hours, keeping for 5 hours after the inorganic base solution is added, standing, removing a lower layer of aqueous phase, adding n-butylamine into an organic phase, and stirring at the temperature of 50-80 DEG C for 2 hours; filtering reaction liquid, carrying out distillation to removal solvent, and drying and smashing to obtain a light green powdery product.The solvent which mutually dissolves with water is introduced, and reaction stability is improved so as to improve the content of the product and accelerate product quality to be stable. The inorganicbase serves as acid-binding agent, n-butylamine and nickel salt are separated, and the pollution of excessive n-butylamine and byproducts generated by the n-butylamine for environment can be lightened.

Description

technical field [0001] The invention relates to a preparation method of 2,2'-thiobis(4-tert-octylphenol) n-butylamine nickel. Background technique [0002] UV absorber UV-1084, the Chinese name is 2,2-thiobis(4-tert-octylphenol) n-butylamine nickel salt; (1-butylamine)[[2,2-(sulfur-KS)di[ 4-(1,1,3,3,-Tetramethylbutyl)phenolate-KO]](2-)]nickel. Light stabilizer UV-1084 is widely used in rubber and plastic products such as polyethylene film, flat wire, or polypropylene film, flat wire, etc. It has good compatibility with polyolefin; it can be used on polyethylene agricultural film and polypropylene shed film Stable application; resistant to pesticides and acid, has a broad market worldwide. [0003] 2,2'-thiobis(4-tert-octylphenol) n-butylamine nickel disclosed preparation method has US3313770 and [light stabilizer 2,2'-thiobis(4-tert-octylphenol) fine petrochemical industry Progress, 2007, Volume 8, No. 12, 9-11], the synthesis method of n-butylamine nickel they adopted is...

Claims

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Application Information

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IPC IPC(8): C07F15/04
CPCC07F15/045
Inventor 高俊峰李迁李河川郭艳成田硕
Owner 乐凯化学材料有限公司
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