Preparation method of 2,2'-thiobis(4-tert-octylphenol) n-butylamine nickel

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: 2021-03-02
乐凯化学材料有限公司
View PDF11 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of 2,2'-thiobis(4-tert-octylphenol) n-butylamine nickel
  • Preparation method of 2,2'-thiobis(4-tert-octylphenol) n-butylamine nickel

Examples

Experimental program
Comparison scheme
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%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a preparation method of 2,2'-thiobis(4-tert-octylphenol) n-butylamine nickel. The method comprises the following steps: (1) Put hydrocarbon solvent, water-miscible solvent and water into the kettle, add 2,2′-thiobis-p-tert-octylphenol and divalent nickel salt under stirring, heat To 40-90°C, evenly drop the inorganic alkali solution from the high-level tank within 1-3 hours, keep it for 5 hours after the addition, let it stand, and separate the lower aqueous phase, add n-butylamine to the organic phase, and store at 50-80°C Stir at low temperature for 2 hours; filter the reaction solution, distill off the solvent, dry and pulverize to obtain a light green powder product. The invention introduces a solvent miscible with water, which improves the reaction stability, further increases the content of the product, and promotes the stability of the product quality. The inorganic base is used as the acid-binding agent to separate the n-butylamine from the nickel salt, which reduces the environmental pollution caused by excessive n-butylamine and its by-products.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap