Synthesis method of 4,4'-thiobis(6-tert-butyl-3-methylphenol)

A technology of methyl phenol and synthesis method, applied in chemical instruments and methods, preparation of sulfides, preparation of organic compounds, etc., to achieve the effects of easy recovery and reuse, environmental protection and safety improvement

Active Publication Date: 2021-08-03
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Description
  • Claims
  • Application Information

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  • Synthesis method of 4,4'-thiobis(6-tert-butyl-3-methylphenol)

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Embodiment 1

[0034] Add 164.2 (1.0 mol) of 2-tert-butyl-5-methylphenol, 169.9 (1.0 mol) of silver nitrate, 253.8 g (1.0 mol) of iodine and 0.7 L of dichloromethane into the reaction kettle, and keep the Stirring, the color of iodine gradually disappears, accompanied by the formation of silver iodide. After 30 minutes, filter and recover the generated silver iodide, wash the filtrate with 1.1L of water and recover the washing water; dry the organic phase with industrial anhydrous magnesium sulfate, add Cu 8.2g, thiourea 38.1g (0.5mol) and triethylamine 200g (about 273ml), then reacted under reflux for 4 hours. Naturally cool to room temperature after the reaction, filter and recover the Cu catalyst, then add water to dilute and wash, separate the water phase, add water to the organic phase and adjust the pH to 6-7 with phosphoric acid, and separate the water phase after standing for stratification. The organic phase was washed once with saturated sodium chloride aqueous solution and water ...

Embodiment 2

[0036] Add 164.2 (1.0 mol) of 2-tert-butyl-5-methylphenol, 220.9 (1.0 mol) of silver trifluoroacetate, 253.8 g (1.0 mol) of iodine and 0.8 L of chloroform into the reaction kettle, and place the Stirring, the color of iodine gradually disappears, accompanied by the formation of silver iodide. After 30 minutes, filter and recover the generated silver iodide, wash the filtrate with 1L of water and recover the washing water; after the organic phase is dried with industrial anhydrous magnesium sulfate, add Cu 8.2g, thiourea 38.1g (0.5mol) and triethylamine 200g (about 273ml), then reacted under reflux for 4 hours. Naturally cool to room temperature after the reaction, filter and recover the Cu catalyst, then add water to dilute and wash, separate the water phase, add water to the organic phase and adjust the pH to 6-7 with phosphoric acid, and separate the water phase after standing for stratification. The organic phase was washed once with saturated sodium chloride aqueous solut...

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Abstract

The invention relates to a synthesis method of 4,4'-thiobis(6-tert-butyl-3-methylphenol). According to the method, chlorine and sulfur dichloride which are necessary to use in a traditional process are avoided, and a large amount of hydrogen chloride tail gas is not generated; a byproduct silver iodide and acid liquor are easy to recover and reuse, the environmental protection property and safety of the reaction are greatly improved, and the problems of equipment corrosion and the like are avoided. Therefore, the method is suitable for industrially synthesizing the 4,4'-thiobis(6-tert-butyl-3-methylphenol).

Description

technical field [0001] The invention relates to the field of antioxidants, in particular to a synthesis method of 4,4'-thiobis(6-tert-butyl-3-methylphenol). Background technique [0002] 4,4'-thiobis(6-tert-butyl-3-methylphenol) (i.e. antioxidant 300), molecular formula C 22 h 30 o 2 S, melting point 161-163°C, white powder appearance, low volatility, low toxicity; soluble in benzene, toluene, acetone, methyl alcohol, ethanol, carbon tetrachloride and other organic solvents, slightly soluble in petroleum solvents, insoluble in water , is a non-polluting high-efficiency phenolic antioxidant, which has the characteristics of low volatility, high antioxidant efficiency, good thermal stability and weather resistance, and has little effect on the electrical properties of products. It is compatible with carbon black and stearyl alcohol It also has a synergistic effect when used in combination. It can be used as an antioxidant for polypropylene, ABS, polystyrene, polyamide, poly...

Claims

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Application Information

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IPC IPC(8): C07C319/14C07C319/28C07C323/20
CPCC07C319/14C07C319/28C07C323/20
Inventor 郭骄阳赵崇鑫
Owner JIANGSU JIYI NEW MATERIAL CO LTD
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