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Method for preparing benzyl hydroxyl amine antioxygen without waste water discharge

A dibenzylhydroxylamine, no waste water technology, applied in the field of preparing N,N-dibenzylhydroxylamine derivative antioxidants, can solve problems such as environmental hazards, product yield decline, environmental pollution, etc., and achieve good quality and product quality. High yield and the effect of solving environmental pollution problems

Active Publication Date: 2014-03-05
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this technique is that water is generated in the reaction process, and p-tert-butylbenzyl bromide is prone to hydrolysis reaction in alkaline solution to generate p-tert-butylbenzyl alcohol, resulting in a decline in product yield; in addition, the reaction solution The mixture of N,N-di-p-tert-butylbenzylhydroxylamine and sodium chloride and other inorganic salts in the product is washed with a large amount of water, resulting in a large amount of industrial wastewater containing dimethylformamide, which seriously pollutes the environment
[0012] The present invention attempts to use benzyl chloride and hydroxylamine hydrochloride as raw materials, anhydrous sodium carbonate as a neutralizing agent, and industrial ethanol as a solvent to prepare N,N-dibenzylhydroxylamine products by reaction, and the solid component in the obtained reaction solution is N,N - The mixture of dibenzylhydroxylamine and inorganic sodium salt can only be separated and purified by washing with a large amount of water to remove the inorganic sodium salt. The production of 1 ton of product will generate about 10 to 15 tons of industrial wastewater, which will cause very serious harm to the environment.

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  • Method for preparing benzyl hydroxyl amine antioxygen without waste water discharge
  • Method for preparing benzyl hydroxyl amine antioxygen without waste water discharge

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] In a reactor equipped with a stirrer, a thermometer, an alkyl benzyl halide addition funnel, and a reflux condenser, 55 g of hydroxylamine hydrochloride, 256 g of triethylamine, and 450 g of toluene were added. Replace the air in the reactor with nitrogen, heat, stir, and raise the temperature to 45°C, keep it constant at this temperature, start to add 230g of benzyl chloride dropwise, and finish dropping in 30 minutes. After the dropwise addition, keep the temperature for 40 minutes. Then the temperature was raised to 110° C., and the reaction was kept for 180 minutes. After the reaction, add 450 g of toluene, heat up to 80° C., heat filter to obtain solid triethylamine hydrochloride, wash and refine with toluene to obtain triethylamine hydrochloride as a by-product. The filtrate and washing liquid were combined, toluene was distilled off, crystallized by cooling, the crystallized product was washed with 80-95% ethanol solution, and dried to obtain 137 g of white cryst...

Embodiment 2

[0041] In a reactor equipped with a stirrer, a thermometer, an alkyl benzyl halide addition funnel, and a reflux condenser, 55 g of hydroxylamine hydrochloride, 240 g of triethylamine, and 450 g of xylene were added. Replace the air in the reactor with nitrogen, heat, stir, and raise the temperature to 45°C, keep it constant at this temperature, start to add 360g of p-tert-butylbenzyl bromide dropwise, and finish dropping in 30 minutes. After the dropwise addition, keep the temperature for 50 minutes. Then the temperature was raised to 100°C, and the reaction was kept for 190 minutes. After the reaction, add 350 g of xylene, heat up to 70° C., heat filter to obtain solid triethylamine hydrochloride, wash and refine with toluene to obtain triethylamine hydrochloride as a by-product. Combine the filtrate and washing liquid, remove xylene by distillation, cool and crystallize, wash the crystalline product with 80-95% ethanol solution, and dry to obtain 166 g of white crystalline pr...

Embodiment 3

[0043] Add 55 g of hydroxylamine hydrochloride, 304 g of triethylamine, and 500 g of benzene into a reactor equipped with a stirrer, a thermometer, an alkyl benzyl halide addition funnel, and a reflux condenser. Replace the air in the reactor with nitrogen, heat, stir, and raise the temperature to 45°C, keep it constant at this temperature, start to add 404g of p-tert-butylbenzyl chloride dropwise, and finish dropping in 40 minutes. After the dropwise addition, keep the temperature for 60 minutes. Then the temperature was raised to 90°C, and the reaction was kept for 200 minutes. After the reaction, 100 g of benzene was added, the temperature was raised to 100° C., the solid matter of triethylamine hydrochloride was obtained by hot filtration, and the by-product triethylamine hydrochloride was obtained by washing and refining with benzene. Combine the filtrate and washing liquid, remove benzene by distillation, cool and crystallize, wash the crystalline product with 80-95% eth...

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Abstract

The invention discloses a method for preparing benzyl hydroxyl amine antioxygen without waste water discharge, and belongs to the technical field of clean chemical synthesis. Alkyl-halogenation benzyl and oxammonium hydrochloride are taken as raw materials, organic amine compound is taken as an acid-binding agent, synthesis reaction is performed in organic solvent, and N, N-dibenzyl hydroxyl amine derivative products can be prepared. Synthesis reaction is performed in an anhydrous system, the production of waste water pollution can be effectively controlled from the source, and problems of environment pollution caused by waste water discharge in a traditional method can be fundamentally solved; in addition, by-product alkyl benzene methanol caused by alkyl-halogenation benzyl hydrolysis reaction can be prevented, and the yield of the N, N dibenzyl hydroxyl amine derivative products is improved. The method disclosed by the invention has the characteristics of simple productive technology, high product yield and good quality, and is convenient for industrial production.

Description

technical field [0001] The invention relates to a process for preparing N,N-dibenzylhydroxylamine derivative antioxidant without wastewater discharge, and belongs to the technical field of clean chemical synthesis. Background technique [0002] N, N-dibenzyl hydroxylamine derivative antioxidant specifically refers to the following formula ( ): [0003] ; [0004] Mode( ) [0005] Mode( ), R=H、C 1 ~C 10 Straight chain alkanes or branched alkanes. [0006] The stabilization process of traditional antioxidants is to terminate the active peroxyl radicals continuously generated in the polymer and effectively decompose hydroperoxides. For this reason, people have developed primary antioxidants such as hindered phenols, auxiliary antioxidants such as phosphites and thiosulfides. Obviously, this binary stabilization system has effectively played a role in the anti-aging process of polymers. [0007] On the one hand, the carbon free radical scavenger inhibits pure ther...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C239/10C07C211/05C07C209/74
Inventor 杜飞刘涛民陆网军范延超
Owner 溧阳常大技术转移中心有限公司