Method for preparing parabenzoquinone dioxime

Abstract

The invention discloses a method for preparing parabenzoquinone dioxime, which comprises the following steps: 1) preparing sodium phenolate solution: mixing 5%-20% of NaOH solution and phenol solution and sodium nitrite solution, preparing the sodium phenolate solution, and adding sodium carbonate with a weight of 1 / 10 of the NaOH weight; 2) preparing parabenzoquinone monoxime, guiding the sodium phenolate solution into 28%-32% of acid liquor through a duct, and adding the sodium nitrite solution for the nitrosation reaction, the whole process being operated under the condition of -3 DEG C to 5 DEG C; 3) cleaning the solution, cleaning the prepared parabenzoquinone monoxime to neutral by using pure water, and measuring a decomposition point; 4) preparing the parabenzoquinone dioxime, adding water into the prepared parabenzoquinone monoxime and stirring, controlling the temperature within 45 DEG C to 62 DEG C, and pouring hydroxylamine and oximating and obtaining the product. The invention has the advantages that the reaction yield is high; the purity of target matter can reach 98 percent; and the content value of the nitrogen element in parabenzoquinone dioxime is not less than 20.26 percent.

Description

technical field [0001] The present invention relates to a method for catalyzing the synthesis of p-benzoquinone dioxime. To be exact, it uses p-benzoquinone dioxime and hydroxylamine hydrochloride as raw materials, and catalyzes the synthesis of p-benzoquinone dioxime at a certain temperature in the next step, which belongs to organic synthesis. technical field. Background technique [0002] P-benzoquinone dioxime is a crosslinking agent, the product is suitable for: butyl rubber, ethylene propylene rubber, natural rubber, styrene butadiene rubber, polysulfide rubber, etc., especially for butyl rubber, ethylene propylene rubber. Product performance: easy to disperse in the rubber compound, fast vulcanization speed, high elongation strength of the rubber compound, heat and weather resistance, ozone resistance and electrical insulation performance, can be used as acrylic acid polymerization inhibitor, and can improve the heat dissipation of polyester fiber tire cord Resistanc...

AI Technical Summary

Problems solved by technology

[0003] In recent years, the industrial production of p-benzoquinone dioxime is mainly as follows: at 0°C, in the presence of a certain concentration of sulfuric acid, sodium nitrite nitrosates phenol dissolved in 30% NaOH solution to prepare p-benzoquinone monoxime, and then prepares p-benzoquinone monoxime. The p-benzoquinone monoxime is added with hydroxamine to produce the final product p-benzoquinone dioxime. The product purity is limited by this synthetic method (≤95%), and contains more impurities, which are specifically reflected in: 1) in the preparation of p-benzoquinone During the process of quinone monoxime, the air in the reactor will oxidize part of p-benzoquinone monoxime to form resin, which affects the quality of p-benzoquinone monoxime and indirectly affects the quality of p-benzoquinone dioxime