阅读说明：本技术 一种间甲基苯甲腈的合成方法 (The synthetic method of one inter-species methyl benzonitrile ) 是由 吴水保 于 2018-05-25 设计创作，主要内容包括：本发明公开了一种间甲基苯甲腈的合成方法,包括以下步骤：(1)取20mL间二甲基苯置于反应釜中,将反应釜加热至130-135℃,依次加入溶剂DMF、催化剂及助催化剂,控制氧气通入量为900mL/min,氢气通入量为100mL/min,反应4-5h；(2)将上述反应液降温至室温,得到的透明无色晶体即为间甲基苯甲腈,使用DMF将得到的晶体洗涤2-3次后,抽滤除去DMF溶剂即可得到纯度高于90%的间甲基苯甲腈；本发明通过间二甲苯常压下液相氨氧化一步法合成间甲基苯甲腈,收率高,产品的纯度高,对设备的要求低,为间甲基苯甲腈的工业化生产提供了一条更为经济和环保的新途径。(The invention discloses the synthetic methods of an inter-species methyl benzonitrile, the following steps are included: (1) takes dimethyl benzene between 20mL to be placed in reaction kettle, reaction kettle is heated to 130-135 DEG C, sequentially add solvent DMF, catalyst and co-catalyst, control oxygen intake is 900mL/min, hydrogen intake is 100mL/min, reacts 4-5h；(2) above-mentioned reaction solution is cooled to room temperature, obtained clear colorless crystals be between methyl benzonitrile, using DMF will obtained crystal wash 2-3 time after, filter remove DMF solvent can be obtained purity be higher than 90% between methyl benzonitrile；The present invention is by methyl benzonitrile between liquid-phase ammoxidation one-step synthesis method under meta-xylene normal pressure, and high income, the purity is high of product, the requirement to equipment is low, and the industrialized production of methyl benzonitrile provides a new way more economical and environmentally friendly between.)

1. the synthetic method of an inter-species methyl benzonitrile, it is characterised in that the following steps are included:

(1) it takes dimethyl benzene between 20mL to be placed in reaction kettle, reaction kettle is heated to 130-135 DEG C, sequentially add solvent N, N- The additional amount of dimethylformamide DMF, catalyst and co-catalyst, the n,N-Dimethylformamide DMF is 20-25mL, is urged Agent and the additional amount of co-catalyst are respectively 2.5-3.0g and 10-15g, and control oxygen intake is 800-900mL/min, hydrogen Gas intake is 100mL/min, reacts 4-5h；

(2) above-mentioned reaction solution is cooled to room temperature, obtained clear colorless crystals be between methyl benzonitrile, using DMF will After the crystal arrived washs 2-3 times, methyl benzonitrile between purity can be obtained higher than 90% in suction filtration removing DMF solvent.

2. the synthetic method of inter-species methyl benzonitrile according to claim 1, it is characterised in that: in the step (1) The intake of oxygen is 860mL/min.

Technical field

The present invention relates to technical field of organic synthesis, the synthetic method of specifically a kind of methyl benzonitrile.

Background technique

Between methyl benzonitrile be one of the primary raw material of fluorescent whitening agent newly developed in recent years, have important purposes, Economic value is very big.The production method of methyl benzonitrile has diazonium salt method, catalytic gas phase oxidation method, dehydration of amide method between at present Deng, but that all there is toxicity is high, process route is long and complicated, industrial application is at high cost and the distinct disadvantages such as yield is low.Between methyl The report of the rarely seen former Soviet Union of benzonitrile phase ammonia oxidation, the country is still in its infancy.This method is simple with raw material, selects Property height, purpose product mononitrile high income, reaction only need to be carried out in a reactor, process route is short, pollution less and poison gently The advantages that.Tolualdehyde and meta-toluic acid are also valuable Organic Chemicals between the by-product of the reaction.This technique Exploitation have huge economic value.

Therefore, for problems existing for above-mentioned synthetic method, the synthetic method for researching and developing an inter-species methyl benzonitrile is The very urgent requirement of the industry.

Summary of the invention

The purpose of the present invention is to many deficiencies existing for the synthetic method of above-mentioned methyl benzonitrile, provide one kind Comprehensive cost of material is low, safety coefficient is high, the three wastes are easily processed, step is few, between high income methyl benzonitrile synthetic method.

The present invention provides the synthetic methods of an inter-species methyl benzonitrile, comprising the following steps:

(1) it takes dimethyl benzene between 20mL to be placed in reaction kettle, reaction kettle is heated to 130-135 DEG C, sequentially add solvent N, N- The additional amount of dimethylformamide DMF, catalyst and co-catalyst, the n,N-Dimethylformamide DMF is 20-25mL, is urged Agent and the additional amount of co-catalyst are respectively 2.5-3.0g and 10-15g, and control oxygen intake is 800-900mL/min, hydrogen Gas intake is 100mL/min, reacts 4-5h；

(2) above-mentioned reaction solution is cooled to room temperature, obtained clear colorless crystals be between methyl benzonitrile, using DMF will After the crystal arrived washs 2-3 times, methyl benzonitrile between purity can be obtained higher than 90% in suction filtration removing DMF solvent.

Preferably, the intake of oxygen is 860mL/min in the heretofore described step (1).

The present invention passes through methyl benzonitrile, high income, product between liquid-phase ammoxidation one-step synthesis method under meta-xylene normal pressure Purity is high, the requirement to equipment is low, and the industrialized production of methyl benzonitrile provides between the synthesis of meta-xylene selective oxidation One new way more economical and environmentally friendly.

Specific embodiment