Novel method of catalytic synthesis of methylhydrazine under normal pressure

A synthesis method and technology of methylhydrazine, applied in the fields of hydrazine preparation and organic chemistry, can solve the problems of high toxicity of dimethyl sulfate, increase of sodium salt treatment cost, difficulty in industrial production, etc., to achieve convenient continuous production, improve Product selectivity, the effect of easy industrial production

Inactive Publication Date: 2015-11-11
UNIV OF JINAN
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Problems solved by technology

However, dimethyl sulfate is highly toxic and has potential safety hazards. At the same time, a large amount of difficult-to-handle sodium salt will remain after the dissociation, which

Method used

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  • Novel method of catalytic synthesis of methylhydrazine under normal pressure
  • Novel method of catalytic synthesis of methylhydrazine under normal pressure
  • Novel method of catalytic synthesis of methylhydrazine under normal pressure

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Slowly add 192.1g (2.0mol) of 38% concentrated hydrochloric acid dropwise to 125g (2.0mol) of 80% hydrazine hydrate. Under the condition of stirring, control the temperature at 20~30°C and keep it warm for 2 hours. After the reaction is complete, measure the pH=6, distill off the water under reduced pressure, mix the obtained hydrazine salt with 138g (3mol) of ethanol, and add coarse porous microspherical silica gel 16.0 g. Raise the reaction temperature to 73° C. and condense to reflux. Chloromethane was slowly introduced into the mixed solution at a rate of 0.56 mL / min to react for 2.3 h. The mixed solution after the reaction is distilled to separate ethanol and a small amount of water, and the ethanol can be recycled. The remaining raffinate was added to 136.0 g of hydrazine hydrate with a mass fraction of 80% for freeing. Finally, the dissociated solution was heated and rectified, and the fraction at 102-110°C was collected to obtain 98.0 g. The content of methylh...

Embodiment 2

[0043] Add 96.05g (1.0mol) of 38% concentrated hydrochloric acid dropwise to 62.5g (1.0mol) of 80% hydrazine hydrate. Under the condition of stirring, control the temperature at 20~30°C and keep it warm for 1.5h. After the reaction is complete, measure the pH=6, distill off the water under reduced pressure, mix the obtained hydrazine salt with 92g (2.0mol) of ethanol and add microporous microspheres Silica gel 8.3g, the reaction temperature was raised to 64°C and condensed to reflux, and methyl chloride was slowly introduced into the mixed solution at a rate of 0.22mL / min to react for 2h. The mixed solution after the reaction is distilled to separate ethanol and water, and the ethanol can be recycled. The remaining raffinate was added to 50 g of hydrazine hydrate with a mass fraction of 80%. Finally, the dissociated solution was heated up and rectified, and the fraction at 102-108°C was collected to obtain 63.3g fraction, with a gas phase detection content of 38.12%. The rem...

Embodiment 3

[0045] Add 134.6g (1.4mol) of 38% concentrated hydrochloric acid dropwise to 127.5g (1.4mol) of 80% hydrazine hydrate. Under the condition of stirring, control the temperature at 20~30°C and keep it warm for 1.0h. After the reaction is complete, measure the pH=6, distill off the water under reduced pressure, mix the obtained hydrazine salt with 96.6g (2.1mol) of ethanol and add coarse-pored microspheres Type 9.3g of silica gel, raise the reaction temperature to 51°C and condense to reflux, slowly inject methyl chloride into the mixed solution at a rate of 0.294mL / min, and react for 1.0h. The mixed solution after the reaction is distilled to separate ethanol and water, and the ethanol can be recycled. The remaining raffinate was added to 130 g of hydrazine hydrate with a mass fraction of 80%. Finally, the dissociated solution was heated up and rectified, and the fraction at 102-108°C was collected to obtain 42.9g fraction, with a gas phase detection content of 32.02%. The rem...

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Abstract

The invention discloses a novel method of catalytic synthesis of methylhydrazine under normal pressure. The method is characterized in that hydrazine hydrate and methane chloride react under normal pressure and 70-74 DEG C by taking hydrochloric acid as a protective agent, silica gel as a catalyst and ethyl alcohol as a solvent, thus generating methylhydrazine hydrochloride. A hydrazine ionization method is adopted, after methylhydrazine is ionized by the hydrazine hydrate, and a methylhydrazine aqueous solution is obtained by a rectification process. The ionized side product hydrazine monohydrochloride can be repeatedly used. The method has the following advantages: equipment cost and raw material price are lower in cost, reaction yield is high, the selectivity is good, three wastes are not generated, environment friendliness is good, and the process realizes internal circulation, continuous production can be conveniently performed, moreover, reaction is performed under normal pressure, operation is simple and production is safe.

Description

technical field [0001] The invention relates to a new method for catalytically synthesizing methylhydrazine under normal pressure. Background technique [0002] Methylhydrazine is also known as monomethylhydrazine, molecular formula: CH 6 N 2 , Molecular weight: 46.07, widely used in pesticides, medicines, dyes, etc., because of its low freezing point, good thermal stability and stable combustion process, it is considered the most promising rocket propellant fuel among hydrazine fuels. [0003] There are many reports on the synthetic method of methylhydrazine, currently according to the existing literature synthetic method mainly contains the following: [0004] Chloramine method [0005] Patent US4192819 first disclosed the process of synthesizing methylhydrazine by chloramine method, which mainly uses sodium hypochlorite and ammonia to react to produce chloramine, and then reacts chloramine and monomethylamine to generate methylhydrazine. [0006] [0007] This tech...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/14
Inventor 郑庚修刘庆东刘悦马志佳杨柳付凯
Owner UNIV OF JINAN
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