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Process for producing methyl hydrazine with hydrazine hydrate method

A technology of hydrazine hydrate and methyl hydrazine, applied in the fields of hydrazine preparation, organic chemistry, etc., can solve the problems of poor product quality, high energy consumption, high pollution, etc., to reduce the cost of three wastes treatment, reduce the consumption of raw materials, and improve the safety factor. Effect

Active Publication Date: 2012-06-27
DONGLI NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The domestic production of methylhydrazine is based on the synthesis process of chlorine ammonia (chlorine gas, liquid ammonia, monomethylammonia, sodium hydroxide), which consumes a lot of energy (about 1.5 tons of standard coal per ton of product) and has a lot of pollution (waste water per ton of product About 12 tons, waste gas about 0.03 tons per ton, waste residue about 0.35 tons per ton) low yield (only 60-75%), poor product quality

Method used

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  • Process for producing methyl hydrazine with hydrazine hydrate method
  • Process for producing methyl hydrazine with hydrazine hydrate method
  • Process for producing methyl hydrazine with hydrazine hydrate method

Examples

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Effect test

Embodiment 1

[0024] Such as figure 1 As shown, the process of producing methylhydrazine by the hydrazine hydrate method of the present invention comprises the following steps: first put 480 parts by mass of hydrazine hydrate with a concentration of 75% into the salt-forming kettle, start stirring, control the temperature to 20°C, and then dropwise add 1051 parts by mass of hydrochloric acid with a concentration of 25%, adjust the pH to 6.5-7.0, after the reaction is completed, heat the temperature to 70°C, carry out dehydration under reduced pressure, and control the pressure to -0.1Mpa to obtain hydrazine hydrochloride; use the obtained hydrazine hydrochloride as a catalyst Transfer to the methylation reaction kettle, then add 900 parts by mass of methanol with a concentration of 95%, then seal the methylation reaction kettle, heat up to 90°C to carry out the methylation reaction, control the reaction pressure to 0.5MPa, react for 2h, and react After the end, the temperature was lowe...

Embodiment 2

[0027] Such as figure 1 As shown, the process for producing methylhydrazine by the hydrazine hydrate method of the present invention comprises the following steps: first put 500 parts by mass of hydrazine hydrate with a concentration of 75% into the salt-forming kettle, start stirring, control the temperature to 30°C, and then dropwise add 912 parts by mass of hydrochloric acid with a concentration of 30%, adjust the pH to be 6.5-7.0, after the reaction is completed, heat the temperature to 80°C, carry out dehydration under reduced pressure, and control the pressure to be -0.1Mpa to obtain hydrazine hydrochloride; the obtained hydrazine hydrochloride is transferred to Add 920 parts by mass of methanol with a concentration of 96% to the methylation reaction kettle, then seal the methylation reaction kettle, raise the temperature to 105°C for the methylation reaction, control the reaction pressure to 0.6MPa, react for 2.5h, and the reaction ends After that, the temperature w...

Embodiment 3

[0029] Such as figure 1 Shown, the technique that hydrazine hydrate method of the present invention produces methylhydrazine comprises the steps:

[0030] First put 520 parts by mass of hydrazine hydrate with a concentration of 80% into the salt-forming kettle, start stirring, control the temperature at 40°C, then add 1012 parts by mass of hydrochloric acid with a concentration of 30% dropwise, adjust the pH to 6.5-7.0, and the reaction is complete Finally, heat the temperature to 90°C, carry out dehydration under reduced pressure, and control the pressure to -0.1Mpa to obtain hydrazine hydrochloride; transfer the obtained hydrazine hydrochloride into a methylation reaction kettle, and then add 950 parts by mass of methanol with a concentration of 98%. Then close the methylation reaction kettle, raise the temperature to 120°C for methylation reaction, control the reaction pressure to 0.7MPa, react for 3 hours, after the reaction is completed, cool down to 55°C, put it into the...

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Abstract

The invention discloses a process for producing methyl hydrazine with a hydrazine hydrate method. The process is characterized by comprising the following steps of: reacting hydrazine chloride with methanol under the protection of an inert gas; isolating methyl hydrazine hydrochloride by using a hydrazine hydrate; and undergoing distilling and rectifying processes to obtain the methyl hydrazine. The process has the advantages of saving in energy, reduction in the emission of waste water, waste gas, waste residues and COD (Chemical Oxygen Demand) emission and high environmental friendliness. Internal circulation and continuous production is realized, the labor intensity of workers is lowered, reaction pressure is lowered from 0.7-1.3 MPa to 0.5-0.7 MPa, and the safe coefficient is increased.

Description

technical field [0001] The invention relates to a process for producing methylhydrazine by a hydrazine hydrate method. Background technique [0002] Methylhydrazine is an important energy material, and at the same time, it is also an important intermediate for the synthesis of some high-quality pesticides and medicines. The domestic production of methylhydrazine is based on the synthesis process of chlorine ammonia (chlorine gas, liquid ammonia, monomethylammonia, sodium hydroxide), which consumes a lot of energy (about 1.5 tons of standard coal per ton of product) and has a lot of pollution (waste water per ton of product About 12 tons, about 0.03 tons of waste gas per ton product, about 0.35 tons of waste residue per ton product) The yield is low (only 60-75%), and the product quality is poor. Therefore, a new technical solution should be provided to solve the above problems. Contents of the invention [0003] The object of the present invention is: aim ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/14C07C241/02
Inventor 蔡炳洋周建陆立新曹长辉王全
Owner DONGLI NANTONG CHEM
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