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Method for preparing m-phenylenediamine by taking meta-position oil as raw material

A technology for meta-oil of m-phenylenediamine and nitrochlorobenzene, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of nitro compounds, etc. Problems such as the yield of nitrochlorobenzene, to achieve the effect of green environmental protection cost, simple process and easy operation

Active Publication Date: 2019-08-09
济宁市金泰利华化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the problem that this patent exists is: sodium methylate solution is in etherification reactor, in order to make p-nitrochlorobenzene fully etherified, usually need to add excess sodium methylate solution, and this just exists excessive sodium methylate to be in p-nitrochlorobenzene At the same time as benzene reacts, it will also react with m-nitrochlorobenzene to produce heavy component impurities, so that m-nitrochlorobenzene cannot be fully and completely extracted, affecting the yield of m-nitrochlorobenzene and causing a waste of resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for preparing m-phenylenediamine from nitrochlorobenzene meta-oil as a raw material comprises two steps: nitrochlorobenzene meta-oil nitration and catalyst hydrogenation.

[0030] Nitrification of nitrochlorobenzene meta-oil: add nitrochlorobenzene meta-oil to the reaction kettle, add concentrated sulfuric acid, raise the temperature to 60-80°C, add fuming nitric acid dropwise, and carry out nitration reaction. After the addition of nitric acid is completed, continue the reaction After standing for 2 hours, the waste acid was separated, and the material was washed twice with water to obtain a mixture of 2,4-nitrochlorobenzene and 3,5-dinitrochlorobenzene.

[0031] Catalytic hydrogenation reaction: use the mixture of 2,4-dinitrochlorobenzene and 3,5-dinitrochlorobenzene as raw material, methanol as solvent, sodium hydroxide, sodium acetate, sodium carbonate, sodium bicarbonate, Alkaline substances such as triethylamine are used as acid-binding agents, and the pr...

Embodiment 2

[0043] Nitration of nitrochlorobenzene meta-oil:

[0044] (1) Add 2000kg of meta oil and 1310kg of concentrated sulfuric acid with a mass fraction of 98% to a 5000L reactor, start stirring and raise the temperature to 75°C.

[0045] (2) Add 833 kg of fuming nitric acid (mass fraction 98%) dropwise at 75°C, the reaction is exothermic, feed circulating water to keep the temperature of the kettle at 75°C, and control it not to exceed 80°C, after the dropwise addition, keep stirring at 75°C 2 hours.

[0046] (3) Stand still to remove the waste acid, transfer the material to the washing kettle for washing, add alkali to adjust the pH value to 9-10 under the first washing and stirring, and let stand to separate the upper washing water, and wash the pH value of the washing material for the second time To neutrality, let stand to separate the upper layer of water, the lower layer of material is the intermediate 2,4-dinitrochlorobenzene and 3,5-dinitrochlorobenzene mixture. Note that t...

Embodiment 3

[0053] Nitration of nitrochlorobenzene meta-oil:

[0054] (1) Add 2000kg of meta oil and 1310kg of concentrated sulfuric acid with a mass fraction of 98% to a 5000L reactor, start stirring and raise the temperature to 75°C.

[0055] (2) Add 833 kg of fuming nitric acid (mass fraction 98%) dropwise at 75°C, the reaction is exothermic, feed circulating water to keep the temperature of the kettle at 75°C, and control it not to exceed 80°C, after the dropwise addition, keep stirring at 75°C 2 hours.

[0056] (3) Stand still to remove the waste acid, transfer the material to the washing kettle for washing, add alkali to adjust the pH value to 9-10 under the first washing and stirring, and let stand to separate the upper washing water, and wash the pH value of the washing material for the second time To neutrality, let stand to separate the upper layer of water, the lower layer of material is the intermediate 2,4-dinitrochlorobenzene and 3,5-dinitrochlorobenzene mixture. Note that...

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Abstract

The invention discloses a method for preparing m-phenylenediamine by taking nitrochlorobenzene meta-position oil as a raw material. The method comprises the following steps of (1) nitrification of thenitrochlorobenzene meta-position oil, wherein the nitrochlorobenzene meta-position oil is added into concentrated sulfuric acid, the temperature rises, fuming nitric acid is added dropwise, a reaction is carried out, standing is carried out for removing waste acid, and a mixture of 2,4-nitrochlorobenzene and 3,5-dinitrochlorobenzene is obtained; (2) a catalytic hydrogenation reaction, wherein themixture of the 2,4-nitrochlorobenzene and the 3,5-dinitrochlorobenzene is taken as a raw material, methyl alcohol is taken as a solvent, an alkaline substance is taken as an acid-binding agent, precious metal palladium carbon is taken as a catalyst, hydrogen is introduced, and the m-phenylenediamine is obtained. The novel method for treating the nitrochlorobenzene meta-position oil is found, which can turn waste into wealth; compared with other methods for treating the meta-position oil, the method is simple and direct, and meets the requirement of the atomic economic benefit; other unnecessary side reactions cannot be generated, and the process is simple and easy to operate; compared with a method for preparing the m-phenylenediamine through the reduction of m-dinitrobenzene, the methodis more environmentally friendly, and low in cost.

Description

technical field [0001] The invention belongs to the field of catalytic hydrogenation in chemical production, and in particular relates to a method for preparing m-phenylenediamine using meta-oil as a raw material. Background technique [0002] M-phenylenediamine, also known as 1,3-diaminobenzene, is a white needle-like crystal. It is an important organic chemical raw material and intermediate, and is widely used in industries such as dyes, washing chemicals, rubber, and national defense. Due to the strong coupling ability of m-phenylenediamine, azo dyes, fur dyes, reactive dyes and sulfur dyes can be produced in the dye industry, and it is also used to produce hair dyes, petroleum additives, rubber antioxidants, etc. It is widely used in various fields. [0003] The traditional method of producing m-phenylenediamine: use m-dinitrobenzene as raw material to prepare m-phenylenediamine by iron powder reduction or alkali sulfide reduction process. These two reduction processes ...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/51
CPCC07C209/36C07C201/08C07C211/51C07C205/12
Inventor 侯卫波韩龙凯王超李娟
Owner 济宁市金泰利华化工科技有限公司
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