Dehalogenation inhibitor

An inhibitor and dehalogenation technology, used in the preparation of amino compounds, the preparation of organic compounds, and the purification/separation of amino compounds, etc., can solve the problems of needing recovery, high price, and large dosage, and achieves low dosage, low price, Good dehalogenation effect

Inactive Publication Date: 2013-08-14
淮安嘉诚高新化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the above-mentioned dehalogenation inhibitors, some have poor dehalogenation inhibition effect, and some have good effect, but post-processing is difficult, the dosage is large, need to be recycled, and the price is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] (1) Weigh 16g of sodium phosphite and 4g of ethanolamine, put them into a beaker, stir and dissolve, and prepare a dehalogenation inhibitor with a weight percentage of 80% sodium phosphite and 20% ethanolamine.

[0012] (2) Add 80g of o-nitrochlorobenzene and 90ml of methanol into a 500ml autoclave, and at the same time add 3g of Raney Ni catalyst (the water content of the catalyst is 20%) and 0.48g of the dehalogenation inhibitor prepared above, airtight In the autoclave, replace the air with nitrogen for three times, then replace the nitrogen with hydrogen for three times, then stir and heat up to 60°C, start to introduce hydrogen to carry out the hydrogenation reduction reaction, maintain the reaction temperature at 60-65°C, and the reaction pressure at 0.8-1.0MPa, Until no hydrogen is absorbed, turn on the cooling water to cool down, stop stirring, after standing still, take out the supernatant, the catalyst stays in the autoclave for mechanical application, the supe...

Embodiment 2

[0015] (1) Weigh 15g of sodium phosphite and 5g of ethanolamine, put them into a beaker, stir and dissolve, and prepare a dehalogenation inhibitor with a weight percentage of 75% sodium phosphite and 25% ethanolamine.

[0016] (2) Add 80g of o-nitrochlorobenzene and 90ml of methanol into a 500ml autoclave, add 3g of Raney Ni catalyst (the water content of the catalyst is 20%), 0.48g of the dehalogenation inhibitor prepared above, and seal In the autoclave, replace the air with nitrogen for three times, then replace the nitrogen with hydrogen for three times, then stir and heat up to 60°C, start to introduce hydrogen to carry out the hydrogenation reduction reaction, maintain the reaction temperature at 60-65°C, and the reaction pressure at 0.8-1.0MPa, Until no hydrogen is absorbed, turn on the cooling water to cool down, stop stirring, after standing, take out the supernatant, the catalyst stays in the autoclave for mechanical application, the supernatant is tested as follows: ...

Embodiment 3

[0019] (1) Weigh 21g of sodium phosphite and 9g of ethanolamine, put them into a beaker, stir and dissolve, and prepare a dehalogenation inhibitor with a weight percentage of 70% sodium phosphite and 30% ethanolamine.

[0020] (2) Add 80g of o-nitrochlorobenzene and 90ml of methanol into a 500ml autoclave, add 3g of Raney Ni catalyst (the water content of the catalyst is 20%), 0.48g of the dehalogenation inhibitor prepared above, and seal In the autoclave, replace the air with nitrogen for three times, then replace the nitrogen with hydrogen for three times, then stir and heat up to 60°C, start to introduce hydrogen to carry out the hydrogenation reduction reaction, maintain the reaction temperature at 60-65°C, and the reaction pressure at 0.8-1.0MPa, Until no hydrogen is absorbed, turn on the cooling water to cool down, stop stirring, after standing, take out the supernatant, the catalyst stays in the autoclave for mechanical application, the supernatant is tested as follows: ...

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PUM

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Abstract

The invention discloses a dehalogenation inhibitor. The dehalogenation inhibitor is prepared by mixing the following ingredients in percentage by weight: 55-80% of sodium phosphite, and 20-45% of ethanol amine. The dehalogenation inhibitor has a good dehalogenation inhibition effect in the process of preparing chlorinated aromatic amine through hydrogenation reduction of chlorinated nitro-aromatics, the content of phenylamine is not more than 1%, the dehalogenation inhibitor is less in usage amount, low in cost and free from recovery, and the usage amount of the dehalogenation inhibitor takes up 0.6% of halogenated nitro-aromatics in weight.

Description

technical field [0001] The invention relates to a dehalogenation inhibitor, in particular to a dehalogenation inhibitor used for suppressing dehalogenation side reactions in the process of catalytic hydrogenation reduction of halogenated aromatic nitro compounds to prepare halogenated aromatic amines. Background technique [0002] Halogenated aromatic amines (such as: o-chloroaniline, 3,4-dichloroaniline, 3,5-dichloroaniline, etc.) are important organic chemical intermediates, widely used in polyurethane, pesticide, pharmaceutical and dye industries. [0003] There are many routes for the synthesis of halogenated aromatic amines, which can be summarized as follows: iron powder reduction method, alkali sulfide reduction method, zinc powder reduction method, electrolytic reduction method, methanol cracking hydrogen reduction method, hydrogenation reduction method, etc. From the comparison of the production process, the iron powder reduction method and the alkali sulfide reduct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/90C07C209/36
Inventor 石祖嘉章燕军沈学军臧维东
Owner 淮安嘉诚高新化工股份有限公司
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