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Method for producing hydroxylamine hydrochloride through continuous method

A continuous method of hydroxylamine hydrochloride, applied in the fields of hydroxylamine, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of small production scale, achieve the effects of increasing production capacity, increasing reaction contact area, and improving compatibility

Active Publication Date: 2016-07-20
ZHEJIANG JINHUA NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, the batch reaction is mainly used, and the production scale is small, so it is necessary to find a continuous production route for improvement

Method used

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  • Method for producing hydroxylamine hydrochloride through continuous method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Step 1 Pretreatment of Stainless Steel Theta Ring Packing

[0020] Add 1Kg stainless steel θ ring packing in 10L reaction kettle, soak 3h in 12Kg ethanol, then add 5g of 1-aminoethyl-3-methylimidazole nitrate in ethanol solution, filter, dry to obtain the described of pretreated fillers.

[0021] Step 2 synthesis reaction

[0022] Mix 10Kg of butanone oxime with hydrochloric acid (concentration: 25% by mass), and pass it into a 2L fixed-bed reactor equipped with 1L of pretreated filler for reaction. The molar ratio of butanone oxime to hydrochloric acid is 1:3, the reaction temperature is 80°C, and the reaction space velocity of the mixed solution is 3h -1 , the reaction pressure is normal pressure, and the reaction product undergoes rectification and crystallization refining process to obtain the refined product of hydroxylamine hydrochloride. Excess hydrochloric acid is recycled as supplementary raw material, numbered M-1.

Embodiment 2

[0024] Step 1 Pretreatment of Stainless Steel Theta Ring Packing

[0025] Add 1Kg stainless steel θ ring packing in 10L reactor, soak 1h in 9Kg ethanol, then add 1-aminoethyl-3-methylimidazole nitrate that is 1g in ethanol solution, filter, dry, obtain described of pretreated fillers.

[0026] Step 2 synthesis reaction

[0027] 10Kg of butanone oxime and hydrochloric acid (mass percentage concentration 20%) were mixed and passed into a 2L fixed-bed reactor equipped with 0.6L of pretreated filler for reaction. The molar ratio of butanone oxime to hydrochloric acid is 1:1, the reaction temperature is 60°C, and the reaction space velocity of the mixed solution is 1h -1 , the reaction pressure is normal pressure, and the reaction product undergoes rectification and crystallization refining process to obtain the refined product of hydroxylamine hydrochloride. Excess hydrochloric acid is recycled as supplementary raw material, coded as M-2.

Embodiment 3

[0029] Step 1 Pretreatment of Stainless Steel Theta Ring Packing

[0030] Add 1Kg stainless steel θ ring filler in 10L reaction kettle, soak in 15Kg ethanol for 5h, then add 10g of 1-aminoethyl-3-methylimidazole nitrate in ethanol solution, filter, dry to obtain the described of pretreated fillers.

[0031] Step 2 synthesis reaction

[0032] Mix 10Kg of butanone oxime with hydrochloric acid (concentration: 30% by mass), and pass it into a 2L fixed-bed reactor equipped with 1.8L of pretreated filler for reaction. The molar ratio of butanone oxime to hydrochloric acid is 1:5, the reaction temperature is 100°C, and the reaction space velocity of the mixed solution is 5h -1 , the reaction pressure is normal pressure, and the reaction product undergoes rectification and crystallization refining process to obtain the refined product of hydroxylamine hydrochloride. Excess hydrochloric acid is recycled as a supplementary raw material, numbered M-3.

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Abstract

Provided is a method for producing hydroxylamine hydrochloride through a continuous method.Diacetylmonoxime and hydrochloric acid are used and continuously reacted in a fixed bed reactor; the surface of filler is pretreated with ionic liquid, compatibility of the filler with hydroxylamine hydrochloride can be improved, and the reaction yield can be increased.

Description

technical field [0001] The invention relates to a method for preparing hydroxylamine hydrochloride, in particular to a method for continuously producing hydroxylamine hydrochloride. Background technique [0002] Hydroxylamine hydrochloride is mainly used as a reducing agent and imaging agent. It is used to prepare oximes in organic synthesis, and is also used as a raw material for the synthesis of anticancer drugs (hydroxyurea), sulfonamides (sulfamethoxazole) and pesticides (methomyl). It is used as a depolarizer in electroanalysis and as a non-coloring short-term stopper in the synthetic rubber industry. The pharmaceutical industry is used as an intermediate of sulfamethoxazole. Synthetic dye industry is used as isatin intermediate preparation. In the oil industry, it is used as an anti-aging agent and antioxidant for fatty acids and soaps. In analytical chemistry, it is used as a reducing agent for the analysis of formaldehyde, furfural, camphor and glucose. Depolariz...

Claims

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Application Information

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IPC IPC(8): C01B21/14
CPCC01B21/1409
Inventor 王金明
Owner ZHEJIANG JINHUA NEW MATERIALS
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