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A kind of method of continuous method production hydroxylamine hydrochloride

A technology of hydroxylamine hydrochloride and hydrochloric acid, which is applied in the field of continuous production of hydroxylamine hydrochloride, can solve the problems of small production scale and achieve the effects of improved production capacity and simple process

Active Publication Date: 2017-08-25
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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  • A kind of method of continuous method production hydroxylamine hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0020] 1Kg stainless steel θ ring packing was added to the 10L reactor, soaked in 12Kg ethanol for 3h, then 5g of 1-aminoethyl-3-methylimidazole nitrate was added to the ethanol solution, filtered and dried to obtain the described of pretreated fillers.

[0021] Step 2 Synthesis Reaction

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

Embodiment 2

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

[0025] 1Kg stainless steel θ ring packing was added to the 10L reactor, soaked in 9Kg ethanol for 1h, then 1g of 1-aminoethyl-3-methylimidazole nitrate was added to the ethanol solution, filtered and dried to obtain the of pretreated fillers.

[0026] Step 2 Synthesis Reaction

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

Embodiment 3

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

[0030] 1Kg stainless steel θ ring packing was added to the 10L reactor, soaked in 15Kg ethanol for 5h, then 10g of 1-aminoethyl-3-methylimidazole nitrate was added to the ethanol solution, filtered and dried to obtain the of pretreated fillers.

[0031] Step 2 Synthesis Reaction

[0032] 10Kg of butanone oxime and hydrochloric acid (30% by mass concentration) were mixed and passed into a 2L fixed-bed reactor equipped with 1.8L of pretreated packing to carry out the reaction. The molar ratio of butanone oxime and 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 is subjected to rectification and crystallization refining process to obtain the refined product of hydroxylamine hydrochloride. Excess hydrochloric acid is recycled as supplementary raw material, numbered as M...

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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 producing hydroxylamine hydrochloride by a continuous method. Background technique [0002] Hydroxylamine hydrochloride is mainly used as a reducing agent and an imaging agent. It is used to prepare oximes in organic synthesis. It is also used as a raw material for synthesizing anticancer drugs (hydroxyurea), sulfa drugs (trimoxazole) and pesticides (methomyl). It is used as a depolarizer in electroanalysis, as a non-coloring short-term stop agent in the synthetic rubber industry, etc. The pharmaceutical industry is used as an intermediate for sulfamethoxazole. Synthetic dye industry is used for the preparation of isatin intermediates. The oil industry is used as an antioxidant 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. Depo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/14
CPCC01B21/1409
Inventor 王金明
Owner ZHEJIANG JINHUA NEW MATERIALS
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