A kind of method for producing hydroxylamine hydrochloride

A technology of hydroxylamine hydrochloride and production equipment, applied in the direction of hydroxylamine, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as difficulty in realizing large-scale industrial production, difficulty in realizing industrial production, complicated process, etc., and achieve large-scale industrialization The effect of production, easy industrialization, and simple process

Active Publication Date: 2018-01-30
ZHEJIANG JINHUA NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that it adopts kettle-type batch reaction, the process is complicated, the cost is high, and it is difficult to realize large-scale industrial production
The disadvantage is that the batch reaction is adopted, the process is complicated, the cost is high, and it is difficult to realize large-scale industrial production

Method used

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  • A kind of method for producing hydroxylamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] First, put butanone oxime and hydrochloric acid into the premixing tank 5 for premixing according to the molar ratio of butanone oxime and hydrochloric acid 1.1:1, and the jacket of the condenser 3 is fed with a cold medium, and then the reaction system is evacuated to -0.07Mpa. Reactor 1 is heated up to the reaction temperature of 80°C, and the feed metering pump 6 is started, and the raw materials in the premix tank 5 are poured into the tubular reactor 1 for reaction, and the residence time is 250s. Distillation and separation tower 2 separates the mixture of methyl ethyl ketone and water, after the mixture of methyl ethyl ketone and water is cooled by condenser 3, part of it is refluxed to rectification and separation tower 2, and part of it is collected in collection tank 4. The tubular reactor discharge pipe 8 at the bottom of the reactor 1 collects, concentrates, filters, and dries to obtain hydroxylamine hydrochloride. The raw materials were injected continuousl...

Embodiment 2

[0029] The residence time is 150s, the system is vacuumed to -0.06Mpa, and the others are the same as in Example 1, 613.6g of hydroxylamine hydrochloride can be obtained, the yield is 98.1%, and the content is 98.9%.

Embodiment 3

[0031] The reaction temperature was 70° C., the residence time was 300 s, the others were the same as in Example 1, and 614.2 g of hydroxylamine hydrochloride could be obtained, with a yield of 98.2% and a content of 99.2%.

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Abstract

The invention discloses a device for producing hydroxylamine hydrochloride. The device comprises a tubular reactor, a rectification separation tower, a condenser, a premixing tank, a metering inlet pump and a collecting tank, wherein the premixing tank, the metering inlet pump, the tubular reactor, the rectification separation tower, the condenser and the collecting tank are sequentially connected, the tube diameter of the tubular reactor is consistent with the tower diameter of the rectification separation tower, and the top of the tubular reactor is vertically connected with the bottom of the rectification separation tower. The invention also discloses a method for producing the hydroxylamine hydrochloride by adopting the device. The device and method disclosed by the invention have the advantages that continuous production of the hydroxylamine hydrochloride is realized, production efficiency is improved, energy consumption is reduced, and cost is saved.

Description

technical field [0001] The present invention relates to the production method of hydroxylamine salt, particularly a kind of method of producing hydroxylamine hydrochloride. Background technique [0002] Hydroxylamine hydrochloride is an important chemical raw material and an organic synthesis intermediate with a wide range of uses. Hydroxylamine hydrochloride is commonly used in the preparation of oximes, especially cyclohexanone oxime for the synthesis of caprolactam. Hydroxylamine hydrochloride can also be used to synthesize a variety of medicines, pesticides and dyes, such as the anticancer drug hydroxyurea, sulfamethoxazole, the pesticide methoxam and the dye isatin; it can also be used to synthesize high-value intermediates with more complex structures, such as hydroxylamine -O-sulfonic acid, p-hydroxybenzonitrile, carboxymethylhydroxylamine hemihydrochloride, N-hydroxysuccinimide; it can also be used as a depolarizer in electrical analysis and a constant viscosity age...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/14
CPCC01B21/1454C01P2006/80
Inventor 张万宏李宏峰周强陈幼坚王彤
Owner ZHEJIANG JINHUA NEW MATERIALS
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