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Processing method for ketoxime type silane byproduct ketoxime salt

A treatment method, ketoxime-type technology, applied in the direction of nitrogen and non-metallic compounds, hydrolysis to prepare carbonyl compounds, hydroxylamine, etc., can solve the problems of high production cost, unfavorable water balance of production system, large sewage discharge, etc., and achieve reduction in treatment cost, benefit process water circulation, and reduce the effect of sewage discharge

Active Publication Date: 2016-02-10
江苏艾科维科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the raw materials used in the preparation of hydroxylamine chloride are limited to ketoxime, and hydrochloric acid is required for hydrolysis. Due to the limitation of hydrochloric acid concentration, it contains a certain amount of water, which is not conducive to the water balance of the production system.
Therefore, the production cost of this method is relatively high, and the amount of sewage discharge is large

Method used

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  • Processing method for ketoxime type silane byproduct ketoxime salt

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Experimental program
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Effect test

Embodiment 1

[0019] In the production process of ketoxime type silane, after the two-phase separator settles and separates layers, the ketoxime hydrochloride precipitate of the lower floor is separated and taken out, and 123.5g butanone oxime hydrochloride (1mol) is added to the mixer, and then Add 360g (20mol) of desalinated water at a high speed to mix thoroughly, feed the material from the feed port in the rectification tower after filtration, and turn on the vacuum pump connected to the vacuum pump port to control the vacuum degree in the tower at 0.05MPa. The internal temperature is controlled at 70-100°C, the reflux ratio in the tower is 4, the kettle liquid is partially circulated, and the produced butanone is discharged from the top of the tower through the cooler in time, part of the kettle liquid is cooled and crystallized by the crystallization tank, and filtered and dried to obtain chlorinated Hydroxylamine 65g, yield 94%, titration content 99.1%.

Embodiment 2

[0021] In the production process of ketoxime type silane, after the two-phase separator settles and separates layers, the ketoxime hydrochloride precipitate in the lower layer is separated and taken out, and 109.5g of acetone oxime hydrochloride (1mol) is added to the mixer, and then at a certain speed Add 360g (20mol) of desalinated water for thorough mixing, feed the material from the feed port in the rectification tower after filtration, turn on the vacuum pump connected to the vacuum pump port, and control the vacuum degree in the tower at 0.05MPa, and the vacuum in the rectification tower still The temperature is controlled at 70-100°C, the reflux ratio in the tower is 4, the kettle liquid is partially circulated, and the butanone produced is discharged from the top of the tower through the cooler in time, part of the kettle liquid is cooled and crystallized by the crystallization tank, and filtered and dried to obtain hydroxylamine chloride 67g, yield 96%, titration conte...

Embodiment 3

[0023] In the production process of ketoxime type silane, after the two-phase separator settles and separates layers, the ketoxime hydrochloride precipitate in the lower layer is separated and taken out, and 149.6g cyclohexanone oxime hydrochloride (1mol) is added to the mixer, and then Add 360g (20mol) of desalted water at a certain speed for thorough mixing, feed the material from the feed port in the rectification tower after filtration, and turn on the vacuum pump connected to the vacuum pump port to control the vacuum degree in the tower at 0.05MPa. The temperature in the kettle is controlled at 70-100°C, the reflux ratio in the tower is 5, the kettle liquid is partially circulated, and the produced butanone is discharged from the top of the tower through the cooler in time, part of the kettle liquid is cooled and crystallized by the crystallization tank, and filtered and dried to obtain chlorine Hydroxylamine 134g, yield 96%, titration content 99.3%.

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Abstract

The invention discloses a processing method for a ketoxime type silane byproduct ketoxime salt. The method comprises the following steps: after settling separation and layering through a two-phase separator in the production process of ketoxime type silane, separating lower-layer ketoxime hydrochloride precipitate, then carrying out complete mixing with water in a mixer, carrying out filtering, allowing the filtered mixture to enter a reactive rectifying column and carrying out hydrolysis reaction so as to generate a mixture of hydroxylammonium chloride and ketone, discharging ketone from the top of the rectifying column, subjecting a part of a hydroxylammonium chloride solution produced from the bottom of the rectifying column to recycling and the other part of the solution to crystallization, filtering and drying so as to obtain a hydroxylammonium chloride product, and allowing obtained filtrate to return to the rectifying column for recycling. According to the invention, the byproduct ketoxime hydrochloride in the production process of ketoxime type silane is used as a raw material, so cost of treating ketoxime hydrochloride in the production process of ketoxime type silane is reduced, and acid cost of production of hydroxylammonium chloride is saved at the same time; and the use of the byproduct ketoxime hydrochloride in the production process of ketoxime type silane as the raw material is favorable for circulation of process water in a production system and greatly reduces wastewater discharge of production equipment.

Description

technical field [0001] The invention relates to the field of chemical and environmental protection, in particular to a method for treating ketoxime salt, a by-product of ketoxime silane. Background technique [0002] Ketoxime silane is a common silicone crosslinking agent. Its body is a colorless or light yellow transparent liquid. It is mainly used in the production of room temperature vulcanized silicone rubber and neutral silicone glass glue. [0003] Synthesis of ketoxime silane, including adding chlorosilane, ketoxime and solvent into the reactor, after the reaction, sedimentation and separation are carried out to obtain the product ketoxime silane and by-product ketoxime hydrochloride. Ketoxime hydrochloride needs to be passed through ammonia water or caustic soda Neutralize to obtain ammonium chloride or sodium chloride and ketoxime. The treatment mode of this ketoxime hydrochloride can cause difficulty in separation and drying of the chloride, and the quality of the...

Claims

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Application Information

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IPC IPC(8): C07C45/42C07C49/04C07C49/08C07C49/403C01B21/14
Inventor 余立新
Owner 江苏艾科维科技股份有限公司
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