阅读说明：本技术 一种酮肟盐酸盐的处理方法 (Method for treating ketoxime hydrochloride ) 是由 徐书群 叶利民 祝俊 叶黎霞 范吉安 王艳霞 于 2020-07-15 设计创作，主要内容包括：本发明公开了一种酮肟盐酸盐的处理方法,该方法具体包括如下步骤：S1:将酮肟盐酸盐分散于有机溶剂中,利用氨中和,形成沉淀并离心；S2:将离心后的清液进行蒸馏回收溶剂、酮肟；S3：将离心后的固体分散于溶剂中进行再次洗涤后离心得到的清液回用,用于溶解酮肟盐酸盐；离心后得到的固体进行干燥回收溶剂,得到固体氯化铵。本发明提供的酮肟盐酸盐的处理方法,生产工艺安全风险小,能耗低,操作方便。(The invention discloses a method for treating ketoxime hydrochloride, which comprises the following steps: s1, dispersing the ketoxime hydrochloride in an organic solvent, neutralizing by ammonia, forming a precipitate and centrifuging; s2, distilling the centrifuged clear liquid to recover the solvent and the ketoxime; s3: dispersing the centrifuged solid in a solvent, washing again, and centrifuging to obtain a clear liquid for recycling, wherein the clear liquid is used for dissolving the ketoxime hydrochloride; and drying the solid obtained after centrifugation to recover the solvent to obtain solid ammonium chloride. The method for treating the ketoxime hydrochloride provided by the invention has the advantages of low production process safety risk, low energy consumption and convenience in operation.)

1. The method for treating the ketoxime hydrochloride is characterized by comprising the following steps of:

s1, dispersing the ketoxime hydrochloride in an organic solvent, neutralizing by ammonia, forming a precipitate and centrifuging;

s2, distilling the centrifuged clear solution to recover the solvent and the ketoxime;

s3: dispersing the centrifuged solid in an organic solvent, washing again, and centrifuging to obtain clear liquid for dissolving the ketoxime hydrochloride; and drying the solid obtained after centrifugation to recover the solvent to obtain solid ammonium chloride.

2. A method of handling a ketoxime hydrochloride according to claim 1 wherein the ketoxime in the ketoxime hydrochloride has the general formula R1(C ═ NOH) R2 wherein R1 and R2 represent hydrogen or C1-C7 alkyl.

3. The method of claim 1, wherein the organic solvent is a ketone.

4. The method for treating ketoxime hydrochloride according to claim 1, wherein the ketoxime is cyclohexanone oxime, acetone oxime, butanone oxime, methyl isobutyl ketoxime, methyl isoamyl ketoxime, or 2-pentanone oxime.

Technical Field

The invention relates to the technical field of chemical synthesis, in particular to a method for treating ketoxime hydrochloride.

Background

A great amount of oxime-containing hydrochloride is generated in the synthesis of an organic silicon oxime-containing cross-linking agent, and an invention patent with the publication number of CN105315139B discloses a method for treating ketoxime salt serving as a byproduct of ketoxime type silane.

At present, the ketoxime hydrochloride is neutralized by liquid alkali to obtain salt and ketone, a large amount of water is brought in the neutralization process to ensure that oxime is easy to hydrolyze, and the method ensures that the subsequent ketoxime recovery and salt crystallization have high energy consumption and large sewage amount.

Disclosure of Invention

Aiming at the problems, the invention provides a method for treating ketoxime hydrochloride, which has the advantages of simple process, low energy consumption and environmental protection.

The technical scheme adopted by the invention is as follows: the invention provides a method for treating ketoxime hydrochloride, which comprises the following steps:

s1, dissolving and dispersing the ketoxime hydrochloride in an organic solvent, neutralizing by ammonia to form a precipitate and centrifuging;

s2, distilling the centrifuged clear liquid to recover the solvent and the ketoxime;

s3: dispersing the centrifuged solid in an organic solvent, washing again, and centrifuging to obtain clear liquid for recycling, wherein the clear liquid is used for dissolving ketoxime hydrochloride; and drying the solid obtained after centrifugation to recover the solvent to obtain solid ammonium chloride.

In the above method for treating ketoxime hydrochloride, the ketoxime hydrochloride has the formula R1(C ═ NOH) R2, wherein R1 and R2 represent hydrogen or alkyl groups of C1 to C7.

In the above method for treating ketoxime hydrochloride, the organic solvent is a ketone.

In the above method for treating ketoxime hydrochloride, the ketoxime is cyclohexanone oxime, propyl ketoxime, butyl ketoxime, methyl isobutyl ketoxime, methyl isoamyl ketoxime or 2-pentanone oxime.

The invention has the beneficial effects that: the invention provides a method for treating ketoxime hydrochloride, which is characterized in that ketoxime hydrochloride is dispersed in an organic solvent, ammonia is utilized for neutralization, and generated ammonium chloride has low solubility in the organic solvent and is precipitated in large quantity to obtain solid ammonium chloride, so that the problems of high separation energy consumption and large wastewater quantity caused by large solubility of the ammonium chloride in an aqueous solution are effectively solved; in addition, hydrolysis of oxime is inhibited in an organic solvent system and in the process, so that free hydroxylamine is difficult to generate, and the safety of the production process is greatly improved.

Detailed Description

The present invention will now be described more fully hereinafter with reference to specific examples.

The technical scheme adopted by the invention is as follows: the invention provides a method for treating ketoxime hydrochloride, which comprises the following steps:

s1, dissolving and dispersing the ketoxime hydrochloride in an organic solvent, neutralizing by ammonia to form a precipitate and centrifuging;

s2, distilling the centrifuged clear liquid to recover the solvent and the ketoxime;

s3: dispersing the centrifuged solid in an organic solvent, washing again, and centrifuging to obtain clear liquid for recycling, wherein the clear liquid is used for dissolving ketoxime hydrochloride; and drying the solid obtained after centrifugation to recover the solvent to obtain solid ammonium chloride.