阅读说明：本技术 一种二氯二苯醚酮的产业化生产方法 (Industrialized production method of dichlorodiphenylene ether ketone ) 是由 马保方 于 2018-05-30 设计创作，主要内容包括：本发明涉及中间体合成技术领域,特别涉及一种二氯二苯醚酮的产业化生产方法,旨在提高产物收率,降低生产成本,减少废液排放量。其包括以下步骤：S1：将二氯二苯醚溶于氯丙烷中,并加入碳钢开式反应釜中,进行搅拌,控制碳钢反应釜内温度稳定；S2：向反应釜中加入氯酸钾催化剂,降温,之后向其中滴加乙酰氯；S3：滴加结束后保温2-2.5h,结束反应,将反应釜逐步降温,并将料液排至水解釜进行水解；S4：将料液经水解、脱溶、脱色、结晶、离心、风干,得到成品。(The invention relates to the technical field of intermediate synthesis, in particular to an industrial production method of dichlorodiphenylene ether ketone, aiming at improving the product yield, reducing the production cost and reducing the discharge amount of waste liquid. Which comprises the following steps: s1: dissolving dichlorodiphenyl ether in chloropropane, adding the solution into an open carbon steel reaction kettle, stirring, and controlling the temperature in the carbon steel reaction kettle to be stable; s2: adding a potassium chlorate catalyst into the reaction kettle, cooling, and then dropwise adding acetyl chloride into the reaction kettle; s3: after the dropwise addition is finished, preserving heat for 2-2.5h, finishing the reaction, gradually cooling the reaction kettle, and discharging the feed liquid to a hydrolysis kettle for hydrolysis; s4: hydrolyzing, desolventizing, decolorizing, crystallizing, centrifuging and air drying the feed liquid to obtain a finished product.)

1. An industrialized production method of dichlorodiphenylene ether ketone is characterized in that: the method comprises the following steps:

S1: dissolving dichlorodiphenyl ether in chloropropane, adding the solution into an open carbon steel reaction kettle, stirring, and controlling the temperature in the carbon steel reaction kettle to be stable;

S2: adding a potassium chlorate catalyst into the reaction kettle, cooling, and then dropwise adding acetyl chloride into the reaction kettle;

S3: after the dropwise addition is finished, preserving heat for 2-2.5h, finishing the reaction, gradually cooling the reaction kettle, and discharging the feed liquid to a hydrolysis kettle for hydrolysis;

S4: hydrolyzing, desolventizing, decolorizing, crystallizing, centrifuging and air drying the feed liquid to obtain a finished product.

2. The industrial production method of dichlorodiphenylene ether ketone according to claim 1, characterized in that: in S1, the stirring speed is 60-80 r/min.

3. The industrial production method of dichlorodiphenylene ether ketone according to claim 1, characterized in that: and S1, controlling the temperature in the carbon steel reaction kettle to be 15-20 ℃.

4. The industrial production method of dichlorodiphenylene ether ketone according to claim 1, characterized in that: and cooling to 8-12 ℃ in S2.

5. the industrial production method of dichlorodiphenylene ether ketone according to claim 1, characterized in that: and cooling to 3-5 ℃ in S3.

Technical Field

The invention relates to the technical field of intermediate synthesis, in particular to an industrial production method of dichlorodiphenylene ether ketone.

Background

The dichlorodiphenylene ether ketone is an important intermediate of pesticide bactericides such as difenoconazole, imidazole, tricyclazole and the like, however, the existing production process of the dichlorodiphenylene ether ketone mainly has the following defects of low reaction conversion rate, high production cost, large consumption of anhydrous aluminum trichloride and large discharge amount of three wastes and waste liquid.

Disclosure of Invention

The invention aims to provide an industrial production method of dichlorodiphenylene ether ketone, aiming at improving the product yield, reducing the production cost and reducing the discharge amount of waste liquid.

The technical purpose of the invention is realized by the following technical scheme:

An industrialized production method of dichlorodiphenylene ether ketone comprises the following steps:

S1: dissolving dichlorodiphenyl ether in chloropropane, adding the solution into an open carbon steel reaction kettle, stirring, and controlling the temperature in the carbon steel reaction kettle to be stable;

S2: adding a potassium chlorate catalyst into the reaction kettle, cooling, and then dropwise adding acetyl chloride into the reaction kettle;

s3: after the dropwise addition is finished, preserving heat for 2-2.5h, finishing the reaction, gradually cooling the reaction kettle, and discharging the feed liquid to a hydrolysis kettle for hydrolysis;

S4: hydrolyzing, desolventizing, decolorizing, crystallizing, centrifuging and air drying the feed liquid to obtain a finished product.

further, the stirring speed in S1 is 60-80 r/min.

Further, in S1, the temperature in the carbon steel reaction kettle is controlled to be 15-20 ℃.

Further, the temperature in S2 is reduced to 8-12 ℃.

Further, the temperature in S3 is reduced to 3-5 ℃.

Detailed Description

The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.

the invention discloses an industrial production method of dichlorodiphenylene ether ketone, and the specific implementation mode is as follows.