CN110551014A - Industrialized production method of dichlorodiphenylene ether ketone - Google Patents
Industrialized production method of dichlorodiphenylene ether ketone Download PDFInfo
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- CN110551014A CN110551014A CN201810541328.2A CN201810541328A CN110551014A CN 110551014 A CN110551014 A CN 110551014A CN 201810541328 A CN201810541328 A CN 201810541328A CN 110551014 A CN110551014 A CN 110551014A
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- reaction kettle
- dichlorodiphenylene
- ether ketone
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/65—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by splitting-off hydrogen atoms or functional groups; by hydrogenolysis of functional groups
Abstract
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.
Description
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.
Example 1
s1: 400kg of dichlorodiphenyl ether and 1200kg of organic solvent chloropropane are added into a dried carbon steel open reaction kettle, a Boolean type stirrer in the reaction kettle is started to stir, the rotating speed of the stirrer is 60 revolutions per minute, and the temperature in the carbon steel reaction kettle is controlled to be 15 ℃.
S2: 100kg of potassium chlorate catalyst with the granularity of 10-20 meshes is added into a reaction kettle, the temperature is reduced to 8 ℃ through frozen brine introduced into an outer jacket of the reaction kettle, then 120kg of acetyl chloride is dropwise added into a slot position of the reaction kettle, and the dropping speed is controlled to keep the temperature between 8 ℃ and 10 ℃.
S3: and (3) preserving the temperature for 2 hours after the dropwise addition, sampling in the period, performing central control analysis, supplementing raw materials or catalysts according to the analysis result, and finishing the reaction. Gradually cooling the reaction kettle to 3 ℃, discharging the materials to a hydrolysis kettle, hydrolyzing the reaction liquid, removing the potassium chlorate catalyst, flushing the reaction kettle with chloropropane, merging the flushing liquid into the reaction liquid for hydrolysis, and introducing steam into a jacket of the reaction kettle for negative pressure drying for the next batch of feeding operation.
S4: the hydrolyzed reaction solution is washed, desolventized, decolored, crystallized, centrifuged and air-dried to obtain 455kg of finished dichlorodiphenyl ether ketone.
Example 2
S1: 400kg of dichlorodiphenyl ether and 1200kg of organic solvent chloropropane are added into a dried carbon steel open reaction kettle, a Boolean type stirrer in the reaction kettle is started to stir, the rotating speed of the stirrer is 80 rpm, and the temperature in the carbon steel reaction kettle is controlled to be 20 ℃.
S2: 100kg of potassium chlorate catalyst with the granularity of 10-20 meshes is added into a reaction kettle, the temperature is reduced to 12 ℃ through frozen brine introduced into an outer jacket of the reaction kettle, then 120kg of acetyl chloride is dropwise added into a slot position of the reaction kettle, and the dropping speed is controlled to keep the temperature between 8 ℃ and 10 ℃.
S3: and (4) preserving the heat for 2.5 hours after the dropwise addition, sampling in the period, performing central control analysis, supplementing raw materials or catalysts according to the analysis result, and finishing the reaction. Gradually cooling the reaction kettle to 5 ℃, discharging to the hydrolysis kettle, hydrolyzing the reaction liquid, removing the potassium chlorate catalyst, flushing the reaction kettle with chloropropane, merging the flushing liquid into the reaction liquid for hydrolysis, and introducing steam into a jacket of the reaction kettle for negative pressure drying for the next batch of feeding operation.
S4: the hydrolyzed reaction solution is washed, desolventized, decolored, crystallized, centrifuged and air-dried to obtain 440kg of finished dichlorodiphenyl ether ketone.
Example 3
S1: 400kg of dichlorodiphenyl ether and 1200kg of organic solvent chloropropane are added into a dried carbon steel open reaction kettle, a Boolean type stirrer in the reaction kettle is started to stir, the rotating speed of the stirrer is 70 r/min, and the temperature in the carbon steel reaction kettle is controlled at 17 ℃.
s2: 100kg of potassium chlorate catalyst with the granularity of 10-20 meshes is added into a reaction kettle, the temperature is reduced to 10 ℃ through frozen brine introduced into an outer jacket of the reaction kettle, then 120kg of acetyl chloride is dropwise added into a slot position of the reaction kettle, and the dropping speed is controlled to keep the temperature between 8 ℃ and 10 ℃.
S3: and (3) preserving the heat for 2.3 hours after the dropwise addition, sampling in the period, performing central control analysis, supplementing raw materials or catalysts according to the analysis result, and finishing the reaction. Gradually cooling the reaction kettle to 4 ℃, discharging the materials to a hydrolysis kettle, hydrolyzing the reaction liquid, removing the potassium chlorate catalyst, flushing the reaction kettle with chloropropane, merging the flushing liquid into the reaction liquid for hydrolysis, and introducing steam into a jacket of the reaction kettle for negative pressure drying for the next batch of feeding operation.
s4: and washing the hydrolyzed reaction solution with water, desolventizing, decolorizing, crystallizing, centrifuging and air-drying to obtain 452kg of finished dichlorodiphenyl ether ketone.
Example 4
S1: 400kg of dichlorodiphenyl ether and 1200kg of organic solvent chloropropane are added into a dried carbon steel open reaction kettle, a Boolean type stirrer in the reaction kettle is started to stir, the rotating speed of the stirrer is 70 r/min, and the temperature in the carbon steel reaction kettle is controlled to be 20 ℃.
s2: adding 110kg of potassium chlorate catalyst with the granularity of 10-20 meshes into a reaction kettle, cooling to 10 ℃ through frozen brine introduced into an outer jacket of the reaction kettle, then dropwise adding 120kg of acetyl chloride into a slot-height position of the reaction kettle, and controlling the dropwise adding speed to keep the temperature between 8-10 ℃.
S3: and (3) preserving the heat for 2.3 hours after the dropwise addition, sampling in the period, performing central control analysis, supplementing raw materials or catalysts according to the analysis result, and finishing the reaction. Gradually cooling the reaction kettle to 4 ℃, discharging the materials to a hydrolysis kettle, hydrolyzing the reaction liquid, removing the potassium chlorate catalyst, flushing the reaction kettle with chloropropane, merging the flushing liquid into the reaction liquid for hydrolysis, and introducing steam into a jacket of the reaction kettle for negative pressure drying for the next batch of feeding operation.
S4: and washing the hydrolyzed reaction solution with water, desolventizing, decolorizing, crystallizing, centrifuging and air drying to obtain 438kg of finished dichlorodiphenyl ether ketone.
Example 5
S1: 400kg of dichlorodiphenyl ether and 1200kg of organic solvent chloropropane are added into a dried carbon steel open reaction kettle, a Boolean type stirrer in the reaction kettle is started to stir, the rotating speed of the stirrer is 70 r/min, and the temperature in the carbon steel reaction kettle is controlled to be 20 ℃.
S2: adding 110kg of potassium chlorate catalyst with the granularity of 10-20 meshes into a reaction kettle, cooling to 10 ℃ through frozen brine introduced into an outer jacket of the reaction kettle, then dropwise adding 120kg of acetyl chloride into a slot-height position of the reaction kettle, and controlling the dropwise adding speed to keep the temperature between 8-10 ℃.
S3: and (4) preserving the heat for 2.5 hours after the dropwise addition, sampling in the period, performing central control analysis, supplementing raw materials or catalysts according to the analysis result, and finishing the reaction. Gradually cooling the reaction kettle to 5 ℃, discharging to the hydrolysis kettle, hydrolyzing the reaction liquid, removing the potassium chlorate catalyst, flushing the reaction kettle with chloropropane, merging the flushing liquid into the reaction liquid for hydrolysis, and introducing steam into a jacket of the reaction kettle for negative pressure drying for the next batch of feeding operation.
S4: and washing the hydrolyzed reaction solution with water, desolventizing, decolorizing, crystallizing, centrifuging and air drying to obtain 450kg of finished dichlorodiphenyl ether ketone.
Claims (5)
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.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113816838A (en) * | 2021-08-05 | 2021-12-21 | 宁夏瑞泰科技股份有限公司 | Synthetic method of 2-chloro-4- (4-chlorophenoxy) -acetophenone |
| CN113861004A (en) * | 2021-11-03 | 2021-12-31 | 山东潍坊双星农药有限公司 | Catalytic synthesis method of difenoconazole intermediate difenone |
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2018
- 2018-05-30 CN CN201810541328.2A patent/CN110551014A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113816838A (en) * | 2021-08-05 | 2021-12-21 | 宁夏瑞泰科技股份有限公司 | Synthetic method of 2-chloro-4- (4-chlorophenoxy) -acetophenone |
| CN113861004A (en) * | 2021-11-03 | 2021-12-31 | 山东潍坊双星农药有限公司 | Catalytic synthesis method of difenoconazole intermediate difenone |
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Application publication date: 20191210 |