CN112516917A - Preparation process of dicamba - Google Patents
Preparation process of dicamba Download PDFInfo
- Publication number
- CN112516917A CN112516917A CN202011486474.3A CN202011486474A CN112516917A CN 112516917 A CN112516917 A CN 112516917A CN 202011486474 A CN202011486474 A CN 202011486474A CN 112516917 A CN112516917 A CN 112516917A
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- CN
- China
- Prior art keywords
- piston
- cauldron
- cauldron body
- kettle
- mounting hole
- Prior art date
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/02—Preparation of carboxylic acid nitriles by reaction of nitrogen oxide with organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/16—Preparation of ethers by reaction of esters of mineral or organic acids with hydroxy or O-metal groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/08—Preparation of carboxylic acids or their salts, halides or anhydrides from nitriles
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation process of dicamba. In each step, putting each material into a reaction kettle, and reacting at a certain temperature and pressure, wherein the reaction kettle adopts the following structure: including the cauldron body, the internal baffle that sets up of cauldron, the cauldron body and the cauldron body down are separated into with the cauldron body to the baffle, the baffle exists one at least and can follow cauldron internal wall up-and-down motion, cauldron body upper portion sets up the air inlet, cauldron body lower part sets up the feed inlet. The invention changes the pressure in the reaction kettle by changing the volume of the reaction kettle, and changes the condition that the pressure in the reaction kettle is changed by filling gas in the traditional way.
Description
Technical Field
The invention relates to a preparation process of dicamba, belonging to the technical field of pesticides.
Background
Dicamba is synthesized under a certain pressure, and the conventional method usually changes the pressure condition by changing the gas pressure in the reaction kettle, i.e. the volume of the reaction kettle is not changed, and the pressure in the reaction kettle is changed by charging the gas, so that the gas consumption is increased, and even if the gas is inert gas, certain treatment is required due to humidity and other factors when the gas is extracted after the reaction is finished, so that improvement is needed.
Disclosure of Invention
The invention aims to overcome the defects and aims to provide a preparation process of dicamba capable of effectively changing pressure.
The technical scheme adopted by the invention is as follows: the preparation process of the dicamba comprises the following process steps: (1) 2, 5-dichlorophenol is taken as an initial raw material to react with dimethyl sulfate, and the reaction formula is as follows:
(2) then the obtained compound 2 is reacted with concentrated nitric acid, and the reaction formula is as follows:
(3) the resulting compound 3 is reductively aminated in the presence of a palladium catalyst and hydrogen, according to the following reaction scheme:
reacting compound 4 with cuprous cyanide, the reaction formula is as follows:
then the compound 5 is hydrolyzed in one step,
the method is characterized in that materials are put into a reaction kettle in each step and react at a certain temperature and pressure, and the reaction kettle adopts the following structure:
including the cauldron body, the internal baffle that sets up of cauldron, the cauldron body and the cauldron body down are separated into with the cauldron body to the baffle, the baffle exists one at least and can follow cauldron internal wall up-and-down motion, cauldron body upper portion sets up the air inlet, cauldron body lower part sets up the feed inlet.
Further, the partition plate comprises a fixing plate fixedly arranged on the inner wall of the kettle body, the fixing plate is provided with a mounting hole, and a piston is arranged in the mounting hole;
the piston comprises a piston cylinder fixedly arranged in the mounting hole and a piston plate arranged in the piston cylinder, an air pipe is arranged in the kettle body, one end of the air pipe is connected with the air inlet, and the other end of the air pipe is connected to the upper side of the kettle body and communicated with the kettle body; the lower surface of the piston plate is connected with a piston rod, the lower part of the piston rod extends out of the lower part of the kettle body, the lower part of the piston rod is connected with a movable plate which is driven by the piston rod to move up and down, and the movable plate and the inner wall of the kettle body form sealing fit.
Furthermore, a sealing gasket is arranged between the piston and the mounting hole, so that sealing connection is formed between the piston and the mounting hole.
The invention has the advantages that: the invention changes the pressure in the reaction kettle by changing the volume of the reaction kettle, and changes the condition that the pressure in the reaction kettle is changed by filling gas in the traditional way.
Drawings
FIG. 1 is a schematic structural view of a reaction vessel according to the present invention.
In the figure, 1 is a reaction kettle, 2 is an air inlet, 3 is an air pipe, 4 is a piston cylinder, 5 is a clapboard, 6 is a piston plate, 7 is a piston rod, 8 is a movable plate, and 9 is a feed inlet.
Detailed Description
The preparation process of the dicamba comprises the following process steps: (1) 2, 5-dichlorophenol is taken as an initial raw material to react with dimethyl sulfate, and the reaction formula is as follows:
(2) then the obtained compound 2 is reacted with concentrated nitric acid, and the reaction formula is as follows:
(3) the resulting compound 3 is reductively aminated in the presence of a palladium catalyst and hydrogen, according to the following reaction scheme:
reacting compound 4 with cuprous cyanide, the reaction formula is as follows:
then the compound 5 is hydrolyzed in one step,
the method is characterized in that materials are put into a reaction kettle in each step and react at a certain temperature and pressure, and the reaction kettle adopts the following structure:
including the cauldron body, the internal baffle that sets up of cauldron, the cauldron body and the cauldron body down are separated into with the cauldron body to the baffle, the baffle exists one at least and can follow cauldron internal wall up-and-down motion, cauldron body upper portion sets up the air inlet, cauldron body lower part sets up the feed inlet.
Further, the partition plate comprises a fixing plate fixedly arranged on the inner wall of the kettle body, the fixing plate is provided with a mounting hole, and a piston is arranged in the mounting hole;
the piston comprises a piston cylinder fixedly arranged in the mounting hole and a piston plate arranged in the piston cylinder, an air pipe is arranged in the kettle body, one end of the air pipe is connected with the air inlet, and the other end of the air pipe is connected to the upper side of the kettle body and communicated with the kettle body; the lower surface of the piston plate is connected with a piston rod, the lower part of the piston rod extends out of the lower part of the kettle body, the lower part of the piston rod is connected with a movable plate which is driven by the piston rod to move up and down, and the movable plate and the inner wall of the kettle body form sealing fit.
Furthermore, a sealing gasket is arranged between the piston and the mounting hole, so that sealing connection is formed between the piston and the mounting hole.
The invention will be further explained below for a better understanding of the invention: according to the invention, reaction raw materials are injected into the reaction kettle through the feeding hole, when the pressure in the reaction kettle needs to be changed, gas is filled into the gas pipe through the gas inlet and is conveyed into the piston cylinder, and the piston plate pushes the movable plate to move downwards under the pressure, so that the purpose of changing the reaction pressure of the materials is achieved; on the contrary, the movable plate moves upwards by pumping out gas, thereby achieving the purpose of changing the reaction pressure of the materials.
The gas introduced through the gas inlet and the raw materials are not contacted all the time, so that the gas and the raw materials are not influenced mutually, the pressure is changed by changing the volume of the reaction kettle, the original pressure changing mode is changed, and the high-pressure reactor has good service performance.
Claims (3)
1. The preparation process of the dicamba comprises the following process steps: (1) 2, 5-dichlorophenol is taken as an initial raw material to react with dimethyl sulfate, and the reaction formula is as follows:
(2) then the obtained compound 2 is reacted with concentrated nitric acid, and the reaction formula is as follows:
(3) the resulting compound 3 is reductively aminated in the presence of a palladium catalyst and hydrogen, according to the following reaction scheme:
reacting compound 4 with cuprous cyanide, the reaction formula is as follows:
then the compound 5 is hydrolyzed in one step,
the method is characterized in that materials are put into a reaction kettle in each step and react at a certain temperature and pressure, and the reaction kettle adopts the following structure:
including the cauldron body, the internal baffle that sets up of cauldron, the cauldron body and the cauldron body down are separated into with the cauldron body to the baffle, the baffle exists one at least and can follow cauldron internal wall up-and-down motion, cauldron body upper portion sets up the air inlet, cauldron body lower part sets up the feed inlet.
2. The dicamba preparation process according to claim 1, wherein the partition comprises a fixing plate fixedly disposed on the inner wall of the kettle body, the fixing plate is provided with a mounting hole, and a piston is disposed in the mounting hole;
the piston comprises a piston cylinder fixedly arranged in the mounting hole and a piston plate arranged in the piston cylinder, an air pipe is arranged in the kettle body, one end of the air pipe is connected with the air inlet, and the other end of the air pipe is connected to the upper side of the kettle body and communicated with the kettle body; the lower surface of the piston plate is connected with a piston rod, the lower part of the piston rod extends out of the lower part of the kettle body, the lower part of the piston rod is connected with a movable plate which is driven by the piston rod to move up and down, and the movable plate and the inner wall of the kettle body form sealing fit.
3. The process for preparing dicamba according to claim 2, wherein a sealing gasket is disposed between the piston and the mounting hole to form a sealing connection therebetween.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN202011486474.3A CN112516917A (en) | 2020-12-16 | 2020-12-16 | Preparation process of dicamba |
Applications Claiming Priority (1)
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CN202011486474.3A CN112516917A (en) | 2020-12-16 | 2020-12-16 | Preparation process of dicamba |
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CN112516917A true CN112516917A (en) | 2021-03-19 |
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CN202011486474.3A Pending CN112516917A (en) | 2020-12-16 | 2020-12-16 | Preparation process of dicamba |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN204865801U (en) * | 2015-06-17 | 2015-12-16 | 宁波大学 | Detachable chemical reaction cauldron |
CN207951385U (en) * | 2018-01-28 | 2018-10-12 | 青岛凤翔新材料有限责任公司 | A kind of reaction kettle compensator |
CN109180439A (en) * | 2018-10-22 | 2019-01-11 | 江苏长青农化股份有限公司 | A kind of synthetic method of dicamba |
CN209934700U (en) * | 2019-03-04 | 2020-01-14 | 张佩佩 | Chemical reaction kettle |
-
2020
- 2020-12-16 CN CN202011486474.3A patent/CN112516917A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN204865801U (en) * | 2015-06-17 | 2015-12-16 | 宁波大学 | Detachable chemical reaction cauldron |
CN207951385U (en) * | 2018-01-28 | 2018-10-12 | 青岛凤翔新材料有限责任公司 | A kind of reaction kettle compensator |
CN109180439A (en) * | 2018-10-22 | 2019-01-11 | 江苏长青农化股份有限公司 | A kind of synthetic method of dicamba |
CN209934700U (en) * | 2019-03-04 | 2020-01-14 | 张佩佩 | Chemical reaction kettle |
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Application publication date: 20210319 |