CN112516917A - Preparation process of dicamba - Google Patents

Preparation process of dicamba Download PDF

Info

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
Authority
CN
China
Prior art keywords
piston
cauldron
cauldron body
kettle
mounting hole
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011486474.3A
Other languages
Chinese (zh)
Inventor
于国权
孙霞林
马长庆
丁华平
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Changqing Agrochemical Co ltd
Original Assignee
Jiangsu Changqing Agrochemical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Changqing Agrochemical Co ltd filed Critical Jiangsu Changqing Agrochemical Co ltd
Priority to CN202011486474.3A priority Critical patent/CN112516917A/en
Publication of CN112516917A publication Critical patent/CN112516917A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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

Landscapes

  • 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

Preparation process of dicamba
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:
Figure 985917DEST_PATH_IMAGE001
；
(2) then the obtained compound 2 is reacted with concentrated nitric acid, and the reaction formula is as follows:
Figure 323358DEST_PATH_IMAGE002
；
(3) the resulting compound 3 is reductively aminated in the presence of a palladium catalyst and hydrogen, according to the following reaction scheme:
Figure 966829DEST_PATH_IMAGE003
；
reacting compound 4 with cuprous cyanide, the reaction formula is as follows:
Figure 301995DEST_PATH_IMAGE004
；
then the compound 5 is hydrolyzed in one step,
Figure 93233DEST_PATH_IMAGE005
；
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:
Figure 735830DEST_PATH_IMAGE001
；
(2) then the obtained compound 2 is reacted with concentrated nitric acid, and the reaction formula is as follows:
Figure 358441DEST_PATH_IMAGE002
；
(3) the resulting compound 3 is reductively aminated in the presence of a palladium catalyst and hydrogen, according to the following reaction scheme:
Figure 818503DEST_PATH_IMAGE003
；
reacting compound 4 with cuprous cyanide, the reaction formula is as follows:
Figure 893776DEST_PATH_IMAGE004
；
then the compound 5 is hydrolyzed in one step,
Figure 776281DEST_PATH_IMAGE005
；
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:
Figure 339153DEST_PATH_IMAGE001
；
(2) then the obtained compound 2 is reacted with concentrated nitric acid, and the reaction formula is as follows:
Figure 344018DEST_PATH_IMAGE002
；
(3) the resulting compound 3 is reductively aminated in the presence of a palladium catalyst and hydrogen, according to the following reaction scheme:
Figure 781953DEST_PATH_IMAGE003
；
reacting compound 4 with cuprous cyanide, the reaction formula is as follows:
Figure 202570DEST_PATH_IMAGE004
；
then the compound 5 is hydrolyzed in one step,
Figure 238921DEST_PATH_IMAGE005
；
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.
CN202011486474.3A 2020-12-16 2020-12-16 Preparation process of dicamba Pending CN112516917A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011486474.3A CN112516917A (en) 2020-12-16 2020-12-16 Preparation process of dicamba

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011486474.3A CN112516917A (en) 2020-12-16 2020-12-16 Preparation process of dicamba

Publications (1)

Publication Number Publication Date
CN112516917A true CN112516917A (en) 2021-03-19

Family

ID=75000743

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011486474.3A Pending CN112516917A (en) 2020-12-16 2020-12-16 Preparation process of dicamba

Country Status (1)

Country Link
CN (1) CN112516917A (en)

Citations (4)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
CN101386564A (en) Technique for synthesizing methanol by hydrogen and carbon dioxide
CN112535999A (en) Synthesis process of hydroxylamine hydrochloride
CN112516917A (en) Preparation process of dicamba
CN101638224B (en) Method for purifying phosphine by-product and application method of phosphine by-product
CN108424358A (en) A kind of device and method producing high-purity dimethoxym ethane using catalytic distillation coupling technique
CN208230684U (en) A kind of fixed bracket bosses stamping die of automobile axle U-shaped oil pipe
CN101327508A (en) Novel assembling die for producing non-welding type water tank die block
CN216713208U (en) Air pressure water supply tank convenient for air pressure supplement
CN108658787A (en) The preparation method of ethamine
CN112337409A (en) Production system of hexamethylene diamine
CN209520267U (en) Molding die knock-out mechanism and stamping die
KR101655829B1 (en) Apparatus for Fabricating the Hydrate using a Controlled Atmosphere Gas and Method Fabricating the Hydrate
CN218573616U (en) Production system of o-tert-butylcyclohexanol
CN202415415U (en) Device for preparing methanethiol by use of hydrogen sulfide-methanol gas-phase catalytic reaction method
CN111253277A (en) Production method of N, N-diethyl acetamide
CN214991231U (en) Reaction device for o-tert-butylcyclohexanol
CN201086107Y (en) Novel composite mold for producing non-soldering water container module
CN213499862U (en) Fertile plant nutrition brick moulding-die
CN214973989U (en) Environment-friendly dye constant-temperature constant-pressure reaction tank
CN212860221U (en) Double-mold-cavity injection mold for producing air conditioner on-hook housing
CN221181690U (en) 2, 2-Di (2-tetrahydrofuranyl) propane synthesis reaction system
CN215611625U (en) Acrylonitrile catalyst apparatus for producing
CN220514169U (en) Dichloropropanol apparatus for producing
CN215841668U (en) Distillation still is used in TGIC processing
CN208839565U (en) A kind of reactor for producing high-concentration formaldehyde by methanol oxidation

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210319