CN214183071U - Production device for difenoconazole intermediate - Google Patents
Production device for difenoconazole intermediate Download PDFInfo
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- CN214183071U CN214183071U CN202022785525.4U CN202022785525U CN214183071U CN 214183071 U CN214183071 U CN 214183071U CN 202022785525 U CN202022785525 U CN 202022785525U CN 214183071 U CN214183071 U CN 214183071U
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Abstract
The utility model provides a apparatus for producing of difenoconazole midbody, includes the elevated tank, the cauldron body, acidylates condenser, phenyl ether ketone receiving tank, the elevated tank include acetyl chloride elevated tank, acidylates the material elevated tank, the cauldron body include phenyl ether ketone synthetic kettle, hydrolysis kettle, washing kettle, acetyl chloride elevated tank, phenyl ether ketone synthetic kettle, acidylates material elevated tank, hydrolysis kettle, washing kettle, phenyl ether ketone receiving tank loop through the pipeline and link to each other. The utility model discloses simple structure, the simple operation between each equipment has realized the semi-continuous steady production of phenyl ether ketone, and the cost is lower, and is easy and simple to handle, is suitable for industrial production.
Description
Technical Field
The utility model belongs to chemical production device field, concretely relates to apparatus for producing of difenoconazole midbody.
Background
Difenoconazole plays an extremely important role in triazole bactericides and has become one of the most widely used bactericides in crop planting. The pure product of difenoconazole is colorless solid, and the molecular formula is as follows: c19H17Cl2N3O3The chemical name is cis, trans-3-chloro-4- [ 4-methyl-2- (1H-1,2, 4-triazole-1-ylmethyl) -1, 3-dioxolan-2-yl]Phenyl 4-chlorophenyl ether.
The difenoconazole is an intermediate for producing difenoconazole, and is prepared by using 3, 4-dichlorodiphenyl ether as a starting material through three steps of acylation, condensation and cyclization. The equation for the phenyl ether ketone reaction is:
in the existing chemical production, the difenoconazole intermediate is usually produced by the method, and a difenoconazole product is obtained through salifying reaction, etherification reaction, washing, Friedel-crafts reaction, ice decomposition, washing, distillation and the like. In the production process of the phenyl ether ketone, wastewater is generated in the production process, the wastewater contains pollutants such as COD (chemical oxygen demand), SS (suspended solid), m-dichlorobenzene and the like, and contains refractory substances due to complex components. The production method has low process controllability and is not environment-friendly, byproducts are easy to generate, the product purity is low, and meanwhile, the operation is complex, and the method is not beneficial to industrial production.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defects in the prior art, and aims to provide a production device of a difenoconazole intermediate, which has the advantages of safe and efficient production method, simple operation, high yield and chemical selectivity, less pollutant discharge, lower production cost and suitability for industrial production.
The utility model discloses a realize above-mentioned technical purpose, provide following technical scheme: a production device of a difenoconazole intermediate comprises an overhead tank, a kettle body, an acylation condenser and a phenylate ketone receiving tank, wherein the overhead tank comprises an acetyl chloride overhead tank and an acylation material overhead tank;
furthermore, a feed port and a pressure gauge are arranged at the upper part of the phenyl ether ketone synthesis kettle, and the feed end of the feed port is connected with a distributor;
furthermore, an acylation condenser is further arranged at the upper part of the phenyl ether ketone synthesis kettle, the acylation condenser is provided with a chilled water inlet and a chilled water outlet, an acylation material transferring pump is arranged on a connecting pipeline of the phenyl ether ketone synthesis kettle and an acylation material elevated tank, the lower part of the hydrolysis kettle is connected with an aluminum chloride wastewater tank and an ethane layer primary receiving tank, an ethane layer primary material transferring pump is arranged on a connecting pipeline of the ethane layer primary receiving tank and the washing kettle, an ethane layer secondary receiving tank is connected at the lower part of the washing kettle, and the washing kettle is sequentially connected with the ethane layer secondary receiving tank, the ethane layer secondary material transferring pump and the phenyl ether ketone receiving tank;
furthermore, a cooling jacket is arranged on the peripheral wall of the kettle body;
further, the cooling jacket is provided with a cooling medium inlet and a cooling medium outlet;
furthermore, an acetyl chloride diaphragm pump is arranged on the acetyl chloride head tank;
furthermore, the phenyl ether ketone synthesis kettle, the hydrolysis kettle and the washing kettle are all provided with stirrers which are respectively a synthesis kettle stirrer, a hydrolysis kettle stirrer and a washing kettle stirrer, and the synthesis kettle stirrer, the hydrolysis kettle stirrer and the washing kettle stirrer are all composed of three U-shaped stirring fans;
further, the pressure gauge is a diaphragm pressure gauge;
furthermore, the distributor is a circular distributor and forms an included angle of 60 degrees with the horizontal plane;
furthermore, the distributor is provided with triangular distribution holes;
furthermore, thermometers are arranged on the right sides of the top ends of the phenyl ether ketone synthesis kettle, the hydrolysis kettle and the washing kettle.
Owing to adopted above technique, the utility model discloses compare with prior art, it is showing the advantage and is:
1) the utility model adopts the synthesis kettle, the hydrolysis kettle and the washing kettle which are connected in series, can realize semi-continuous operation, complete one-step salifying reaction and improve the reaction rate;
2) the utility model discloses difenoconazole intermediate apparatus for producing production stability is good, and production cycle is short, and simple process pollutes few energy consumption low grade advantage, is suitable for industrial production.
3) The distributor 22 of the utility model is a circular distributor and is arranged at an included angle of 60 degrees with the horizontal plane, thus effectively avoiding the blockage of the distributor and realizing uniform dispersion;
4) the utility model has simple integral structure, simple and convenient operation among devices, safety, controllability and environmental protection;
drawings
FIG. 1 is a schematic view of the structure of a production apparatus for a difenoconazole intermediate;
FIG. 2 is a schematic view of the partial structure of the present invention;
FIG. 3 is a schematic view of a distributor according to the present invention;
in the figure: 1-acetyl chloride elevated tank, 11-acetyl chloride diaphragm pump, 2-phenyl ether ketone synthesis kettle, 21-synthesis kettle stirrer, 22-distributor, 221-distribution hole, 23-feeding port, 24-sampling port, 25-synthesis kettle temperature meter, 26-diaphragm pressure gauge, 27-synthesis kettle cooling jacket, 3-acylation condenser, 31-chilled water inlet, 32-chilled water outlet, 4-acylation material elevated tank, 41-acylation transferring pump, 5-hydrolysis kettle, 51-hydrolysis kettle stirrer, 52-hydrolysis kettle thermometer, 53-hydrolysis kettle cooling jacket, 54-aluminum chloride waste water tank, 55-ethane layer primary receiving tank, 56-ethane layer primary transferring pump, 6-water washing kettle, 61-water washing kettle stirrer, 62-a washing kettle thermometer, 63-a washing kettle cooling jacket, 64-an ethane layer secondary receiving tank, 65-an ethane layer secondary transfer pump and 7-phenyl ether ketone receiving tank.
Detailed Description
In order to make the technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to specific embodiments, but the scope of the present invention is not limited thereto.
Example 1
As shown in fig. 1, the present invention provides the following technical solutions to achieve the above technical objectives: the utility model provides a apparatus for producing of difenoconazole midbody, includes overhead tank, the cauldron body, acylation condenser 3, phenyl ether ketone receiving tank 7, the overhead tank include acetyl chloride overhead tank 1, acylation material overhead tank 4, the cauldron body include phenyl ether ketone synthetic kettle 2, hydrolysis kettle 5, washing kettle 6, acetyl chloride overhead tank 1, phenyl ether ketone synthetic kettle 2, acylation material overhead tank 4, hydrolysis kettle 5, washing kettle 6, phenyl ether ketone receiving tank 7 loop through the pipeline and link to each other, and process flow includes friedel-crafts reaction, ice and tear, the layering that stews, washing etc..
Be provided with acetyl chloride diaphragm pump 11 on acetyl chloride elevated tank 1, thereby the round trip of 11 main diaphragm pumps that rely on a diaphragm pieces of acetyl chloride changes the studio volume and inhales and discharge liquid, and acetyl chloride diaphragm pump 11 can be according to the change control acetyl chloride flow of exit resistance, and 11 small, the simple installation economy of acetyl chloride diaphragm pump in addition is portable material delivery pump.
The upper part of the phenyl ether ketone synthesis kettle 2 is provided with a feeding port 23, a pressure gauge and a sampling port 24, the pressure gauge is a diaphragm pressure gauge 26, the diaphragm pressure gauge 26 is connected with equipment through a flange, and the pressure gauge is the diaphragm pressure gauge 26 and has the characteristics of convenient connection, difficult accumulation of precipitate, corrosion resistance, high temperature resistance, convenient cleaning and the like; a sample can be withdrawn through the sampling port 24 for analysis.
The feeding end of the feeding port 23 is connected with a distributor 22, the distributor 22 is a circular distributor and forms an included angle of 60 degrees with the horizontal plane, in the Friedel-crafts reaction process, a catalyst needs to be fed downwards through the feeding port 23 and is fed downwards to the phenyl ether ketone synthesis kettle 2 through the distributor 22, triangular distribution holes 221 are formed in the distributor 22,the catalyst can be uniformly distributed, for example, AlCl catalyst is used in the reaction process3Uniform dispersion can be achieved by the distributor 22.
An acylation condenser 3 is further arranged at the upper part of the phenyl ether ketone synthesis kettle 2, the acylation condenser 3 is provided with a chilled water inlet 31 and a chilled water outlet 32, an acylation material transfer pump 41 is arranged on a connecting pipeline of the phenyl ether ketone synthesis kettle 2 and the acylation material head tank 4, the lower part of the hydrolysis kettle is connected with an aluminum chloride wastewater tank 54 and an ethane layer primary receiving tank 55, an ethane layer primary receiving tank 56 is arranged on a connecting pipeline of the ethane layer primary receiving tank 55 and the washing kettle 6, and the lower part of the washing kettle 6 is sequentially connected with an ethane layer secondary receiving tank 64, an ethane layer secondary material transfer pump 65 and a phenyl ether ketone receiving tank 7;
the peripheral wall of the kettle body is provided with a cooling jacket which comprises a synthesis kettle cooling jacket 27, a hydrolysis kettle cooling jacket 53 and a water washing kettle cooling jacket 63, each cooling jacket is provided with an inlet and an outlet, and the internal cooling medium is cold brine.
The synthetic cauldron 2 of phenyl ether ketone, hydrolysis kettle 5, washing cauldron 6 all are provided with the agitator, are synthetic cauldron agitator 21, hydrolysis kettle agitator 51, washing cauldron agitator 61 respectively, synthetic cauldron agitator 21, hydrolysis kettle agitator 51, washing cauldron agitator 61 constitute by three "U" type stirring fan, can be with each material misce bene. Thermometers are respectively arranged on the right sides of the top ends of the phenyl ether ketone synthesis kettle 2, the hydrolysis kettle 5 and the washing kettle 6, and are respectively a synthesis kettle thermometer 25, a hydrolysis kettle thermometer 52 and a washing kettle thermometer 63.
The specific operation flow is as follows:
adding the measured 3, 4-dichlorodiphenyl ether and dichloroethane into the phenyl ether ketone synthesis kettle 2, stirring by using a synthesis kettle stirrer 21, adding aluminum trichloride (catalyst) through a feeding port 23, continuously stirring uniformly, controlling the temperature to be about 50 ℃, controlling the flow rate by using an acetyl chloride diaphragm pump 11, dropwise adding acetyl chloride in an acetyl chloride head tank into the phenyl ether ketone synthesis kettle 2, and preserving heat for 2 hours after dropwise adding; and then introducing the reaction liquid into an acylation condenser 3, introducing chilled water through a chilled water inlet, returning from a chilled water outlet, controlling the temperature to be not more than 30 ℃, then introducing into an acylation material head tank 4, then introducing into a hydrolysis kettle 5, standing for layering, separating out and separating aluminum trichloride hexahydrate in a water layer into an aluminum chloride wastewater tank 54, adding the separated aluminum trichloride into a concentration kettle, heating to about 105 ℃, concentrating, cooling, crystallizing, and centrifugally recovering an aluminum trichloride hexahydrate byproduct.
The organic layer was washed with water, and the washing vessel 6 was sealed during washing. Washing with water to neutrality, standing for layering, and separating out the wastewater. Distilling the organic layer, controlling the temperature to be about 85 ℃ and the pressure to be-0.09 MPa, removing dichloroethane to an ethane layer secondary receiving tank 64, and obtaining a crude product to a phenylate ketone receiving tank 7.
The above-mentioned embodiments are merely preferred technical solutions of the present invention, and should not be regarded as limitations of the present invention, and the protection scope of the present invention should be protected by the technical solutions described in the claims, and equivalent alternatives including technical features in the technical solutions described in the claims are also within the protection scope of the present invention.
Claims (9)
1. The production device of the difenoconazole intermediate is characterized by comprising an elevated tank, a kettle body, an acylation condenser and a phenylate ketone receiving tank, wherein the elevated tank comprises an acetyl chloride elevated tank and an acylation material elevated tank;
the upper part of the phenylate ketone synthesis kettle is provided with a feed port and a pressure gauge, the feed port is connected with a blanking end and a distributor, the upper part of the phenylate ketone synthesis kettle is further provided with an acylation condenser, the acylation condenser is provided with a chilled water inlet and a chilled water outlet, an acylation material transferring pump is arranged on a connecting pipeline of the phenylate ketone synthesis kettle and an acylation material elevated tank, the lower part of the hydrolysis kettle is connected with an aluminum chloride waste water tank and an ethane layer one-level receiving tank, the connecting pipeline of the ethane layer one-level receiving tank and the washing kettle is provided with an ethane layer one-level material transferring pump, the lower part of the washing kettle is connected with an ethane layer two-level receiving tank, and the washing kettle is sequentially connected with the ethane layer two-level receiving tank, the ethane layer two-level material transferring pump and the phenylate ketone receiving tank.
2. The apparatus for producing a difenoconazole intermediate as claimed in claim 1, wherein a cooling jacket is provided on the peripheral wall of the vessel.
3. The apparatus for producing a difenoconazole intermediate according to claim 2, wherein the cooling jacket is provided with a cooling medium inlet and a cooling medium outlet.
4. The apparatus for producing a difenoconazole intermediate as claimed in claim 1, wherein an acetyl chloride diaphragm pump is provided on the acetyl chloride head tank.
5. The apparatus for producing a difenoconazole intermediate according to claim 1, wherein the difenoconazole synthesis kettle, the hydrolysis kettle and the washing kettle are provided with stirrers, respectively a synthesis kettle stirrer, a hydrolysis kettle stirrer and a washing kettle stirrer, and each of the synthesis kettle stirrer, the hydrolysis kettle stirrer and the washing kettle stirrer is composed of three "U" -shaped stirring fans.
6. The apparatus for producing a difenoconazole intermediate as claimed in claim 1, wherein the pressure gauge is a diaphragm pressure gauge.
7. The apparatus for producing a difenoconazole intermediate according to claim 1, wherein the distributor is a circular distributor and is arranged at an angle of 60 ° with the horizontal plane.
8. The apparatus for producing a difenoconazole intermediate as claimed in claim 1, wherein the distributor is provided with triangular distribution holes.
9. The apparatus for producing a difenoconazole intermediate as claimed in claim 1, wherein thermometers are arranged on the right side of the top of the difenoconazole synthesis kettle, the hydrolysis kettle and the washing kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022785525.4U CN214183071U (en) | 2020-11-26 | 2020-11-26 | Production device for difenoconazole intermediate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022785525.4U CN214183071U (en) | 2020-11-26 | 2020-11-26 | Production device for difenoconazole intermediate |
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| Publication Number | Publication Date |
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| CN214183071U true CN214183071U (en) | 2021-09-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202022785525.4U Active CN214183071U (en) | 2020-11-26 | 2020-11-26 | Production device for difenoconazole intermediate |
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| CN (1) | CN214183071U (en) |
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- 2020-11-26 CN CN202022785525.4U patent/CN214183071U/en active Active
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