CN116459783A - Preparation method of difenoconazole - Google Patents
Preparation method of difenoconazole Download PDFInfo
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- CN116459783A CN116459783A CN202310520801.XA CN202310520801A CN116459783A CN 116459783 A CN116459783 A CN 116459783A CN 202310520801 A CN202310520801 A CN 202310520801A CN 116459783 A CN116459783 A CN 116459783A
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- reciprocating screw
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- difenoconazole
- driving
- pipe
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- 239000005760 Difenoconazole Substances 0.000 title claims abstract description 56
- BQYJATMQXGBDHF-UHFFFAOYSA-N difenoconazole Chemical compound O1C(C)COC1(C=1C(=CC(OC=2C=CC(Cl)=CC=2)=CC=1)Cl)CN1N=CN=C1 BQYJATMQXGBDHF-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000012535 impurity Substances 0.000 claims abstract description 59
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000011343 solid material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000012043 crude product Substances 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 78
- 230000007246 mechanism Effects 0.000 claims description 76
- 238000007789 sealing Methods 0.000 claims description 57
- 238000000926 separation method Methods 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 25
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 15
- 230000000903 blocking effect Effects 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000011344 liquid material Substances 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011265 semifinished product Substances 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 5
- 230000006835 compression Effects 0.000 claims description 4
- 238000007906 compression Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000575 pesticide Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000007363 ring formation reaction Methods 0.000 description 3
- 241000233866 Fungi Species 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 2
- 238000005893 bromination reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000006266 etherification reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 150000003852 triazoles Chemical class 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OILXMJHPFNGGTO-UHFFFAOYSA-N (22E)-(24xi)-24-methylcholesta-5,22-dien-3beta-ol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(C)C(C)C)C1(C)CC2 OILXMJHPFNGGTO-UHFFFAOYSA-N 0.000 description 1
- RQOCXCFLRBRBCS-UHFFFAOYSA-N (22E)-cholesta-5,7,22-trien-3beta-ol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CCC(C)C)CCC33)C)C3=CC=C21 RQOCXCFLRBRBCS-UHFFFAOYSA-N 0.000 description 1
- XMCRWEBERCXJCH-UHFFFAOYSA-N 1-(2,4-dichlorophenyl)ethanone Chemical compound CC(=O)C1=CC=C(Cl)C=C1Cl XMCRWEBERCXJCH-UHFFFAOYSA-N 0.000 description 1
- WXNZTHHGJRFXKQ-UHFFFAOYSA-N 4-chlorophenol Chemical compound OC1=CC=C(Cl)C=C1 WXNZTHHGJRFXKQ-UHFFFAOYSA-N 0.000 description 1
- OQMZNAMGEHIHNN-UHFFFAOYSA-N 7-Dehydrostigmasterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CC(CC)C(C)C)CCC33)C)C3=CC=C21 OQMZNAMGEHIHNN-UHFFFAOYSA-N 0.000 description 1
- DNVPQKQSNYMLRS-NXVQYWJNSA-N Ergosterol Natural products CC(C)[C@@H](C)C=C[C@H](C)[C@H]1CC[C@H]2C3=CC=C4C[C@@H](O)CC[C@]4(C)[C@@H]3CC[C@]12C DNVPQKQSNYMLRS-NXVQYWJNSA-N 0.000 description 1
- 241000221785 Erysiphales Species 0.000 description 1
- 206010039509 Scab Diseases 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000017858 demethylation Effects 0.000 description 1
- 238000010520 demethylation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- DNVPQKQSNYMLRS-SOWFXMKYSA-N ergosterol Chemical compound C1[C@@H](O)CC[C@]2(C)[C@H](CC[C@]3([C@H]([C@H](C)/C=C/[C@@H](C)C(C)C)CC[C@H]33)C)C3=CC=C21 DNVPQKQSNYMLRS-SOWFXMKYSA-N 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229940090668 parachlorophenol Drugs 0.000 description 1
- 229960004063 propylene glycol Drugs 0.000 description 1
- 150000003431 steroids Chemical class 0.000 description 1
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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/28—Moving reactors, e.g. rotary drums
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D405/00—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom
- C07D405/02—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing two hetero rings
- C07D405/06—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing two hetero rings linked by a carbon chain containing only aliphatic carbon atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a preparation method of difenoconazole, which relates to the technical field of pesticide raw material preparation, and is realized by preparation equipment of difenoconazole. According to the invention, the mixed solution of the p-toluene and the difenoconazole crude product is not required to be washed while removing the water-soluble impurities, and the water-soluble impurities can be synchronously dried and output during subsequent drying of the solid materials, so that the water resource is saved, the preparation cost of the difenoconazole is reduced, the treatment difficulty of the water-soluble impurities is reduced, and the method is more suitable for industrial production of the difenoconazole.
Description
Technical Field
The invention relates to the technical field of pesticide raw material preparation, in particular to a preparation method of difenoconazole.
Background
The difenoconazole is a novel high-efficiency triazole fungicide, is a steroid demethylation inhibitor, has the characteristics of high efficiency, broad spectrum, low toxicity and low dosage, has a unique action mechanism, and mainly inhibits the biosynthesis of cell ergosterol, thereby destroying the cell structure and function, and can prevent and treat scab, powdery mildew, leaf spot and rust caused by pathogenic bacteria such as fungi and fungi imperfecti on various crops.
The invention patent of the issued publication number CN 102898422B discloses a preparation method of difenoconazole, which comprises the steps of cyclization reaction, bromination reaction, condensation reaction and etherification reaction which are sequentially carried out, wherein: the cyclization reaction is to make 2, 4-dichloro acetophenone and 1, 2-propylene glycol react in a solvent in the presence of an acid catalyst to generate ketal; the bromination reaction is to drop liquid bromine into a system after the cyclization reaction, so that brominated ketal is generated by the reaction; the condensation reaction is to make brominated ketal react with triazole potassium in solvent N, N-dimethylformamide to generate methyl cycloazole; the etherification reaction is to make the difenoconazole react with the potassium parachlorophenol in a solvent at the temperature of 100-180 ℃ to generate the difenoconazole.
However, the preparation method has some defects found by the practical application of the technical personnel in the field, and obviously, in order to remove water-soluble impurities in the crude difenoconazole when the crude difenoconazole is refined, the mixed solution of the p-toluene and the crude difenoconazole is required to be subjected to water washing operation after the crude difenoconazole is dissolved by the toluene, so that a large amount of water resources are consumed in the water washing process, the preparation cost of the difenoconazole is increased, a large amount of cleaning wastewater is generated, the preparation cost of the difenoconazole is further increased by the subsequent treatment of the cleaning wastewater, and the preparation method is not effectively applicable to the industrial production of the difenoconazole.
Therefore, it is necessary to invent a preparation method of difenoconazole to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of difenoconazole, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the difenoconazole is realized by the preparation equipment of the difenoconazole, the preparation equipment of the difenoconazole comprises a reaction kettle, a driving mechanism is arranged in the reaction kettle, a first separating mechanism, a second separating mechanism, a filtering mechanism and a drying impurity removing mechanism are sequentially arranged outside the driving mechanism from top to bottom, and an inner cavity of the reaction kettle is divided into an upper cavity, a middle cavity and a lower cavity by the second separating mechanism and the filtering mechanism;
the driving mechanism comprises a reciprocating screw, a driving motor, a sealing box, a hot air input pipe, a discharging hole and an air inlet hole;
the reciprocating screw is arranged inside the reaction kettle in a penetrating manner and is in rotary connection with the reaction kettle through a bearing, the driving motor is fixedly arranged at the bottom of the reaction kettle and is in transmission connection with the reciprocating screw, the sealing box is arranged at the bottom end outside the reciprocating screw in a rotary sleeving manner through the bearing and is fixedly connected with the reaction kettle, the hot air input pipe is fixedly arranged on the right side of the sealing box in a penetrating manner, two discharging holes are formed, the two discharging holes are respectively formed in the tops of two sides of the reciprocating screw, and the air inlet hole is formed in the bottom of the back of the reciprocating screw;
the first separation mechanism comprises a reaction cylinder, a separation hole, a sealing sleeve and an extension rod;
the reaction cylinder is rotatably nested to be arranged at the top of the reaction kettle through a bearing and fixedly sleeved on the outer side of the reciprocating screw rod, a plurality of separation holes are formed, the separation holes are uniformly formed in the bottom of the outer side of the reaction cylinder, the sealing sleeve is slidably sleeved on the outer side of the reaction cylinder, two extension rods are arranged, and the two extension rods are respectively fixedly arranged on two sides of the bottom of the sealing sleeve.
Preferably, the second separation mechanism comprises a guide hopper, a guide pipe, a plugging plate, a first spring and a driving plate.
Preferably, the water conservancy diversion fill, stand pipe, shutoff board, first spring and drive plate cup joint in proper order from top to bottom and set up in the reciprocating screw outside, the water conservancy diversion is fought fixedly and is set up in the inboard middle part of reation kettle, the inside heating resistor that is provided with of water conservancy diversion fill, the stand pipe is fixed to be set up in the water conservancy diversion fill bottom, the shutoff board slides and cup joints in the reciprocating screw outside and carries out the shutoff to the stand pipe bottom, first spring one end and shutoff board fixed connection and the other end and drive plate fixed connection, drive plate and reciprocating screw pass through reciprocating screw drive connection, the extension rod slides and runs through the water conservancy diversion fill and with drive plate fixed connection.
Preferably, the filtering mechanism comprises a filter plate, a rotating block, a push plate, a sliding rod, a top ring and an annular plate.
Preferably, the filter plate is fixedly arranged in the middle of the inner side of the reaction kettle, the rotary block is fixedly sleeved on the outer side of the reciprocating screw and is rotationally arranged on the inner side of the filter plate through a bearing, a plurality of push plates are arranged on the outer side of the rotary block uniformly and fixedly, a plurality of sliding rods are arranged on the sliding rods uniformly and slidably penetrate through the top of the rotary block, the top ring is slidably sleeved on the outer side of the reciprocating screw and fixedly connected with a plurality of sliding rods, and the annular plate is slidably sleeved on the outer side of the reciprocating screw and fixedly arranged at the bottom ends of the sliding rods.
Preferably, the drying and impurity removing mechanism comprises a hollow disc, a second spring, a sealing sleeve, a connecting column and an impurity removing pipe.
Preferably, the hollow disc slides along the vertical direction and sets up in reation kettle inner chamber bottom and seals up the filter plate, the annular plate rotates nested setting in hollow disc top through the bearing, hollow disc top evenly fixed nest is provided with a plurality of valves, the second spring is provided with two, two the second spring is fixed connection respectively in hollow disc bottom both sides, the sealing sleeve sliding sleeve sets up in the reciprocating screw outside and sets up in hollow disc bottom through the bearing rotation sleeve, the spliced pole is provided with two, two the spliced pole slides nested setting respectively in the inside both sides of reciprocating screw and all with sealing sleeve fixed connection, the edulcoration pipe is fixed to be set up between two spliced poles, the edulcoration pipe bottom runs through the seal box and extends to the seal box bottom, the sealing pipe is fixed to cup joint and is set up in the sealing box outside top and slide and inside the reciprocating screw, the shutoff pipe is to the discharge opening.
Preferably, the preparation method specifically comprises the following steps:
s1, adding a difenoconazole crude product and toluene into the inner part of a reaction cylinder from an opening at the top of the reaction cylinder, adding propanol, triethylamine and a crystallization aid BPO into a middle chamber through a pipeline at the side surface of the reaction kettle, simultaneously starting a driving motor, driving a reciprocating screw to continuously rotate after the driving motor is started, and gradually dissolving the difenoconazole crude product into toluene to form a solution in the rotating process of the reciprocating screw, wherein water-soluble impurities insoluble in toluene remain in the solution;
s2, driving the driving plate to continuously descend when the reciprocating screw rod rotates, gradually releasing compression on the plugging plate when the driving plate descends, simultaneously driving the sealing sleeve to descend through the extension rod, and releasing plugging of the separation hole on the reaction cylinder by the sealing sleeve when the descending distance of the driving plate reaches a first threshold value, wherein under the continuous rotation of the reaction cylinder, the solution in the reaction cylinder passes through the separation hole to be output, and water-soluble impurities insoluble in toluene remain in the reaction cylinder;
s3, outputting the solution and then falling the solution on the top of the guide hopper, continuously heating the solution by a heating resistor in the guide hopper, evaporating toluene in the solution to obtain a difenoconazole semi-finished product, and manually condensing and recycling the evaporated toluene at the top opening of the reaction cylinder;
s4, when the descending distance of the driving plate reaches a second threshold value, the toluene is completely steamed, the plugging plate is driven by the driving plate and the first spring to remove the plugging of the opening at the bottom of the guide pipe, then the difenoconazole semi-finished product at the top of the guide hopper penetrates through the guide pipe and falls into propanol, triethylamine and crystallization auxiliary agent BPO in the middle chamber, and the reciprocating screw drives a plurality of pushing plates to stir the mixed solution through the rotating block;
s5, when the descending distance of the driving plate reaches a third threshold value, the bottom of the driving plate is contacted with the top of the top ring, the driving plate pushes the hollow disc through the top ring, the sliding rod and the annular plate along with the continuous descending of the driving plate, the hollow disc descends to compress the second spring, the blocking of the filter plate is relieved, liquid materials at the top of the filter plate penetrate through the filter plate and enter the lower chamber, then the liquid materials are output, and the solid materials remain at the top of the filter plate;
s6, when the hollow disc descends, the impurity removing pipe is driven to synchronously descend through the sealing sleeve and the connecting column, when the impurity removing pipe descends, the plugging pipe is driven to synchronously descend, when the descending distance of the driving plate reaches a fourth threshold value, liquid materials are all output, meanwhile, the hollow disc is sleeved outside the air inlet hole, the plugging pipe synchronously unblocks the discharge hole, then hot air input pipe and hot air input into the reciprocating screw through the sealing box enter the hollow disc through the air inlet hole, then the valve is opened, and solid materials at the top of the filter plate are dried through the filter plate, so that a difenoconazole finished product is prepared;
s7, the hot air flow continues to move upwards after drying the solid materials, then enters the reaction cylinder through the separation hole, dries the water-soluble impurities in the reaction cylinder, enters the impurity removing pipe through the discharging hole, and is output and collected through the impurity removing pipe;
and S8, when the descending distance of the driving plate reaches a fifth threshold value, the driving plate moves to the bottommost end of the outer side reciprocating thread of the reciprocating screw rod, and then the driving plate moves upwards to reset along with the continuous movement of the reciprocating screw rod.
The invention has the technical effects and advantages that:
according to the invention, the driving mechanism, the first separating mechanism, the second separating mechanism, the filtering mechanism and the drying impurity removing mechanism are arranged, so that the driving mechanism is used for driving the second separating mechanism, the second separating mechanism is used for triggering the first separating mechanism, the first separating mechanism is used for removing the blocking of the first separating mechanism, then under the driving of the driving mechanism, the first separating mechanism inputs the solution into the second separating mechanism and simultaneously separates the water-soluble impurities, then the second separating mechanism driven by the driving mechanism inputs the semi-finished difenoconazole into the solvent of the middle cavity after the solution is evaporated, after the treatment is finished, the second separating mechanism triggers the drying impurity removing mechanism through the filtering mechanism, so that the filtering mechanism is used for completing the filtering of the solid material, and the drying impurity removing mechanism is used for drying and outputting the solid material and the water-soluble impurities along with the extension of the triggering time of the drying impurity removing mechanism.
Drawings
Fig. 1 is a schematic diagram of the overall front sectional structure of the present invention.
Fig. 2 is a schematic cross-sectional elevation view of a first separating mechanism according to the present invention.
Fig. 3 is a schematic cross-sectional front view of a second separation mechanism according to the present invention.
Fig. 4 is a schematic cross-sectional front view of the filter mechanism of the present invention.
Fig. 5 is a schematic diagram showing a cross-sectional front view of the drying and impurity removing mechanism of the present invention.
In the figure: 1. a reaction kettle; 2. a driving mechanism; 21. a reciprocating screw; 22. a driving motor; 23. a seal box; 24. a hot air input pipe; 25. a discharge hole; 26. an air inlet hole; 3. a first separation mechanism; 31. a reaction cylinder; 32. a separation hole; 33. a sealing sleeve; 34. an extension rod; 4. a second separation mechanism; 41. a diversion bucket; 42. a guide tube; 43. a plugging plate; 44. a first spring; 45. a driving plate; 5. a filtering mechanism; 51. a filter plate; 52. a rotating block; 53. a push plate; 54. a slide bar; 55. a top ring; 56. an annular plate; 6. a drying and impurity removing mechanism; 61. a hollow disc; 62. a second spring; 63. sealing the sleeve; 64. a connecting column; 65. a impurity removing pipe; 66. the tube was plugged.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The invention provides a preparation method of difenoconazole, which is shown in figures 1-5, wherein the preparation method of difenoconazole is realized by preparation equipment of difenoconazole, the preparation equipment of difenoconazole comprises a reaction kettle 1, a driving mechanism 2 is arranged in the reaction kettle 1, a first separating mechanism 3, a second separating mechanism 4, a filtering mechanism 5 and a drying and impurity removing mechanism 6 are sequentially arranged outside the driving mechanism 2 from top to bottom, and the inner cavity of the reaction kettle 1 is divided into an upper cavity, a middle cavity and a lower cavity by the second separating mechanism 4 and the filtering mechanism 5.
As shown in fig. 2, fig. 4 and fig. 5, the driving mechanism 2 comprises a reciprocating screw 21, a driving motor 22, a sealing box 23, a hot air input pipe 24, discharge holes 25 and air inlet holes 26, wherein the reciprocating screw 21 is penetrated and arranged in the reaction kettle 1 and is rotationally connected with the reaction kettle 1 through a bearing, the driving motor 22 is fixedly arranged at the bottom of the reaction kettle 1 and is in transmission connection with the reciprocating screw 21, the sealing box 23 is rotationally sleeved and arranged at the bottom of the outer side of the reciprocating screw 21 and is fixedly connected with the reaction kettle 1 through a bearing, the hot air input pipe 24 is fixedly penetrated and arranged on the right side of the sealing box 23, the two discharge holes 25 are arranged, the two discharge holes 25 are respectively arranged at the tops of two sides of the reciprocating screw 21, and the air inlet holes 26 are arranged at the bottom of the back of the reciprocating screw 21.
As shown in fig. 2, the first separation mechanism 3 includes a reaction cylinder 31, separation holes 32, a sealing sleeve 33 and an extension rod 34, where the reaction cylinder 31 is rotatably nested at the top of the reaction kettle 1 through a bearing and fixedly sleeved at the outer side of the reciprocating screw 21, the separation holes 32 are provided with a plurality of separation holes 32 uniformly formed at the bottom of the outer side of the reaction cylinder 31, the sealing sleeve 33 is slidably sleeved at the outer side of the reaction cylinder 31, the extension rod 34 is provided with two extension rods, and the two extension rods 34 are respectively fixedly arranged at two sides of the bottom of the sealing sleeve 33.
As shown in fig. 3, the second separation mechanism 4 includes a guide funnel 41, a guide tube 42, a blocking plate 43, a first spring 44 and a driving plate 45, where the guide funnel 41, the guide tube 42, the blocking plate 43, the first spring 44 and the driving plate 45 are sequentially sleeved on the outer side of the reciprocating screw 21 from top to bottom, the guide funnel 41 is fixedly arranged in the middle of the inner side of the reaction kettle 1, a heating resistor is arranged in the guide funnel 41, the guide tube 42 is fixedly arranged at the bottom end of the guide funnel 41, the blocking plate 43 is slidably sleeved on the outer side of the reciprocating screw 21 and blocks the bottom end of the guide tube 42, one end of the first spring 44 is fixedly connected with the blocking plate 43, the other end of the first spring is fixedly connected with the driving plate 45, the driving plate 45 is in transmission connection with the reciprocating screw 21 through reciprocating threads, and the extension rod 34 is slidably penetrating the guide funnel 41 and is fixedly connected with the driving plate 45.
By arranging the first separation mechanism 3 and the second separation mechanism 4 so as to drive the driving plate 45 to continuously descend when the reciprocating screw 21 rotates, gradually releasing the compression of the plugging plate 43 when the driving plate 45 descends and simultaneously driving the sealing sleeve 33 to descend through the extension rod 34, when the descending distance of the driving plate 45 reaches a first threshold value, the sealing sleeve 33 releases the plugging of the separation hole 32 on the reaction cylinder 31, and at the moment, under the continuous rotation of the reaction cylinder 31, the solution inside the reaction cylinder 31 is output through the separation hole 32, and water-soluble impurities insoluble in toluene remain inside the reaction cylinder 31.
As shown in fig. 4 and 5, the filtering mechanism 5 includes a filter plate 51, a rotating block 52, a pushing plate 53, sliding rods 54, a top ring 55 and an annular plate 56, wherein the filter plate 51 is fixedly disposed in the middle of the inner side of the reaction kettle 1, the rotating block 52 is fixedly sleeved on the outer side of the reciprocating screw 21 and is rotatably disposed on the inner side of the filter plate 51 through a bearing, the pushing plate 53 is provided with a plurality of uniformly fixed rollers disposed on the outer side of the rotating block 52, the sliding rods 54 are provided with a plurality of uniformly sliding rods 54, the top ring 55 is slidably sleeved on the outer side of the reciprocating screw 21 and is fixedly connected with the sliding rods 54, and the annular plate 56 is slidably sleeved on the outer side of the reciprocating screw 21 and is fixedly disposed at the bottom ends of the sliding rods 54.
Through setting up above-mentioned structure to in the reciprocating screw rod 21 rotation in-process drive a plurality of push plates 53 through rotatory piece 52 and rotate, and then stir the material, follow-up solid material is dried simultaneously afterwards, along with the rotation of push plate 53, the push plate 53 promotes the solid material to the position that is close to the discharge gate and removes.
As shown in fig. 4 and fig. 5, the drying and impurity removing mechanism 6 includes a hollow disc 61, a second spring 62, a sealing sleeve 63, a connecting column 64 and an impurity removing tube 65, wherein the hollow disc 61 is slidably disposed at the bottom of the inner cavity of the reaction kettle 1 along the vertical direction and is fixedly connected with the sealing sleeve 63, the annular plate 56 is rotatably nested and disposed at the top of the hollow disc 61 through a bearing, a plurality of valves are uniformly and fixedly nested at the top of the hollow disc 61, two second springs 62 are disposed at two, the second springs 62 are fixedly connected to two sides of the bottom of the hollow disc 61, the sealing sleeve 63 is slidably sleeved and disposed at the outer side of the reciprocating screw 21 and rotatably sleeved and disposed at the bottom of the hollow disc 61 through the bearing, the connecting column 64 is disposed at two connecting columns 64 and is fixedly connected with the sealing sleeve 63, the impurity removing tube 65 is fixedly disposed between the two connecting columns 64, the bottom of the impurity removing tube 65 penetrates through the sealing box 23 and extends to the bottom of the sealing box 23, the sealing sleeve 66 is fixedly disposed at the top of the impurity removing tube 65 and is rotatably sleeved and disposed at the outer side of the reciprocating screw 21, and the discharging hole is plugged and sealed by the sealing sleeve 25.
By arranging the driving mechanism 2, the filtering mechanism 5 and the drying and impurity removing mechanism 6 so that the hollow disc 61 descends to compress the second spring 62 and simultaneously unblock the filter plate 51, liquid materials at the top of the filter plate 51 pass through the filter plate 51 and enter the lower chamber and are then output, solid materials remain at the top of the filter plate 51, in addition, the hollow disc 61 descends while driving the impurity removing pipe 65 through the sealing sleeve 63 and the connecting column 64, the impurity removing pipe 65 descends while driving the blocking pipe 66 while descending, when the hollow disc 61 is sheathed outside the air inlet 26, the blocking pipe 66 synchronously unblocks the discharge hole 25, hot air input pipe 24 and the sealing box 23 input into the reciprocating screw 21 enter the hollow disc 61 through the air inlet 26 and then wash out the valve and pass through the filter plate 51 to dry solid materials at the top of the filter plate 51, thereby obtaining difenoconazole finished products, the hot air continues to move upwards after drying the solid materials, the hot air enters the inside the reaction cylinder 31 through the separating hole 32, water-soluble impurities inside the reaction cylinder 31 are dried, the discharged water-soluble impurities enter the impurity removing pipe 65 through the impurity removing pipe 65 after drying, and the discharged water-soluble impurities enter the inside the impurity removing pipe 65 through the impurity removing pipe 65.
Example 2
The preparation method specifically comprises the following steps:
s1, adding a difenoconazole crude product and toluene into a reaction cylinder 31 from the top opening of the reaction cylinder 31 in the year, adding propanol, triethylamine and a crystallization aid BPO into a middle chamber through a pipeline on the side surface of a reaction kettle 1, simultaneously starting a driving motor 22, driving a reciprocating screw 21 to continuously rotate after the driving motor 22 is started, and gradually dissolving the difenoconazole crude product into toluene to form a solution in the rotating process of the reciprocating screw 21, wherein water-soluble impurities insoluble in toluene remain in the solution;
s2, driving the driving plate 45 to continuously descend when the reciprocating screw 21 rotates, gradually releasing the compression of the plugging plate 43 when the driving plate 45 descends, simultaneously driving the sealing sleeve 33 to descend through the extension rod 34, and releasing the plugging of the separation hole 32 on the reaction cylinder 31 by the sealing sleeve 33 when the descending distance of the driving plate 45 reaches a first threshold value, wherein under the continuous rotation of the reaction cylinder 31, the solution in the reaction cylinder 31 passes through the separation hole 32 to be output, and water-soluble impurities insoluble in toluene remain in the reaction cylinder 31;
s3, outputting the solution, then, placing the solution at the top of the guide hopper 41, continuously heating the solution by a heating resistor in the guide hopper 41, evaporating toluene in the solution to obtain a difenoconazole semi-finished product, and manually condensing and recycling the evaporated toluene at the top opening of the reaction cylinder 31;
s4, when the descending distance of the driving plate 45 reaches a second threshold value, the toluene is completely steamed, and simultaneously the plugging plate 43 is driven by the driving plate 45 and the first spring 44 to release the plugging of the bottom opening of the guide pipe 42, and then the difenoconazole semi-finished product at the top of the guide bucket 41 passes through the guide pipe 42 and falls into propanol, triethylamine and crystallization auxiliary agent BPO in the middle chamber, and the reciprocating screw 21 drives the plurality of pushing plates 53 to stir the mixed solution through the rotating block 52;
s5, when the descending distance of the driving plate 45 reaches a third threshold value, the bottom of the driving plate 45 is contacted with the top of the top ring 55, then the driving plate 45 pushes the hollow disc 61 through the top ring 55, the sliding rod 54 and the annular plate 56 along with the continuous descending of the driving plate 45, the hollow disc 61 descends to compress the second spring 62, meanwhile, the blocking of the filter plate 51 is relieved, liquid materials at the top of the filter plate 51 pass through the filter plate 51 to enter the lower chamber and then are output, and solid materials remain at the top of the filter plate 51;
s6, when the hollow disc 61 descends, the impurity removing pipe 65 is driven to synchronously descend through the sealing sleeve 63 and the connecting column 64, the plugging pipe 66 is driven to synchronously descend when the impurity removing pipe 65 descends, when the descending distance of the driving plate 45 reaches a fourth threshold value, liquid materials are all output, meanwhile, the hollow disc 61 is sleeved on the outer side of the air inlet hole 26, at the moment, the plugging pipe 66 synchronously releases plugging of the discharge hole 25, then hot air input pipe 24 and the hot air input pipe 23 input into the reciprocating screw 21 enter the hollow disc 61 through the air inlet hole 26, then a valve is opened by flushing and solid materials at the top of the filter plate 51 are dried by passing through the filter plate 51, and a difenoconazole finished product is prepared;
s7, the hot air flow continues to move upwards after drying the solid materials, then enters the reaction cylinder 31 through the separation hole 32, dries the water-soluble impurities in the reaction cylinder 31, enters the impurity removing pipe 65 through the discharging hole 25, and is output and collected through the impurity removing pipe 65;
and S8, when the descending distance of the driving plate 45 reaches a fifth threshold value, the driving plate 45 moves to the bottommost end of the outer side reciprocating thread of the reciprocating screw rod 21, and then the driving plate 45 moves upwards to reset along with the continuous movement of the reciprocating screw rod 21.
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.
Claims (8)
1. A preparation method of difenoconazole is characterized in that: the preparation method of the difenoconazole is realized by the preparation equipment of the difenoconazole, the preparation equipment of the difenoconazole comprises a reaction kettle (1), a driving mechanism (2) is arranged in the reaction kettle (1), a first separating mechanism (3), a second separating mechanism (4), a filtering mechanism (5) and a drying impurity removing mechanism (6) are sequentially arranged outside the driving mechanism (2) from top to bottom, and the inner cavity of the reaction kettle (1) is divided into an upper cavity, a middle cavity and a lower cavity by the second separating mechanism (4) and the filtering mechanism (5);
the driving mechanism (2) comprises a reciprocating screw (21), a driving motor (22), a sealing box (23), a hot air input pipe (24), a discharging hole (25) and an air inlet hole (26);
the reciprocating screw (21) is arranged inside the reaction kettle (1) in a penetrating manner and is rotationally connected with the reaction kettle (1) through a bearing, the driving motor (22) is fixedly arranged at the bottom of the reaction kettle (1) and is in transmission connection with the reciprocating screw (21), the sealing box (23) is sleeved at the bottom end outside the reciprocating screw (21) in a rotating manner through the bearing and is fixedly connected with the reaction kettle (1), the hot air input pipe (24) is fixedly arranged on the right side of the sealing box (23) in a penetrating manner, the two discharging holes (25) are formed, the two discharging holes (25) are respectively formed in the tops of two sides of the reciprocating screw (21), and the air inlet hole (26) is formed in the bottom of the back of the reciprocating screw (21);
the first separation mechanism (3) comprises a reaction cylinder (31), a separation hole (32), a sealing sleeve (33) and an extension rod (34);
the reaction cylinder (31) rotates the nested setting in reation kettle (1) top and fixed sleeve joint in reciprocating screw (21) outside through the bearing, separation hole (32) are provided with a plurality ofly, a plurality of separation hole (32) are evenly offered in reaction cylinder (31) outside bottom, sealed sleeve (33) slip sleeve sets up in reaction cylinder (31) outside, extension rod (34) are provided with two, two extension rod (34) are fixed respectively and are set up in sealed sleeve (33) bottom both sides.
2. The method for preparing difenoconazole according to claim 1, wherein: the second separation mechanism (4) comprises a guide hopper (41), a guide pipe (42), a blocking plate (43), a first spring (44) and a driving plate (45).
3. The method for preparing difenoconazole according to claim 2, wherein: the utility model provides a flow guide fill (41), stand pipe (42), shutoff board (43), first spring (44) and drive plate (45) cup joint in proper order from top to bottom in the reciprocating screw (21) outside, flow guide fill (41) are fixed to be set up in reation kettle (1) inboard middle part, inside heating resistor that is provided with of flow guide fill (41), stand pipe (42) are fixed to be set up in flow guide fill (41) bottom, shutoff board (43) slide cup joint set up in reciprocating screw (21) outside and to carry out the shutoff to stand pipe (42) bottom, first spring (44) one end and shutoff board (43) fixed connection and other end and drive plate (45) fixed connection, drive plate (45) are connected through reciprocating screw (21) transmission, extension rod (34) slip run through flow guide fill (41) and with drive plate (45) fixed connection.
4. A process for the preparation of difenoconazole as claimed in claim 3, wherein: the filtering mechanism (5) comprises a filter plate (51), a rotating block (52), a push plate (53), a sliding rod (54), a top ring (55) and an annular plate (56).
5. The method for preparing difenoconazole according to claim 4, wherein: the utility model discloses a filter plate, including rotatory piece (52), rotatory piece (52) are fixed to be cup jointed in the reciprocating screw (21) outside and rotate through the bearing and set up in filter plate (51) inboard, push pedal (53) are provided with a plurality of and even fixed settings in rotatory piece (52) outside, slide bar (54) are provided with a plurality of, a plurality of slide bar (54) evenly slip runs through and sets up in rotatory piece (52) top, top ring (55) slip cup joint set up in reciprocating screw (21) outside and with a plurality of slide bar (54) fixed connection, annular plate (56) slip cup joint set up in reciprocating screw (21) outside and fixed settings in a plurality of slide bar (54) bottom.
6. The method for preparing difenoconazole according to claim 5, wherein: the drying impurity removing mechanism (6) comprises a hollow disc (61), a second spring (62), a sealing sleeve (63), a connecting column (64) and an impurity removing pipe (65).
7. The method for preparing difenoconazole according to claim 6, wherein: the utility model provides a sealing device for sealing a discharge hole of a reactor, including hollow dish (61), sealing sleeve (63) and sealing sleeve (66), hollow dish (61) are slided along vertical direction and are set up in reation kettle (1) inner chamber bottom and carry out the shutoff to filter plate (51), annular plate (56) rotate the nestification through the bearing and set up in hollow dish (61) top, hollow dish (61) top evenly fixed nestification is provided with a plurality of valves, second spring (62) are provided with two, second spring (62) are fixed connection respectively in hollow dish (61) bottom both sides, sealing sleeve (63) slip cup joint set up in reciprocating screw (21) outside and through the bearing rotation set up in hollow dish (61) bottom, spliced pole (64) are provided with two spliced pole (64) slip nestification respectively set up in reciprocating screw (21) inside both sides and all with sealing sleeve (63) fixed connection, edulcoration pipe (65) fixed set up between two spliced pole (64), sealing box (23) are run through to sealing box (23) bottom, sealing sleeve (66) are fixed to be set up in reciprocating screw (65) outside and sealing sleeve (25) slip top (25).
8. The preparation method of difenoconazole as recited in claim 7, wherein said preparation method comprises the steps of:
s1, adding a difenoconazole crude product and toluene into a reaction cylinder (31) from the top opening of the reaction cylinder (31) in the year, adding propanol, triethylamine and a crystallization aid BPO into a middle chamber through a pipeline on the side surface of the reaction kettle (1), simultaneously starting a driving motor (22), driving a reciprocating screw (21) to continuously rotate after the driving motor (22) is started, and gradually dissolving the difenoconazole crude product into toluene to form a solution in the rotating process of the reciprocating screw (21), wherein water-soluble impurities insoluble in toluene remain in the solution;
s2, driving a driving plate (45) to continuously descend when a reciprocating screw (21) rotates, gradually releasing compression on a blocking plate (43) when the driving plate (45) descends, simultaneously driving a sealing sleeve (33) to descend through an extension rod (34), and releasing blocking of a separation hole (32) on a reaction cylinder (31) by the sealing sleeve (33) when the descending distance of the driving plate (45) reaches a first threshold value, wherein under the continuous rotation of the reaction cylinder (31), a solution in the reaction cylinder (31) passes through the separation hole (32) to be output, and water-soluble impurities insoluble in toluene remain in the reaction cylinder (31);
s3, outputting the solution, then, putting the solution on the top of a guide hopper (41), continuously heating the solution by a heating resistor in the guide hopper (41), evaporating toluene in the solution to obtain a difenoconazole semi-finished product, and manually condensing and recycling the evaporated toluene at the top opening of a reaction cylinder (31);
s4, when the descending distance of the driving plate (45) reaches a second threshold value, the toluene is completely steamed, the plugging plate (43) is driven by the driving plate (45) and the first spring (44) to remove the plugging of the bottom opening of the guide pipe (42), and then the difenoconazole semi-finished product at the top of the guide hopper (41) passes through the guide pipe (42) and falls into propanol, triethylamine and crystallization auxiliary agent BPO in the middle chamber, and the reciprocating screw (21) drives a plurality of pushing plates (53) to stir the mixed solution through the rotating block (52);
s5, when the descending distance of the driving plate (45) reaches a third threshold value, the bottom of the driving plate (45) is contacted with the top of the top ring (55), then the driving plate (45) is pushed by the top ring (55), the sliding rod (54) and the annular plate (56) along with the continuous descending of the driving plate (45), the hollow plate (61) descends to compress the second spring (62), the blocking of the filter plate (51) is relieved, the liquid material at the top of the filter plate (51) passes through the filter plate (51) to enter the lower chamber and is then output, and the solid material remains at the top of the filter plate (51);
s6, when the hollow disc (61) descends, the impurity removing pipe (65) is driven to synchronously descend through the sealing sleeve (63) and the connecting column (64), the plugging pipe (66) is driven to synchronously descend when the impurity removing pipe (65) descends, when the descending distance of the driving plate (45) reaches a fourth threshold value, liquid materials are all output, meanwhile, the hollow disc (61) is sleeved on the outer side of the air inlet hole (26), at the moment, the plugging pipe (66) synchronously releases plugging of the discharging hole (25), then hot air input pipe (24) and hot air input into the reciprocating screw (21) through the sealing box (23) enter the hollow disc (61) through the air inlet hole (26), then a valve is opened by flushing, and solid materials at the top of the filter plate (51) are dried through the filter plate (51), so that a difenoconazole finished product is obtained;
s7, enabling the hot air flow to continuously move upwards after drying the solid materials, enabling the hot air flow to enter the reaction cylinder (31) through the separation hole (32), drying water-soluble impurities in the reaction cylinder (31), enabling the dried water-soluble impurities to enter the impurity removing pipe (65) through the discharging hole (25), and then outputting and collecting the impurities through the impurity removing pipe (65);
and S8, when the descending distance of the driving plate (45) reaches a fifth threshold value, the driving plate (45) moves to the bottommost end of the outer side reciprocating thread of the reciprocating screw rod (21), and then the driving plate (45) moves upwards to reset along with the continuous movement of the reciprocating screw rod (21).
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| CN116983911A (en) * | 2023-09-25 | 2023-11-03 | 河北彩客新材料科技股份有限公司 | Continuous preparation device and preparation method for biphenyl tetracarboxylic dianhydride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116983911A (en) * | 2023-09-25 | 2023-11-03 | 河北彩客新材料科技股份有限公司 | Continuous preparation device and preparation method for biphenyl tetracarboxylic dianhydride |
| CN116983911B (en) * | 2023-09-25 | 2024-01-02 | 河北彩客新材料科技股份有限公司 | Continuous preparation device and preparation method for biphenyl tetracarboxylic dianhydride |
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