Preparation system of pyraclostrobin

Abstract

The utility model discloses a pyraclostrobin preparation system which comprises a bromination reaction kettle, an etherification reaction kettle, a reduction device, an acylation device and a methylation device, and purification devices are arranged on a material conveying pipeline between the etherification reaction kettle and the reduction device and a material conveying pipeline of the methylation device. The purification device consists of an impurity removal crystallizing tank, a washing tank and a drying box, an ethanol storage cylinder is arranged on the side edge of the impurity removal crystallizing tank, a temperature control jacket is wrapped on the outer wall of the impurity removal crystallizing tank, and a filter box is further arranged on the side edge of the impurity removal crystallizing tank. According to the utility model, pyrazole benzyl ether generated by the etherification reaction kettle is put into the purification device for purification treatment, so that higher purity can be obtained, the content of impurities in subsequent products is reduced, and meanwhile, pyraclostrobin generated by reaction of the methylation device is also put into the purification device for purification treatment, so that the purity of pyraclostrobin is improved. The content of impurities in a finished product is further reduced, so that pyraclostrobin with higher purity is prepared and generated.

Description

Technical Field

[0001] The utility model relates to the technical field of pyraclostrobin preparation, in particular to a pyraclostrobin preparation system. Background Art

[0002] Pyraclostrobin is a methoxyacrylate fungicide that can prevent and treat plant diseases caused by Ascomycetes, Basidiomycetes, Deuteromycetes and Oomycetes, while also improving the plant's tolerance to the environment. According to its synthetic process characteristics, it is mainly divided into the first condensation route and the second condensation route. Regardless of the first condensation method or the second condensation method, the process involves two steps: bromination and etherification.

[0003] According to the patent document with application number 202322325289.1 retrieved from the patent website, a system for preparing pyraclostrobin is disclosed. A continuous passage for preparing pyraclostrobin is formed between a bromination reactor, a filtration device, a temporary storage tank for benzyl bromide organic phase, an etherification reactor, a centrifuge I, a washing tank, a drying device, a temporary storage barrel for pyrazole benzyl ether, a reduction device, an acylation device and a methylation device, thereby ensuring the continuity, sustainability and stability of the preparation process of pyraclostrobin.

[0004] However, no purification structure is provided in the preparation system, resulting in more internal impurities and lower purity of the pyraclostrobin produced.

[0005] Therefore, we propose a preparation system of pyraclostrobin to solve the above problems. Utility Model Content

[0006] The purpose of the utility model is to provide a preparation system of pyraclostrobin to solve the problems raised in the above background technology.

[0007] In order to achieve the above purpose, the utility model provides the following technical solutions:

[0008] A pyraclostrobin preparation system comprises a bromination reaction kettle, an etherification reaction kettle, a reduction device, an acylation device and a methylation device, wherein a purification device is provided on a feed pipeline between the etherification reaction kettle and the reduction device and on a feed pipeline of the methylation device, the purification device comprises an impurity removal crystallization tank, a washing tank and a drying box, and the impurity removal crystallization tank, the washing tank and the drying box are sequentially connected through a transmission pipeline;

[0009] An ethanol storage cylinder is provided on the side of the impurity removal crystallization tank, the input end of the ethanol storage cylinder is connected to the top of the impurity removal crystallization tank through a condenser, and the output end of the ethanol storage cylinder is connected to the inside of the impurity removal crystallization tank through a conveying pipeline, a temperature control jacket is wrapped on the outer wall of the impurity removal crystallization tank, and the temperature control jacket is respectively connected to a heating liquid cylinder and a cooling liquid cylinder through two groups of circulating conveying pipelines, a filter box is also provided on the side of the impurity removal crystallization tank, the bottom output end of the filter box is connected to the top input end of the impurity removal crystallization tank through a conveying pipeline, and the top input end of the filter box is connected to the bottom output end of the impurity removal crystallization tank through a conveying pipeline.

[0010] In a further embodiment, metering pumps are installed on the delivery pipelines from the etherification reaction kettle and the methylation device to the purification device respectively.

[0011] In a further embodiment, a metering pump is installed on the delivery pipeline from the ethanol storage cylinder to the impurity removal crystallization tank.

[0012] In a further embodiment, a stirring device is also provided inside the impurity removal crystallization tank.

[0013] In a further embodiment, a heating component and a temperature detector are provided inside the heating liquid cylinder.

[0014] In a further embodiment, a refrigeration component and a temperature detector are provided inside the coolant cylinder.

[0015] In a further embodiment, a circulation pump is installed on each of the heating liquid cylinder and the cooling liquid cylinder and the circulation delivery pipeline of the temperature control jacket.

[0016] In a further embodiment, solenoid valves are respectively installed on one end of the circulating delivery pipelines of the heating liquid cylinder and the cooling liquid cylinder close to the temperature control jacket.

[0017] Compared with the prior art, the beneficial effects of the utility model are:

[0018] The utility model puts the pyrazolyl benzyl ether generated by the etherification reaction kettle into a purification device for purification treatment, so that the pyrazolyl benzyl ether can obtain higher purity before being put into a reduction device for reaction, thereby reducing the content of impurities in subsequent products. At the same time, the pyraclostrobin generated by the methylation device reaction is also put into the purification device for purification treatment, which is beneficial to further reduce the impurity content in the finished product, so as to prepare and generate pyraclostrobin with higher purity. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a structural block diagram of the preparation system in the utility model;

[0020] Figure 2 It is a structural block diagram of the purification device in the utility model.

[0021] In the figure: 1. Bromination reactor; 2. Etherification reactor; 3. Reduction device; 4. Acylation device; 5. Methylation device; 6. Purification device; 61. Impurity removal crystallization tank; 611. Ethanol storage cylinder; 6111. Condenser; 612. Temperature control jacket; 6121. Heating liquid cylinder; 6122. Cooling liquid cylinder; 6123. Circulation pump; 6124. Solenoid valve; 613. Filter box; 62. Washing tank; 63. Drying box; 7. Heating component; 8. Refrigeration component; 9. Temperature detector. DETAILED DESCRIPTION

[0022] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention. In the description of the present invention, unless otherwise specified, "multiple" means two or more.

[0023] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installation", "connection" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood by specific circumstances.

[0024] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0025] See also Figure 1-2A system for preparing pyraclostrobin comprises a bromination reactor 1, an etherification reactor 2, a reduction device 3, an acylation device 4 and a methylation device 5. The reactions in the bromination reactor 1, the etherification reactor 2, the reduction device 3, the acylation device 4 and the methylation device 5 are consistent with the prior art. A purification device 6 is provided on the feed pipeline between the etherification reactor 2 and the reduction device 3 and on the feed pipeline of the methylation device 5, so that the pyrazolyl benzyl ether generated by the reaction in the etherification reactor 2 can be obtained by the purification device 6 before being put into the reduction device 3 for reaction. Similarly, the pyraclostrobin generated by the reaction in the methylation device 5 is also put into the purification device 6 for purification treatment, which is conducive to further reducing the impurity content in the finished product.

[0026] In order to facilitate the purification process, a purification device 6 is provided, which is composed of an impurity removal crystallization tank 61, a washing tank 62 and a drying box 63, and the impurity removal crystallization tank 61, the washing tank 62 and the drying box 63 are connected in sequence through a conveying pipeline. An ethanol storage cylinder 611 is provided on the side of the impurity removal crystallization tank 61, and ethanol is stored in the ethanol storage cylinder 611. The output end of the ethanol storage cylinder 611 is connected to the impurity removal crystallization tank 61 through a conveying pipeline, and then ethanol can be added to the impurity removal crystallization tank 61 to dissolve the pyrazolylbenzyl The input end of the ethanol storage cylinder 611 is connected to the top of the impurity removal crystallization tank 61 through a condenser 6111, so that when pyrazol benzyl ether or pyrazostrobin is crystallized, the ethanol is first volatilized, and the volatilized ethanol enters the condenser 6111 for condensation, so that it can be recovered into the ethanol storage cylinder 611 for reuse. The outer wall of the impurity removal crystallization tank 61 is wrapped with a temperature control jacket 612, and the temperature control jacket 612 is respectively connected to a heating liquid cylinder 6121 and a cooling liquid cylinder 6121 through two sets of independent circulation transmission pipelines. The cylinder 6122 allows the heating liquid cylinder 6121 and the cooling liquid cylinder 6122 to exchange liquids with the temperature control jacket 612 through their respective circulation pipelines. The heating liquid cylinder 6121 transports the heated liquid to the temperature control jacket 612, thereby driving the temperature inside the impurity removal crystallization tank 61 to rise, so as to accelerate the dissolution of pyrazolyl benzyl ether or pyraclostrobin, while the cooling liquid cylinder 6122 transports the cooled liquid to the temperature control jacket 612, thereby driving the temperature inside the impurity removal crystallization tank 61 to drop, so as to control the dissolution of pyrazolyl benzyl ether or pyraclostrobin. Or pyraclostrobin cooling crystallization, a filter box 613 is also provided on the side of the impurity removal crystallization tank 61, which is used to filter impurities in the dissolved liquid, and then remove insoluble impurities from the solution to achieve the effect of impurity removal and purification. The bottom output end of the filter box 613 is connected to the top input end of the impurity removal crystallization tank 61 through a conveying pipeline, and the top input end of the filter box 613 is connected to the bottom output end of the impurity removal crystallization tank 61 through a conveying pipeline, and centrifugal pumps are provided on the two conveying pipelines to provide transmission power for the conveyed liquid.

[0027] In order to improve the purification effect, the etherification reaction kettle 2 and the methylation device 5 are respectively provided with metering pumps on the delivery pipelines to the purification device 6. Correspondingly, the ethanol storage cylinder 611 is provided with a metering pump on the delivery pipeline to the impurity removal crystallization tank 61, so that pyrazolyl benzyl ether or pyraclostrobin and ethanol can be added to the impurity removal crystallization tank 61 in proportion, which is conducive to the full dissolution of pyrazolyl benzyl ether.

[0028] Furthermore, in order to accelerate the efficiency of impurity removal and purification, a stirring device is also provided inside the impurity removal crystallization tank 61. The stirring device is a stirring rod-like structure of conventional technology, which can help the product dissolve faster and more fully.

[0029] In order to facilitate more accurate control of the temperature of the impurity removal crystallization tank 61, a heating component 7 and a temperature detector 9 are provided inside the heating liquid cylinder 6121. The heating component 7 can adopt an electric heating rod or an electric heating block. The cooling liquid cylinder 6122 is provided inside with a refrigeration component 8 and a temperature detector 9. The refrigeration component 8 can adopt a semiconductor refrigeration sheet. Through the detection of the temperature detector 9, the heating or cooling temperature can be better controlled.

[0030] In order to prevent mutual interference between the two groups of circulation pipelines, a circulation pump 6123 is respectively installed on the circulation conveying pipeline of the heating liquid cylinder 6121 and the cooling liquid cylinder 6122 and the temperature control jacket 612, so that the circulation pump 6123 can be used to drive the liquid to circulate, thereby ensuring the uniformity of temperature. At the same time, an electromagnetic valve 6124 is respectively installed on the end of the circulation conveying pipeline of the heating liquid cylinder 6121 and the cooling liquid cylinder 6122 close to the temperature control jacket 612, so that when one of the heating liquid cylinder 6121 and the cooling liquid cylinder 6122 is supplying liquid, the electromagnetic valve 6124 on the circulation pipeline of the other one is closed, thereby preventing the cooling liquid and the heating liquid from mixing.

[0031] It is obvious to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be regarded as exemplary and non-restrictive from any point of view, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention. Any reference numeral in a claim should not be regarded as limiting the claim to which it relates.

[0032] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A system for preparing pyraclostrobin, comprising a bromination reactor (1), an etherification reactor (2), a reduction device (3), an acylation device (4) and a methylation device (5), characterized in that: A purification device (6) is provided on the feed pipeline between the etherification reaction kettle (2) and the reduction device (3) and the feed pipeline of the methylation device (5), wherein the purification device (6) is composed of an impurity removal crystallization tank (61), a washing tank (62) and a drying box (63), and the impurity removal crystallization tank (61), the washing tank (62) and the drying box (63) are sequentially connected through a transmission pipeline; An ethanol storage cylinder (611) is provided on the side of the impurity removal crystallization tank (61), the input end of the ethanol storage cylinder (611) is connected to the top of the impurity removal crystallization tank (61) through a condenser (6111), and the output end of the ethanol storage cylinder (611) is connected to the inside of the impurity removal crystallization tank (61) through a delivery pipeline, the outer wall of the impurity removal crystallization tank (61) is wrapped with a temperature control jacket (612), and the temperature control jacket (612) is respectively connected to a heating liquid cylinder (6121) and a cooling liquid cylinder (6122) through two groups of circulating delivery pipelines, and a filter box (613) is also provided on the side of the impurity removal crystallization tank (61), the bottom output end of the filter box (613) is connected to the top input end of the impurity removal crystallization tank (61) through a delivery pipeline, and the top input end of the filter box (613) is connected to the bottom output end of the impurity removal crystallization tank (61) through a delivery pipeline.

2. A system for preparing pyraclostrobin according to claim 1, characterized in that: The etherification reaction kettle (2) and the methylation device (5) are both equipped with metering pumps on the delivery pipelines to the purification device (6).

3. A system for preparing pyraclostrobin according to claim 1, characterized in that: A metering pump is installed on the delivery pipeline from the ethanol storage cylinder (611) to the impurity removal crystallization tank (61).

4. A system for preparing pyraclostrobin according to claim 1, characterized in that: The impurity removal crystallization tank (61) is also provided with a stirring device inside.

5. A system for preparing pyraclostrobin according to claim 1, characterized in that: The interior of the heating liquid cylinder (6121) is provided with a heating component (7) and a temperature detector (9).

6. A system for preparing pyraclostrobin according to claim 5, characterized in that: A refrigeration component (8) and a temperature detector (9) are provided inside the cooling liquid cylinder (6122).

7. A system for preparing pyraclostrobin according to claim 1, characterized in that: The heating liquid cylinder (6121) and the cooling liquid cylinder (6122) are each respectively provided with a circulation pump (6123) on the circulation delivery pipeline of the temperature control jacket (612).

8. A system for preparing pyraclostrobin according to claim 1, characterized in that: Solenoid valves (6124) are respectively installed on one end of the circulating delivery pipelines of the heating liquid cylinder (6121) and the cooling liquid cylinder (6122) close to the temperature control jacket (612).

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