CN215464449U - Tower reactor for preparing prothioconazole - Google Patents
Tower reactor for preparing prothioconazole Download PDFInfo
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- CN215464449U CN215464449U CN202121333990.2U CN202121333990U CN215464449U CN 215464449 U CN215464449 U CN 215464449U CN 202121333990 U CN202121333990 U CN 202121333990U CN 215464449 U CN215464449 U CN 215464449U
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Abstract
The utility model relates to a tower reactor for preparing prothioconazole, which comprises a tower kettle, a packed tower, a condenser and a circulating pump, wherein the tower kettle, the packed tower and the condenser are sequentially arranged from bottom to top and are communicated with each other. The tower reactor is suitable for synthesizing prothioconazole, materials can be fully contacted and reacted through the matching of material circulation, the packed tower and the condenser, and the reaction efficiency and the yield of prothioconazole are greatly improved; the device has simple structure and is particularly suitable for industrial production of prothioconazole.
Description
Technical Field
The utility model relates to a tower reactor, in particular to a tower reactor for preparing prothioconazole.
Background
Prothioconazole is a novel broad-spectrum triazolethione bactericide developed by Bayer companies, is mainly used for preventing and treating a plurality of diseases of cereals, wheat and bean crops and the like, has low toxicity, no teratogenicity, no mutation type, no toxicity to embryos and safety to people and environment.
The existing industrial production process mostly takes acetylbutyrolactone as a starting raw material to synthesize an intermediate 2- (1-chloro-cyclopropyl-1-yl) -1- (2-chloro-phenyl) -2-hydroxy-3-1, 2, 4-triazolidine-5-thion-1-yl) -propane, and then the intermediate is oxidized with an oxidant to obtain a target product, wherein the oxidant can be ferric trichloride, oxygen, air and the like. The air is used as the oxidant, so the cost is low, the raw materials are easy to obtain, three wastes are not generated, and the method is very suitable for industrial production.
At present, although air is used as an oxidant to synthesize prothioconazole, the synthesis of prothioconazole involves two-phase or even three-phase reaction, the reaction system is relatively complex, the high yield of prothioconazole is difficult to directly obtain only by air oxidation, and the reaction is generally directly carried out in a tower kettle 1, so the reaction efficiency is low.
Disclosure of Invention
The utility model aims to provide a tower reactor for preparing prothioconazole.
In order to achieve the purpose, the utility model adopts the technical scheme that:
the utility model provides a tower reactor for preparing prothioconazole, which comprises a tower kettle for containing reaction raw materials and reaction products, a packed tower filled with packing, a condenser for cooling and refluxing evaporated reactants in a reaction system, and a circulating pump capable of conveying the materials in the tower kettle to the top of the packed tower;
one end of the packed tower is communicated with the tower kettle, the other end of the packed tower is communicated with the condenser, an inlet of the circulating pump is communicated with the tower kettle, and an outlet of the circulating pump is communicated with the top of the packed tower;
the tower kettle is provided with a feeding hole which can be used for introducing air, 2- (1-chloro-cyclopropyl-1-yl) -1- (2-chloro-phenyl) -2-hydroxy-3- (1, 2, 4-triazolidine-5-thion-1-yl) -propane, a catalyst and a diluent, and the tower kettle is also provided with a discharging hole which can be used for discharging prothioconazole.
Preferably, the tower kettle, the packed tower and the condenser are arranged from bottom to top, the bottom of the tower kettle and the top of the packed tower are further connected with a material circulating pipeline, the material circulating pipeline is provided with the circulating pump, and one end of the condenser, which is far away from the packed tower, is connected with an air outlet pipeline for discharging air in the reactor.
The synthesis of prothioconazole generally adopts a kettle-type reactor, and because of the strong oxidizing property of oxygen, prothioconazole prepared by the kettle-type reactor generally faces to the excessive oxidation of raw materials, so that the prepared prothioconazole has low yield. This application makes the material can be from up down in tower reactor, from last down constantly circulating through the circulating pump, and then makes the material fully react, simultaneously, utilizes the air pump condenser to cool off the material of evaporation constantly, makes its backward flow to the packed tower, avoids the material to evaporate and influences the reaction effect.
Preferably, the feed inlet is connected with an air source device for introducing air, the air source device comprises an air compressor, a filter for filtering impurities is installed at an air inlet of the air compressor, and an air flow regulating valve is installed at an air outlet of the air compressor.
The air is continuously fed through the air source device, so that materials in the filler are continuously and fully contacted with the air, the reaction time is shortened, and the reaction efficiency is improved.
Preferably, the tower reactor further comprises a first storage tank for storing the (2-chloro-phenyl) -2-hydroxy-3- (1, 2, 4-triazolidin-5-thione-1-yl) -propane, a second storage tank for storing the catalyst, a third storage tank for storing the diluent, and a fourth storage tank for receiving the prothioconazole, wherein the first storage tank, the second storage tank and the third storage tank are respectively communicated with the feeding hole, and the fourth storage tank is communicated with the discharging hole.
Preferably, the filler comprises one or more of metal filler, ceramic filler, glass filler, molecular sieve, activated carbon, diatomite and chromatographic silica gel.
Preferably, the filling height of the filling material filled in the filled tower is not lower than 2/3 of the total length of the tower body. The setting of this application filling height makes the raw materials can be by abundant oxidation and can not be by excessive oxidation when, and then improves prothioconazole's yield.
According to some preferred embodiments, a packing support device for supporting the packing is further installed in the packed tower.
Preferably, the packing support device is detachably connected with the packing tower.
Further preferably, the packing support device comprises a circular plate, the outer diameter of the circular plate is smaller than or equal to the inner diameter of the packing tower, and a plurality of through holes are formed in the circular plate.
Preferably, a stirrer for mixing and stirring materials is arranged in the tower kettle.
Further preferably, a heating jacket for heating and insulating the material is arranged outside the tower kettle.
Preferably, the outer periphery of the packed tower is provided with a heat insulation sleeve.
Due to the application of the technical scheme, compared with the prior art, the utility model has the following advantages: the tower reactor is suitable for synthesizing prothioconazole, materials can be fully contacted and reacted through the matching of material circulation, the packed tower and the condenser, and the reaction efficiency and the yield of prothioconazole are greatly improved; the device has simple structure and is particularly suitable for industrial production of prothioconazole.
Drawings
FIG. 1 is a schematic diagram of a tower reactor according to the present invention;
FIG. 2 is a schematic structural view of a packing support device according to the present invention;
in the above drawings: 1. a tower kettle; 2. a packed tower; 3. a circulation pump; 4. a condenser; 5. an air intake duct; 6. a material circulation pipeline; 7. an air outlet pipe; 8. a filler support means; 9. and a through hole.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the embodiments of the utility model. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
In the description of the embodiments of the present invention, it should be understood that the terms "upper", "lower", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in fig. 1, and are only used for convenience in describing the embodiments of the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have specific orientations, be constructed in specific orientations, and be operated, and thus, should not be construed as limiting the embodiments of the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the embodiments of the present invention, "a plurality" means two or more unless specifically limited otherwise.
In the embodiments of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," "fixed," and the like are to be construed broadly, e.g., as being fixedly connected, detachably connected, or integrated; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. Specific meanings of the above terms in the embodiments of the present invention can be understood by those of ordinary skill in the art according to specific situations.
In embodiments of the utility model, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may comprise the first and second features being in direct contact, or the first and second features being in contact, not directly, but via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly above and obliquely above the second feature, or simply meaning that the first feature is at a lesser level than the second feature.
The following disclosure provides many different embodiments or examples for implementing different configurations of embodiments of the utility model. To simplify the disclosure of embodiments of the utility model, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit embodiments of the utility model. Furthermore, embodiments of the present invention may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed.
The utility model will be further described with reference to examples of embodiments shown in the drawings to which the utility model is attached.
The tower reactor comprises a tower kettle 1, a packed tower 2, a condenser 4 and a circulating pump 3, wherein the tower kettle 1, the packed tower 2 and the condenser 4 are sequentially arranged from bottom to top and are communicated with each other.
A stirrer is arranged in the tower kettle 1, and the stirrer can be a magnetic stirrer or a stirring paddle.
The heating mode of the tower kettle 1 can be electromagnetic heating, infrared heating or resistance heating. For example, the column bottom 1 is heated and maintained at a constant temperature by fitting a heating jacket around the outer periphery of the column bottom 1. For another example, a resistance wire heating rod is arranged in the tower kettle 1, and the resistance wire heating rod is used for heating and insulating the tower kettle.
The first feed inlet has been seted up at the top of tower cauldron 1, and air can let in tower cauldron 1 through first feed inlet to from bottom to top through packed tower 2, react with the material in packed tower 2. Of course, in certain embodiments, the first inlet port may also be used to feed the reaction mass (2- (1-chloro-cyclopropyl-1-yl) -1- (2-chloro-phenyl) -2-hydroxy-3- (1, 2, 4-triazolidin-5-thione-1-yl) -propane, catalyst, diluent) and, after the reaction mass is complete, the first inlet port is used again to admit air. Or, the tower kettle 1 is provided with an opening specially used for feeding and discharging materials. In some embodiments, the opening is further connected to a first reservoir (not shown) for storing (2-chloro-phenyl) -2-hydroxy-3- (1, 2, 4-triazolidin-5-thione-1-yl) -propane, a second reservoir (not shown) for storing a catalyst, a third reservoir (not shown) for storing a diluent, and a fourth reservoir (not shown) for receiving prothioconazole. The valve and the transmission pump for controlling feeding and discharging can be arranged on the connecting pipelines of the first storage tank, the second storage tank, the third storage tank, the fourth storage tank and the tower kettle 1 according to actual needs.
Preferably, the first feeding hole is connected with an air inlet pipe 5, and air enters the tower kettle through the air inlet pipe 5. The air inlet pipe 5 is connected with an air source device (not shown in the figure), the air source device comprises an air compressor, a filter for filtering impurities is installed at an air inlet of the air compressor, and an air flow regulating valve is installed at an air outlet of the air compressor. The air can move from bottom to top uninterruptedly under the drive of the air source device and react with the materials in the packed tower 2. The gas source device may be a commercially available gas source device. In addition, the air inlet pipeline can also be connected with an air transmission pump, and air is continuously transmitted to the tower kettle through the air transmission pump.
Still set up the first discharge gate that is used for discharging prothioconazole on the tower cauldron 1, prothioconazole discharges through first discharge gate after the reaction finishes. The second discharge gate has still been seted up to the bottom of tower cauldron 1, and the second feed inlet has been seted up at the top of packed tower 2, and second discharge gate, second feed inlet are linked together through material circulating line 6 to be equipped with circulating pump 3 on the material circulating line 6, the material enters into the top of packed tower 2 from tower cauldron 1 through circulating pump 3, and top-down and air reaction. In some embodiments, a flow meter is further disposed on the material circulation pipeline 6 for monitoring and adjusting the flow rate of the material entering the packed tower 2.
The packed tower 2 can be directly connected to the tower kettle 1 or connected with the tower kettle 1 through a pipeline. And a filler supporting device 8 for supporting filler is further arranged in the filler tower 2, and the filler supporting device 8 can be fixedly connected with the filler tower 2 and can also be detachably connected with the filler tower 2. The packing supporting device 8 comprises a circular plate, the outer diameter of the circular plate is smaller than or equal to the inner diameter of the packing tower 2, and a plurality of through holes 81 which penetrate through the circular plate are formed in the circular plate, so that the materials can flow out conveniently. The circular plate is preferably a mesh plate, and the shape of the mesh on the mesh plate is not limited, as long as the filler in the filler tower 2 can be prevented from falling off, and the size of the mesh is also not limited.
In some embodiments, the outer periphery of the packed tower 2 is further wrapped with an insulation jacket, including but not limited to insulation cotton, for insulating the packed tower 2. In other embodiments, a heating device is arranged on the outer periphery of the packed tower 2, and the heating device can be a heating resistance wire or a heating jacket.
The filler filled in the packed tower 2 can be one or more of metal filler, ceramic filler, glass filler, molecular sieve, activated carbon, diatomite and chromatographic silica gel. When the filler is a metallic filler, the metal may be one or more of carbon steel, 304 stainless steel, 316 stainless steel, monel, and other alloys. The filling height of the filling material is not lower than 2/3 of the total length of the tower body.
And one end of the condenser 4 far away from the packed tower 2 is connected with an air outlet pipeline 7 for discharging air in the reactor. The condenser 4 may be a water-cooled condenser, for example, a vertical shell-and-tube condenser or a double-tube condenser.
The tower reactor can be used for preparing prothioconazole with high yield, the specific preparation process is as follows, and the material of the metal filler in the embodiment is 304L stainless steel.
10.00g (mass content is 83.0%) of 2- (1-chloro-cyclopropyl-1-yl) -1- (2-chloro-phenyl) -2-hydroxy-3-1, 2, 4-triazolidine-5-thione-1-yl) -propane, 40g of methanol and 0.6g of benzyl trimethyl ammonium chloride are put into a tower kettle 1, a stirrer is started for stirring, a heater outside the tower kettle 1 is started to heat materials in the tower kettle to 50 ℃, a circulating pump 3 is started to start material circulation, the materials enter a packed tower 2 filled with metal packing from bottom to top from the tower kettle 1, and air is introduced from a first feeding hole. After 4h, HLPC detection shows that the content of the raw materials is lower than 1%, and discharging. Methanol is removed at 70 ℃, 20g of toluene is added, and the mixture is cooled to room temperature for recrystallization, so that 8.17g (the mass content is 98.0%) of prothioconazole is obtained, and the molar yield is 97.1%.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A tower reactor for preparing prothioconazole, which is characterized in that: the tower reactor comprises a tower kettle (1) used for containing reaction raw materials and reaction products, a packed tower (2) filled with packing, a condenser (4) used for cooling and refluxing evaporated reactants in a reaction system, and a circulating pump (3) capable of conveying materials in the tower kettle (1) to the top of the packed tower (2);
one end of the packed tower (2) is communicated with the tower kettle (1), the other end of the packed tower (2) is communicated with the condenser (4), an inlet of the circulating pump (3) is communicated with the tower kettle (1), and an outlet of the circulating pump (3) is communicated with the top of the packed tower (2);
the tower kettle (1) is provided with a feeding hole for introducing air, 2- (1-chloro-cyclopropyl-1-yl) -1- (2-chloro-phenyl) -2-hydroxy-3- (1, 2, 4-triazolidine-5-thion-1-yl) -propane, a catalyst and a diluent, and the tower kettle (1) is also provided with a discharging hole for discharging prothioconazole.
2. The tower reactor for preparing prothioconazole of claim 1, wherein: the tower kettle (1), the packed tower (2), condenser (4) set up from bottom to top, the bottom of tower kettle (1) the top of packed tower (2) still is connected with material circulating line (6), be equipped with on material circulating line (6) circulating pump (3), condenser (4) are kept away from the one end of packed tower (2) is connected with pipeline (7) of giving vent to anger that is used for discharging the air in the reactor.
3. The column reactor for the preparation of prothioconazole according to claim 1 or 2, characterized in that: the feed inlet is connected with the air source device who is used for letting in the air, the air source device includes air compressor, the filter that is used for filtering impurity is installed to air compressor's air inlet, gas flow control valve is installed to air compressor's gas outlet.
4. The tower reactor for preparing prothioconazole of claim 1, wherein: the tower reactor further comprises a first storage tank for storing the (2-chloro-phenyl) -2-hydroxy-3- (1, 2, 4-triazolidine-5-thione-1-yl) -propane, a second storage tank for storing the catalyst, a third storage tank for storing the diluent and a fourth storage tank for receiving the prothioconazole, wherein the first storage tank, the second storage tank and the third storage tank are respectively communicated with the feeding hole, and the fourth storage tank is communicated with the discharging hole.
5. The tower reactor for preparing prothioconazole of claim 1, wherein: the filler comprises one or more of metal filler, ceramic filler, glass filler, molecular sieve, activated carbon, diatomite and chromatographic silica gel.
6. The column reactor for the preparation of prothioconazole according to claim 1 or 5, characterized in that: the filling height of the filler filled in the packed tower (2) is not lower than 2/3 of the total length of the tower body.
7. The tower reactor for preparing prothioconazole of claim 1, wherein: and a filler supporting device (8) for supporting the filler is further installed in the filler tower (2), and the filler supporting device (8) is detachably connected with the filler tower (2).
8. The tower reactor for preparing prothioconazole of claim 6, wherein: the packing supporting device (8) comprises a circular plate, the outer diameter of the circular plate is smaller than or equal to the inner diameter of the packing tower (2), and a plurality of through holes (81) are formed in the circular plate in a penetrating mode.
9. The tower reactor for preparing prothioconazole of claim 1, wherein: a stirrer for mixing and stirring the materials is arranged in the tower kettle (1).
10. The tower reactor for preparing prothioconazole of claim 1, wherein: a heating sleeve for heating and insulating the materials is sleeved outside the tower kettle (1); and/or a heat insulation sleeve is arranged on the outer peripheral side of the packed tower (2).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121333990.2U CN215464449U (en) | 2021-06-16 | 2021-06-16 | Tower reactor for preparing prothioconazole |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121333990.2U CN215464449U (en) | 2021-06-16 | 2021-06-16 | Tower reactor for preparing prothioconazole |
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| CN215464449U true CN215464449U (en) | 2022-01-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805228A (en) * | 2022-07-01 | 2022-07-29 | 江苏七洲绿色科技研究院有限公司 | Preparation method of prothioconazole |
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2021
- 2021-06-16 CN CN202121333990.2U patent/CN215464449U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805228A (en) * | 2022-07-01 | 2022-07-29 | 江苏七洲绿色科技研究院有限公司 | Preparation method of prothioconazole |
| CN114805228B (en) * | 2022-07-01 | 2022-09-27 | 江苏七洲绿色科技研究院有限公司 | Preparation method of prothioconazole |
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