Purification device for producing metconazole

Abstract

The application provides a purification device for metconazole production, comprising a reaction kettle, a first filter, an alkalization kettle, a desolventizing kettle, a crystallization kettle, a second filter and a product storage bin which are connected in series; the reaction kettle is further connected with a clean water storage tank and an acid metering pump; the first filter is further connected with a filtrate treatment device; the alkalization kettle is further connected with a toluene storage tank and an alkali metering pump; the desolventizing kettle is connected with the toluene storage tank through a condenser, and the condenser is further connected with a first vacuum unit and a first tail gas treatment device in sequence; and the crystallization kettle is further connected with a crystallization solvent storage tank. The device of the application is used in cooperation with the above-mentioned devices, and metconazole reaction liquid is purified in a mode of washing, acidification to form a salt, filtration, alkalization, desolventizing and crystallization to obtain a metconazole product with high purity, and the problem of large product loss in the prior art of purifying metconazole by using multiple recrystallization is overcome.

Description

Technical Field

[0001] This application relates to the field of pesticide production technology, and in particular to a purification device for the production of tebuconazole. Background Technology

[0002] Metconazole (trade name Caramba) is a triazole fungicide. As a novel broad-spectrum systemic fungicide, it possesses excellent protective and curative effects and is an inhibitor of C-14 demethylase in ergosterol biosynthesis. Although its mechanism of action is similar to other triazole fungicides, its activity differs significantly. Metconazole has a very broad fungicidal spectrum and excellent activity, showing remarkable effectiveness against *Nematocystis*, *Nematocystis*, and *Stenocystis* rusts in cereal crops when applied in the field. Compared to traditional fungicides, metconazole requires extremely low dosages while controlling a wide range of cereal diseases. It is suitable for crops such as wheat, barley, oats, rye, and triticale, exhibiting low toxicity to non-target organisms, requiring low dosages, and possessing high fungicidal activity. It is widely used in the pesticide industry.

[0003] There are multiple synthetic routes for tebuconazole. Regardless of the route used to synthesize tebuconazole, it must go through a purification stage. The current method is to purify it by recrystallization multiple times. However, due to the large number and complexity of impurities in the system after the synthesis of tebuconazole, the product loss is significant after recrystallization. Utility Model Content

[0004] This application provides a purification device for the production of tebuconazole, which solves the problem of significant product loss when using multiple recrystallization methods to purify tebuconazole.

[0005] This application provides a purification device for the production of tebuconazole, comprising a reaction vessel, a first filter, an alkalization vessel, a solvent removal vessel, a crystallization vessel, a second filter, and a product storage silo connected in series. The reactor is also connected to a clean water storage tank and an acid metering pump, respectively. The first filter is also connected to the filtrate treatment device; The alkalization reactor is also connected to a toluene storage tank and an alkali metering pump, respectively. The desolventizing vessel is connected to the toluene storage tank via a condenser, which is also connected in sequence to the first vacuum unit and the first tail gas treatment device. The crystallization vessel is also connected to a crystallization solvent storage tank.

[0006] Optionally, the second filter is also connected to the mother liquor treatment device; The mother liquor treatment unit is also connected to the crystallization kettle and the crystallization solvent storage tank, respectively.

[0007] Optionally, the mother liquor treatment device includes a concentration kettle, a second condenser, a second vacuum unit, and a second tail gas treatment device; The concentration vessel is connected to the second filter and the crystallization vessel, respectively. The second condenser is also connected to the crystallization solvent storage tank.

[0008] Optionally, the filtrate treatment device includes a filtrate storage tank, a reverse osmosis filter, and a freshwater storage tank connected in series. The reverse osmosis filter is also connected to the concentrate storage tank; A transfer pump is also installed between the filtrate storage tank and the reverse osmosis filter.

[0009] Optionally, the first filter includes a housing with an open top. The interior of the housing is divided into an upper filtration zone and a lower liquid receiving zone by an inclined perforated plate; A discharge port is provided on one side of the filtration zone, and the opening is located on the side where the orifice plate is at its lowest point. A drain outlet is provided on one side of the bottom of the liquid receiving area; A clamping structure is provided on the upper part of the perforated plate to clamp the filter cloth. The clamping structure is located on the other three sides of the filtration zone where there is no discharge port.

[0010] Optionally, the pressing structure includes a pressing strip and a pair of limiting blocks disposed at both ends of the pressing strip, the limiting blocks being fixedly connected to the inner wall of the filter area; An elastic block is connected to the bottom of the clamping strip, and the elastic block is set along the length of the clamping strip. The bottom of the limiting block has a limiting groove that matches the width of the clamping strip.

[0011] Optionally, the first exhaust gas treatment device is an adsorption tower or an incinerator.

[0012] This application provides a purification apparatus for the production of tebuconazole. Water is added to the reaction solution from the reaction mixture via a water storage tank to wash away salts. Dilute acid is then added to the reaction vessel via an acid metering pump to react the tebuconazole in the reaction solution into salts, which precipitate out. Simultaneously, a first filter separates the inorganic acid salts of tebuconazole. The separated inorganic acid salts are then added to an alkali treatment vessel, where alkali is added via an alkali metering pump to convert the inorganic acid salts back into tebuconazole. Toluene is added to a toluene storage tank for extraction. The extract is then transferred to a solvent removal vessel to remove the solvent. The solvent-removed tebuconazole is added to a crystallization vessel for crystallization. The crystallized liquid is then filtered using a second filter to obtain pure tebuconazole. This apparatus, through the combined use of the above-mentioned devices, purifies the tebuconazole reaction solution through washing, acidification to salt formation, filtration, alkali treatment, solvent removal, and crystallization to obtain a high-purity tebuconazole product. This overcomes the drawback of significant product loss associated with existing methods that involve multiple recrystallizations for purifying tebuconazole. Attached Figure Description

[0013] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0014] Figure 1 A schematic diagram of a purification apparatus for producing tebuconazole according to an embodiment of this application; Figure 2 A schematic diagram of a purification apparatus for producing tebuconazole according to another embodiment of this application; Figure 3 A schematic diagram of a purification apparatus for producing tebuconazole according to yet another embodiment of this application; Figure 4 This is a schematic diagram of a filtrate treatment apparatus provided in an embodiment of this application; Figure 5 A three-dimensional structural schematic diagram of a first filter provided in an embodiment of this application; Figure 6 A three-dimensional structural schematic diagram of the first filter provided in one embodiment of this application from another angle; Figure 7 This is a schematic diagram of a clamping structure provided in an embodiment of this application.

[0015] Explanation of reference numerals in the attached figures: 1. Reactor; 2. First filter; 3. Alkalization reactor; 4. Solvent removal reactor; 5. Crystallization reactor; 6. Second filter; 7. Product storage silo; 10. Acid metering pump; 11. Clean water storage tank; 20. Alkali metering pump; 21. Filtrate treatment device; 22. Shell; 31. Toluene storage tank; 41. Condenser; 42. First vacuum unit; 43. First tail gas treatment device; 51. Crystallization solvent storage tank; 61. Mother liquor treatment device; 210 211. Transfer pump; 212. Filtrate storage tank; 213. Reverse osmosis filter; 214. Freshwater storage tank; 225. Concentrated water storage tank; 226. Orifice plate; 227. Pressing structure; 618. Concentrator; 619. Second condenser; 610. Second vacuum unit; 611. Second tail gas treatment device; 2201. Drain outlet; 2202. Limiting groove; 2221. Pressing strip; 2222. Limiting block; 2223. Elastic pressure block. Detailed Implementation

[0016] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application are described clearly and completely below. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without creative effort are also within the scope of protection of this application.

[0017] like Figure 1 As shown, this application provides a purification device for the production of tebuconazole, comprising a reaction vessel 1, a first filter 2, an alkalization vessel 3, a solvent removal vessel 4, a crystallization vessel 5, a second filter 6, and a product storage silo 7 connected in series. The reactor 1 is also connected to the clean water storage tank 11 and the acid metering pump 10 respectively; The first filter 2 is also connected to the filtrate treatment device 21; The alkalization reactor 3 is also connected to the toluene storage tank 31 and the alkali metering pump 20, respectively; The desolventizing vessel 4 is connected to the toluene storage tank 31 via a condenser 41. The condenser 41 is also connected in sequence to the first vacuum unit 42 and the first tail gas treatment device 43. The crystallization vessel 5 is also connected to the crystallization solvent storage tank 51.

[0018] In operation, clean water from the clean water storage tank 11 is added to the quenched reaction solution in the reaction vessel 1 (the solvent used in the reaction process is a benzene-based solvent). Since the reaction solvent and water are immiscible, the mixture will separate into layers after the water is added. The water washes away the salts generated during the reaction process, i.e., after the reaction is quenched. Then, sulfuric acid aqueous solution (concentration of 10~15 wt%) is added to the reaction vessel 1 through the acid metering pump 10 to adjust the reaction system to acidity (pH 1~2). At this time, the tebuconazole in the reaction solution will form sulfate and precipitate from the organic solvent, and then precipitate in the aqueous solution (tebuconazole sulfate is also insoluble in water). The above steps can also be performed by washing away the salts in the reaction solution with clean water, draining the water layer, adding clean water again, and then performing the acid adjustment operation. The aqueous phase containing the tebuconazole sulfate precipitate is separated from the reaction vessel 1 and transferred to the first filter 2 for filtration.

[0019] The filtrate obtained from filtration is transferred to filtrate treatment device 21 for processing. The filter cake obtained from filtration, which is the sulfate of tebuconazole, is transferred to alkalization reactor 3. Toluene is added using toluene storage tank 31 (at this time, the sulfate of tebuconazole is insoluble in toluene). Then, alkali solution (an aqueous solution of sodium hydroxide or potassium hydroxide) is added to alkalization reactor 3 through alkali metering pump 20. Through acid-base neutralization, the sulfate of tebuconazole is converted into tebuconazole. At this time, the tebuconazole will gradually dissolve in toluene (that is, toluene acts as an extractant). The toluene layer is separated by liquid separation, and the aqueous phase is transferred to the corresponding wastewater treatment section for treatment (for example, it is combined with the filtrate treatment device 21 for treatment). The separated toluene layer is transferred to desolvation reactor 4 and desolvation is performed by first vacuum unit 42. The distilled toluene is condensed by first condenser 41 and transferred to toluene storage tank 31 for reuse. The non-condensable gases that cannot be condensed are transferred to first tail gas treatment device 43 through first vacuum unit 42 for harmless treatment (incineration or adsorption).

[0020] The crude tebuconazole obtained after solvent removal is added to crystallization vessel 5. Crystallization solvent (methylcyclohexanone is used in this application) is added to crystallization solvent storage tank 51 for crystallization. The resulting crystal-solvent mixture is transferred to the second filter 6 for filtration. The filter cake, which is pure tebuconazole, is transferred to product storage silo 7 for subsequent drying and packaging processes. The filtrate is processed separately for recovery.

[0021] This application provides a purification device for the production of tebuconazole. Water is added to the reaction solution via a water storage tank 11 to wash away salts. Dilute acid is added to the reaction vessel 1 via an acid metering pump 10 to react the tebuconazole in the reaction solution into salts, which then precipitate out. Simultaneously, a first filter 2 separates the inorganic acid salts of tebuconazole. The separated inorganic acid salts are then added to an alkali treatment vessel 3, where alkali is added via an alkali metering pump 20 to convert the inorganic acid salts of tebuconazole back into tebuconazole. Toluene is added to a toluene storage tank 31 for extraction. The extract is then transferred to a solvent removal vessel 4 to remove the solvent. The solvent-removed tebuconazole is added to a crystallization vessel 5 for crystallization. The crystallized liquid is then filtered using a second filter 6 to obtain pure tebuconazole. The apparatus described in this application, through the combined use of the aforementioned devices, purifies the tebuconazole reaction solution by washing, acidifying to salt, filtering, alkalizing, desolvating, and crystallizing to obtain a high-purity tebuconazole product. This overcomes the drawback of significant product loss when using existing methods of purifying tebuconazole through multiple recrystallizations.

[0022] like Figure 2 As shown, optionally, the second filter 6 is also connected to the mother liquor treatment device 61; The mother liquor treatment device 61 is also connected to the crystallization kettle 5 and the crystallization solvent storage tank 51, respectively.

[0023] In this application, the mother liquor treatment device 61 concentrates the filtered mother liquor, and the solvent obtained during the concentration process is recovered into the crystallization solvent storage tank 51, while the concentrated liquid is returned to the crystallization kettle 5.

[0024] like Figure 3 As shown, optionally, the mother liquor treatment device 61 includes a concentration vessel 611, a second condenser 612, a second vacuum unit 613, and a second tail gas treatment device 614. The concentration vessel 611 is connected to the second filter 6 and the crystallization vessel 5, respectively; The second condenser 612 is also connected to the crystallization solvent storage tank 51.

[0025] In this application, the filtrate obtained from the second filter 6, which is also the crystallization mother liquor, is transferred to the concentration vessel 611 and concentrated by vacuum distillation using the second vacuum unit 613. During the concentration process, the distilled solvent is condensed in the second condenser 612 and recovered to the crystallization solvent storage tank 51 for reuse. The non-condensable gases that fail to condense are transferred to the second tail gas treatment device 614 through the second vacuum unit 613 for harmless treatment (incineration or adsorption). The concentrated liquid is then returned to the crystallization vessel 5 to recrystallize with subsequent batches of tebuconazole.

[0026] like Figure 4 As shown, optionally, the filtrate treatment device 21 includes a filtrate storage tank 211, a reverse osmosis filter 212 and a freshwater storage tank 213 connected in series. The reverse osmosis filter 212 is also connected to the concentrate storage tank 214; A transfer pump 210 is also installed between the filtrate storage tank 211 and the reverse osmosis filter 212.

[0027] In this application, during use, the filtrate separated by the first filter 2 contains a large amount of organic matter and salt, so it is temporarily stored in the filtrate storage tank 211. After being pressurized by the transfer pump 210, it is transferred to the reverse osmosis filter 212 to filter out the organic matter, salt, etc. The output fresh water is stored in the fresh water storage tank 213, while the concentrated water is transferred to the concentrated water storage tank 214 for further purification treatment.

[0028] like Figure 5 and Figure 6 As shown, optionally, the first filter 2 includes a housing 22 with an open top; The housing 22 is divided into an upper filtration zone and a lower liquid receiving zone by an inclined perforated plate 221. A discharge port is provided on one side of the filtration zone, and the opening is located on the side where the orifice plate 221 is at its lowest point; A drain outlet 2201 is provided on one side of the bottom of the liquid receiving area; A pressing structure 222 is provided on the upper part of the perforated plate 221 for pressing the filter cloth. The pressing structure 222 is provided on the other three sides of the filtration zone where no discharge port is opened.

[0029] In this application, the tilt angle of the orifice plate 221 is 5~10°.

[0030] In this application, during use, filter cloth should be laid on the perforated plate 221 and fixed by the clamping structure 222. The aqueous phase mixed with the sulfate precipitate of tebuconazole is poured onto the filter cloth from a position away from the discharge port, and solid-liquid separation is achieved through filtration.

[0031] like Figure 7 As shown, optionally, the pressing structure 222 includes a pressing strip 2221 and a pair of limiting blocks 2222 disposed at both ends of the pressing strip 2221, the limiting blocks 2222 being fixedly connected to the inner wall of the filter area; The bottom of the clamping strip 2221 is connected to an elastic block 2223, which is arranged along the length of the clamping strip 2221. The bottom of the limiting block 2222 is provided with a limiting groove 2202 that matches the width of the pressing strip 2221.

[0032] In this application, it should be noted that the total thickness of the clamping strip 2221 and the elastic pressure block 2223 should be greater than the distance between the limiting groove 2202 and the perforated plate 221 (the specific value can be designed according to actual needs, such as 1.1 to 1.2 times the distance between the limiting groove 2202 and the perforated plate 221). This allows the filter cloth to be fixed in place by the elastic force generated by the elastic pressure block 2223 after compression during use. The elastic pressure block 2223 can be made of rubber or other elastic materials.

[0033] In this application, when laying the filter cloth, the filter cloth is laid flat on the upper surface of the perforated plate 221 and adhered to the perimeter of the perforated plate 221. The clamping strip 2221 is placed on the upper surface of the perforated plate 221 near the limiting block 2222. After pressing the clamping strip 2221 to compress the elastic block 2223, the clamping strip 2221 is inserted into the limiting groove 2202 by translation, thereby achieving the fastening of the filter cloth.

[0034] Optionally, the first exhaust gas treatment device 43 is an adsorption tower or an incinerator.

[0035] In this application, the first exhaust gas treatment device 43 is an adsorption tower or an incinerator, which can treat the exhaust gas to be harmless through incineration or adsorption, so as to avoid environmental pollution caused by exhaust gas emissions.

[0036] Optionally, the second exhaust gas treatment device 614 is an adsorption tower or an incinerator.

[0037] A purification device for the production of tebuconazole, the working process of which is as follows: In operation, clean water from the clean water storage tank 11 is added to the quenched reaction solution in the reaction vessel 1 (the solvent used in the reaction process is a benzene-based solvent). Since the reaction solvent and water are immiscible, the mixture will separate into layers after the water is added. The water washes away the salts generated during the reaction process, i.e., after the reaction is quenched. Then, sulfuric acid aqueous solution (concentration of 10~15 wt%) is added to the reaction vessel 1 through the acid metering pump 10 to adjust the reaction system to acidity (pH 1~2). At this time, the tebuconazole in the reaction solution will form sulfate and precipitate from the organic solvent, and then precipitate in the aqueous solution (tebuconazole sulfate is also insoluble in water). The above steps can also be performed by washing away the salts in the reaction solution with clean water, draining the water layer, adding clean water again, and then performing the acid adjustment operation. The aqueous phase containing the tebuconazole sulfate precipitate is separated from the reaction vessel 1 and transferred to the first filter 2 for filtration.

[0038] During filtration in the first filter 2, filter cloth should be laid on the perforated plate 221 and fixed by the clamping structure 222. The aqueous phase mixed with the sulfate precipitate of tebuconazole is poured onto the filter cloth from a position away from the discharge port, and solid-liquid separation is achieved through filtration. The separated filtrate contains a large amount of organic matter and salt, so it is temporarily stored in the filtrate storage tank 211. After being pressurized by the transfer pump 210, it is transferred to the reverse osmosis filter 212 to remove the organic matter, salt, etc. The output fresh water is stored in the fresh water storage tank 213, and the concentrated water is transferred to the concentrated water storage tank 214 for further purification treatment.

[0039] The filter cake obtained from filtration, which is the sulfate of tebuconazole, is transferred to the alkalization reactor 3. Toluene is added using the toluene storage tank 31 (at this point, the sulfate of tebuconazole is insoluble in toluene). Then, alkali solution (an aqueous solution of sodium hydroxide or potassium hydroxide) is added to the alkalization reactor 3 through the alkali metering pump 20. Through acid-base neutralization, the sulfate of tebuconazole is converted back to tebuconazole. At this time, the tebuconazole gradually dissolves in the toluene (that is, the toluene acts as an extractant). The toluene layer is separated by liquid separation, and the aqueous phase is transferred to the corresponding wastewater treatment section for treatment (for example, it is combined with the filtrate treatment device 21 for treatment). The separated toluene layer is transferred to the desolvation reactor 4 and desolvated under reduced pressure using the first vacuum unit 42. The distilled toluene is condensed by the first condenser 41 and transferred to the toluene storage tank 31 for reuse. The non-condensable gases that cannot be condensed are transferred to the first tail gas treatment device 43 through the first vacuum unit 42 for harmless treatment (incineration or adsorption).

[0040] The crude tebuconazole obtained after solvent removal is added to crystallization vessel 5. Crystallization solvent (methylcyclohexanone is used in this application) is added to crystallization solvent storage tank 51 for crystallization. The resulting crystal-solvent mixture is transferred to the second filter 6 for filtration. The filter cake, i.e., pure tebuconazole, is transferred to product storage silo 7 for subsequent drying and packaging processes. The filtrate, i.e., crystallization mother liquor, is transferred to concentration vessel 611 for vacuum distillation using the second vacuum unit 613. The solvent distilled during concentration is condensed in the second condenser 612 and recovered to crystallization solvent storage tank 51 for reuse. Uncondensed non-condensable gases are transferred through the second vacuum unit 613 to the second tail gas treatment device 614 for harmless treatment (incineration or adsorption). The concentrated liquid is then returned to crystallization vessel 5 for recrystallization with subsequent batches of tebuconazole.

[0041] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

Claims

1. A purification apparatus for the production of tebuconazole, characterized in that, It includes a reaction vessel (1), a first filter (2), an alkalization vessel (3), a solvent removal vessel (4), a crystallization vessel (5), a second filter (6), and a product storage silo (7) connected in series. The reactor (1) is also connected to a clean water storage tank (11) and an acid metering pump (10), respectively; The first filter (2) is also connected to the filtrate treatment device (21); The alkalization reactor (3) is also connected to the toluene storage tank (31) and the alkali metering pump (20), respectively; The desolventizing vessel (4) is connected to the toluene storage tank (31) via a condenser (41), and the condenser (41) is also connected in sequence to the first vacuum unit (42) and the first tail gas treatment device (43); The crystallization vessel (5) is also connected to the crystallization solvent storage tank (51).

2. The purification apparatus for the production of tebuconazole according to claim 1, characterized in that, The second filter (6) is also connected to the mother liquor treatment device (61); The mother liquor treatment device (61) is also connected to the crystallization kettle (5) and the crystallization solvent storage tank (51), respectively.

3. The purification apparatus for the production of tebuconazole according to claim 2, characterized in that, The mother liquor treatment device (61) includes a concentration kettle (611), a second condenser (612), a second vacuum unit (613), and a second tail gas treatment device (614). The concentration vessel (611) is connected to the second filter (6) and the crystallization vessel (5) respectively; The second condenser (612) is also connected to the crystallization solvent storage tank (51).

4. The purification apparatus for the production of tebuconazole according to claim 1, characterized in that, The filtrate treatment device (21) includes a filtrate storage tank (211), a reverse osmosis filter (212), and a freshwater storage tank (213) connected in series. The reverse osmosis filter (212) is also connected to the concentrate storage tank (214); A transfer pump (210) is also provided between the filtrate storage tank (211) and the reverse osmosis filter (212).

5. The purification apparatus for the production of tebuconazole according to claim 1, characterized in that, The first filter (2) includes a housing (22) with an open top. The housing (22) is divided into an upper filtration zone and a lower liquid receiving zone by an inclined perforated plate (221); A discharge port is provided on one side of the filtration zone, and the opening is located on the side where the perforated plate (221) is at a lower position; A drain port (2201) is provided on one side of the bottom of the liquid receiving area. The upper part of the perforated plate (221) is provided with a pressing structure (222) for pressing the filter cloth. The pressing structure (222) is provided on the other three sides of the filtration zone where no discharge port is opened.

6. The purification apparatus for the production of tebuconazole according to claim 5, characterized in that, The pressing structure (222) includes a pressing strip (2221) and a pair of limiting blocks (2222) disposed at both ends of the pressing strip (2221), wherein the limiting blocks (2222) are fixedly connected to the inner wall of the filter area; The bottom of the clamping strip (2221) is connected to an elastic block (2223), and the elastic block (2223) is arranged along the length direction of the clamping strip (2221); The bottom of the limiting block (2222) is provided with a limiting groove (2202) that matches the width of the pressing strip (2221).

7. The purification apparatus for the production of tebuconazole according to any one of claims 1-6, characterized in that, The first exhaust gas treatment device (43) is an adsorption tower or an incinerator.

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