Isoprothiolane mother liquor treatment device

Abstract

According to the isoprothiolane mother liquor treatment device, an organic solvent in isoprothiolane mother liquor is removed by arranging the desolventizing kettle, the removed organic solvent is condensed by utilizing the condenser and then is mixed with kettle residues in the kettle residue storage box, and the mixture is recycled into the crystallization kettle, so that the use of the solvent in the crystallization process is reduced, and the crystallization efficiency is improved. After kettle residues obtained in the desolventizing kettle are cleaned by an alkali washing kettle to remove impurities, the kettle residues are transferred into a kettle residue storage box after being subjected to secondary desolventizing, and are recycled into a crystallization kettle, so that the waste of isoprothiolane in mother liquor is reduced. The isoprothiolane mother liquor recycling device has the advantages that the isoprothiolane mother liquor recycling device can continuously run, accordingly, the isoprothiolane mother liquor recycling device is high in treatment capacity, the isoprothiolane mother liquor can be treated and recycled by the aid of cooperative use of the equipment, and the shortcomings of material waste and difficulty in treatment of a large quantity of isoprothiolane mother liquor in existing modes can be overcome.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of pesticide production, in particular to a processing device for isoprothiolane mother liquor. BACKGROUND

[0002] Isoprothiolane is also known as isoprothiolane, Fuji No. 1, and its chemical name is 1,3-dithiolane-2-ylidene malonic acid diisopropyl ester. It is a fungicide which is stable to light and heat and lowly toxic to human and livestock. At present, all domestic manufacturers adopt the production process that diisopropyl malonate reacts with carbon disulfide and sodium hydroxide to obtain sodium salt (hereinafter referred to as sodium salt), and then diisopropyl malonate reacts with the sodium salt and dichloroethane to synthesize isoprothiolane. In the above production process, dichloroethane is both a solvent and a reactant. After isoprothiolane is synthesized, dichloroethane in isoprothiolane is removed by distillation and desolventization, and then methanol is added as a solvent for crystallization. The mother liquor obtained after crystallization is a mixed system with methanol as a solvent. The existing method is to distill and recover the solvent methanol in the mother liquor, and the kettle residue is treated as waste liquid. Since the kettle residue still contains part of isoprothiolane, it will cause waste of materials in the kettle residue. Since a certain amount of isoprothiolane and other active by-products exist in the mother liquor, some manufacturers configure it into a crude emulsion for sale as a by-product. However, due to the limited use of the by-product, it is difficult to handle a large amount of isoprothiolane mother liquor. Therefore, it is necessary to develop a method for effectively treating isoprothiolane mother liquor to solve the problems of material waste and difficulty in handling a large amount of isoprothiolane mother liquor in the existing method. CONTENT OF THE UTILITY MODEL

[0003] The application provides an isoprothiolane mother liquor processing device to solve the problems of material waste and difficulty in handling a large amount of isoprothiolane mother liquor in the existing method.

[0004] The application provides an isoprothiolane mother liquor processing device, which comprises a crystallization kettle, a desolventization kettle, a condenser and a vacuum unit connected in sequence.

[0005] The desolventization kettle is further connected with an alkali washing kettle, an oil phase storage tank, a distillation device, a kettle residue storage tank and the crystallization kettle in sequence.

[0006] The condenser is further connected with a first solvent storage tank and the kettle residue storage tank in sequence.

[0007] The alkali washing kettle is further connected with a second solvent storage tank, an alkali storage tank and a brine storage tank respectively.

[0008] The distillation device is further connected with the second solvent storage tank and a gas input end of the vacuum unit respectively.

[0009] Optionally, the vacuum unit is connected with the condenser and the distillation device respectively through a filter.

[0010] Optionally, the gas output end of the vacuum unit is connected with the tail gas treatment device.

[0011] Optionally, the brine storage tank is further connected with a brine treatment device.

[0012] Optionally, the brine treatment device comprises, in sequence, an evaporator, a thickener, a crystallization kettle, a dehydration device and a filter cake storage bin.

[0013] The dehydration device is further connected with the evaporator.

[0014] The evaporator is further connected with the brine storage tank.

[0015] Optionally, an adsorption tower is arranged between the brine storage tank and the evaporator.

[0016] Optionally, a heat exchanger is arranged between the oil phase storage tank and the distillation device.

[0017] The steam output end of the evaporator is further connected with the heat exchange medium input end of the heat exchanger.

[0018] The condensate water output end of the heat exchanger is further connected with the lye storage tank.

[0019] The application provides a kind of edifenphos mother liquor treatment device, by setting up desolventizing kettle, remove organic solvent in edifenphos mother liquor, and the organic solvent removed is condensed using condenser again, then with kettle residue storage tank and kettle residue are mixed and recovered in crystallization kettle, to reduce the use of solvent in crystallization process, the kettle residue obtained in desolventizing kettle is washed by alkali washing kettle again, and then after secondary desolventizing, it is transferred into kettle residue storage tank, and recovered to crystallization kettle, to reduce the waste of edifenphos in mother liquor.The above-mentioned device can be continuously operated and thus has the characteristics of large processing capacity.The device of the application processes and recovers edifenphos mother liquor by using the above-mentioned equipment, overcoming the drawbacks of the existing method that easily causes material waste and is difficult to process a large amount of edifenphos mother liquor. BRIEF DESCRIPTION OF DRAWINGS

[0020] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, a brief introduction of the drawings needed to be used in the embodiments or prior art description will be given below. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0021] Figure 1 a schematic diagram of the edifenphos mother liquor treatment device provided by an embodiment of the present application;

[0022] Figure 2 a schematic diagram of the edifenphos mother liquor treatment device provided by another embodiment of the present application;

[0023] Figure 3 A schematic diagram of a treatment device for an edifenphos mother liquor according to another embodiment of the present application is provided;

[0024] Figure 4 A schematic diagram of a salt water treatment device according to an embodiment of the present application is provided;

[0025] Figure 5 A schematic diagram of a salt water treatment device according to another embodiment of the present application is provided;

[0026] Figure 6 A schematic diagram of a treatment device for an edifenphos mother liquor according to another embodiment of the present application is provided.

[0027] Explanation of reference signs:

[0028] 1, crystallization kettle; 2, desolventizing kettle; 3, alkali washing kettle; 4, distillation device; 5, kettle residue storage tank; 6, salt water treatment device; 21, condenser; 22, vacuum unit; 23, first solvent storage tank; 24, filter; 25, tail gas treatment device; 31, oil phase storage tank; 32, second solvent storage tank; 33, lye storage tank; 34, salt water storage tank; 41, heat exchanger; 61, evaporator; 62, thickener; 63, crystallization kettle; 64, dehydration device; 65, filter cake storage bin; 66, adsorption tower. DETAILED DESCRIPTION

[0029] In order to make the purpose, technical scheme and advantages of the embodiments of the present application more clear, the technical scheme in the embodiments of the present application is described clearly and completely below. Obviously, the described embodiments are some embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor also belong to the scope of protection of the present application.

[0030] As shown in Figure 1 The present application provides a treatment device for an edifenphos mother liquor, which comprises a crystallization kettle 1, a desolventizing kettle 2, a condenser 21 and a vacuum unit 22 connected in series;

[0031] The desolventizing kettle 2 is further connected with an alkali washing kettle 3, an oil phase storage tank 31, a distillation device 4, a kettle residue storage tank 5 and the crystallization kettle 1 in sequence;

[0032] The condenser 21 is further connected with a first solvent storage tank 23 and the kettle residue storage tank 5 in sequence;

[0033] The alkali washing kettle 3 is further connected with a second solvent storage tank 32, a lye storage tank 33 and a salt water storage tank 34 respectively;

[0034] The distillation device 4 is further connected with the second solvent storage tank 32 and a gas input end of the vacuum unit 22 respectively.

[0035] In use, the solution of the crude product of anilofos, after crystallization in the crystallization kettle 1, the mother liquor obtained is transferred to the desolventizing kettle 2 for heating desolventizing (in this application, anilofos is crystallized by using methanol, and the solvent removed in the desolventizing kettle 2 is methanol), at the same time, the vacuum unit 22 pumps the desolventizing kettle 2 to the state of the kettle pressure, so as to reduce the boiling point of the solvent, and the solvent removed in the desolventizing kettle 2 is gaseous, which is condensed into liquid by the condenser 21 and then input into the first solvent storage tank 23 for temporary storage, and the gas not condensed in the condenser 21 is discharged from the condenser 21 and then subjected to subsequent harmless treatment.

[0036] The residual liquid obtained after desolventizing, containing part of anilofos and acidic by-products generated in the reaction, is transferred into the alkali washing kettle 3, and the acidic substances (such as HCl generated in the reaction) in the residual liquid are converted into salts by adding alkali liquor through the alkali liquor storage tank 33, and dissolved in water, at the same time, the second solvent storage tank 32 adds water-immiscible organic solvent (such as dimethylbenzene) to the alkalinized residual liquid for extraction, and the organic substances in the residual liquid are extracted into the organic phase, and after the extraction is completed, the liquid is allowed to stand to separate into the water phase containing salts and the organic phase, the organic phase is transferred into the oil phase storage tank 31, and the water phase containing salts is transferred into the brine storage tank 34 for temporary storage.

[0037] The organic phase stored in the oil phase storage tank 31 is transferred into the distillation device 4 (distillation kettle or distillation column in this application) for distillation, and the solvent is separated and recovered into the second solvent storage tank 32 for reuse after being condensed and cooled, and at the same time, the distillation device 4 is pumped by the vacuum unit 22 to reduce the boiling point of the solvent, so as to facilitate the distillation. The kettle residue obtained after distillation in the distillation device 4 is transferred into the kettle residue storage tank 5, mixed with the solvent (i.e. methanol) received by the first solvent storage tank 23, and then transferred into the crystallization kettle 1 to mix with the solution of the crude product of anilofos for crystallization.

[0038] The present application provides a device for treating the mother liquor of anilofos, which removes the organic solvent in the mother liquor of anilofos by the desolventizing kettle 2, and condenses the removed organic solvent by the condenser 21, and then mixes the condensed organic solvent with the kettle residue in the kettle residue storage tank 5 and recovers the mixture into the crystallization kettle 1, so as to reduce the use of solvent in the crystallization process, and the kettle residue obtained in the desolventizing kettle 2 is cleaned by the alkali washing kettle 3 to remove impurities, and then transferred into the kettle residue storage tank 5 after secondary desolventizing, and recovered into the crystallization kettle 1, so as to reduce the waste of anilofos in the mother liquor, and the above device can be continuously operated, thus having the characteristics of large processing capacity. The device of the present application processes and recovers the mother liquor of anilofos by the cooperation of the above devices, and overcomes the drawbacks of the prior art that the material is easily wasted and it is difficult to process a large amount of mother liquor of anilofos.

[0039] Optionally, as Figure 2As shown, the vacuum unit 22 is connected with the condenser 21 and the distillation device 4 through the filter 24 respectively.

[0040] In the present application, since other substances are evaporated together with the solvent, the substances have lower boiling points and cannot be condensed in the condenser 21, that is, form non-condensable gas. The non-condensable gas contains a small amount of organic substances. If the non-condensable gas is sucked into the vacuum unit 22, it may cause the equipment in the vacuum unit 22 to malfunction, affecting the operation and service life of the equipment. The filter 24 filled with adsorbent (such as activated carbon) can adsorb and remove the organic substances in the non-condensable gas, avoiding damage to the vacuum unit 22.

[0041] Optionally, the gas output end of the vacuum unit 22 is connected with the tail gas treatment device 25.

[0042] In the present application, the non-condensable gas can be further treated to prevent the substances mixed in the non-condensable gas from polluting the environment.

[0043] Optionally, as shown in the figure, Figure 3 As shown, the brine storage tank 34 is also connected with the brine treatment device 6.

[0044] In the present application, the brine treatment device 6 is arranged to treat and recycle the brine generated in the alkali washing process, avoiding waste of materials.

[0045] Optionally, as shown in the figure, Figure 4 As shown, the brine treatment device 6 includes an evaporator 61, a thickener 62, a crystallization kettle 63, a dehydration device 64 and a filter cake storage bin 65 connected in series.

[0046] The dehydration device 64 is also connected with the evaporator 61;

[0047] The evaporator 61 is also connected with the brine storage tank 34.

[0048] In use, the brine stored in the brine storage tank 34 is neutralized to neutral, and then transferred to the evaporator 61 (a multi-effect evaporator in the present application) for evaporation and concentration to obtain a concentrated liquid. The concentrated liquid is then transferred to the thickener 62 for gradual cooling and enrichment (in the present application, if potassium hydroxide is used as the alkali, the salt is mainly potassium chloride). The concentrated liquid treated by the thickener 62 is then transferred to the crystallization kettle 63 for cooling and final crystallization. The completely crystallized liquid is dehydrated by the dehydration device 64 (such as a centrifuge or a filter press) to obtain a filter cake which is the salt, and then transferred to the filter cake storage bin 65 for temporary storage. The liquid obtained after dehydration is recycled to the evaporator 61 for further evaporation and concentration.

[0049] Optionally, as shown in the figure, Figure 5 As shown, an adsorption tower 66 is arranged between the brine storage tank 34 and the evaporator 61.

[0050] In the present application, since the brine is obtained from the neutralized residual liquid and is subjected to solvent extraction and liquid separation during the neutralization process, a small amount of organic matter and colored substances inevitably mix into the brine. The mixing of these substances into the brine is not conducive to the subsequent treatment of the brine. Therefore, it is necessary to set up an adsorption tower 66 (which is filled with activated carbon or adsorption resin as adsorbent) to treat the brine, so as to avoid the mixing of secondary steam generated during the evaporation and concentration process into the organic matter.

[0051] Optionally, as shown in Figure 6 A heat exchanger 41 is arranged between the oil phase storage tank 31 and the distillation device 4;

[0052] The steam output end of the evaporator 61 is also connected to the heat exchange medium input end of the heat exchanger 41;

[0053] The condensate output end of the heat exchanger 41 is also connected to the lye storage tank 33.

[0054] In the present application, the brine stored in the brine storage tank 34 is neutralized to neutral during use, and then transferred to the evaporator 61 (which is a multi-effect evaporator in the present application) for evaporation and concentration. The secondary steam obtained during the evaporation and concentration process is transferred to the heat exchanger 41 to exchange heat with the organic phase output from the oil phase storage tank 31. The secondary steam after heat exchange is condensed into liquid, and these condensed liquids are recycled to the lye storage tank 33 for preparation of lye (sodium hydroxide aqueous solution or potassium hydroxide aqueous solution).

[0055] A process for treating a mother liquor of an isoprothiolane solution is as follows:

[0056] In use, the mother liquor obtained after crystallization of the isoprothiolane crude product solution in the crystallization kettle 1 is transferred to the desolventizing kettle 2 for heating and desolventizing (in the present application, isoprothiolane is crystallized by using methanol, and the solvent to be removed in the desolventizing kettle 2 is methanol). At the same time, the vacuum unit 22 pumps the desolventizing kettle 2 to a state of kettle pressure, so as to reduce the boiling point of the solvent. The solvent to be removed in the desolventizing kettle 2 is in gaseous state, which is condensed into liquid state by the condenser 21 and then input into the first solvent storage tank 23 for temporary storage. The gas that fails to be condensed in the condenser 21 is discharged from the condenser 21, adsorbed by the filter 24 to remove the organic matter entrained therein, and then discharged into the tail gas treatment device 25 by the vacuum unit 22 for harmless treatment, such as incineration.

[0057] The residual liquid obtained after desolventizing, which contains part of the unconverted rice bud blight and the acidic by-products generated in the reaction, is transferred into the caustic washing kettle 3, and the acidic substances (such as HCl generated in the reaction) in the residual liquid are converted into salts by adding caustic solution through the caustic solution storage tank 33, and dissolved in water. Meanwhile, the second solvent storage tank 32 adds water-immiscible organic solvent (such as xylene) to extract the alkalized residual liquid, and the organic substances in the alkalized residual liquid are extracted into the organic phase. After extraction, the organic phase and the water phase containing the salts are separated by standing, and the organic phase is transferred into the oil phase storage tank 31, while the water phase containing the salts is transferred into the brine storage tank 34 for temporary storage.

[0058] The organic phase stored in the oil phase storage tank 31 is heated by heat exchange with the steam output from the evaporator 61 through the heat exchanger 41, and then transferred into the distillation device 4 (distillation kettle or distillation column in this application) for distillation to separate the solvent therefrom. The separated solvent is condensed and cooled, and then recycled to the second solvent storage tank 32 for reuse. At the same time, the distillation device 4 is pumped by the vacuum unit 22 to reduce the boiling point of the solvent, facilitating distillation. The kettle residue obtained after distillation in the distillation device 4 is transferred into the kettle residue storage tank 5, mixed with the solvent (i.e. methanol) received by the first solvent storage tank 23, and then transferred into the crystallization kettle 1 to mix with the rice bud blight crude solution for crystallization.

[0059] The brine stored in the brine storage tank 34 is neutralized to neutral, and then the colored impurities or organic substances are removed by the adsorption column 66, and then transferred into the evaporator 61 (multi-effect evaporator in this application) for evaporation and concentration. The secondary steam obtained in the evaporation and concentration process is transferred into the heat exchanger 41 to exchange heat with the organic phase output from the oil phase storage tank 31. The secondary steam after heat exchange is condensed into liquid, which is recycled to the caustic solution storage tank 33 for preparation of caustic solution (aqueous sodium hydroxide solution or aqueous potassium hydroxide solution). The concentrated liquid obtained after evaporation in the evaporator 61 is transferred into the thickener 62 for gradual cooling and enrichment (in this application, if the caustic solution is aqueous potassium hydroxide, the salt is mainly potassium chloride). The concentrated liquid treated by the thickener 62 is then transferred into the crystallization kettle 63 for cooling and final crystallization. The completely crystallized liquid is dehydrated by the dehydration device 64 (such as centrifuge or filter press, etc.) to obtain the filter cake as the salt. The liquid obtained after dehydration is recycled to the evaporator 61 for further evaporation and concentration.

[0060] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, and are not limited thereto; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand; it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement to part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A device for treating a technical-grade molinate solution, characterized in that it comprises: The crystallization kettle (1), the desolventizing kettle (2), the condenser (21) and the vacuum unit (22) are connected in series. The desolventizing kettle (2) is further connected with the alkali washing kettle (3), the oil phase storage tank (31), the distillation device (4), the kettle residue storage tank (5) and the crystallization kettle (1) in series. The condenser (21) is further connected with the first solvent storage tank (23) and the kettle residue storage tank (5) in series. The alkali washing kettle (3) is further connected with the second solvent storage tank (32), the alkali storage tank (33) and the brine storage tank (34) respectively. The distillation device (4) is further connected with the second solvent storage tank (32) and the gas input end of the vacuum unit (22) respectively.

2. The pronamiphos stock solution treatment device according to claim 1, characterized by The vacuum unit (22) is connected with the condenser (21) and the distillation device (4) through the filter (24) respectively.

3. The pronamiphos stock solution treatment device according to claim 1, characterized by, The gas output end of the vacuum unit (22) is connected with the tail gas treatment device (25).

4. The pronamiphos stock solution treatment device according to claim 1, characterized by, The brine storage tank (34) is further connected with the brine treatment device (6).

5. The pronamiphos stock solution treatment device according to claim 4, characterized by The brine treatment device (6) comprises an evaporator (61), a thickener (62), a crystallization kettle (63), a dehydration device (64) and a filter cake storage (65) connected in series. The dehydration device (64) is further connected with the evaporator (61). The evaporator (61) is further connected with the brine storage tank (34).

6. The pronamiphos stock solution treatment device according to claim 5, characterized by An adsorption tower (66) is arranged between the brine storage tank (34) and the evaporator (61).

7. The pronamid mother liquor treatment device according to claim 5, characterized in that, A heat exchanger (41) is arranged between the oil phase storage tank (31) and the distillation device (4). The steam output end of the evaporator (61) is further connected with the heat exchange medium input end of the heat exchanger (41). The condensate output end of the heat exchanger (41) is further connected with the alkali storage tank (33).

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