A method for extracting oxadiazine through oxadiazine wastewater

Abstract

The present application discloses a kind of method of extracting oxadiazine by oxadiazine wastewater, oxadiazine wastewater is injected in extraction kettle, injecting oxadiazine wastewater water yield is 1 / 3rd of kettle volume, add extraction solvent, open stirring, stir after 1h, close stirring, the waste water having stirred is proceeded to layering tank and is left standstill 30min, after leaving standstill, the water layer of upper strata is put into wastewater storage tank, the organic layer of lower floor is collected, the organic layer collected is proceeded to precipitation crystallization kettle, precipitation crystallization kettle is with condensing device and vacuum system, heats up with hot water, removes solvent under negative pressure, adds distilled water after removing solvent, is cooled to 0 10 DEG C with ice water in precipitation crystallization kettle, has crystallization to separate out, and is filtered to obtain oxadiazine recycled material.The oxadiazine wastewater collected is carried out multi-step process, extracts the oxadiazine dissolved in wastewater, not only oxadiazine product is recycled, saves oxadiazine production cost, also reduces the pollution of oxadiazine wastewater to environment, the damage to land.

Description

Technical Field

[0001] The present application relates to the field of pesticide intermediate synthesis, and in particular to a method for extracting oxadiazine from oxadiazine wastewater. Background Art

[0002] Oxadiazine is an important intermediate of the insecticide thiamethoxam. Thiamethoxam is a second-generation nicotinoid insecticide with a new structure, which is highly effective and low-toxic. It has good preventive effects on piercing-sucking pests such as aphids, planthoppers, leafhoppers, whiteflies, etc., and shows low toxicity to fish, birds and mammals. Therefore, oxadiazine insecticides have developed rapidly in the domestic and foreign markets.

[0003] A large amount of oxadiazine wastewater is generated during the production and use of oxadiazine. Direct sewage treatment of oxadiazine wastewater not only pollutes the environment but also causes waste of oxadiazine. Therefore, a method for extracting oxadiazine from oxadiazine wastewater is designed. Summary of the Invention

[0004] The present application provides a method for extracting oxadiazine from oxadiazine wastewater, wherein the collected oxadiazine wastewater is subjected to multi-step treatment to extract the oxadiazine dissolved in the wastewater. This not only recovers the oxadiazine raw material and reduces the production cost of oxadiazine, but also reduces the pollution to the environment and damage to the land caused by the direct discharge of oxadiazine wastewater.

[0005] The present application provides a method for extracting oxadiazine from oxadiazine wastewater, characterized in that it comprises the following steps:

[0006] Prepare an extraction kettle with stirring;

[0007] Fully cleaning the extraction kettle;

[0008] injecting the oxadiazine wastewater into the extraction kettle, wherein the amount of the injected oxadiazine wastewater is one third of the kettle volume;

[0009] adding an extraction solvent;

[0010] Start stirring at room temperature and pressure, and turn off stirring after stirring for 1 hour;

[0011] Place the stirred wastewater into a stratification tank and let it stand for 30 minutes;

[0012] After standing, the upper aqueous layer is placed in a wastewater storage tank and the lower organic layer is collected;

[0013] The collected organic layer is transferred into a desolventizing and crystallizing kettle;

[0014] The desolventizing and crystallizing kettle is equipped with a condensing device and a vacuum system, and heated in a water bath;

[0015] Remove organic matter under reduced pressure, remove the solvent and add distilled water;

[0016] Cool down the crystallization in the desolventizing crystallization kettle and use ice water to cool down to 0-10℃ for crystallization.

[0017] After the crystals are precipitated, they are placed in a filter for filtration. The mother liquor after filtration is sent to the oxadiazine mother liquor storage tank for re-extraction; the filter cake is recovered, and the filter cake obtained after drying is the extracted oxadiazine solid. The oxadiazine content after drying is 80%-98%.

[0018] In summary, the beneficial effects produced by this application are as follows:

[0019] 1. This application conducts multi-step treatment on the collected oxadiazine wastewater, extracts the oxadiazine dissolved in the wastewater, and recovers the oxadiazine product, thereby reducing the production cost of oxadiazine.

[0020] 2. The collected oxadiazine wastewater is subjected to multi-step treatment to extract the oxadiazine dissolved in the wastewater, thereby reducing the pollution of the oxadiazine wastewater to the environment and the damage to the land.

[0021] 3. This application solves the problem that the effective ingredient oxadiazine in oxadiazine wastewater is difficult to extract. The extraction technology of oxadiazine in oxadiazine wastewater is of great significance to the long-term development of oxadiazine. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the technical solution of this application, the following is a brief introduction to the drawings required for the implementation cases. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0023] Figure 1 A process flow diagram of a method for extracting oxadiazine from oxadiazine wastewater according to the present invention;

[0024] Figure 2 This is a chromatogram of the product in Example 1 of the present invention;

[0025] Figure 3 This is a chromatogram of the product in Example 2 of the present invention;

[0026] Figure 4 This is a chromatogram of the product in Example 3 of the present invention;

[0027] Figure 5 This is a chromatogram of the product in Example 4 of the present invention;

[0028] Figure 6 This is the chromatogram of the oxadiazine standard sample of the present invention. DETAILED DESCRIPTION

[0029] In order to enable people skilled in the art to better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the accompanying drawings.

[0030] See the above technical solution Figures 1-6 :

[0031] A method for extracting oxadiazine from oxadiazine wastewater, characterized by comprising the following steps:

[0032] Prepare an extraction kettle with stirring;

[0033] Fully cleaning the extraction kettle;

[0034] injecting the oxadiazine wastewater into the extraction kettle, wherein the amount of the injected oxadiazine wastewater is one third of the kettle volume;

[0035] adding an extraction solvent;

[0036] Start stirring at room temperature and pressure, and turn off stirring after stirring for 1 hour;

[0037] Place the stirred wastewater into a stratification tank and let it stand for 30 minutes;

[0038] After standing, the upper aqueous layer is placed in a wastewater storage tank and the lower organic layer is collected;

[0039] The collected organic layer is transferred into a desolventizing and crystallizing kettle;

[0040] The desolventizing and crystallizing kettle is equipped with a condensing device and a vacuum system, and heated in a water bath;

[0041] Remove organic matter under reduced pressure, remove the solvent and add distilled water;

[0042] Cool down the crystallization in the desolventizing crystallization kettle and use ice water to cool down to 0-10℃ for crystallization.

[0043] After the crystals are precipitated, they are placed in a filter for filtration. The mother liquor after filtration is sent to the oxadiazine mother liquor storage tank for re-extraction; the filter cake is recovered, and the filter cake obtained after drying is the extracted oxadiazine solid. The oxadiazine content after drying is 80%-98%.

[0044] As a preferred embodiment, the weight ratio of oxadiazine wastewater to extraction solvent is 1:1-4, wherein the extraction solvent used includes toluene, ethyl acetate, carbon tetrachloride, and petroleum ether.

[0045] As a preferred embodiment, the pressure under reduced pressure is controlled at -0.080-0.09 MPa, the desolventizing temperature is maintained at 60-90°C, and a set proportion of distilled water is added after the solvent is completely removed. The weight ratio of the remaining material to the distilled water is: 1:1-3.

[0046] As a preferred embodiment, the filter is specifically a suction filtration funnel, the suction filtration funnel is vacuum filtered until there is no moisture, and the filter cake is dried to obtain the finished oxadiazine.

[0047] Example 1, see Figure 1 、 Figure 2 :

[0048] A method for extracting oxadiazine from oxadiazine wastewater comprises the following steps:

[0049] (1) Add 500 g of oxadiazine wastewater into a 1000 ml stirred extraction kettle, add 1000 g of extraction solvent at room temperature, the types of extraction solvents include: toluene, ethyl acetate, carbon tetrachloride, petroleum ether, the weight ratio is 1:1-4, and stop stirring after stirring for 1 hour;

[0050] (2) After standing for 30 minutes, separate the water layer and pour the water layer into the wastewater storage tank; the organic layer is placed in a 2000ml removal crystallization kettle, and the solvent is evaporated under reduced pressure on a rotary evaporator. The water bath temperature is set at 70°C and the vacuum degree is controlled at less than -0.08MPa. After the solvent is basically removed, 10g of distilled water is added;

[0051] (3) Transfer the water-added solution into a stirred extraction kettle and cool it to 5°C in an ice bath;

[0052] (4) Pour the crystallized material into a suction filtration funnel, filter it with vacuum until it is dry, scrape out the filter cake, and put it into an oven to dry.

[0053] Dry weight: 5.4g; Content: 95.3%;

[0054] The product chromatogram is as follows Figure 2 shown.

[0055] Example 2, see Figure 1 、 Figure 3 :

[0056] A method for extracting oxadiazine from oxadiazine wastewater comprises the following steps:

[0057] (1) Add 1000 g of oxadiazine wastewater into a 2000 ml stirred extraction kettle, add 1000 g of extraction solvent at room temperature, and the weight ratio of toluene, ethyl acetate, carbon tetrachloride, and petroleum ether in the extraction solvent is 2:2:1:1. Stir for 1 hour and then stop stirring;

[0058] (2) After standing for 30 minutes, the water layer was separated and poured into the wastewater storage tank; the organic layer was placed in a 2000ml removal crystallization kettle, and the solvent was evaporated under reduced pressure on a rotary evaporator. The water bath temperature was set at 70°C and the vacuum degree was controlled at less than -0.08MPa. After the solvent was basically removed, 20g of distilled water was added;

[0059] (3) Transfer the water-added solution into a stirred extraction kettle and cool it to 5°C in an ice bath;

[0060] (4) Pour the crystallized material into a suction filtration funnel, filter it with vacuum until it is dry, scrape out the filter cake, and put it into an oven to dry.

[0061] Dry weight: 9.6g; Content: 96.4%;

[0062] The product chromatogram is as follows Figure 3 shown.

[0063] Example 3, see Figure 1 、 Figure 4 :

[0064] A method for extracting oxadiazine from oxadiazine wastewater comprises the following steps:

[0065] (1) Add 500 g of oxadiazine wastewater into a 1000 ml stirred extraction kettle, add 500 g of extraction solvent at room temperature, and the weight ratio of toluene, ethyl acetate, carbon tetrachloride, and petroleum ether in the extraction solvent is 1:1:1:1. Stir for 1 hour and then stop stirring;

[0066] (2) After standing for 30 minutes, separate the water layer and pour the water layer into the wastewater storage tank; the organic layer is placed in a 2000ml removal crystallization kettle, and the solvent is evaporated under reduced pressure on a rotary evaporator. The water bath temperature is set at 70°C and the vacuum degree is controlled at less than -0.08MPa. After the solvent is basically removed, 10g of distilled water is added;

[0067] (3) Transfer the water-added solution into a stirred extraction kettle and cool it to 5°C in an ice bath;

[0068] (4) Pour the crystallized material into a suction filtration funnel, filter it with vacuum until it is dry, scrape out the filter cake, and put it into an oven to dry.

[0069] Dry weight: 3.5g; Content: 85.8%;

[0070] The product chromatogram is as follows Figure 4 shown.

[0071] Example 4, see Figure 1 、 Figure 5 :

[0072] A method for extracting oxadiazine from oxadiazine wastewater comprises the following steps:

[0073] (1) Add 500 g of oxadiazine wastewater into a 1000 ml stirred extraction kettle, add 1000 g of extraction solvent at room temperature, and the weight ratio of toluene, ethyl acetate, carbon tetrachloride, and petroleum ether in the extraction solvent is 1:1:1:1. Stir for 1 hour and then stop stirring;

[0074] (2) After standing for 30 minutes, separate the water layer and pour the water layer into the wastewater storage tank; the organic layer is placed in a 2000ml removal crystallization kettle, and the solvent is evaporated under reduced pressure on a rotary evaporator. The water bath temperature is set at 70°C and the vacuum degree is controlled at less than -0.08MPa. After the solvent is basically removed, 10g of distilled water is added;

[0075] (3) Transfer the water-added solution into a stirred extraction kettle and cool it to 5°C in an ice bath;

[0076] (4) Pour the crystallized material into a suction filtration funnel, filter it with vacuum until it is dry, scrape out the filter cake, and put it into an oven to dry.

[0077] Dry weight: 3.7g; Content: 84.6%;

[0078] The product chromatogram is as follows Figure 5 shown.

[0079] Those skilled in the art will readily appreciate other embodiments of the present application after considering the specification and practicing the application disclosed herein. This application is intended to cover any variations, uses, or adaptations of the present application that follow the general principles of this application and include common knowledge or customary techniques in the art not disclosed herein. The description and examples are to be considered merely as exemplary, and the true scope of this application is indicated by the claims.

[0080] It should be understood that the present application is not limited to the precise structure described above and shown in the drawings, and various modifications and changes can be made without departing from the scope thereof. The above-described embodiments of the present application do not constitute a limitation on the scope of protection of the present application.

Claims

1. A method for extracting oxadiazine from oxadiazine wastewater, characterized in that: The method comprises the following steps: preparing an extraction kettle with stirring; Fully cleaning the extraction kettle; injecting the oxadiazine wastewater into the extraction kettle, wherein the amount of the injected oxadiazine wastewater is one third of the kettle volume; adding an extraction solvent; Start stirring at room temperature and pressure, and turn off stirring after stirring for 1 hour; Place the stirred wastewater into a stratification tank and let it stand for 30 minutes; After standing, the upper aqueous layer is placed in a wastewater storage tank and the lower organic layer is collected; The collected organic layer is transferred into a desolventizing and crystallizing kettle; The desolventizing and crystallizing kettle is equipped with a condensing device and a vacuum system, and heated in a water bath; Remove organic matter under reduced pressure, remove the solvent and add distilled water; Cool down the crystallization in the desolventizing crystallization kettle and use ice water to cool down to 0-10℃ for crystallization; After the crystals are precipitated, they are placed in a filter for filtration. The mother liquor after filtration is sent to the oxadiazine mother liquor storage tank for re-extraction; the filter cake is recovered and the filter cake obtained after drying is the extracted oxadiazine solid. The oxadiazine content after drying is 80%-98%; The weight ratio of the oxadiazine wastewater to the extraction solvent is 1:1-4, wherein the extraction solvent used is toluene, ethyl acetate, carbon tetrachloride, and petroleum ether.

2. The method for extracting oxadiazine from diazine wastewater according to claim 1, characterized in that: The pressure under the reduced pressure state is controlled at -0.080-0.09 MPa, and the desolventizing temperature is maintained at 60-90° C., and a set proportion of distilled water is added after the solvent is completely removed. The weight ratio of the remaining material to the distilled water is 1:1-3.

3. The method for extracting oxadiazine from diazine wastewater according to claim 1, characterized in that: The filter is specifically a flat plate centrifuge, which is used to dry the solid material by centrifugal force, and the obtained filter cake is dried to obtain a recovered oxadiazine product.

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