CN113023988A - Method for treating methomyl process wastewater - Google Patents
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Abstract
The invention discloses a method for treating methomyl process wastewater, which comprises the following steps: mixing the methomyl process wastewater with an organic solvent, extracting, separating and collecting organic extract liquor; mixing the organic extraction liquid with water and activated carbon, recovering the organic solvent in the obtained mixed liquid, and filtering to obtain filtrate; and crystallizing the filtrate, filtering, drying and recovering the methomyl to finish the treatment of the methomyl process wastewater. The method for treating the methomyl process wastewater has the advantages of simple process, convenience in operation, low treatment cost, high safety and the like, can realize effective pretreatment of the methomyl process wastewater on the premise of not increasing the wastewater yield, obviously reduces the subsequent treatment difficulty of the methomyl process wastewater, has the characteristics of high recovery rate of the methomyl, recycling of an organic solvent and the like, improves the product yield, obtains a high-quality methomyl recovered product, reduces the treatment cost, and is suitable for industrial popularization.
Description
Technical Field
The invention relates to a method for treating methomyl process wastewater.
Background
Methomyl is an oxime carbamate insecticide, acaricide, nematicide and molluscicide, is developed by DuPont in 1966, has the effects of contact poisoning, stomach poisoning and ovicidal action, has strong killing power, quick response, wide insecticidal spectrum, low residual quantity, wide applicable crops and safe use, and is widely applied to more than thirty crops such as cotton, cabbage, tobacco, orange, soybean, peanut and the like. Methomyl is a high-grade pesticide, is about to be banned, and can still be used as an important intermediate for synthesizing thiodicarb. Thiodicarb, also known as thiodicarb, is a second-generation carbamate pesticide, and is one of low-toxicity derivatives obtained by further improving on the basis of methomyl, namely, two methomyl molecules are connected through a thioether chain to form dicarbamate, the toxicity is only about one tenth of that of methomyl, and the thiodicarb is a high-efficiency, broad-spectrum, low-toxicity and systemic stomach toxicity pesticide. To date, they have been registered in thirty-few countries of the world, with annual sales of thousands of tons. The pesticide is widely used for crops such as cotton, vegetables, fruit trees, tea, tobacco, forest, wheat and the like, is particularly effective for larvae of pests such as lepidoptera, homoptera, hymenoptera, diptera, coleoptera and the like, and is an excellent medicament for preventing and controlling resistant cotton bollworms at present in China.
In the existing preparation process of methomyl, a large amount of process wastewater containing methomyl is generated, however, a treatment process of the process wastewater of the methomyl is not seen in the prior art. In addition, because the methomyl has poor thermal stability and is easy to cause explosion of a methomyl waste liquid treatment device, the methomyl manufacturers at home and abroad directly abandon the recovery of the methomyl or adopt a salting-out method to recover the methomyl. However, when methomyl is recovered by salting out, the following problems still remain: (1) the solubility of the industrial salt in water is about 36g, namely about 3600 tons of industrial salt is required to be added for treating 10000 tons of methomyl wastewater, so that the production cost and the total amount of the wastewater are increased; (2) the high-concentration salt-containing wastewater after the methomyl is recovered by the salting-out method has high treatment difficulty and high cost. Therefore, the recovery of methomyl by the salting-out method is not considered to be economically effective. However, with the increasing market demand of methomyl and the increasing requirement of environmental protection, there is an urgent need to develop a method for treating the methomyl process wastewater with simple process, convenient operation, low treatment cost and high safety, which can recover the methomyl product in the process wastewater while reducing the generation of three wastes, thereby not only reducing the adverse effect of the methomyl process wastewater on the environment, but also realizing the goal of improving the economic benefit and social benefit of enterprises.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for treating the waste water of the methomyl process, which has the advantages of simple process, convenient operation, low treatment cost and high safety.
In order to solve the technical problems, the invention adopts the technical scheme that:
a method for treating methomyl process wastewater comprises the following steps:
s1, mixing the methomyl process wastewater with an organic solvent, extracting, separating and collecting organic extract liquor;
s2, mixing the organic extraction liquid collected in the step S1 with water and activated carbon, recovering the organic solvent in the obtained mixed liquid, and filtering to obtain filtrate;
s3, crystallizing the filtrate obtained in the step S2, filtering, drying and recovering the methomyl to finish the treatment of the methomyl process wastewater.
In the step S1, the mass ratio of the organic solvent to the methomyl process wastewater is 0.2-0.6: 1.
In step S1, the organic solvent is at least one of dichloromethane, chloroform, 1, 2-dichloroethane, and ethyl acetate.
In step S1, the method for treating methomyl process wastewater is further improved in that the mass percentage of methomyl in the methomyl process wastewater is 1% to 5%.
In the step S1, the extraction temperature is 5-30 ℃; the extraction time is 0.5 h-2 h; the extraction times are 1 to 3.
The method for treating the methomyl process wastewater is further improved, and the mass ratio of the water to the methomyl process wastewater is 0.05-0.1: 1.
In the method for treating the methomyl process wastewater, the mass ratio of the activated carbon to the methomyl process wastewater is further improved to be 0.0005-0.002: 1.
In a further improvement of the above method for treating methomyl process wastewater, in step S2, the method for recovering the organic solvent includes the following steps: heating the obtained mixed solution to 50 ℃, and performing suction filtration under reduced pressure to complete the recovery of the organic solvent in the mixed solution.
In the above method for treating methomyl process wastewater, in a further improvement, in step S3, the drying is performed under vacuum condition; the drying temperature is 50 ℃; the drying time is 12 h.
Compared with the prior art, the invention has the advantages that:
(1) the invention provides a method for treating waste water of methomyl process, which comprises the steps of firstly extracting methomyl in the waste water by using an organic solvent, transferring the methomyl into an organic phase, adding water and activated carbon, then realizing the transfer of the methomyl from the organic phase to a water phase by using different solubilities of the methomyl in the water and the organic phase, recovering the organic solvent, and finally completing the effective treatment of the waste water of the methomyl process while recovering the methomyl product by crystallization, filtration and drying. In the invention, before the organic solvent is treated and recovered, because water with larger specific heat capacity is added, the concentration degree of the methomyl solution can be effectively controlled in the recovery process of the organic solvent, the explosion risk caused by poor stability of the methomyl is greatly reduced, combustion explosion cannot be caused by the presence of the water, the safety of the recovery process is obviously improved, and meanwhile, the recovery rates of the methomyl product and the organic solvent can also be improved; meanwhile, water generated in the crystallization process can be reused in the process of transferring methomyl from an organic phase to a water phase, the generation of waste water is reduced, the treatment cost can be reduced, and the cost required by treatment can be reduced by recovering methomyl products; on the other hand, the wastewater generated in the organic phase recovery process can greatly reduce the treatment difficulty and safety risk of the wastewater on the premise of not increasing the wastewater yield due to the great reduction of the content of the methomyl (the COD concentration in the wastewater is greatly reduced), so that the subsequent treatment of the wastewater is facilitated on the premise of not increasing the wastewater yield as a whole, and meanwhile, the treatment cost can be further reduced due to the recovery of the organic solvent, so that the effective pretreatment of the methomyl process wastewater is realized. The method for treating the methomyl process wastewater has the advantages of simple process, convenience in operation, low treatment cost, high safety and the like, can realize effective pretreatment of the methomyl process wastewater on the premise of not increasing the wastewater yield, obviously reduces the subsequent treatment difficulty of the methomyl process wastewater, has the characteristics of high recovery rate of the methomyl, recycling of an organic solvent and the like, improves the product yield, obtains a high-quality methomyl recovered product, reduces the treatment cost, and is suitable for industrial popularization.
(2) In the invention, the extraction conditions are optimized, and the method specifically comprises the following steps: mixing an organic solvent and the methomyl process wastewater according to the mass ratio of 0.2-0.6: 1, extracting for 0.5-2 h at the temperature of 5-30 ℃, and extracting for 1-3 times, so that the methomyl can be efficiently recovered from the methomyl process wastewater, and the recovery rate is 86.3-95.1%.
(3) In the invention, the use amount of water and activated carbon is optimized, specifically, the mass ratio of water to the methomyl process wastewater is 0.05-0.1: 1, and the mass ratio of the activated carbon to the methomyl process wastewater is 0.0005-0.002: 1, so that the quality of the recovered methomyl product can be ensured, and the content is 98.06-98.35%.
(4) In the invention, the recovery condition of the organic solvent is optimized, the organic solvent is recovered under reduced pressure at 50 ℃, the organic solvent can be efficiently recovered, and the methomyl has good stability at the temperature and can be completely dissolved in water, so that the impurities can be conveniently adsorbed by the activated carbon.
Detailed Description
The invention is further described below with reference to specific preferred embodiments, without thereby limiting the scope of protection of the invention.
The mass percentage of the methomyl in the wastewater from the methomyl process, which is treated in the following examples, is 1.72% by sampling and analyzing.
Example 1:
a method for treating methomyl process wastewater comprises the following steps:
1000g of methomyl process wastewater and 200g of 1, 2-dichloroethane are added into a 2L three-neck flask, stirred for 0.5 hour at 25 ℃, then the material is transferred into a 2L pear-shaped separating funnel, and after standing for 20 minutes, the lower organic extract and the upper aqueous phase are separated. And transferring the upper water phase into a 2L three-neck flask, adding 200g of 1, 2-dichloroethane, repeating the operation, and performing secondary extraction, wherein the COD concentration in the separated water phase after extraction is greatly reduced, and the treatment difficulty and safety risk are greatly reduced. And combining the organic extraction liquids separated in the two times, adding the combined organic extraction liquids into a 1L three-neck flask, adding 100g of tap water and 2g of activated carbon, heating the mixture in a water bath to 50 ℃, decompressing, filtering, recovering 1, 2-dichloroethane, filtering while the mixture is hot, cooling, crystallizing (crystallizing) the obtained filtrate, filtering, drying the filter cake for 12 hours at 50 ℃ in a vacuum drying oven, recovering 16.13g of white crystals, namely the methomyl product, and finishing the treatment of the methomyl process wastewater. The mass percentage of the methomyl in the product is 98.31 percent and the recovery rate is 92.2 percent by analyzing the product by a liquid chromatography external standard method. In the embodiment, water generated in the crystallization process can be reused in the process of transferring methomyl from an organic phase to a water phase, so that the wastewater is reduced, and the treatment cost can be reduced. In this embodiment, the treatment method adopted does not increase the yield of wastewater as a whole.
Example 2
A method for treating methomyl process wastewater comprises the following steps:
1000g of methomyl process wastewater and 200g of dichloromethane are added into a 2L three-neck flask, stirred for 0.5 hour at 5 ℃, then transferred into a 2L pear-shaped separating funnel, and after standing for 20 minutes, the lower organic extract and the upper aqueous phase are separated. And transferring the upper water phase into a 2L three-neck flask, adding 200g of dichloromethane, repeating the operation, and performing secondary extraction, wherein the COD concentration in the separated water phase after extraction is greatly reduced, and the treatment difficulty and the safety risk are greatly reduced. And combining the organic extraction liquids separated in the two times, adding the combined organic extraction liquids into a 1L three-neck flask, adding 80g of tap water and 1g of activated carbon, heating the mixture in a water bath to 50 ℃, decompressing, pumping, filtering, recovering dichloromethane, filtering while the mixture is hot, cooling, crystallizing and filtering the filtrate, drying the filter cake for 12 hours at 50 ℃ by using a vacuum drying oven, recovering and obtaining 16.33g of white crystals, namely the methomyl product, and finishing the treatment of the methomyl process wastewater. The mass percentage of the methomyl in the product is 98.25 percent and the recovery rate is 93.3 percent by analyzing the product by a liquid chromatography external standard method. In the embodiment, water generated in the crystallization process can be reused in the process of transferring methomyl from an organic phase to a water phase, so that the wastewater is reduced, and the treatment cost can be reduced. In this embodiment, the treatment method adopted does not increase the yield of wastewater as a whole.
Example 3
A method for treating methomyl process wastewater comprises the following steps:
1000g of methomyl process wastewater and 200g of chloroform are added into a 2L three-neck flask, stirred for 0.5 hour at 30 ℃, then transferred into a 2L pear-shaped separating funnel, and after standing for 20 minutes, the lower organic extract and the upper aqueous phase are separated. And transferring the upper water phase into a 2L three-neck flask, adding 200g of trichloromethane, repeating the operation, and performing secondary extraction, wherein the COD concentration in the separated water phase after extraction is greatly reduced, and the treatment difficulty and the safety risk are greatly reduced. And combining the organic extraction liquids separated in the two times, adding the combined organic extraction liquids into a 1L three-neck flask, adding 50g of tap water and 0.5g of activated carbon, heating the mixture in a water bath to 50 ℃, decompressing, pumping and filtering to recover the trichloromethane, filtering while the mixture is hot, cooling and crystallizing the filtrate, filtering, drying the filter cake for 12 hours at 50 ℃ in a vacuum drying oven, and recovering 16.61g of white crystals, namely the methomyl product, thereby finishing the treatment of the methomyl process wastewater. The mass percentage of the methomyl in the product is 98.06% and the recovery rate is 94.7% by analyzing the product by a liquid chromatography external standard method. In the embodiment, water generated in the crystallization process can be reused in the process of transferring methomyl from an organic phase to a water phase, so that the wastewater is reduced, and the treatment cost can be reduced. In this embodiment, the treatment method adopted does not increase the yield of wastewater as a whole.
Example 4
A method for treating methomyl process wastewater comprises the following steps:
1000g of methomyl process wastewater and 200g of chloroform are added into a 2L three-neck flask, stirred for 0.5 hour at 25 ℃, then transferred into a 2L pear-shaped separating funnel, and after standing for 20 minutes, the lower organic extract and the upper aqueous phase are separated. And transferring the upper water phase into a 2L three-neck flask, adding 200g of trichloromethane, repeating the operation, and performing secondary extraction, wherein the COD concentration in the separated water phase after extraction is greatly reduced, and the treatment difficulty and the safety risk are greatly reduced. And combining the organic extraction liquids separated in the two times, adding the combined organic extraction liquids into a 1L three-neck flask, adding 50g of tap water and 1g of activated carbon, heating the mixture in a water bath to 50 ℃, decompressing, pumping, filtering, recovering the trichloromethane, filtering while the mixture is hot, cooling, crystallizing and filtering the filtrate, drying the filter cake for 12 hours at 50 ℃ by using a vacuum drying oven, recovering and obtaining 16.55g of white crystals, namely the methomyl product, and finishing the treatment of the methomyl process wastewater. The mass percentage of the methomyl in the product is 98.22 percent and the recovery rate is 94.5 percent by analyzing the product by a liquid chromatography external standard method. In the embodiment, water generated in the crystallization process can be reused in the process of transferring methomyl from an organic phase to a water phase, so that the wastewater is reduced, and the treatment cost can be reduced. In this embodiment, the treatment method adopted does not increase the yield of wastewater as a whole.
Example 5
A method for treating methomyl process wastewater comprises the following steps:
1000g of methomyl process wastewater and 200g of ethyl acetate are added into a 2L three-neck flask, stirred for 0.5 hour at 25 ℃, then transferred into a 2L pear-shaped separating funnel, and after standing for 20 minutes, an upper organic extract and a lower aqueous phase are separated. And transferring the lower water phase into a 2L three-neck flask, adding 200g of ethyl acetate, repeating the operation, and performing secondary extraction, wherein the COD concentration in the separated water phase after extraction is greatly reduced, and the treatment difficulty and the safety risk are greatly reduced. And combining the organic extraction liquids separated in the two times, adding the combined organic extraction liquids into a 1L three-neck flask, adding 100g of tap water and 2g of activated carbon, heating the mixture in a water bath to 50 ℃, decompressing, pumping, filtering, recovering ethyl acetate, filtering while the mixture is hot, cooling, crystallizing and filtering the filtrate, drying the filter cake for 12 hours at 50 ℃ by using a vacuum drying oven, recovering and obtaining 16.13g of white crystals, namely the methomyl product, and finishing the treatment of the methomyl process wastewater. The mass percentage of the methomyl in the product is 98.31 percent and the recovery rate is 92.2 percent by analyzing the product by a liquid chromatography external standard method. In the embodiment, water generated in the crystallization process can be reused in the process of transferring methomyl from an organic phase to a water phase, so that the wastewater is reduced, and the treatment cost can be reduced. In this embodiment, the treatment method adopted does not increase the yield of wastewater as a whole.
Example 6
A method for treating methomyl process wastewater comprises the following steps:
1000g of methomyl process wastewater and 200g of 1, 2-dichloroethane are added into a 2L three-neck flask, stirred for 0.5 hour at 25 ℃, then the material is transferred into a 2L pear-shaped separating funnel, and after standing for 20 minutes, the lower organic extract and the upper aqueous phase are separated. And transferring the upper water phase into a 2L three-neck flask, adding 200g of 1, 2-dichloroethane, repeating the above operations, and performing second and third extraction, wherein the COD concentration in the separated water phase after extraction is greatly reduced, and the treatment difficulty and safety risk are greatly reduced. And combining the organic extraction liquids separated out in the three times, adding the combined organic extraction liquids into a 1L three-neck flask, adding 80g of tap water and 0.5g of activated carbon, heating the mixture in a water bath to 50 ℃, decompressing, pumping, filtering, recovering 1, 2-dichloroethane, filtering while the mixture is hot, cooling, crystallizing and filtering the filtrate, drying the filter cake for 12 hours at 50 ℃ in a vacuum drying oven, recovering 16.65g of white crystals, namely the methomyl product, and finishing the treatment of the methomyl process wastewater. The mass percentage of the methomyl in the product is 98.27 percent and the recovery rate is 95.1 percent by analyzing the product by a liquid chromatography external standard method. In the embodiment, water generated in the crystallization process can be reused in the process of transferring methomyl from an organic phase to a water phase, so that the wastewater is reduced, and the treatment cost can be reduced. In this embodiment, the treatment method adopted does not increase the yield of wastewater as a whole.
Example 7
A method for treating methomyl process wastewater comprises the following steps:
adding 1000g of methomyl process wastewater and 200g of 1, 2-dichloroethane into a 2L three-neck flask, stirring for 2 hours at 25 ℃, transferring the materials into a 2L pear-shaped separating funnel, standing for 20 minutes, and separating out a lower organic extract and an upper aqueous phase, wherein the COD concentration in the aqueous phase separated after extraction is greatly reduced, and the treatment difficulty and the safety risk are greatly reduced. Adding the lower organic extract into a 1L three-neck flask, adding 50g of tap water and 1g of activated carbon, heating in a water bath to 50 ℃, decompressing, filtering, recovering 1, 2-dichloroethane, filtering while hot, cooling and crystallizing the filtrate, filtering, drying the filter cake for 12 hours at 50 ℃ by using a vacuum drying oven, recovering to obtain 15.13g of white crystals, namely the methomyl product, and finishing the treatment of the methomyl process wastewater. The mass percentage of the methomyl in the product is 98.13 percent and the recovery rate is 86.3 percent by analyzing the product by a liquid chromatography external standard method. In the embodiment, water generated in the crystallization process can be reused in the process of transferring methomyl from an organic phase to a water phase, so that the wastewater is reduced, and the treatment cost can be reduced. In this embodiment, the treatment method adopted does not increase the yield of wastewater as a whole.
The embodiment shows that the treatment method of the methomyl process wastewater has the advantages of simple process, convenience in operation, low treatment cost, high safety and the like, can realize effective pretreatment of the methomyl process wastewater on the premise of not increasing the wastewater yield, obviously reduces the subsequent treatment difficulty of the methomyl process wastewater, has the characteristics of high recovery rate of the methomyl, recycling of an organic solvent and the like, improves the product yield, obtains a high-quality methomyl recovered product, reduces the treatment cost, and is suitable for industrial popularization.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (9)
1. A treatment method of methomyl process wastewater is characterized by comprising the following steps:
s1, mixing the methomyl process wastewater with an organic solvent, extracting, separating and collecting organic extract liquor;
s2, mixing the organic extraction liquid collected in the step S1 with water and activated carbon, recovering the organic solvent in the obtained mixed liquid, and filtering to obtain filtrate;
s3, crystallizing the filtrate obtained in the step S2, filtering, drying and recovering the methomyl to finish the treatment of the methomyl process wastewater.
2. The method for treating methomyl process wastewater as claimed in claim 1, wherein in step S1, the mass ratio of the organic solvent to the methomyl process wastewater is 0.2-0.6: 1.
3. The method for treating methomyl process wastewater as claimed in claim 2, wherein in step S1, the organic solvent is at least one of dichloromethane, trichloromethane, 1, 2-dichloroethane, and ethyl acetate.
4. The method for treating methomyl process wastewater as claimed in claim 2, wherein in step S1, the mass percentage of methomyl in the methomyl process wastewater is 1% -5%.
5. The method for treating methomyl process wastewater as claimed in any one of claims 1 to 4, wherein in step S1, the temperature of the extraction is 5 ℃ to 30 ℃; the extraction time is 0.5 h-2 h; the extraction times are 1 to 3.
6. The method for treating methomyl process wastewater as claimed in any one of claims 1 to 4, wherein the mass ratio of the water to the methomyl process wastewater is 0.05-0.1: 1.
7. The method for treating methomyl process wastewater as claimed in any one of claims 1 to 4, wherein the mass ratio of the activated carbon to the methomyl process wastewater is 0.0005 to 0.002: 1.
8. The method for treating methomyl process wastewater as claimed in any one of claims 1 to 4, wherein in step S2, the method for recovering the organic solvent comprises the steps of: heating the obtained mixed solution to 50 ℃, and performing suction filtration under reduced pressure to complete the recovery of the organic solvent in the mixed solution.
9. The method for treating methomyl process wastewater as claimed in any one of claims 1 to 4, wherein in step S3, the drying is performed under vacuum conditions; the drying temperature is 50 ℃; the drying time is 12 h.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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