A phoxim solution and its preparation method

Abstract

This application relates to the technical field of veterinary drugs. Specifically, it relates to a phoxim solution and a preparation method thereof. Among them, the phoxim solution, calculated by weight, includes components: 50 - 150 parts of compound phoxim emulsifiable concentrate, 50 - 150 parts of ethanol. Among them, the compound phoxim emulsifiable concentrate contains 30 - 80% phoxim, 5 - 10% polyethylene glycol, and 1 - 3% diethylamine, and the balance is solvent. The phoxim solution provided by this application can significantly delay the reproduction rate of algae after phoxim degradation, thereby ensuring the stability of dissolved oxygen content in the water body and improving the safety of phoxim application.

Description

Technical Field

[0001] This application relates to the technical field of veterinary drugs. Specifically, it relates to a phoxim solution and a preparation method thereof. Background Art

[0002] Phoxim is an organophosphorus insecticide that disrupts normal nerve conduction by inhibiting the activity of cholinesterase in insects, causing the insects to become paralyzed and eventually die. In addition, phoxim also has an inhibitory effect on the activity of host cholinesterase, enhancing the gastrointestinal peristalsis of the host and accelerating the excretion of the insects from the body.

[0003] Phoxim is widely used in water bodies to kill or expel parasites such as Sinergasilus, Lernaea, Argulus, Ergasilus, Gyrodactylus, Dactylogyrus, and nematodes parasitizing on fish such as black carp, grass carp, silver carp, bighead carp, common carp, crucian carp, and bream, and can achieve good results. However, the phoxim solution in the prior art is prone to cause a large reproduction of algae after degradation, affecting the dissolved oxygen content in the water body, and thus having an impact on the growth and reproduction of fish.

[0004] Therefore, there is an urgent need in the art for a phoxim solution and a preparation method thereof, so this application is proposed. Summary of the Invention

[0005] The purpose of this application is to provide a phoxim solution and a preparation method thereof to solve at least one of the technical problems described in the background art.

[0006] Specifically, in the first aspect of this application, a phoxim solution is provided, which includes the following components by weight:

[0007] 50 - 150 parts of compound phoxim emulsifiable concentrate,

[0008] 50 - 150 parts of ethanol,

[0009] Among them, the compound phoxim emulsifiable concentrate contains 30 - 80% phoxim, 5 - 10% polyethylene glycol, and 1 - 3% diethylamine, and the balance is solvent.

[0010] By adopting the above technical solution, adding polyethylene glycol and diethylamine to the compound phoxim emulsifiable concentrate can significantly delay the reproduction rate of algae after phoxim degradation, thereby ensuring the stability of the dissolved oxygen content in the water body and improving the safety of phoxim application.

[0011] Preferably, the compound phoxim emulsifiable concentrate contains 40 - 60% phoxim, 6 - 8% polyethylene glycol, and 1.5 - 2.5% diethylamine, and the balance is solvent.

[0012] Preferably, the compound phoxim emulsifiable concentrate includes 1 - 5% auxiliary agent.

[0013] Preferably, the auxiliary agent is selected from one or more of styrylphenol polyoxyethylene ether, calcium dodecylbenzenesulfonate, and trifluoroacetic acid.

[0014] Preferably, the solvent is selected from one or more of tetramethylbenzene, tristearate glyceryl, and sec-butyl acetate.

[0015] Preferably, the polyethylene glycol is polyethylene glycol 4000.

[0016] Preferably, the water content of the composite phoxim emulsifiable concentrate is 0.6%-0.8%.

[0017] Preferably, the acidity of the composite phoxim emulsifiable concentrate is less than 0.5%.

[0018] Preferably, the phoxim solution further comprises 0.02-1 part of sodium hypochlorite. More preferably, the phoxim solution further comprises 0.05-0.2 part of sodium hypochlorite.

[0019] Preferably, the degradation rate of the phoxim solution is 45-55% within 14 days under the ultraviolet light intensity of 100 W / m2.

[0020] In a second aspect of the present application, a method for preparing a phoxim solution is provided, comprising the steps of:

[0021] Weigh appropriate amounts of diethylamine and polyethylene glycol, mix thoroughly, and prepare a mixed solution A;

[0022] Dissolve the mixed solution A and an appropriate amount of phoxim technical in an appropriate amount of solvent to prepare a mixed solution B;

[0023] Add appropriate amount of auxiliary agent to mixed solution B, adjust pH to 6-7, and emulsify by shearing to obtain composite phoxim emulsifiable concentrate.

[0024] Preferably, the method for preparing the phoxim solution further comprises the steps of:

[0025] The compound phoxim emulsifiable concentrate is mixed with ethanol and sodium hypochlorite to prepare the phoxim solution.

[0026] Preferably, in the shear emulsification step, the shear rate is 100-200 r / min and lasts for 20-40 min.

[0027] In summary, this application has the following beneficial effects:

[0028] 1. The phoxim solution provided in the present application can significantly slow down the reproduction rate of algae after phoxim degradation by adding polyethylene glycol and diethylamine to the composite phoxim emulsifiable concentrate, thereby ensuring the stability of the dissolved oxygen content in the water body and improving the safety of phoxim application.

[0029] 2. The phoxim solution provided by this application can further control the growth rate of algae and improve the stability of dissolved oxygen in water by controlling the degradation rate of the phoxim solution to be 50 - 60% after 14 days under the ultraviolet light intensity of 100 W / m2.

[0030] 3. The preparation method of the phoxim solution provided by this application prepares mixture A and mixture B successively, which can ensure that the product has good stability, and then it can be fully dispersed after being applied to water bodies, obtaining a better insecticidal effect. Detailed implementation manners

[0031] Here, the exemplary embodiments will be described in detail. The implementation manners described in the following exemplary embodiments do not represent all implementation manners consistent with this application. On the contrary, they are merely examples of devices and methods consistent with some aspects of this application as detailed in the appended claims.

[0032] The terms used in this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The singular forms "a", "the", and "said" used in this application and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise. It should also be understood that the term "and / or" used herein refers to and includes any or all possible combinations of one or more of the associated listed items.

[0033] The following will describe this application in detail through examples.

[0034] The phoxim solution in the prior art is prone to cause a large reproduction of algae after being applied to water bodies, affecting the dissolved oxygen content in water bodies, and then affecting the growth and reproduction of fish. In view of this, the inventive concept of this application is to provide a phoxim solution and its preparation method that can solve the above technical problems. Among them, the phoxim solution includes components in parts by weight: 50 - 150 parts of compound phoxim emulsifiable concentrate, 50 - 150 parts of ethanol. Among them, the compound phoxim emulsifiable concentrate contains 30 - 60% phoxim, 5 - 10% polyethylene glycol, and 3 - 5% diethylamine. According to this inventive concept, by adding polyethylene glycol and diethylamine to the compound phoxim emulsifiable concentrate, the reproduction rate of algae after phoxim degradation can be significantly delayed, thereby ensuring the stability of dissolved oxygen in water bodies and improving the safety of phoxim application.

[0035] Before introducing the technical solution of this application, the main components involved in this application will be introduced first. It should be noted that the compounds not particularly emphasized in this application can be purchased through commercial channels and are not limited to the several introduced below.

[0036] Polyethylene Glycol 4000: It is a white waxy solid flake or granular powder; slightly having a special odor. It is readily soluble in water or ethanol and insoluble in ether.

[0037] Styrylphenol Polyoxyethylene Ether: This product is a light yellow or orange-yellow oily liquid. It becomes semi-fluid state after cooling. It is readily soluble in water and various organic solvents, does not electrolyze in water, and is stable in acid and alkali solutions. It is prone to cracking when contacting with oxidants at high temperature and has good emulsifying properties.

[0038] Tetramethylbenzene: Also known as sym-tetramethylbenzene, it is an organic compound with the chemical formula C10H14, a white crystalline powder, insoluble in water, soluble in ethanol, ether, benzene, and acetone.

[0039] Glyceryl Tristearate: The chemical formula is C57H110O6, which is a natural oil and fat, soluble in hot alcohol, chloroform, benzene, and carbon disulfide, insoluble in water, petroleum ether, ether, and cold alcohol.

[0040] sec-Butyl Acetate: Also known as sec-butyl acetate, it is an organic compound with the chemical formula C6H12O2, a colorless transparent liquid, insoluble in water, miscible with most organic solvents such as ethanol and ether.

[0041] In order to better understand the above technical solutions, the following will describe the above technical solutions in detail in combination with specific implementation manners.

[0042] Experimental Example 1 Test on the Change of Dissolved Oxygen in Water

[0043] This example introduces the experimental method of the test on the change of dissolved oxygen in water in this application. Unless otherwise specified, the test on the change of dissolved oxygen in water in this application is implemented according to the method of this experimental example.

[0044] Specifically, collect the pond water of a certain fish pond, filter it with a 40-mesh sieve and reserve it for use.

[0045] Add 0.1 ml of phoxim solution to 1 m3 of water body. Control the experimental temperature at 25 °C, use a magnetic stirrer to stir the water body at a rate of 30 r / min; irradiate the water body with a fluorescent lamp and control the light intensity at 500 W / m2; for 14 days continuously.

[0046] Detect the dissolved oxygen in the water body on the 0th day, 3rd day, 6th day, 9th day, 12th day, and 14th day respectively.

[0047] Experimental Example 2 Stability Test

[0048] This example introduces the experimental method of the stability test in this application. Unless otherwise specified, the stability test in this application is implemented according to the method of this experimental example.

[0049] Specifically, collect the pond water of a certain fish pond, filter it with a 40-mesh sieve and reserve it for use.

[0050] Add 0.1 ml of phoxim solution to 1 m3 of water body. Control the experimental temperature at 25 °C, and use a magnetic stirrer to stir the water body at a rate of 30 r / min; irradiate the water body with an ultraviolet lamp, and control the light intensity at 30 W / m2 for 14 days.

[0051] Detect the phoxim content in the water body on the 1st day, 2nd day, 3rd day, 7th day, and 14th day respectively.

[0052] Experimental Example 3 Acute Toxicity Experiment

[0053] Conduct an acute toxicity test on juvenile Odontobutis potamophila. The test is carried out in a dark water tank with a total water volume of 1 m3. The top is under normal light during the day and covered with a black sunshade net at night. The breeding water is purified water aerated for 3 days, with a pH of 7.0 - 8.0, a test temperature of (24 ± 2) °C, and a dissolved oxygen ≥ 6.5 mg / L. To prevent the influence of feeding, no bait is fed during the test, and the juveniles grow normally during domestication and the test.

[0054] Adopt the static water biological test method. Put 30 test juvenile fish into each water tank and set up a blank control group. Calculate the safety concentration according to the median lethal concentration at 24 h, 48 h, and 72 h.

[0055] Experimental Example 4 Efficacy Experiment

[0056] The test is carried out in a dark water tank with a total water volume of 1 m3. The top is under normal light during the day and covered with a black sunshade net at night. The breeding water is pond water with fish diseases, and the test temperature is (24 ± 2) °C.

[0057] Put 30 test juvenile Odontobutis potamophila into each water tank and set up a blank control group. Statistically analyze the survival rate of the juvenile fish after 7 days.

[0058] Experimental Example 4

[0059] The applicant found in production that if the input amount of the existing phoxim solution is slightly larger, it may reduce the dissolved oxygen content in the water body, thereby affecting the growth and reproduction of organisms in the water, especially fish.

[0060] Scheme A

[0061] Take 100 parts of phoxim emulsifiable concentrate and 100 parts of ethanol. Among them, the phoxim emulsifiable concentrate contains 50% phoxim, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is the solvent xylene.

[0062] Dissolve the above-mentioned weight parts of phoxim technical in an appropriate amount of xylene solvent weighed, fully mix, add an appropriate amount of auxiliary agent, and adjust the pH to 6, then shear and emulsify to obtain phoxim emulsifiable concentrate.

[0063] The above-mentioned weight parts of phoxim emulsifiable concentrate are mixed with ethanol to prepare a phoxim solution.

[0064] Plan B

[0065] Take 100 parts of compound phoxim emulsifiable concentrate and 100 parts of ethanol, wherein the compound phoxim emulsifiable concentrate contains 50% phoxim, 6% polyethylene glycol, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the remainder is solvent tetramethylbenzene.

[0066] The polyethylene glycol and phoxim technical in the above proportions are weighed and dissolved in an appropriate amount of tetramethylbenzene solvent, and after being fully mixed, an appropriate amount of auxiliary agent is added, and the pH is adjusted to 6, and shear emulsification is performed to obtain a composite phoxim emulsifiable concentrate.

[0067] The above-mentioned weight parts of the composite phoxim emulsifiable concentrate are mixed with ethanol to prepare a phoxim solution.

[0068] Plan C

[0069] Take 100 parts of compound phoxim emulsifiable concentrate and 100 parts of ethanol, wherein the compound phoxim emulsifiable concentrate contains 50% phoxim, 2% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the remainder is solvent tetramethylbenzene.

[0070] The above-mentioned weight portions of diethylamine and phoxim technical are weighed according to the above-mentioned proportion and dissolved in a weighed appropriate amount of tetramethylbenzene solvent. After fully mixing, an appropriate amount of auxiliary agent is added, and the pH is adjusted to 6. Shear emulsification is performed to obtain a composite phoxim emulsifiable concentrate.

[0071] The above-mentioned weight parts of the composite phoxim emulsifiable concentrate are mixed with ethanol to prepare a phoxim solution.

[0072] Plan D

[0073] Take 100 parts of compound phoxim emulsifiable concentrate and 100 parts of ethanol, wherein the compound phoxim emulsifiable concentrate contains 50% phoxim, 6% polyethylene glycol, 2% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is solvent tetramethylbenzene.

[0074] The above-mentioned weight portions of diethylamine, polyethylene glycol and phoxim technical are weighed according to the above-mentioned proportions and dissolved in a weighed appropriate amount of tetramethylbenzene solvent. After fully mixing, an appropriate amount of auxiliary agent is added, and the pH is adjusted to 6. Shear emulsification is performed to obtain a composite phoxim emulsifiable concentrate.

[0075] The above-mentioned weight parts of the composite phoxim emulsifiable concentrate are mixed with ethanol to prepare a phoxim solution.

[0076] Plan E

[0077] Take 100 parts of compound phoxim emulsifiable concentrate and 100 parts of ethanol, wherein the compound phoxim emulsifiable concentrate contains 50% phoxim, 6% polyethylene glycol, 2% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is solvent tetramethylbenzene.

[0078] Weigh the above-mentioned parts by weight of diethylamine and polyethylene glycol according to the above-mentioned proportion, mix them thoroughly, and prepare a mixed solution A;

[0079] Dissolve the mixed solution A and the above-mentioned parts by weight of phoxim technical in a weighed appropriate amount of tetramethylbenzene solvent to prepare a mixed solution B;

[0080] Add appropriate amount of auxiliary agent to mixed solution B, adjust pH to 6, and emulsify by shearing to obtain composite phoxim emulsifiable concentrate.

[0081] The above-mentioned weight parts of the composite phoxim emulsifiable concentrate are mixed with ethanol to prepare a phoxim solution.

[0082] Blank control group

[0083] Add 0.2 ml of deionized water to 1 m3 of water. Control the experimental temperature to 25°C, stir the water at a rate of 30 r / min with a magnetic stirrer, irradiate the water with a fluorescent lamp, and control the light intensity to 500 W / m2 for 14 days.

[0084] Among them, the components selected in Schemes AE are all from the same batch, and the polyethylene glycol is polyethylene glycol 4000. The phoxim solution prepared according to Schemes AE was tested for changes in dissolved oxygen in water according to the method in Experimental Example 1. The oxygen content in the water was measured to be 7.8 mg / L before the experiment. The experimental results are shown in Table 1.

[0085] Table 1 Effect of Scheme AE on dissolved oxygen content in water

[0086]

[0087] In the process of studying this application, the applicant found that the prior art phoxim solution (Scheme A), if added in large amounts and under sufficient light conditions, can easily induce the reproduction of algae and other organisms during degradation, thereby reducing the amount of dissolved oxygen in the water.

[0088] However, the applicant unexpectedly found that when specific components (phoxim, polyethylene glycol, diethylamine, and adjuvant) were used to prepare the composite phoxim emulsifiable concentrate, the reduction in the amount of dissolved oxygen in the water was reduced (Scheme D and Scheme E), which was more conducive to its use in water deworming. Among them, Scheme E adopted a method for preparing phoxim solution that was different from the prior art, which further reduced the amount of dissolved oxygen reduction in the water.

[0089] Experimental Example 5

[0090] Plan F

[0091] Take 100 parts of compound phoxim emulsifiable concentrate, 100 parts of ethanol and 0.1 parts of sodium hypochlorite. The compound phoxim emulsifiable concentrate contains 50% phoxim, 6% polyethylene glycol, 2% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is solvent tetramethylbenzene.

[0092] Weigh the above-mentioned parts by weight of diethylamine and polyethylene glycol according to the above-mentioned proportion, mix them thoroughly, and prepare a mixed solution A;

[0093] Dissolve the mixed solution A and the above-mentioned parts by weight of phoxim technical in a weighed appropriate amount of tetramethylbenzene solvent to prepare a mixed solution B;

[0094] Add appropriate amount of auxiliary agent to mixed solution B, adjust pH to 6, and emulsify by shearing to obtain composite phoxim emulsifiable concentrate.

[0095] The above-mentioned weight parts of the composite phoxim emulsifiable concentrate are mixed with ethanol and sodium hypochlorite to prepare a phoxim solution.

[0096] Plan G

[0097] Take 100 parts of compound phoxim emulsifiable concentrate, 100 parts of ethanol and 0.1 parts of potassium permanganate. The compound phoxim emulsifiable concentrate contains 50% phoxim, 6% polyethylene glycol, 2% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the remainder is solvent tetramethylbenzene.

[0098] Weigh the above-mentioned parts by weight of diethylamine and polyethylene glycol according to the above-mentioned proportion, mix them thoroughly, and prepare a mixed solution A;

[0099] Dissolve the mixed solution A and the above-mentioned parts by weight of phoxim technical in a weighed appropriate amount of tetramethylbenzene solvent to prepare a mixed solution B;

[0100] Add appropriate amount of auxiliary agent to mixed solution B, adjust pH to 6, and emulsify by shearing to obtain composite phoxim emulsifiable concentrate.

[0101] The above weight parts of the composite phoxim emulsifiable concentrate are mixed with ethanol and potassium permanganate to prepare a phoxim solution.

[0102] Scheme H

[0103] Take 100 parts of compound phoxim emulsifiable concentrate, 100 parts of ethanol and 0.1 parts of sodium sulfite. The compound phoxim emulsifiable concentrate contains 50% phoxim, 6% polyethylene glycol, 2% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the remainder is solvent tetramethylbenzene.

[0104] Weigh the above-mentioned parts by weight of diethylamine and polyethylene glycol according to the above-mentioned proportion, mix them thoroughly, and prepare a mixed solution A;

[0105] Dissolve the mixed solution A and the above-mentioned parts by weight of phoxim technical in a weighed appropriate amount of tetramethylbenzene solvent to prepare a mixed solution B;

[0106] Add appropriate amount of auxiliary agent to mixed solution B, adjust pH to 6, and emulsify by shearing to obtain composite phoxim emulsifiable concentrate.

[0107] The above-mentioned weight parts of the composite phoxim emulsifiable concentrate are mixed with ethanol and sodium sulfite to prepare a phoxim solution.

[0108] Scheme I

[0109] Take 100 parts of compound phoxim emulsifiable concentrate, 100 parts of ethanol and 0.1 parts of sodium thiosulfate. The compound phoxim emulsifiable concentrate contains 50% phoxim, 6% polyethylene glycol, 2% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the remainder is solvent tetramethylbenzene.

[0110] Weigh the above-mentioned parts by weight of diethylamine and polyethylene glycol according to the above-mentioned proportion, mix them thoroughly, and prepare a mixed solution A;

[0111] Dissolve the mixed solution A and the above-mentioned parts by weight of phoxim technical in a weighed appropriate amount of tetramethylbenzene solvent to prepare a mixed solution B;

[0112] Add appropriate amount of auxiliary agent to mixed solution B, adjust pH to 6, and emulsify by shearing to obtain composite phoxim emulsifiable concentrate.

[0113] The above-mentioned weight parts of the composite phoxim emulsifiable concentrate are mixed with ethanol and sodium thiosulfate to prepare a phoxim solution.

[0114] Plan J

[0115] Take 100 parts of phoxim emulsifiable concentrate, 100 parts of ethanol and 0.1 parts of sodium hypochlorite, wherein the phoxim emulsifiable concentrate contains 50% phoxim, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the remainder is solvent tetramethylbenzene.

[0116] The above-mentioned weight portion of phoxim technical is dissolved in a weighed appropriate amount of tetramethylbenzene solvent, mixed thoroughly, added with an appropriate amount of auxiliary agent, and the pH is adjusted to 6, and sheared and emulsified to obtain phoxim emulsifiable concentrate.

[0117] The above-mentioned weight parts of phoxim emulsifiable concentrate are mixed with ethanol and sodium hypochlorite to prepare a phoxim solution.

[0118] The components selected in Schemes FJ are from the same batch, and the polyethylene glycol is polyethylene glycol 4000. The phoxim solution prepared according to Schemes AJ was tested for content change of the phoxim solution according to the method in Experimental Example 2, and characterized by degradation. The experimental results are shown in Table 2.

[0119] Table 2 Degradation rate of Scheme AI under UV light

[0120]

[0121]

[0122] According to Table 2, the applicant found in further research that: although the technical solution provided by Solution E of the present application can effectively reduce the reduction of dissolved oxygen in water, when the ultraviolet intensity is relatively high, its degradation rate is too fast (the degradation amount in the first 3 days is close to 50%), resulting in difficulty in achieving sufficient disinfection and killing of parasites in water.

[0123] The applicant unexpectedly found that adding an appropriate amount of sodium hypochlorite to the compound phoxim emulsifiable concentrate component of Solution E can delay its degradation rate and can reach or be slightly better than the degradation rate of the existing phoxim solution (Solution F).

[0124] Furthermore, adding the same amount of sodium hypochlorite to the existing phoxim solution component (Solution A) cannot obtain the technical effect of significantly reducing the degradation rate of the phoxim solution similar to that of Solution F (Solution J).

[0125] Example 1

[0126] Weigh the compound phoxim emulsifiable concentrate component according to the following weight ratio: 30% phoxim, 10% polyethylene glycol 4000, 3% diethylamine, 1% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is solvent xylene.

[0127] Weigh diethylamine, polyethylene glycol, and phoxim technical according to the above ratio, dissolve them in the weighed appropriate amount of xylene solvent, fully mix them, add an appropriate amount of auxiliary agent, adjust the pH to 6, and perform shear emulsification at a shear rate of 100 r / min for 20 min to prepare the compound phoxim emulsifiable concentrate.

[0128] Take 50 parts of the compound phoxim emulsifiable concentrate prepared by the above method and mix it with 150 parts of ethanol to prepare a phoxim solution.

[0129] Example 2

[0130] Weigh the compound phoxim emulsifiable concentrate component according to the following weight ratio: 40% phoxim, 6% polyethylene glycol 4000, 1.5% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is solvent xylene.

[0131] Weigh diethylamine, polyethylene glycol, and phoxim technical according to the above ratio, dissolve them in the weighed appropriate amount of xylene solvent, fully mix them, add an appropriate amount of auxiliary agent, adjust the pH to 6, and perform shear emulsification at a shear rate of 150 r / min for 30 min to prepare the compound phoxim emulsifiable concentrate.

[0132] Take 100 parts of the compound phoxim emulsifiable concentrate prepared by the above method and mix it with 100 parts of ethanol to prepare a phoxim solution.

[0133] Example 3

[0134] The composite phoxim emulsifiable concentrate components were weighed according to the following weight ratio: 60% phoxim, 8% polyethylene glycol 4000, 2.5% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance was solvent tetramethylbenzene.

[0135] According to the above proportion, diethylamine, polyethylene glycol and phoxim technical were weighed and dissolved in an appropriate amount of tetramethylbenzene solvent, and after thorough mixing, an appropriate amount of auxiliary agent was added, and the pH was adjusted to 7. Shear emulsification was performed at a shear rate of 150 r / min for 30 minutes to obtain a composite phoxim emulsifiable concentrate.

[0136] 100 parts of the composite phoxim emulsifiable concentrate prepared according to the above method were taken and mixed with 100 parts of ethanol to prepare a phoxim solution.

[0137] Example 4

[0138] The composite phoxim emulsifiable concentrate components were weighed according to the following weight ratio: 80% phoxim, 5% polyethylene glycol 4000, 1% diethylamine, 5% auxiliary agent styrylphenol polyoxyethylene ether, and the balance was solvent tetramethylbenzene.

[0139] According to the above proportion, diethylamine, polyethylene glycol and phoxim technical were weighed and dissolved in an appropriate amount of tetramethylbenzene solvent, and after fully mixing, an appropriate amount of auxiliary agent was added, and the pH was adjusted to 7. Shear emulsification was carried out at a shear rate of 200 r / min for 40 minutes to obtain a composite phoxim emulsifiable concentrate.

[0140] 150 parts of the composite phoxim emulsifiable concentrate prepared according to the above method were taken and mixed with 50 parts of ethanol to prepare a phoxim solution.

[0141] Example 5

[0142] The composite phoxim emulsifiable concentrate components were weighed according to the following weight ratio: 30% phoxim, 10% polyethylene glycol 4000, 3% diethylamine, 1% auxiliary agent styrylphenol polyoxyethylene ether, and the balance was solvent tetramethylbenzene.

[0143] The above-mentioned parts by weight of diethylamine and polyethylene glycol are fully mixed to prepare a mixed solution A;

[0144] Dissolve the mixed solution A and the above-mentioned parts by weight of phoxim technical in a weighed appropriate amount of tetramethylbenzene solvent to prepare a mixed solution B;

[0145] Add appropriate amount of auxiliary agent to mixed solution B, adjust pH to 6, perform shear emulsification at a shear rate of 100 r / min for 20 min, and obtain composite phoxim emulsifiable concentrate.

[0146] Take 50 parts of the compound phoxim emulsifiable concentrate prepared by the above method and mix it with 150 parts of ethanol to obtain a phoxim solution.

[0147] Example 6

[0148] Weigh the components of the compound phoxim emulsifiable concentrate according to the following weight ratio: 40% phoxim, 6% polyethylene glycol 4000, 1.5% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is the solvent pseudocumene.

[0149] Fully mix the above-mentioned parts by weight of diethylamine and polyethylene glycol to obtain a mixed solution A;

[0150] Dissolve the mixed solution A and the above-mentioned parts by weight of phoxim technical in an appropriate amount of pseudocumene solvent weighed to obtain a mixed solution B;

[0151] Add an appropriate amount of auxiliary agent to the mixed solution B, adjust the pH to 6, and perform shear emulsification at a shear rate of 150 r / min for 30 min to obtain the compound phoxim emulsifiable concentrate.

[0152] Mix the above-mentioned parts by weight of the compound phoxim emulsifiable concentrate with ethanol to obtain a phoxim solution.

[0153] Take 100 parts of the compound phoxim emulsifiable concentrate prepared by the above method and mix it with 100 parts of ethanol to obtain a phoxim solution.

[0154] Example 7

[0155] Weigh the components of the compound phoxim emulsifiable concentrate according to the following weight ratio: 60% phoxim, 8% polyethylene glycol 4000, 2.5% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is the solvent pseudocumene.

[0156] Fully mix the above-mentioned parts by weight of diethylamine and polyethylene glycol to obtain a mixed solution A;

[0157] Dissolve the mixed solution A and the above-mentioned parts by weight of phoxim technical in an appropriate amount of pseudocumene solvent weighed to obtain a mixed solution B;

[0158] Add an appropriate amount of auxiliary agent to the mixed solution B, adjust the pH to 7, and perform shear emulsification at a shear rate of 150 r / min for 30 min to obtain the compound phoxim emulsifiable concentrate.

[0159] Take 100 parts of the compound phoxim emulsifiable concentrate prepared by the above method and mix it with 100 parts of ethanol to obtain a phoxim solution.

[0160] Example 8

[0161] Weigh the components of the compound phoxim emulsifiable concentrate according to the following weight ratios: 80% phoxim, 5% polyethylene glycol 4000, 1% diethylamine, 5% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is the solvent pseudocumene.

[0162] Fully mix the above-mentioned weight portions of diethylamine and polyethylene glycol to obtain a mixed solution A;

[0163] Dissolve the mixed solution A and the above-mentioned weight portion of phoxim technical in an appropriate amount of pseudocumene solvent weighed to obtain a mixed solution B;

[0164] Add an appropriate amount of auxiliary agent to the mixed solution B, adjust the pH to 7, and perform shear emulsification at a shear rate of 200 r / min for 40 min to obtain the compound phoxim emulsifiable concentrate.

[0165] Mix the above-mentioned weight portion of the compound phoxim emulsifiable concentrate with ethanol to obtain a phoxim solution.

[0166] Take 150 parts of the compound phoxim emulsifiable concentrate prepared by the above method and mix it with 50 parts of ethanol to obtain a phoxim solution.

[0167] Example 9

[0168] Weigh the components of the compound phoxim emulsifiable concentrate according to the following weight ratios: 40% phoxim, 6% polyethylene glycol 4000, 1.5% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is the solvent pseudocumene.

[0169] Fully mix the above-mentioned weight portions of diethylamine and polyethylene glycol to obtain a mixed solution A;

[0170] Dissolve the mixed solution A and the above-mentioned weight portion of phoxim technical in an appropriate amount of pseudocumene solvent weighed to obtain a mixed solution B;

[0171] Add an appropriate amount of auxiliary agent to the mixed solution B, adjust the pH to 6, and perform shear emulsification at a shear rate of 150 r / min for 30 min to obtain the compound phoxim emulsifiable concentrate.

[0172] Mix the above-mentioned weight portion of the compound phoxim emulsifiable concentrate with ethanol to obtain a phoxim solution.

[0173] Take 100 parts of the compound phoxim emulsifiable concentrate prepared by the above method, mix it with 100 parts of ethanol and 0.02 part of sodium hypochlorite to obtain a phoxim solution.

[0174] Example 10

[0175] It is basically the same as the technical solution of Example 9, the difference is only that the phoxim solution is obtained by mixing 100 parts of the compound phoxim emulsifiable concentrate, 100 parts of ethanol and 0.05 part of sodium hypochlorite.

[0176] Example 11

[0177] It is basically the same as the technical solution of Example 9, except that the phoxim solution is obtained by mixing 100 parts of compound phoxim emulsifiable concentrate, 100 parts of ethanol, and 0.2 part of sodium hypochlorite.

[0178] Example 12

[0179] It is basically the same as the technical solution of Example 9, except that the phoxim solution is obtained by mixing 100 parts of compound phoxim emulsifiable concentrate, 100 parts of ethanol, and 1 part of sodium hypochlorite.

[0180] Comparative Example 1

[0181] Weigh the phoxim emulsifiable concentrate components according to the following weight ratio: 50% phoxim, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is the solvent xylene.

[0182] Dissolve the above-mentioned weight parts of phoxim technical in the weighed appropriate amount of xylene solvent, fully mix, add an appropriate amount of auxiliary agent, adjust the pH to 6, and perform shear emulsification at a shear rate of 150 r / min for 30 min to obtain phoxim emulsifiable concentrate.

[0183] Take 100 parts of the compound phoxim emulsifiable concentrate prepared by the above method and mix it with 100 parts of ethanol to obtain a phoxim solution.

[0184] Comparative Example 2

[0185] Weigh the compound phoxim emulsifiable concentrate components according to the following weight ratio: 40% phoxim, 6% polyethylene glycol 4000, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is the solvent xylene.

[0186] Weigh polyethylene glycol and phoxim technical according to the above ratio and dissolve them in the weighed appropriate amount of xylene solvent, fully mix, add an appropriate amount of auxiliary agent, adjust the pH to 6, and perform shear emulsification at a shear rate of 150 r / min for 30 min to obtain compound phoxim emulsifiable concentrate.

[0187] Take 100 parts of the compound phoxim emulsifiable concentrate prepared by the above method and mix it with 100 parts of ethanol to obtain a phoxim solution.

[0188] Comparative Example 3

[0189] Weigh the compound phoxim emulsifiable concentrate components according to the following weight ratio: 40% phoxim, 1.5% diethylamine, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance is the solvent xylene.

[0190] Weigh diethylamine and phoxim technical according to the above ratio and dissolve them in the weighed appropriate amount of xylene solvent, fully mix, add an appropriate amount of auxiliary agent, adjust the pH to 6, and perform shear emulsification at a shear rate of 150 r / min for 30 min to obtain compound phoxim emulsifiable concentrate.

[0191] 100 parts of the composite phoxim emulsifiable concentrate prepared according to the above method were taken and mixed with 100 parts of ethanol to prepare a phoxim solution.

[0192] Comparative Example 4

[0193] The components of phoxim emulsifiable concentrate were weighed according to the following weight ratio: 50% phoxim, 2% auxiliary agent styrylphenol polyoxyethylene ether, and the balance was solvent tetramethylbenzene.

[0194] The above-mentioned weight portion of phoxim technical was dissolved in a weighed appropriate amount of tetramethylbenzene solvent, mixed thoroughly, added with an appropriate amount of auxiliary agent, and the pH was adjusted to 6. Shear emulsification was performed at a shear rate of 150 r / min for 30 minutes to obtain phoxim emulsifiable concentrate.

[0195] 100 parts of the composite phoxim emulsifiable concentrate prepared according to the above method were taken and mixed with 100 parts of ethanol and 0.05 parts of sodium hypochlorite to prepare a phoxim solution.

[0196] Test Example 1

[0197] The phoxim solutions prepared by the methods of Examples 1-12 and Comparative Examples 1-4 were tested for safety concentration and efficacy by the methods of Experimental Examples 3 and 4. It can be understood that the same batch of products was selected for the same group of experiments.

[0198] The experimental results are shown in Table 3-1.

[0199] Table 3-1 Quality indicators of phoxim solution-1

[0200]

[0201]

[0202] According to the records in Table 3-1, it can be seen that: First, the safe concentration of the embodiments provided in this application is basically consistent with the existing technology (Comparative Example 1), indicating that its safety for use is qualified; Second, the survival rate of young fish in the embodiments provided in this application is higher than that of the existing technology under the same conditions, proving that the technical solution provided in this application has good application prospects.

[0203] Test Example 2

[0204] The phoxim solutions prepared by the methods of Examples 1-12 and Comparative Examples 1-4 were respectively tested for dissolved oxygen content in the water of the phoxim solutions after 14 days according to the method of Experimental Example 1, and the efficacy was determined according to the method of Experimental Example 4 (the results were the same as those of Test Example 1); further, the phoxim solutions were treated according to the method of Experimental Example 2 for 14 days, and the efficacy was determined again according to the method of Experimental Example 4. It can be understood that the same batch of products was selected for the same group of experiments.

[0205] The experimental results are shown in Table 3-2.

[0206] Table 3-2 Quality Indexes of Phoxim Solution - 2

[0207]

[0208]

[0209] According to the records in Table 3-2, first, for Examples 1-12 provided in this application, after application, it can ensure that the water body has better dissolved oxygen content, which is significantly superior to the prior art, proving that the technical solution provided in this application can better ensure the water body stability and has good application prospects.

[0210] Second, comparing Examples 5-8 with Examples 1-4, Examples 5-8 have higher dissolved oxygen content. It shows that by using the preparation method of Examples 5-8, the phoxim solution with the same components can have a smaller impact on the dissolved oxygen content of the water body, proving that the preparation method of the phoxim solution provided in this application has better technical effects compared with the prior art.

[0211] Third, comparing Examples 9-12 with Examples 1-8, Examples 9-12 have higher juvenile fish survival rates. It shows that by using the technical solution of Examples 9-12, the stability of the phoxim solution in this application under ultraviolet light can be improved, proving that the phoxim solution provided in Examples 9-12 of this application has good stability and a wider application range.

[0212] In addition, after multiple experiments, in Examples 5-12 of this application, the water content in the compound phoxim emulsifiable concentrate is 0.6% - 0.8%, and the acidity is less than 0.5%. However, Examples 1-4 cannot be stably controlled within the above parameter ranges after multiple experiments.

[0213] In summary, the phoxim solution and its preparation method provided in this application can keep the water body solution amount at a higher level on the basis of obtaining qualified products, improving the water body stability; further, the phoxim solution provided in this application has stronger tolerance to ultraviolet light in the water body, and has good stability and application prospects.

[0214] It should be noted that, first, the auxiliary agent in the examples of this application can be replaced by calcium dodecylbenzenesulfonate or trifluoroacetic acid without affecting the conclusion of this application; second, the solvent in the examples of this application can be replaced by glyceryl tristearate or sec-butyl acetate without affecting the conclusion of this application.

[0215] For those of ordinary skill in the art, the technical features in the above examples can be freely combined, and the formed technical solutions also belong to the disclosed examples of this application.

[0216] Furthermore, without departing from the principle of the present application, several improvements and modifications can also be made to the present application, and these improvements and modifications also fall within the protection scope of the claims of the present application.

Claims

1. A phoxim solution, Features: In parts by weight, the components include: 50-150 parts of compound phoxim emulsifiable concentrate, 50-150 parts of ethanol, The composite phoxim emulsifiable concentrate contains 30-80% phoxim, 5-10% polyethylene glycol, and 1-3% diethylamine, and the remainder is solvent.

2. The phoxim solution according to claim 1, Features: The composite phoxim emulsifiable concentrate contains 40-60% phoxim, 6-8% polyethylene glycol, and 1.5-2.5% diethylamine, and the remainder is solvent.

3. The phoxim solution according to claim 2, Features: The composite phoxim emulsifiable concentrate further comprises 1-5% of an auxiliary agent.

4. The phoxim solution according to claim 3, Features: The auxiliary agent is selected from one or more of styrylphenol polyoxyethylene ether, calcium dodecylbenzenesulfonate and trifluoroacetic acid.

5. The phoxim solution according to claim 1, Features: The solvent is selected from one or more of tetramethylbenzene, tristearate glyceryl, and sec-butyl acetate.

6. The phoxim solution according to claim 1, Features: The polyethylene glycol is polyethylene glycol 4000.

7. The phoxim solution according to claim 1, Features: The phoxim solution has a degradation rate of 45-55% in 14 days under the ultraviolet light intensity of 100 W / m 2 .

8. The phoxim solution according to any one of claims 1 to 7, Features: The phoxim solution also includes 0.02-1 parts of sodium hypochlorite.

9. A method for preparing the phoxim solution as claimed in claims 1 to 8, Features: Includes steps: Weigh appropriate amounts of diethylamine and polyethylene glycol, mix thoroughly, and prepare a mixed solution A; Dissolve the mixed solution A and an appropriate amount of phoxim technical in an appropriate amount of solvent to prepare a mixed solution B; Add appropriate amount of auxiliary agent to mixed solution B, adjust pH to 6-7, and emulsify by shearing to obtain composite phoxim emulsifiable concentrate.

10. The method for preparing phoxim solution according to claim 9, Features: The preparation method of the phoxim solution also includes the steps of: The compound phoxim emulsifiable concentrate is mixed with ethanol and sodium hypochlorite to prepare the phoxim solution.

Images