CN107686777B

CN107686777B - Water-soluble granules of methoxone salt and preparation method thereof

Info

Publication number: CN107686777B
Application number: CN201610630582.0A
Authority: CN
Inventors: 孙国庆; 侯永生; 吴勇; 路雪林; 陈帅
Original assignee: Shandong Weifang Rainbow Chemical Co Ltd
Current assignee: Shandong Weifang Rainbow Chemical Co Ltd
Priority date: 2016-08-03
Filing date: 2016-08-03
Publication date: 2020-09-25
Anticipated expiration: 2036-08-03
Also published as: AU2017100484A4; AU2017100484B4; AU2016101531A4; CN107686777A

Abstract

The invention relates to the technical field of pesticides, and discloses a methoxone salt water-soluble granule and a preparation method thereof. The water dispersible granule consists of dimethyl tetrachloro salt, a specific surfactant, a chelating agent and a filler. The methoxone salt water-soluble granule can achieve better storage stability, solubility and dissolution stability and lasting foamability in high-concentration hard water by adjusting the type of the methoxone salt water-soluble granule assistant and combining and using proper accessories, and is particularly suitable for countries and regions with higher water hardness.

Description

Water-soluble granules of methoxone salt and preparation method thereof

Technical Field

The invention relates to the technical field of pesticides, in particular to a methoxone salt water-soluble granule and a preparation method thereof.

Background

The methoxone is a methoxone phenoxy carboxylic acid selective herbicide, has strong systemic conductivity, is mainly used for post-emergence stem and leaf treatment, the medicament penetrates through a cuticle and a cytoplasmic membrane and is finally conducted to each part, different influences are generated on nucleic acid and protein synthesis at different parts, nucleic acid metabolism and protein synthesis are inhibited at the top of a plant, a growth point stops growing, young and tender leaves cannot stretch until photosynthesis can not be normally carried out; the medicament is conducted to the lower part of the plant, so that the synthesis of nucleic acid and protein of the stem tissue of the plant is increased, the abnormal division of cells is promoted, the root tip is expanded, the capability of absorbing nutrients is lost, the stem is distorted and deformed, the sieve tube is blocked, the phloem is damaged, and the transportation of organic matters is blocked, so that the normal living capability of the plant is damaged, and finally the plant is dead. For many years, methoxone is widely used in wheat fields, corn fields, rice paddy fields, urban lawns, hemp crops to control annual or perennial broadleaf weeds and parts of sedges; can also be used as a rice root removing agent and can improve the seedling pulling effect. The compound fertilizer is used for soil treatment, and has certain control effect on annual grass and perennial weed sprouts propagated by seeds. The fertilizer is widely used due to the advantages of low cost, high speed, no residue, safety to succeeding crops and the like.

The pure product of the methoxone is non-volatile colorless crystals, and the industrial product is yellow to white solid powder. The solubility in water at 25 ℃ is about 300mg, and the organic solvent is easy to dissolve. Because the solubility of the methoxone in water is very low, the methoxone is generally required to be prepared into water-soluble salts or oil-soluble esters in practical application, such as: methoxone dimethylamine salt, methoxone isooctyl, methoxone sodium, methoxone thioethyl ester, methoxone thioester, methoxone isopropylamine salt, methoxone ethyl butyrate, and the like. At present, main preparations of methoxone are water aqua, water soluble powder and missible oil. The effective content of the aqueous solution is 13%, the rest components are mainly water, the preparation increases the transportation cost, the effective components are low in dosage, and the environmental protection and resource waste are not facilitated; the water soluble powder mainly comprises 56% sodium salt, although the water soluble powder is a solid preparation, the powder material is easy to form dust, and potential safety hazards exist to producers and users; the missible oil contains a large amount of organic solvents, belongs to an environmentally-friendly preparation, and has great damage to the environment, wherein part of the solvents have great potential safety hazards to producers and users.

Under the condition of reasonable formula, the Water soluble granule (SG or WSG) can be quickly disintegrated after entering Water, the formed solution is stable, and the solubility is higher, so that the utilization rate of the effective components is also higher. The water-soluble granules have higher requirements on the formula and the preparation process, the selection of auxiliary materials is matched with that of the main medicine, and WSG prepared by selecting improper auxiliary materials cannot achieve good solubility, so that the prepared water-soluble granules have long disintegration time and low suspension rate.

Chinese patent CN104705301A discloses a methoxone salt water-soluble granule and a preparation method thereof, wherein the methoxone salt water-soluble granule is prepared from methoxone salt, a specific surfactant and a water-soluble filler, the suspension rate of the preparation is improved, and the disintegration time and the foaming property are reduced. However, the product is tested and researched, and found that the beneficial effects of the product in all aspects are only suitable for countries and regions with low water hardness, and like australia, countries with common high-concentration hard water still have the phenomena of poor product quality, such as poor storage stability, poor solubility and dissolution stability and low lasting foamability, so that the drug effect of methoxone cannot be fully exerted.

Disclosure of Invention

In view of the above, an object of the present invention is to provide water-soluble granules of methoxone salt and a method for preparing the same, which have better storage stability, solubility and dissolution stability, and persistent foaming properties under conditions of high concentration hard water.

In order to achieve the above purpose, the invention provides the following technical scheme:

the water soluble granule of methoxone salt is characterized in that the granule consists of methoxone salt, surfactant, chelating agent and filler;

the surfactant is one of alkylphenol polyoxyethylene polyoxypropylene ether, lauryl alcohol polyoxyethylene ether, fatty amine polyoxyethylene ether, alkyl naphthalene sulfonate, fatty alcohol polyoxyethylene ether alkyl naphthalene sulfonic acid formaldehyde condensate and dodecyl sulfate; or ethylene oxide-propylene oxide block copolymers and alkyl glycosides; or both a polycarboxylate and polyethylene glycol; or both methyl ethylene oxide and polyoxyethylene fatty acid esters;

the chelating agent is one or more than two of ethylene diamine tetraacetic acid, ethylene diamine tetraacetic acid disodium, ethylene diamine tetraacetic acid tetrasodium and sodium tripolyphosphate.

Aiming at the defect that the existing water-soluble granules of the methoxone salt cannot be suitable for high-concentration hard water, the invention adjusts the types of auxiliary materials, increases a chelating agent, and limits the specific matching combination of a surfactant and the chelating agent, thereby solving the problem that the performance of the methoxone salt water-soluble granules is poor under the condition of high-concentration hard water.

Preferably, the surfactant and chelating agent are used in one of the following combinations:

(1) alkyl naphthalene sulfonate and disodium edetate;

(2) ethylene oxide-propylene oxide block copolymers, alkyl glycosides and ethylene diamine tetraacetic acid;

(3) methyl oxirane, polyoxyethylene fatty acid esters, and tetrasodium ethylenediaminetetraacetate;

(4) alkylphenol polyoxyethylene polyoxypropylene ether and ethylenediamine tetraacetic acid;

(5) polyoxyethylene lauryl ether and tetrasodium ethylene diamine tetraacetate;

(6) fatty alcohol-polyoxyethylene ether and sodium tripolyphosphate;

(7) fatty alcohol-polyoxyethylene ether alkyl naphthalene sulfonic acid formaldehyde condensate and ethylene diamine tetraacetic acid tetrasodium;

(8) sodium lauryl sulfate and sodium tripolyphosphate;

(9) polycarboxylates, polyethylene glycols and sodium tripolyphosphate.

Preferably, in the water-soluble granules, by weight, 10-90% of dimethyltetrachloro salt, 1-20% of surfactant, 1-10% of chelating agent and the balance of filler are contained; more preferably, 30-90% of dimethyl tetrachloro salt, 1-10% of surfactant, 1-6% of chelating agent and the balance of filler; further preferably, 50-90% of dimethyl tetrachloro salt, 1-5% of surfactant, 1.5% of chelating agent and the balance of filler; most preferably, the dimethyl tetrachloro salt is 90%, the surfactant is 2%, the chelating agent is 1.5%, and the balance is the filler.

In some embodiments of the present invention, the weight percentages of the components may be selected as follows:

(1) 90% of dimethyl tetrachloro salt, 2% of surfactant, 1.5% of chelating agent and the balance of filler;

(2) 80% of dimethyl tetrachloro salt, 2% of surfactant, 1.5% of chelating agent and the balance of filler;

(3) 50% of dimethyl tetrachloro salt, 10% of surfactant, 6% of chelating agent and the balance of filler;

(4) 30% of dimethyl tetrachloro salt, 2% of surfactant, 1.5% of chelating agent and the balance of filler;

(5) 10% of dimethyl tetrachloro salt, 2% of surfactant, 1.5% of chelating agent and the balance of filler;

(6) 50% of dimethyl tetrachloro salt, 2% of surfactant, 1.5% of chelating agent and the balance of filler;

(7) 90% of dimethyl tetrachloro salt, 3.5% of surfactant, 0.5% of chelating agent and the balance of filler;

(8) 70% of dimethyl tetrachloro salt, 9.5% of surfactant, 3.5% of chelating agent and the balance of filler;

(9) 40% of dimethyl tetrachloro salt, 12% of surfactant, 4% of chelating agent and the balance of filler;

(10) 10% of dimethyl tetrachloro salt, 20% of surfactant, 6% of chelating agent and the balance of filler;

(11) 60% of dimethyl tetrachloro salt, 12% of surfactant, 3% of chelating agent and the balance of filler;

(12) 40% of dimethyl tetrachloro salt, 15% of surfactant, 5% of chelating agent and the balance of filler;

(13) 20% of dimethyl tetrachloro salt, 20% of surfactant, 6% of chelating agent and the balance of filler;

preferably, the alkyl naphthalene sulfonate is Morwet EFW, available from akzo nobel; the ethylene oxide-propylene oxide block copolymer is PE6200, available from Basff; the polyoxyethylene fatty acid ester is selected from A (OEO) series emulsifiers, preferably A-105 series emulsifiers, which are commercially available; preferably, the polycarboxylate is TERSPERSE-2700 available from huntman.

Preferably, the dimethyltetrachloro salt of the present invention is a dimethyltetrachloropotassium salt, a dimethyltetrachlorosodium salt, a dimethyltetrachlorodimethylamine salt, a dimethyltetrachloroethylamine salt, a dimethyltetrachloroisopropylammonium salt, a dimethyltetrachlorocholine salt or a dimethyltetrachlorotriisopropanolate salt. The respective methoxone salt may be purchased or made by oneself, and the method for making by oneself may be referred to as follows:

mixing methoxone with alkaline substance for 10-15min, adding 12-16% water, and reacting at 45-55 deg.C for 50-70min to obtain methoxone salt. Wherein the alkaline substance is selected from sodium hydroxide, potassium carbonate, potassium hydroxide, potassium bicarbonate, ammonium bicarbonate, ammonia, isopropylamine, sodium carbonate, sodium bicarbonate, dimethylamine, triisopropanol and choline according to the type of the desired dimethyltetrachloro salt. The molar ratio of the methoxone to the basic substance is 1 (1-1.1), preferably 1: 1.04.

Preferably, the filler is one or more of ammonium sulfate, diammonium hydrogen phosphate, sodium sulfate, sodium chloride, urea, potassium nitrate, ammonium chloride, dipotassium hydrogen phosphate, sucrose, potassium sulfate and sodium tripolyphosphate.

Meanwhile, the invention also provides a preparation method of the water-soluble granules of the methoxone salt, which comprises the steps of uniformly mixing the methoxone salt with the surfactant, the chelating agent and the filler, then adding water for mixing, extruding, granulating and drying to obtain the methoxone salt water-soluble granules.

Preferably, the drying is drying at 50-75 ℃.

The comparison of the water-soluble granules of the tetrachloro dimethylmethane salt and products of examples 13-47 in the prior patent CN104705301A on the storage stability, the solubility, the dissolution stability and the lasting foamability in high-concentration hard water shows that the water-soluble granules of the tetrachloro dimethylmethane salt are obviously higher than the products in the prior patent.

Meanwhile, the chelating agent different from the chelating agent adopted by the invention and different types of surfactants are selected for comparative tests, and the results show that the excellent product performance can be exerted in a high-concentration hard water environment only on the premise of the compatibility of the selected surfactant and the chelating agent.

According to the technical scheme, the methoxone salt water-soluble granule which can achieve better storage stability, solubility, dissolution stability and lasting foamability in high-concentration hard water is prepared by adjusting the type of the methoxone salt water-soluble granule auxiliary agent and combining and using appropriate auxiliary materials, and is particularly suitable for countries and regions with higher water hardness.

Detailed Description

The embodiment of the invention discloses a methoxone salt water-soluble granule and a preparation method thereof, and a person skilled in the art can appropriately improve process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to those skilled in the art are deemed to be included within the invention. The methoxone water soluble granules of the present invention and the method of making the same have been described in terms of preferred embodiments, and it will be apparent to those skilled in the art that modifications, or appropriate variations and combinations of the products and methods described herein may be made to implement and use the techniques of the present invention without departing from the spirit, scope and content of the invention.

The water soluble granules are in percentage by mass of the components in the total feeding, but the water soluble granules are generally not 100% pure in purchased or prepared tetrachlor, the feeding amount of the tetrachlor in the total feeding refers to the tetrachlor containing impurities, and the weight percentage of the tetrachlor is the pure tetrachlor in the total feeding.

The water-soluble granules of methoxone salt and the preparation method thereof provided by the present invention are further described below.

Example 1: preparation of dimethyltetrachloro salt

421.1g of raw methoxone (with the purity of 95%) and alkaline substances (with the purity of more than 99%) are put into a 1L kneader with a heating device, mixed for 10min to 15min at normal temperature and normal pressure, added with 12% to 16% of water, heated to 45 ℃ to 55 ℃, and reacted for 50min to 70min to obtain the tetrachlor. Wherein the reaction conditions of the respective dimethyltetrachloro salts are shown in Table 1;

TABLE 1 preparation conditions of dimethyltetrachloro salt

Example 2: 90% water soluble granules of potassium methoxone

93.75g of dimethyl tetrachloro potassium salt (with the purity of 96 percent), 2g of Morwet EFW (Akzo Nobel, alkyl naphthalene sulfonate), 1.5g of EDTA disodium and 2.75g of cane sugar are weighed, mixed, added with 3 percent of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to obtain the finished product of the dimethyl tetrachloro potassium salt soluble granule with the mass fraction of 90 percent, and the yield of 99.7 percent.

Example 3: 80% water soluble granules of methoxone potassium salt

83.3g of methoxone potassium salt (with the purity of 96 percent), 2g of Morwet EFW (Akzo Nobel, alkyl naphthalene sulfonate), 1.5g of EDTA disodium and 13.2g of cane sugar are weighed, mixed, added with 3 percent of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to obtain the finished methoxone potassium salt soluble granule product with the mass fraction of 80 percent, and the yield is 99.5 percent.

Example 4: 50% water soluble granules of potassium methoxone

52.1g of methoxone potassium salt (with the purity of 96 percent), 2g of Morwet EFW (Akzo Nobel, alkyl naphthalene sulfonate), 1.5g of EDTA disodium and 44.4g of cane sugar are weighed, mixed, added with 2.5 percent of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to obtain the finished methoxone potassium salt soluble granule product with the mass fraction of 50 percent, and the yield is 99.3 percent.

Example 5: 30% water soluble granules of potassium methoxone

31.3g of methoxone potassium salt (with the purity of 96 percent), 2g of Morwet EFW (Akzo Nobel, alkyl naphthalene sulfonate), 1.5g of EDTA disodium and 65.2g of cane sugar are weighed, mixed, added with 1.5 percent of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to obtain the finished product of the methoxone potassium salt soluble granule with the mass fraction of 30 percent, and the yield is 99.1 percent.

Example 6: 10% water soluble granules of potassium methoxone

After 110.4g of methoxone potassium salt (with the purity of 96%), 2g of Morwet EFW (Akzo Nobel, alkyl naphthalene sulfonate), 1.5g of EDTA disodium and 86.1g of cane sugar are weighed and mixed, 0.5% of water is added, the mixture is put into a 1L kneader to be fully kneaded, extruded, granulated and dried, and the finished methoxone potassium salt soluble granule product with the mass fraction of 10% is prepared, and the yield is 99.0%.

Example 7: 90% water soluble granule of dimethyl tetrachloro dimethylamine salt

93.75g of dimethyldichlorodimethylamine salt (with the purity of 96 percent), 2g of Morwet EFW (Akzo Nobel, alkyl naphthalene sulfonate), 2.75g of EDTA disodium and 1.8g of cane sugar are weighed, mixed, added with 4 percent of water, put into a 1L kneader to be fully kneaded, extruded, granulated and dried to prepare the finished product of the dimethyldichlorodimethylamine salt soluble granules with the mass fraction of 90 percent, and the yield is 99.0 percent.

Example 8: 80% water soluble granule of metoclopramide

83.3g of dimethyl tetrachloro isopropylammonium salt (with the purity of 96%), 2g of Morwet EFW (Akzo Nobel, alkyl naphthalene sulfonate), 1.5g of EDTA disodium and 13.2g of cane sugar are weighed, mixed, added with 3.5% of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to obtain the finished product of the dimethyl tetrachloro isopropylammonium salt soluble granule with the mass fraction of 80%, and the yield is 98.7%.

Example 9: 50% water soluble granule of methoxone choline salt

52.1g of methoxone choline salt (with the purity of 96%), 2g of Morwet EFW (Akzo Nobel, alkyl naphthalene sulfonate), 1.5g of EDTA disodium and 44.4g of cane sugar are weighed, mixed, added with 4.5% of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to obtain the finished product of the methoxone choline salt soluble granule with the mass fraction of 50%, and the yield is 98.5%.

Example 10: 90% water soluble granules of potassium methoxone

993.75g of dimethyl tetrachloro potassium salt (with the purity of 96%), 1.5g of PE6200 (basf, ethylene oxide-propylene oxide block copolymer), 2% of APG (alkyl glycoside), 0.5g of EDTA and 2.25g of ammonium sulfate are weighed, mixed, added with 3.2% of water, put into a 1L kneader to be fully kneaded, extruded, granulated and dried to prepare the finished product of the dimethyl tetrachloro potassium salt soluble granule with the mass fraction of 90%, and the yield is 99.2%.

Example 11: 70% water soluble granules of potassium methoxone

72.9g of methoxone potassium salt (with the purity of 96 percent), 6.5g of T-2700(Hunstman, polycarboxylate), 3g of polyethylene glycol, 3.5g of sodium tripolyphosphate, 5g of sodium chloride and 9.1g of potassium nitrate are weighed, mixed, added with 4.2 percent of water, put into a 1L kneader to be fully kneaded, extruded, granulated and dried to obtain the finished methoxone potassium salt soluble granule product with the mass fraction of 70 percent, and the yield is 98.8 percent.

Example 12: 40% water soluble granules of potassium methoxone

41.7g (with the purity of 96%) of the dimethyltetrachloro potassium salt, 10g of methyl ethylene oxide, 2g of A-105 (emulsifier A (OEO) series), 4.0g of tetrasodium EDTA, 20g of ammonium nitrate and 22.3g of dipotassium hydrogen phosphate are weighed, mixed, added with 8.2% of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to prepare a finished product of the dimethyltetrachloro potassium salt soluble granule with the mass fraction of 40%, and the yield is 98.5%.

Example 13: 10% water soluble granules of potassium methoxone

Weighing 10.4g of dimethyl tetrachloro potassium salt (with the purity of 96%), 20g of alkylphenol polyoxyethylene polyoxypropylene ether, 6.0g of EDTA6, 40g of ammonium chloride and 23.6g of diammonium hydrogen phosphate, mixing, adding 10.0% of water, fully kneading in a 1L kneader, extruding, granulating and drying to obtain a finished product of the dimethyl tetrachloro potassium salt soluble granule with the mass fraction of 10%, wherein the yield is 98.1%.

Example 14: 60% water soluble granule of sodium methoxone

62.5g of sodium methoxone (with the purity of 96 percent), 12g of polyoxyethylene lauryl ether, 3.0g of tetrasodium EDTA, 20g of sodium chloride and 2.5g of urea are weighed, mixed, added with 5.0 percent of water, put into a 1L kneader to be fully kneaded, extruded, granulated and dried to obtain the finished product of the sodium methoxone soluble granule with the mass fraction of 60 percent, and the yield is 98.3 percent.

Example 15: 50% water soluble granule of dimethyl tetrachloroammonium salt

Weighing 52.1g of dimethyl tetrachloroammonium salt (with the purity of 96 percent), 10g of fatty alcohol-polyoxyethylene ether, 6.0g of sodium tripolyphosphate and 31.9g of sodium sulfate, mixing, adding 6.0 percent of water, putting into a 1L kneader, fully kneading, extruding, granulating and drying to obtain a finished product of dimethyl tetrachloroammonium salt soluble granules with the mass fraction of 50 percent, wherein the yield is 98.0 percent.

Example 16: 40% water soluble granule of methoxone triisopropanolamine salt

41.7g of MCPA (purity of 96%), 15g of fatty alcohol-polyoxyethylene ether alkyl naphthalene sulfonate formaldehyde condensate, 5.0g of EDTA tetrasodium, 30g of potassium sulfate and 8.3g of potassium sulfate are weighed, mixed, added with 7.0% of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to obtain a finished product of MCPA (mass fraction) triisopropanol amine salt soluble granules with the yield of 98.1%.

Example 17: 20% water soluble granules of methoxone choline

Weighing 20.8g of methoxone triisopropanol ammonium salt (with the purity of 96 percent), 20g of sodium dodecyl sulfate, 6.0g of sodium tripolyphosphate, 40g of potassium sulfate and 13.2g of ammonium chloride, mixing, adding 9.0 percent of water, fully kneading in a 1L kneader, extruding, granulating and drying to obtain the finished product of the methoxone triisopropanol salt soluble granule with the mass fraction of 20 percent, wherein the yield is 98.0 percent.

Example 18: comparative test

Comparison: 1. CN104705301A example 13-example 47 product (hereinafter abbreviated CN13-CN 47);

2. the chelating agents other than the chelating agents in the invention are replaced on the basis of the formulas of the example 2, the example 10, the example 11 and the example 15, and the dosage is unchanged, and the chelating agents are respectively the chelating agents of the example 2: citric acid; example 10: tartaric acid; example 11: calcium gluconate; example 15: sodium metaphosphate; (hereinafter abbreviated as controls 1 to 4);

3. the formulation of example 2 was replaced with alkylnaphthalene sulfonates other than Morwet EFW in the same amounts as Tamol NN 8906 (basf), Morwet D-400 (Acksonobel), TP04 (British grass David); (hereinafter abbreviated as control 5-7);

4. on the basis of the formula of CN13-CN17, other chelating agents except the chelating agent are added, the dosage is 1.5 percent, and the chelating agents are CN 13: tartaric acid; CN 14: sodium gluconate; CN 15: monosodium diacetate; CN 16: sorbitol; CN 17: sodium metaphosphate; (hereinafter abbreviated as control 8-12);

all examples of the invention and the above 4-type control were placed in the same high concentration hard water: (3 times of D water, the hardness of 1026mg/L, the pH value of 6.0-7.0 and Ca²⁺:Mg²⁺4:1), and the detection refers to a method provided in CIPAC manual, namely physical and chemical methods of pesticide raw materials and preparations, and the quality standard refers to FAO pesticide standard formulation and instruction manual and pesticide soluble powder product standard writing standard, which are specifically shown in Table 2.

TABLE 2 test standards

Inspection item	Inspection method	Standard of merit
			Water content%	MT30.5	≤2.0
pH	MT75.3	5-10
			Solubility and solubility stability	MT179	5min≤2.0％；18h≤2.0％
Long-lasting foamability	MT47.2	≤30ml
			Storage stability	MT46.3	54℃±2℃14d

The results are shown in Table 3.

TABLE 3 test results

As is obvious from the results in Table 3, the water-soluble granules of the methoxone salt of the present invention meet the requirements in three product performances of storage stability, solubility, dissolution stability and persistent foamability and have performances far better than the standard requirements in a high concentration hard water environment; the existing patent products and the comparison products basically do not meet the standard requirements, and the effect of the invention is obviously different from that of the invention.

While the results of the controls 1-4 show that not all chelating agents in combination with the other components of the invention are able to achieve the desired product performance; the results of controls 5-7 show that only suitable surfactant and chelant combinations of the present invention can achieve superior results; the controls 8-12 show that even if some chelating agents outside the range defined by the present invention are added to the products of the prior patents, the product performance cannot be improved.

Example 19: test of drug efficacy

The product of the embodiment of the invention is used for carrying out the drug effect test in New south Wales in Australia (high-concentration hard water quality), the crop is Wheat (Wheat), and the control object is Wild radish (Wild radish raphanacross); when the wild radish grows to 2-leaf stage, the control is carried out, the daily temperature of the application is 11 ℃, the humidity is 79 percent, the test field is acid red soil, the pH is 5.4, the dosage is 2175g a.i/ha, and the result is shown in the table 4:

TABLE 4 comparison of drug effects (35 days after application)

Examples	Control of wild radish%
		2	95.0
3	94.5
		4	94.3
5	94.1
		6	94.7
7	92.2
		8	91.7
9	91.1
		10	86.8
11	85.8
		12	86.1
13	85.2
		14	82.5
15	80.8
		16	80.2
17	80.3
		CN13	76.2
Clear water control	0

As can be seen from the control effect test in Table 4, the water-soluble granules of methoxone salt of the invention have significantly higher control effect on wild radish than the products of the control patents in the high-concentration hard water environment.

The foregoing is only for the purpose of understanding the method of the present invention and the core concept thereof, and it will be understood by those skilled in the art that various changes and modifications may be made without departing from the principle of the invention, and the invention also falls within the scope of the appended claims.

Claims

1. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

93.75g of methoxone potassium salt with the purity of 96 percent, alkyl naphthalene sulfonate Morwet EFW2g purchased from Akzo Nobel, 1.5g of EDTA disodium and 2.75g of cane sugar are weighed and mixed, then 3 percent of water is added, the mixture is put into a 1L kneader to be fully kneaded, extruded, granulated and dried, and the finished methoxone potassium salt soluble granule product with the mass fraction of 90 percent is prepared, and the yield is 99.7 percent.

2. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

83.3g of methoxone potassium salt with the purity of 96 percent, 2g of alkyl naphthalene sulfonate Morwet EFW purchased from Akzo Nobel, 1.5g of EDTA disodium and 13.2g of cane sugar are weighed, mixed, added with 3 percent of water, put into a 1L kneader and fully kneaded, extruded, granulated and dried to prepare the finished methoxone potassium salt soluble granule product with the mass fraction of 80 percent, and the yield is 99.5 percent.

3. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

52.1g of the methoxone potassium salt with the purity of 96 percent, 2g of alkyl naphthalene sulfonate Morwet EFW purchased from Akzo Nobel, 1.5g of EDTA disodium and 44.4g of cane sugar are weighed and mixed, 2.5 percent of water is added, the mixture is put into a 1L kneader to be fully kneaded, extruded, granulated and dried, and the finished methoxone potassium salt soluble granule product with the mass fraction of 50 percent is prepared, and the yield is 99.3 percent.

4. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

31.3g of the methoxone potassium salt with the purity of 96 percent, 2g of alkyl naphthalene sulfonate Morwet EFW purchased from Akzo Nobel, 1.5g of EDTA disodium and 65.2g of cane sugar are weighed and mixed, 1.5 percent of water is added, the mixture is put into a 1L kneader to be fully kneaded, extruded, granulated and dried, and the finished product of the methoxone potassium salt soluble granule with the mass fraction of 30 percent is prepared, and the yield is 99.1 percent.

5. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

110.4g of the methoxone potassium salt with the purity of 96 percent, the alkyl naphthalene sulfonate Morwet EFW2g purchased from Akzo Nobel, 1.5g of EDTA disodium and 86.1g of cane sugar are weighed and mixed, 0.5 percent of water is added, the mixture is put into a 1L kneader to be fully kneaded, and the finished product of the methoxone potassium salt soluble granule is prepared by extrusion granulation and drying, wherein the yield is 99.0 percent.

6. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

93.75g of the dimethyldichlorodimethylamine salt with the purity of 96 percent, 2g of alkyl naphthalene sulfonate Morwet EFW purchased from Akzo Nobel, 2.75g of EDTA disodium and 1.8g of cane sugar are weighed and mixed, 4 percent of water is added, the mixture is put into a 1L kneader to be fully kneaded, extruded, granulated and dried, and the finished product of the dimethyldichlorodimethylamine salt soluble granule with the mass fraction of 90 percent is prepared with the yield of 99.0 percent.

7. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

83.3g of the dimethyl tetrachloroisopropylamine salt with the purity of 96 percent, 1.5g of alkyl naphthalene sulfonate Morwet EFW2g purchased from Akzo Nobel, 1.5g of EDTA disodium and 13.2g of cane sugar are weighed, mixed, added with 3.5 percent of water, put into a 1L kneader to be fully kneaded, extruded, granulated and dried to prepare the finished product of the dimethyl tetrachloroisopropylamine salt soluble granules with the mass fraction of 80 percent, and the yield is 98.7 percent.

8. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

52.1g of methoxone choline salt with the purity of 96 percent, Morwet EFW2g of alkyl naphthalene sulfonate purchased from Akzo Nobel, 1.5g of EDTA disodium and 44.4g of cane sugar are weighed and mixed, 4.5 percent of water is added, the mixture is put into a 1L kneader to be fully kneaded, extruded, granulated and dried, and the finished product of the methoxone choline salt soluble granule with the mass fraction of 50 percent is prepared, and the yield is 98.5 percent.

9. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

72.9g of potassium methoxone with the purity of 96 percent, T-27006.5 g of polycarboxylate purchased from Hunstman, 3g of polyethylene glycol, 3.5g of sodium tripolyphosphate, 5g of sodium chloride and 9.1g of potassium nitrate are weighed, mixed, added with 4.2 percent of water, put into a 1L kneader to be fully kneaded, extruded, granulated and dried to prepare the finished product of the potassium methoxone soluble granule with the mass fraction of 70 percent, and the yield is 98.8 percent.

10. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

weighing 10.4g of methoxone potassium salt with the purity of 96%, 20g of alkylphenol polyoxyethylene polyoxypropylene ether, 6.0g of EDTA, 40g of ammonium chloride and 23.6g of diammonium hydrogen phosphate, mixing, adding 10.0% of water, fully kneading in a 1L kneader, extruding, granulating and drying to obtain the finished product of methoxone potassium salt soluble granules with the mass fraction of 10%, wherein the yield is 98.1%.

11. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

62.5g of MCPA sodium salt with the purity of 96%, 12g of polyoxyethylene lauryl ether, 3.0g of EDTA tetrasodium, 20g of sodium chloride and 2.5g of urea are weighed, mixed, added with 5.0% of water, put into a 1L kneader to be fully kneaded, extruded, granulated and dried to obtain the MCPA sodium salt soluble granule finished product with the mass fraction of 60%, and the yield is 98.3%.

12. The water-soluble granules of the methoxone salt are characterized by being prepared by the following preparation method:

weighing 52.1g of the methoxone amine salt with the purity of 96%, 10g of fatty alcohol-polyoxyethylene ether, 6.0g of sodium tripolyphosphate and 31.9g of sodium sulfate, mixing, adding 6.0% of water, putting into a 1L kneader, fully kneading, extruding, granulating and drying to obtain the finished product of the methoxone amine salt soluble granule with the mass fraction of 50%, wherein the yield is 98.0%.