CA2470595A1

CA2470595A1 - Glyphosate herbicide composition and method for preparing the same

Info

Publication number: CA2470595A1
Application number: CA 2470595
Authority: CA
Inventors: Pen-Wen Tseng; Jeff Liu; Chi-Chang Wang
Original assignee: Sinon Corp
Current assignee: Sinon Corp
Priority date: 2004-04-20
Filing date: 2004-06-09
Publication date: 2005-10-20
Also published as: BRPI0402224A; TW200534787A; TWI291329B

Abstract

A glyphosate herbicide composition and method for preparing the same are provided. The glyphosate herbicide composition comprises 1 ~ 98% (w/w) water-soluble glyphosate salt derivative, 2 ~ 99% (w/w) organic extender and 0.5 ~ 4% (w/w) water.
The herbicide according to the present invention uses an organic compound as an extender, hence providing a safe, environmentally friendly and effective glyphosate herbicide.

Description

Glyphosate Herbicide Composition and Method for Preparing the Same BACKGROUND OF THE INVENTION
FIELD OF THE INVENTION
The present invention relates to a glyphosate herbicide composition and a method for preparing the same.
DESCRIPTION OF RELATED ART
Glyphosate is a non-selective systemic herbicide widely applied in post-seeding weed control. After application for a period of time, glyphosate is absorbed by leafs and non-ligneous stems and transferred to the interior of the plant. It is very effective against deep-rooted perennial weeds and evergreen or annual or biannual Cyperaceae, Gramineae and broadleaf weed.
Glyphosate has a low water solubility at approximately 10.5 g/l (pH 1.9, 20°C).
Thus, glyphosate herbicide is commonly turned into a salt derivative and then prepared in a liquid formulation before it is marketed. Commonly seen salt derivatives of glyphosate include glyphosate ammonium salt, glyphosate isopropylammonium salt, glyphosate sodium salt, and glyphosate trimesium salt, etc. The glyphosate product in liquid formulation is diluted with water before use; product in the water-soluble granule (WSG) or water dispersible granule(WDG) formulation is added with water to let the granules be dissolved or dispersed in water 'before use.
_1_ The weed control effect of glyphosate and its manufacturing process have been disclosed in US Patent No. 3,799,758, and the process for salt derivatives of glyphosate has been disclosed in US Patent No. 4,405,531. Other published methods for preparing glyphosate herbicide are disclosed in EPO Publication No. 0378985 and US
Patent No.
5,872,078, which respectively relates to admixing glyphosate salt acquired by adding bases to glyphosate acid, the surfactant of ethoxylated tallow amine containing 15 ~ 18 moles of ethylene oxideand inorganic extender, such as ammonium sulfate, potassium sulfate, potassium chloride, sodium sulfate or urea, and then extruding the mixture to obtain a dry water soluble agriculturally acceptable composition. The US
Patent No.
5,612,285 discloses the use of polyethylene glycol having an average molecular weight of from about 7000 ~ 9000 as extrusion aid.
However, the long-term and massive use of the inorganic extender in glyphosate herbicide will lead to acidification or salination of soil. For example, ammonium sulfate is physiologically acidic. This inorganic salt will break down into ammonia and sulfate upon contacting with the moisture in soil. The ammonia will be absorbed by the plant, while the sulfate will be left in the soil and gradually cause the acidic caking of soil, hence lowering the pH of soil. Potassium sulfate and potassium chloride also produce salt, sulfate and chlorine ion after application and gradually cause the acidification of soil.
Urea produces nitrate in the soil after application and its long-term use also lowers the pH
of soil. Sodium sulfate is a main ingredient in saline soil, which is hydrolyzed in soil and exhibits alkalinity to raise gradually the pH of soil to as high as 8.5. If the soil contains large amount of water-soluble salts, such as Na2S04, NaCI, MgS04, CaS04, and MgCl2, it becomes saline soil when the total content of water-soluble salts reaches 0.2% of dry soil amount, and is suitable for the growth of only a few adaptive plants. The addition of surfactant in herbicide or auxiliary agent will cause eye irntation and foaming. Thus, there is a need for developing novel herbicide for weed killing or control without the problem of soil acidification caused by the use of inorganic salt.
SUMMARY OF THE INVENTION
To address the drawback of prior arts, the present invention provides a glyphosate herbicide composition, comprising 1 ~ 98% (w/w) water-soluble glyphosate salt derivative; 2 ~ 99% (w/w) organic extender; and 0.5 ~ 4% {w/w) water.
The glyphosate herbicide composition according to the present invention comprises preferably 41 ~ 85% (w/w) water-soluble glyphosate salt derivative, 13 ~ 57%
(w/w) organic extender; and 1 ~ 2% (w/w) water.
The organic extender in the glyphosate herbicide composition preferably includes 1 ~ 25% monosodium L-glutamate, and more preferably 3 ~ 8% monosodium L-glutamate.
The glyphosate herbicide composition of the present invention is preferably in the form of water-soluble granule, wherein the glyphosate salt is preferably dried glyphosate ammonium salt. If necessary, the glyphosate herbicide of the present invention can be further mixed with other herbicide to enhance the weed control effect, or mixed with insecticide, dustmite rniticide, nematicide, fungicide, or plant growth regulator, The other object of the present invention is to provide a method for preparing _3-water-soluble granules of glyphosate herbicide, comprising the steps of (1) mixing 1 98% (w/w) water-soluble glyphosate salt derivative with 2 ~ 99% (w/w) organic extender into a pre-mixture; (2) milling the pre-mixture into ultrafine powder with at least 90% of powder passing 0.075mm mesh; (c) adding proper amount of water with total weight of 3 ~ 20% (w/w) to the ultrafine powder and mix uniformly; and (d) extruding and drying mixture resulted in step (c) to obtain the water-soluble granules of glyphosate herbicide.
In a preferred embodiment of the present invention, the method for preparing water-soluble granules of glyphosate herbicide comprises the steps of: (1) mixing 41 85% (w/w) water-soluble glyphosate salt derivative with 13 ~ S7% (w/w) organic extender into a pre-mixture; (2) milling the pre-mixture into ultrafine powder with at least 90% of powder passing 0.045 mm mesh; (c) adding a proper amount of water with total weight of 6 ~ 14% (w/w) to the ultrafine powder and mix uniformly; and (d) extruding and drying mixture resulted in step (c) to obtain the water-soluble granules of glyphosate herbicide.
The water-soluble granules of glyphosate prepared according to the aforementioned method preferably have particle size of 0.1 ~ 2.0 mm and length of 0.5 l5mm; more preferably particle size of 0.5 ~ 1.0 mm and length of 1 ~ 6 mm.
The moisture content of aforementioned water-soluble granules is preferably 0.5 ~-4% (w/w), and more preferably 1 ~ 2% (w/w).
The water-soluble glyphosate salt derivative used in the invention includes, but not limited to, glyphosate ammonium salt, glyphosate isopropylammonium salt, glyphosate sodium salt, or glyphosate trimesium salt, preferably dried glyphosate ammonium salt.
The extender or water used in the invention its for modifying the physical properties of the herbicide composition, including attrition resistance, persistent foaming after dilution in water, disintegration in water, and heat storage stability of main ingredient. The organic extender used in the invention. includes, but not limited to, monosodium L-glutamate, glutamic acid, glutamine, lactose, sucrose, glucose, fructose, mannitol, D (+)-xylose, xylitol, xylose, sorbitol, arabinose, or mixtures thereof.
Yet another object of the present invention is to provide a weed control method, comprising the step of applying an effective amount of aforesaid glyphosate herbicide composition pre-emergence or post-emergence to a plant, partial plant, seeds of plant or plant growing area.
The glyphosate herbicide composition according to the present invention is characterized by replacing the conventional inorganic extender, binder, or extrusion aid with organic substances without the addition of auxiliary agent or surfactant.
This simpler formulation will not produce the problems of eye irritation or foaming property with the addition of auxiliary agent or surfactant, nor will it cause acidification of soil with the addition of inorganic salt, while providing excellent weed control effect. It is a new kind of glyphosate herbicide that is safe, environmentally friendly and effective.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to a glyphosate herbicide composition, comprising 1 98% (w/w) water-soluble glyphosate salt derivative, preferably 41 ~ 85% (w/w);

99% (w/w) organic extender, preferably 13 ~ 57% (w/w); and 0.5 ~ 4% (w/w) water, preferably 1 ~ 2% (w/w). If necessary, the glyphosate herbicide of the present invention can be further mixed with other herbicide, including insecticide, dustmite miticide, nematicide, fungicide, or plant growth regulator, to enhance the weed control effect.
The glyphosate herbicide composition is preferably water-soluble granules, wherein the water-soluble glyphosate salt derivative is preferably glyphosate ammonium salt; the organic extender is preferably 1 ~ 25% monosodium L-glutamate, and more preferably 3 ~ 8% monosodium L-glutamate.
The glyphosate herbicide composition uses organic; compounds (e.g. monosodium L-glutamate) or mixtures thereof as extender; the organic compound has functions of extender, binder and extrusion aid that no additional binder, extrusion aid or disintegrating agent is needed in the process to achieve extrusion and formation with ease.
The use of aforementioned organic compound also helps to reduce the attrition resistance of finished product after drying and enhancing the dispersibility of finished product when diluted in water.
The invention further provides a method for preparing water-soluble granules of glyphosate herbicide, comprising the steps of (1) mixing 1 ~ 98% (w/w) water-soluble glyphosate salt derivative with 2 ~ 99% (w/w) organic extender into a pre-mixture, preferably mixing 41 ~ 85% (w/w) water-soluble glyphosate salt derivative with 13~ 57%
(w/w) organic extender; (2) milling said pre-mixture into ultrafine powder with at least 90% of powder passing 0.075mm mesh, preferably 0.045mm mesh to increase the water solubility of the finished product; (c) adding a proper amount of water with total weight of 3 ~ 20% (w/w), preferably 6 ~ 14% (w/w) to said ultrafine powder and mixing uniformly;
and (d) extruding and drying mixture resulted in step (c) to obtain the water-soluble granule of glyphosate herbicide.
'The water-soluble granules of glyphosate herbicide prepared in the aforementioned method preferably have particle size of 0.1 ~ 2.0 mm and length of 0.5 l5mm; more preferably particle size of 0.5 ~ 1.0 mm and length of 1 ~ 6 mm.
The moisture content of said water-soluble granules is preferably 0.5 ~ 4% (w/w), and more preferably 1 ~ 2% (w/w).
'The method for preparing glyphosate herbicide composition and test results are depicted in examples below. These examples of glyphosate herbicide composition and method for preparing the same are meant to illustrate the advantages of the invention, and should not be construed as a limitation on the actual application of the present invention.
Example: Method for preparing water-soluble granules of glyphosate The water-soluble granules of glyphosate herbicide in the examples disclosed herein are prepared by the following steps:
(a) Adding a proper amount of extender to water-soluble glyphosate salt and mixing them with a ribbon blender or an instrument having equivalent function into a pre-mixture of specific concentration;
(b) Subjecting the pre-mixture to the jet miller or are equipment having equivalent function under dry air pressure of 6-8 kg/cm2 to let the granules of the pre-mixture collide with each other and crush into ultrafine powder. After this step, the pre-_7_ mixture has smaller particle sizes with at least 90% of particles passing 0.075mm mesh, preferably 0.045mm mesh, and obtain bigger surface area to increase the water solubility of finished product;
(c) Adding a proper amount of water to the resulting ultrafine powder of water-soluble glyphosate salt and subjecting the mixture to kneading in a kneader to obtain an uniform mixture; theamount of water added is 3 ~~ 20% (w/w) of total mixture weights, preferably 6 ~ 14% (w/w);
(d) Passing the mixture obtained in step (c) through an extrusion granulator to obtain granules with cylindrical shape and particle size of 0.1 ~ 2.Omm, preferably 0.5 l.Omm, and length in the range of 0.5 ~ l5mm, preferably 1 ~ 6mm, depending on the size of mesh used in the extrusion process;
(e) After granulation is achieved, drying the granules in a fluid-bed dryer, oven or a device having equivalent function under 40 ~ 60°C to form dried granules as finished product; the moisture content of the finished product is 0.5 ~ 4%
(w/w), preferably 1 ~ 2% (w/w).
(f) After drying, sieving the resulting granules and returning granules that do not meet the aforesaid specifications to the granulation process; and (g) Putting the finished product to a heat resistance test under 54~2°C, and taking out the product after 14 days for analysis of the main ingredient content (glyphosate salt).
The decomposition rate of the glyphosate salt after drying meets the specification of Food and Agriculture Organization of the United Nations (FAO), that is, not higher than 5%.
_8_ Example 1: Preparing water-soluble granules containing active ingredient of 10%
(w/w) glyphosate ammonium salt Pxe-mixture of water-soluble granules of 10% (w/w)~ly~hosate ammonium salt Composition Weight ratio % (w/w) 95% glyphosate ammonium salt technical 12.00 Monosodium L-glutamate 8.00 Sucrose 80.00 According to the method described in Example, firstly mixing the above ingredients by the indicated ratio with a ribbon blender to obtain a pre-mixture of water-soluble granules of 10% (w/w) glyphosate ammonium salt; subjecting the pre-mixture to a jet miller to crush it into ultrafine powder with at least 90% of powder passing 0.045mm mesh; feeding the ultrafine powder to ribbon blender and introducing water by spraying to obtain a mixture with water content of 9 ~ 11% (w/w); subjecting the mixture to a kneader to obtain uniform distribution of water. Using an extrusion granulator installed with l.Omm mesh to produce cylindrical granules with particle size of 0.8 ~
l.Omm and length of 3 ~ 4mm. Drying the granules in a fluid bed dryer under 40 ~
50°C to remove water in the granules. The final dried granules have a moisture content of approximately 1 2% (w/w). Dried granules that do not meet the aforementioned specifications after sieving are returned to the granulation process.
According to the method described above, water-soluble granules containing active ingredient of 10%w/w glyphosate ammonium salt are obtained.

Example 2: Preparing water-soluble granules containing active ingredient of 41 (wlw) glyphosate ammonium salt Pre-mixture of water-soluble granules o f 41 % (w/w) ~Ivnhosate ammonium salt Composition Wei ht ratio % (w/w~
95% glyphosate ammonium salt technical 45.00 Monosodium L-glutamate $.00 Lactose 47.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 41%w/w glyphosate ammonium salt are obtained.
Example 3: Preparing water-soluble granules containing active ingredient of 50%
(wlw) glyphosate ammonium salt Pre-mixture of water-soluble Qranules of 50% (w/w) glyphosate ammonium salt Composition, Weight ratio % (w/w~
95% gl3rphosate ammonium salt technical 55.00 Monosodium L-glutamate $.00 Glucose 37.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 50%(w/w) glyphosate ammonium salt are obtained.

Example 4: Preparing water-soluble granules containing active ingredient of 60%
(w/w) glyphosate ammonium salt Pre-mixture ofwater-soluble granules of 60% (w/w) ~lvnhosate ammonium salt Com~,osition Weight ratio % (w/w) 95% glyphosate ammonium salt technical 65.00 Monosodium L-glutamate 5.00 Sucrose 30.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 60%w/w glyphosate ammonium salt are obtained.
Example 5: Preparing water-soluble granules containing active ingredient of 74.7%
(w/w) glyphosate ammonium salt Pre-mixture of water-soluble gxanules of 74.7% w/w)~lynhosate ammonium salt Composition V4~ei~ht ratio % (w/w) 95% glyphosate ammonium salt technical 80.00 Monosodium L-glutamate 20.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 74.7%w/w glyphosate ammonium salt are obtained.
Example 6: Preparing water-soluble granules containing active ingredient of 74.7%

(w/w) glyphosate ammonium salt Pre-mixture of water-soluble granules of 74.7% (w/w) ~lvahosate ammonium salt Composition W'ei~ht ratio % yw/w) 95% glyphosate ammonium salt technical 80.00 Monosodium L-glutamate 3.00 Lactose 17.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 74.7%w/w glyphosate ammonium salt are obtained.
Example 7: Preparing water-soluble granules containing active ingredient of 74.7%
(w/w) glyphosate ammonium salt Pre-mixture of water-solubl~anules of 74.7% (w/w~ gl hyp orate ammonium salt Composition ~Nei~ht ratio %~w/w) 95% glyphosate ammonium salt technical 80.00 Monosodium L-glutamate 3.00 Glucose 17.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 74.7%w/w glyphosate ammonium salt are obtained.
Example 8: Preparing water-soluble granules containing active ingredient of 74.7%

(w/w) glyphosate ammonium salt Pre-mixture of water-soluble granules of 74.7% (w/w) glyphosate ammonium salt Composition Weight ratio % w/w 95% glyphosate ammonium salt technical 80.00 Monosodium L-glutamate 3.00 Sucrose 17.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 74.7%w/w glyphosate ammonium salt are obtained.
Example 9: Preparing water-soluble granules containing active ingredient of 74.7%
(wlw) glyphosate ammonium salt Pre-mixture of water-soluble . r~anules of 74.7% (w/w~glyphosate ammonium salt Composition Weight ratio % (w/w) 95% glyphosate ammonium salt technical 80.00 Monosodium L-glutamate 3.00 Fructose 17.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 74.7%w/w glyphosate ammonium salt are obtained.
Example 10: Preparing water-soluble granules containing active ingredient of 74.7%

(w/w) glyphosate ammonium salt Pre-mixture of water-soluble granules of 74.7% (w/w) glvahosate ammonium salt Composition Weight ratio % w/w 95% glyphosate ammonium salt technical 80.00 Monosodium L-glutamate 3.00 Mannitol 17.00 Mixing the above ingredients according to indicated ratios and following the steps in Example 1, water-soluble granules containing active ingredient of 74.7%w/w glyphosate ammonium salt are obtained.
Example 11: Comparison of physical properties The physical properties of glyphosate herbicide prepared in Examples 5 ~ 8 in the aspect of attrition resistance, persistent foaming and disintegration in water and those of glyphosate ammonium salt (GAS) herbicide available on the market are compared in accordance with the guidelines described in the CIPAD Handbook, and the results are depicted in Table 1.
Test methods:
Attrition resistance test method Firstly screening the test samples to 32 mesh and retain 100 g of test sample with particles larger than 32 mesh. Putting the retained sample along with three magnetic balls into a vessel (100mm long and 100rnm in diameter) for hardness testing.
Sealing the vessel and then putting it into a rolling blender. Setting the rotation speed of blender at 75rpm and let the vessel roll for 15 minutes. Taking out the test sample and removing powder adhered to the walls of vessel. Sieving the sample using 32 mesh.
Setting the weight of granules smaller than 32 mesh as A to calculate the attrition resistance by the following formula:
Attrition resistance = A/100 x 100%
Attrition resistance test method Refer to Collaborative International Pesticides Analytical Council Handbook (CIPAC Handbook MT47.1 on persistent foaming) Disinte ation in water test method Adding 100rn1 of 342ppm hard water (in reference to CIPAC MT 18 Standard Waters) into a 250m1 beaker. Weighing 0.2 g of a test sample and pouring it into the beaker from Scm above the water level. Observing the time required for the test sample to transform from granules to powder and recording it; the time observed is the measure of disintegration in water.
Table 1: Comparison of Physical Properties of Water-soluble Granules off 74.7%
Glyphosate Ammonium Salt No. Sample Attrition Persistent Persistent Disintegration foaming foaming in resistance(diluted (diluted water (sec) (%) 50X) (ml) 200X) (ml) 1 74.7% GAS 0.3 5 0 135 (Example 5) 2 74.7% GAS 0.8 24 10 140 (Example 6) 3 74.7% GAS 0.6 0 0 100 (Example 7) 4 74.7% GAS 0.5 4 0 125 (Example 8) 5 74.7% GAS 64.0 65 40 180 (Market brand) -IS-As shown in Table l, the attrition resistance of the market brand was 64.0%, while that of glyphosate ammonium salt herbicide of the invention ranged from 0.3 ~
0.8%.
With regarding to persistent foaming diluted 50 times, that of the market brand was 65m1, S while that of the herbicide of this invention ranged from 0 ~ 24m1; for persistent foaming diluted 200 times, that of market brand was 40m1, while that of Example 6 was only lOml, and that of Examples 5, 7 and 8 were Oml. With regarding to disintegration in water, that of market brand was 180 sec, while herbicide of this invention needed only 100 ~ 140 sec to attain the same level of dispersion. Thus, the glyphosate ammonium salt herbicide according to the present invention is superior to market brand in attrition resistance, persistent foaming and disintegration in water, suggesting that the organic extender in the herbicide composition of the invention can effectively prevent foaming associated with surfactant or auxiliary agent, and provide excellent dispersibility.
Field Test:
Field test was carried out to test the weed control effect of glyphosate herbicide (water-soluble granules containing 74.7% (w/w) glyphosate ammonium salt) prepared in Examples 5, 6 and 7.
A. Materials and method Dividing the Sm x 2m test area (lOM2) into 18 blocks. Applying the test material around fast growing and flowering stage of weeds (see Table 2 for test materials) to 3 blocks per treatment. Prior to application, observing the weed canopy, and species and names of weeds in the test area.
B. Evaluation standards Examining visually the percentage of weed yellowing in each block on day 7, day 15, day 22 and day 29 after application; on day 29 after application, selecting 2 representative sampling spots in each block to collect weeds within 1 square meter of area.
Investigating the number of weeds and their fresh weight.
Weed control rate: Evaluating the effect on 3 ~ 5 major weeds by visual observation (e.g, drying, dwarfing, inhibited growth, number of weeds, weight of weed), and expressing by percentage.
Table 2: Dose of Water-soluble Granules of 74.7% Glyphosate Ammonium Salt and Dose of Active Ingredient in the Field Test No. Sample lFormulation Dose per block Dose of active Dose/hectare (g or rnl) ingredientlhectare (kg or L) (g or ml}
1 Blank control NA 0 0 0 2 74.7% GAS (Example Water-soluble granule 3.3 2460 3.3 5) 3 74.7% GAS (Example Water-soluble granule 3.3 2460 3.3 6) 4 74.7% GAS (Example Water-soluble granule 3.3 2460 3.3 7) 5 85% GAS Water-soluble granule 2.9 2460 2.9 (another brand) 6 41 % glyphosate Liquid 6.0 2460 6.0 isopropylammonium salt (Liquid) 7 74.7% GAS (market Water-soluble granule 3.3 2460 3.3 brand) Group 1 was blank control; Groups 2, 3, and 4 used the formulation of this invention; Group 6 was the liquid formulation control; Groups 5 and 7 were water-soluble granules of other brands. The results of field test axe illustrated in Table 3, 4 and 5 below.
Table 3: Major Weed Species and Canopy (%) of Test Area before Application of Herbicide Weed species Group No.
1 2 3 4 ' S 6 7 Southern crabgrass87 87 87 87.3 85.7 87 86.3 (Digitaria adscendens) Bermudagrass 12.3 12 12 11.3 13.3 12.3 13 (Cynodon dactylon) Purple nutgrass0.7 1 1 1.4 1 0.7 0.7 (Cyperus rotundus) Percentage 100 100 100 100 100 100 100 oftotal ~ ~ ~ ~

canopy Table 4: Change of Percentage of Yellowing (%) No. Sample FormulationDose/hectareDays after application fig' 7 15 22 29 L) 1 Blank controlNA - -b -b -b -b 2 74.7% GAS Water-soluble3.3 51.7a 69.7a 88.7a 100a (Example S) granule 3 74.7% GAS Water-soluble3.3 52.7a 69.Oa 88.7a 100a (Example 6) granule 4 74.7% GAS Water-soluble3.3 52.Oa 69.3a 88.7a 100a (Example 7) granule 5 85% GAS Water-soluble2.9 52.3a 69.3a 89.7a 100a (another granule brand) 6 41% glyphosateLiquid 6.0 52.7a 69.7a 89.7a 100a isopropyiammonium salt (liquid) 7 74.7% GAS Water-soluble3.3 52.3a 70.Oa 90.Oa 100a (market brand) ~ ~ ~ ~
granule IO

Table 5: Fresh Weight of Weeds on Day 29 after Application No. Sample Formulation Dose/hectareFresh weight (kg, L) (gram/m2) 1 Blank controlNA 0 2280a 2 74,7% GAS Water-soluble3.3 1596b (Example granule 5) 3 74.7% GAS Water-soluble3.3 1583b (Example granule 6) 4 74.7% GAS Water-soluble3.3 1224b (Example granule 7) 85% GAS Water-soluble2.9 1332b granule (another brand) 6 41% glyphosate Liquid 6.0 1242b isopropylammonium salt (liquid) 7 74.7% GAS (market Water-soluble granule 3.3 1452b brand) * Statistical analysis used Duncan's Multiple Range Test at 5% significance level; a and b indicate significant difference between treatment blocks.

C. Results 1. Test time and first observation Test material was applied on 09/24/2003. Test field was observed the first time on 10/1/2003 (day 7 after application) and no herbicide toxicity was found.
2. Species of weed Weeds in the test area included: 1. southern crabgrass, 2, bermudagrass, 3.
purple nutgrass.
3. First observation:
Treatment blocks were observed on 10/1/2003 (day 7 after application) and no significant difference among different groups was found, indicating that the herbicide according to the present invention had good preliminary result.

4. The second, third and fourth observations In subsequent observations taken place on 10/912003 and 10/16/2003 (day 15 and day 22 after application), the percentage of yellowing in each treatment block was close without significant difference.
S. The fifth observation In the observation conducted on 10/2312003 (day 29 after application), yellowing in each treatment block reached 100%, indicating excellent weed control effect.
D. Conclusion In the field test, weed control effect in different treatment blocks observed did not show significant difference, indicating that the simpler formulation and process disclosed in the present invention provides the same effect as liquid and granular products available on the market, while offering the advantages of not causing acidification and salination of soil or eye irritation, and the advantage of low foaming.
OTHER EMBODIMENTS
The embodiments of the present invention have been disclosed in the examples.
Anybody familiar with the skills in this field may change or modify the aforesaid steps and conditions and use equipment or methods having identical or equivalent purpose and functions to produce water-soluble granules of glyphosate herbicide or use glyphosate salt derivatives of similar nature or organic compounds to produce glyphosate herbicide composition of this invention. Therefore, other embodiments without departing from the spirits of the invention and appended claim shall remain within the protected scope and claims of the invention.

Claims

1. A glyphosate herbicide composition, comprising 1 ~ 98% (w/w) water-soluble glyphosate salt derivative;

2 ~ 99% (w/w) organic extender; and 0.5 ~ 4% (w/w) water.
2. The glyphosate herbicide composition according to Claim 1, wherein said composition comprises: 41 ~ 85% (w/w) water-soluble glyphosate salt derivative; 13 ~
57% (w/w) organic extender; and 1 ~ 2% (w/w) water.

3. The glyphosate herbicide composition according to Claim 1, wherein said water-soluble glyphosate salt derivative comprises glyphosate ammonium salt, glyphosate isopropylammonium salt, glyphosate sodium salt, or glyphosate trimesium salt.

4. The glyphosate herbicide composition according to Claim 3, wherein said water-soluble glyphosate salt derivative is dried glyphosate ammonium salt.

5. The glyphosate herbicide composition according to Claim 1, wherein said organic extender comprises monosodium L-glutamate, glutamic acid, glutamine, lactose, sucrose, glucose, fructose, mannitol, D (+)-xylose, xylitol, xylose, sorbitol, arabinose, or mixtures thereof.

6. The glyphosate herbicide composition according to Claim 1, wherein said organic extender is 1 ~ 25% monosodium L-glutamate.

7. The glyphosate herbicide composition according to Claim 6, wherein said organic extender is 3 ~ 8% monosodium L-glutamate.

8. The glyphosate herbicide composition according to Claim 1, wherein said herbicide composition is water-soluble granules.

9. The glyphosate herbicide composition according to Claim 1, wherein said herbicide composition is further mixed with other herbicide, insecticide, dustmite miticide, nematicide, fungicide, or plant growth regulator.

10. The glyphosate herbicide composition according to Claim 8, wherein said water-soluble granules have particle size of 0.1 ~ 2.0mm and length of 0.5 ~
15mm.

11. The glyphosate herbicide composition according to Claim 10, wherein said water-soluble granules have particle size of 0.5 ~ 1.0mm and length of 1 ~
6mm.

12. A method for preparing water-soluble granules of glyphosate herbicide, comprising the steps of:
(a) mixing 1 ~ 98% (w/w) water-soluble glyphosate salt derivative with 2 ~ 99%
(w/w) organic extender into a pre-mixture;
(2) milling said pre-mixture into ultrafine powder with at least 90% of powder passing 0.075mm mesh;
(c) adding a proper amount of water with total weight of 3 ~ 20% (w/w) to said ultrafine powder and mixing uniformly; and (d) extruding and drying mixture resulted in step (c) to obtain. the water-soluble granules of glyphosate herbicide.

13. The method according to Claim 12, wherein said ultrafine powder in step (b) is at least 90% passing 0.045 mesh.

14. The method according to Claim 12, wherein total weight of water added in step (c) is 6 ~ 14% (w/w).

15. The method according to Claim 12, wherein the drying temperature in step (d) is 40 ~ 60°C.

16. The method according to Claim 12, wherein in step (a) 41 ~ 85% (w/w) water-soluble glyphosate salt derivative is mixed with 13 ~ 57% (w/w) organic extender into a pre-mixture.

17. The method according to Claim 12, wherein the moisture content of water-soluble granules in step (d) is 0.5 ~ 4% (w/w).

18. The method according to Claim 17, wherein the moisture content of water-soluble granules in step (d) is 1 ~ 2% (w/w).

19. The method according to Claim 12, wherein the water-soluble glyphosate salt derivative in step (a) comprises glyphosate ammonium salt, glyphosate isopropylammonium salt, glyphosate sodium salt, or glyphosate trimesium salt.

20. The method according to Claim 19, wherein the water-soluble glyphosate salt derivative in step (a) is dried glyphosate ammonium salt.

21. The method according to Claim 12, wherein the organic extender in step (a) comprises monosodium L-glutamate, glutamic acid, glutamine, lactose, sucrose, glucose, fructose, mannitol, D (+)-xylose, xylitol, xylose, sorbitol, arabinose, or mixtures thereof.

22. The method according to Claim 12, wherein the organic extender in step (a) is 1 ~ 25% monosodium L-glutamate.

23. The method according to Claim 22, wherein the organic extender in step (a) is 3 ~ 8% monosodium L-glutamate.

24. The method according to Claim 12, wherein the method further comprises the step of mixing other herbicide, insecticide, dustmite miticide, nematicide, fungicide, or plant growth regulator.

25. A method for weed control, comprising the step of applying an effective amount of glyphosate herbicide composition of Claim 1 pre-emergence or post-emergence to a plant, partial plant, seeds of plant or plant growing area.