Liquid composition and process thereof

Abstract

The present invention provides a liquid composition for defoliation of crop plants comprising a metal chlorate and alkali metal halide. The invention also provides a process for preparing the liquid composition for defoliation of crop plants and a method of defoliating crop plants.

Claims

1. A liquid composition for defoliation of crop plants, the liquid composition consisting of: about 10 wt % to about 80 wt % magnesium chlorate; about 2 wt % to about 30 wt % of sodium chloride, each based on a total weight of the liquid composition, and water.

2. The liquid composition as claimed in claim 1, wherein the sodium chloride is present in an amount from about 2% to about 10% of the total weight of the liquid composition.

3. The liquid composition as claimed in claim 1, wherein the sodium chloride is present in an amount less than 20% by the total weight of the liquid composition.

4. The liquid composition as claimed in claim 1, wherein the sodium chloride is present in an amount less than 10% by the total weight of the liquid composition.

5. The liquid composition as claimed in claim 1, wherein the sodium chloride is present in an amount less than 7.5% by the total weight of the liquid composition.

6. A process for preparing a liquid composition for defoliation of crop plants, wherein the process comprising: a) dissolving an alkali metal chlorate and alkali metal halide separately in water at a temperature of less than or equal to about 40° C. to provide a solution; and b) heating the solution to a temperature not less than about 90° C. and adding magnesium chloride to the heated solution to obtain a reaction mixture; c) heating the reaction mixture at a temperature not less than about 100° C. for at least about four hours to obtain a first product; d) removing water from the first product to form a second product; e) adding acetone to the second product and stirring for at least 60 minutes at a temperature of not less than 50° C. to form a third product, and further cooling the third product; f) filtering the third product after cooling to obtain a precipitate; g) removing acetone from the precipitate at a temperature not exceeding 90° C. obtain a fourth product, and adding water to the fourth product thereby forming the liquid composition.

7. The process for preparing a liquid composition as claimed in claim 6, wherein the alkali metal chlorate consists of of sodium chlorate and the alkali metal halide consists of sodium chloride.

8. A method of defoliating crop plants, said method comprising applying, to the crop plants that are required to be defoliated, a liquid composition consisting of about 10 wt % to about 80 wt % of magnesium chlorate; about 2 wt % to about 30 wt % of sodium chloride, each based on a total weight of the composition; and water.

9. The liquid composition of claim 1, wherein the liquid composition consists of: about 20 wt % to about 70 wt % of the magnesium chlorate; about 2 wt % to about 10 wt % of the sodium chloride, each based on the total weight of the liquid composition; and water.

10. The liquid composition of claim 9, wherein the sodium chloride is present in an amount of about 2 wt % to less than 7.5 wt. % based on the total weight of the liquid composition.

11. The method of claim 7, wherein the liquid composition consists of: about 10 wt % to about 80 wt % of the magnesium chlorate; about 2 wt % to about 30 wt % of the sodium chloride, each based on the total weight of the liquid composition; and water.

12. The method of claim 7, wherein the liquid composition consists of: about 20 wt % to about 70 wt % of the magnesium chlorate; about 2 wt % to about 10 wt % of the sodium chloride, each based on the total weight of the liquid composition; and water.

13. The method of claim 12, wherein the sodium chloride is present in an amount of about 2 wt % to less than 7.5 wt. % based on the total weight of the liquid composition.

14. The method of claim 8, wherein the liquid compositions consists of: about 20 wt % to about 70 wt % of the magnesium chlorate; about 2 wt % to about 10 wt % of the sodium chloride, each based on the total weight of the liquid composition; and water.

15. The method of claim 14, wherein the sodium chloride is present in an amount of about 2 wt % to less than 7.5 wt. % based on the total weight of the liquid composition.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 shows evaluation of defoliation activity of exemplary liquid formulations of the disclosure with different concentrations of magnesium cholorate on a bean crop.

(2) FIG. 2 shows evaluation of burndown activity of exemplary liquid formulations of disclosure with different concentration of magnesium chlorate on a bean crop.

DESCRIPTION OF THE INVENTION

(3) It has now been found, surprisingly, that these disadvantages of magnesium chlorate are overcome and liquid magnesium chlorate performs well when the relative percentage of halide salt is lesser in the defoliant composition in comparison to the conventional compositions. This composition of Magnesium chlorate and sodium chloride defoliate crop plants, even in relatively cool weather.

(4) Thus, in an aspect, the present invention provides a liquid composition for defoliation of crop plants, the composition comprising: (a) a metal chlorate; and (b) a reduced quantity of an alkali metal halide.

(5) It has now been found that a defoliant composition containing a metal chlorate as the defoliant is more physico-chemically stable and demonstrates better defoliant and burndown activity when the quantity of the metal halide in the composition is reduced in comparison to the conventional defoliant compositions. All the conventional defoliant compositions included an appreciable quantity of the ‘contaminant_ alkali metal halide. It was found that when liquid defoliant compositions were prepared comprising reduced quantities of the alkali metal halide in comparison to the conventional defoliant compositions, the resultant compositions surprisingly possessed better physicochemical stability in addition to improved defoliant and burndown activity.

(6) The term ‘reduced quantity_ of alkali metal halide as used herein denotes a quantity of the alkali metal halide that is less than 30% by total weight of the composition, preferably less than 20% by total weight of the composition, more preferably less than 10% of weight of the composition, and most preferably less than 7.5% by total weight of the composition.

(7) According to another embodiment of the present invention, the liquid composition for defoliation of crop plants comprises from about 0.1% to about 95% and preferably from about 10% to about 80% of the metal chlorate by total weight of the composition.

(8) In a preferred embodiment of the present invention, the metal chlorate is present in an amount from about 20% to about 70% of the total weight of the defoliant composition.

(9) In an embodiment, the metal chlorate defoliant may be selected from the group consisting of sodium chlorate, magnesium chlorate, calcium chlorate, calcium-magnesium chlorate and potassium chlorate.

(10) In an embodiment, the metal chlorate defoliant is magnesium chlorate.

(11) In an embodiment, the metal chlorate defoliant may include trace amounts of inherent phosphorus.

(12) In an embodiment, the defoliant composition of the present invention comprises a reduced quantity of an alkali metal halide than is present in all known defoliant compositions.

(13) In an embodiment, the defoliant composition of the present invention comprises a reduced quantity of sodium halide.

(14) In an embodiment, the defoliant composition of the present invention comprises a reduced quantity of sodium chloride.

(15) According to another embodiment of the present invention, the liquid composition for defoliation of crop plants comprises from about 0.1% to about 30% and preferably from about 1% to about 20% of sodium chloride by the total weight of the composition.

(16) In a preferred embodiment of the present invention, sodium chloride is present in an amount from about 2% to about 10% of the total weight of the herbicide formulation.

(17) In an embodiment, the defoliant composition of the present invention comprises water.

(18) In an embodiment, water is used in a sufficient quantity to enable stable compositions of the metal chlorate defoliant of a desired strength to be prepared. The percentage quantity of water present in the liquid compositions of the present inventions is not particularly limiting and may be conveniently decided by a person skilled in the art.

(19) In an embodiment, the liquid composition of the present invention is in the form of an aqueous formulation. The aqueous formulation of the invention has greater ease of application in defoliant actions, greater ease of application in burndown actions, can be used to defoliate crop plants even in relatively cool weather, has a normal spraying moment without any drift and therefore does not cause any harm to the neighbouring crops, and does not produce foam during application of the composition on the crop plants.

(20) In an aspect, the present invention provides a process for preparing a liquid composition for defoliation of crop plants.

(21) The process for preparing the liquid composition comprises: (a) dissolving an alkali metal chlorate and alkali metal halide in water; and (b) adding a second metal halide to the reaction mass.

(22) The alkali metal chlorate and alkali metal halide form the cation portion of the metal halide component of the composition, while the second metal halide provides the metal portion of the final metal chlorate defoliant.

(23) In an embodiment, sodium chlorate and sodium chloride are dissolved in water, to which an alkaline earth halide is added to form the corresponding alkaline earth chlorate defoliant.

(24) In an embodiment, sodium chlorate and sodium chloride are dissolved in water, to which magnesium chloride is added to form the corresponding magnesium chlorate defoliant. This composition comprises sodium chloride as the salt.

(25) In another embodiment, the liquid composition remains stable at low temperature.

(26) In an embodiment, the defoliant composition of the present invention may be prepared by a non-limiting process comprising the steps of: (a) dissolving sodium chlorate and sodium chloride in charged water at temperature not exceeding 40° C. in a suitable assembly; (b) heating the mixture to a temperature not less than 90° C. and adding magnesium chloride solution for 60 minutes and continue heating for at least one hour to obtain reaction mass; (c) cooking the reaction mass at temperature not less than 100° C. for atleast 4 hours; (d) recovering water upon completion of reaction by applying pressure; (e) adding acetone to the reaction mass and stirring for atleast 60 minutes at a temperature not less than 50° C. and further cooling the reaction mass; (f) filtering the reaction mass and washing it with acetone; (g) recovering the acetone at a temperature not exceeding 90° C. atmospherically; and adding water to magnesium chloride to obtain desired strength.

(27) In another aspect, the present invention also provides a method of defoliating crop plants, said method comprising applying, to the crop plants that are required to be defoliated, a liquid composition comprising a metal chlorate; and a reduced quantity of an alkali metal halide.

(28) In another embodiment, the liquid composition is effective in defoliating crop plants even at relatively cool weather.

(29) The preferred embodiments of the liquid composition used in this aspect of the invention are as described hereinabove in respect of the preferred embodiments for the liquid compositions of the invention.

(30) The process of preparing liquid composition containing magnesium chlorate is ascertained by the experiments as exemplified below. These examples are merely illustrations and are not to be understood as limiting the scope and underlying principles of the invention in anyway. Indeed, various modifications of the invention in addition to those shown and described herein will become apparent to those skilled in the art from the following examples and foregoing description.

Example 1

(31) Equipped assembly with overhead stirrer, condenser, and an addition funnel in Oil-Bath. Sodium chlorate crystal and sodium chloride were dissolved in charged water at 30-35éC. The quantity of ingredients is according to Table 1. Magnesium chloride solution was added to the mixture and further heated for 1 hour at 90éC to obtain reaction mass of magnesium chlorate. The reaction mass was continued to cook for at least 4 hours at temperature not less than 100éC. At the completion of reaction, water was removed under vacuum and wet cake was obtained. Acetone wash was applied to the wet cake at least for 1 hour at temperature not exceeding 70éC and kept for drying. After acetone wash, wet cake was filtered and dried and finally 50-52% magnesium chlorate was obtained from the above procedure.

(32) TABLE-US-00001 TABLE 1 Ingredients Quantity Sodium chlorate 661 g Sodium chloride  39 g Magnesium 1000 g  chloride solution Charged water 808 g

(33) Test for Storage Stability

(34) The liquid magnesium chlorate composition according to present invention was tested for storage stability. Stability of the solid magnesium chlorate was also ascertained for comparative assessment of the liquid and solid magnesium chlorate preparations. The storage stability of solid magnesium chlorate and liquid magnesium chlorate according to the present invention is presented in the below tables (Table 2):

(35) TABLE-US-00002 TABLE 2 REAL TIME STABILITY DATA OF MAGNESIUM CHLORATE (50% SOLUTION) STABILITY AT RT Batch No. 0 15 30 60 90 UPA/890-009/#177 days days days days days % Mg(ClO.sub.3).sub.2 51.86 51.70 51.80 51.75 51.81 % NaCl 5.90 5.97 5.99 6.00 6.00 REAL TIME STABILITY DATA OF MAGNESIUM CHLORATE SOLID STABILITY AT RT Batch No. 0 60 90 120 180 UPA/879-113/#165 days days days days days % Mg(ClO.sub.3).sub.2 42.75 42.18 41.72 41.11 40.18 % NaCl 25.75 25.90 26.15 26.20 26.23

(36) The results of the above table show that samples UPA/890-009/#177 prepared according to method described in the present invention and UPA/879-113/#165 was prepared according to the standard conventional procedure. It can be seen from the table that liquid magnesium chlorate, comprising the reduced amount of sodium chloride, was quite stable from 0-90 days with very less degradation. The amount of sodium chloride also remained almost stable from 0-90 days. A clear solution was thus maintained over the scale of 0-90 days.

(37) Similarly, solid magnesium chlorate was assessed for real time stability on the scale of 0-180 days. A little deterioration of magnesium chlorate was observed. There was negligible deterioration in the amount of sodium chloride.

Preparation of Liquid Magnesium Chlorate with Higher Amount of Sodium Chloride

(38) With an objective to study the effect of quantity of sodium chloride in the liquid compositions, the liquid composition of magnesium chlorate with 5% sodium chloride was compared with a liquid composition of magnesium chlorate with 10% sodium chloride. Liquid compositions (Table 3) were prepared according to the process disclosed in the present invention with 5% and 10% sodium chloride respectively.

(39) Physical observations (Table 4) were made to identify critical features with liquid composition of magnesium chlorate with 10% sodium chloride. It was observed that the liquid composition of magnesium chlorate remains stable at ambient conditions but sodium chloride crystallize at low temperature. A separate layer of sodium chloride crystals settled at the bottom of the flask with liquid magnesium chlorate composition with 10% sodium chloride.

(40) TABLE-US-00003 TABLE 3 Ingredients Quantity (%) Magnesium 52 52 Chloride Sodium 5 10 Chloride Water q.s. q.s. Total 100 100 

(41) TABLE-US-00004 TABLE 4 Liquid composition of Liquid composition of magnesium chlorate with magnesium chlorate with Observations 5% sodium chloride 10% sodium chloride Physical Clear Translucent Appearance at Ambient Physical Clear Layer of Sodium Chloride Appearance settled at the bottom. at Low Temperature Hygroscopicity 1.28 1.64

(42) Field Trial

Example 1

(43) Test in Beans-Pre-Harvesting

(44) Details of experiment: a) Treatments: 8 (Eight) b) Test Crop: Beans c) Time of application: Pre-harvest d) Observation days: 2 days after application e) Treatment details: This study was performed on beans crop where the crop was ready for harvest. The aim of study was to evaluate the efficacy of liquid composition of magnesium chlorate in defoliation and also its burndown effect Field study was conducted to evaluate performance of the liquid composition of the present invention in comparison to the conventional solid. To observe the burn down and defoliation effect, a portion of land with standing crops without receiving any kind of treatment was considered as control.

(45) Various liquid compositions (Aq1, Aq2 and Aq3) were prepared at different dosages of magnesium chlorate (3 Kg/Ha, 4 Kg/Ha and 5 Kg/Ha) to optimize effective dose of magnesium chlorate in the liquid composition as defoliant. Similarly, solid compositions (SI1, SI2, SI3 and SI4) were prepared with varied dosages (3 Kg/Ha, 4 Kg/Ha and 5 Kg/Ha) of magnesium chlorate. All these compositions were evaluated for defoliation activity. The bean crop was evaluated on second day after treatment for defoliation action of liquid composition (Table 5 and FIG. 1). Crop received three treatments with different dosages vis. 3 kg/Ha as Aq1, 4 Kg/Ha as Aq2 and 5 Kg/Ha as Aq3 of the liquid composition. Similarly, three treatments of different dosages vis. 3 kg/Ha as SI1, 4 Kg/Ha as SI2 and 5 Kg/Ha as SI3 of conventional solid composition were given to the crop. Upon evaluating defoliation effect on 2DAT, it was found that liquid composition resulted in better defoliation in comparison to untreated control and the conventional solid composition.

(46) Comparative study of liquid Magnesium Chlorate composition and Solid Magnesium Chlorate composition to evaluate defoliant activity.

(47) TABLE-US-00005 TABLE 5 Crop Defoliation 2DAT Product # (Kg-L/Ha) Block 1 Block 2 Block 3 Block 4 Average 1 Check 0 0 0 0 0 2 Aq1 (3.0) 60 60 70 70 65 3 Aq2 (4.0) 75 60 60 65 65 4 Aq3 (5.0) 70 70 60 65 66.25 5 Sl1 (3.0) 40 40 65 60 51.25 6 Sl2 (4.0) 65 60 50 35 52.5 7 Sl3 (5.0) 70 75 50 50 61.25

(48) Similarly, liquid composition (Aq1, Aq2 and Aq3) were prepared at different dosages of magnesium chlorate (3 Kg/Ha, 4 Kg/Ha and 5 Kg/Ha) to optimize effective dose of magnesium chlorate in the liquid composition as burndown. Solid composition (SI1, SI2, SI3 and SI4) were prepared with varied dosages (3 Kg/Ha, 4 Kg/Ha and 5 Kg/Ha) of magnesium chlorate. All these compositions were evaluated for burndown activity. The bean crop was evaluated on second day after treatment for defoliation action of liquid composition (Table 6 and FIG. 2). Crop received three treatments with different dosages vis. 3 kg/Ha as Aq1, 4 Kg/Ha as Aq2 and 5 Kg/Ha as Aq3 of the liquid composition. Three treatments of different dosages vis. 3 kg/Ha as SI1, 4 Kg/Ha as SI2 and 5 Kg/Ha as SI3 of conventional solid composition were also given to the crop. Upon evaluating burndown effect on 2DAT, it was found that liquid composition resulted in better burndown in comparison to untreated control and the conventional solid composition.

(49) Comparative study of liquid Magnesium Chlorate composition and Solid Magnesium Chlorate composition to evaluate burndown activity.

(50) TABLE-US-00006 TABLE 6 Crop Burndown 2 DAT Product # (Kg-L/Ha) Block 1 Block 2 Block 3 Block 4 Average 1 Check 0 0 0 0 0 2 Aq1 (3.0) 50 60 50 60 55 3 Aq2 (4.0) 80 60 70 60 67.5 4 Aq3 (5.0) 80 70 60 70 70 5 Sl1 (3.0) 30 40 60 50 45 6 Sl2 (4.0) 70 70 60 40 60 7 Sl3 (5.0) 60 80 40 60 60

(51) Therefore, it was concluded that the liquid composition having lesser sodium salt content of the present invention showed far more superior effect in both defoliation action as well as burndown action. The liquid composition with lesser sodium salt content does not affect the plant adversely. The liquid composition is found better than the solid conventional composition of Magnesium chlorate in terms of efficacy.

(52) While the foregoing written description of the invention enables one of ordinary skill to make and use what is considered presently to be the best mode thereof, those of ordinary skill will understand and appreciate the existence of variations, combinations, and equivalents of the specific embodiment, method, and examples herein. The invention should therefore not be limited by the above described embodiment, method, and examples, but by all embodiments and methods within the scope and spirit of the invention.