Title of Invention

A PROCESS FOR THE PREPARATION OF PESTICIDE

Abstract

"A process for preparation of pesticide". This invention relates to a process for preparation of pesticide comprising treating cut and crushed leaves, flowers, fruits and tender stem of calotropis, gigantean and/or calotropis procera, nerium oleander and hydrocarpus each separately with dichloro ethane to get the extract and solid parts thereof, the residual masses obtained after treatments of the above cut and crushed leaves, flower, tender stem, fruits and/or stems, each of which is dissolved in diethylene glycols or polyethylene glycol separately and filtered, the filtrates so obtained are mixed in the range of 40-60% Calotropis extract, 20-30% Hydrocarpus extract, 20-30% Oleander extract in order to prepare the pesticide formulation, taking the said formulation in a glass beaker separately and adding 30% hydrochloric acid with or without zinc chloride thereof, stirring said beaker for a period of 1-3 hours at a temperature of 15-50°C and cooled, an ionic emulsifier and nonyl phenol ethylene oxide is then added therein and mixed well, to which antioxidants alongwith para amino benzoic acid is mixed in order to obtain amber liquid or turbid liquid for use as a pesticide.

Full Text

Field of Invention This invention relates to a process for the preparation of a pesticide for use in the agriculture and horticulture fields. The use of phytochemical pesticides is known in the art. Such pesticides are like pyrethrum from chrysanthemum and neem used pesticides from neem kernal and neem oil. There are certain disadvantages associated with the chemical pesticide. One of the main disadvantages is that these pesticides are toxic in nature and thus the product become toxic. Another disadvantage is that the conventional chemical pesticides are not biodegradable. Another disadvantage associated with the neem-based pesticide is that it is not so effective and it is required for use. Therefore, the main object of this invention is to provide a natural pesticide, which obviates the disadvantage associated with the prior art. Another object of this invention is to provide a pesticide, which is not toxic in nature. Still another object of the present invention is to provide a pesticide, which does not damage the fertility of the soil. According to this invention there is provided a process for preparation of pesticide comprising treating cut and crushed leaves, flowers, fruits and tender stem of calotropis, gigantean and/or calotropis procera, nerium oleander and hydrocarpus each separately with dichloro ethane to get the extract and solid parts thereof, the residual masses obtained after treatments of the above cut and crushed leaves, flower, tender stem, fruits and/or stems, each of which is dissolved in diethylene glycols or polyethylene glycol separately and filtered, the filtrates so obtained are mixed in the range of 40-60% Calotropis extract, 20-30% Hydrocarpus extract, 20-30% Oleander extract in order to prepare the pesticide formulation, taking the said formulation in a glass beaker separately and adding 30% hydrochloric acid with or without zinc chloride thereof, stirring said beaker for a period of 1-3 hours at a temperature of 15-50°C and cooled, an ionic emulsifier and nonyl phenol ethylene oxide is then added therein and mixed well, to which antioxidants alongwith para amino benzoic acid is mixed in order to obtain amber liquid or turbid liquid for use as a pesticide. In accordance with this invention leaves, flowers, tender stem and fruits, seeds of calotropis, oleander and hydrocarpus are cut into small pieces and crushed gently. The crushed leaves flowers, tender stem, fruits and seeds are subjected to the step of extraction/treatment separately by using dichloroethane or methanol in the ratio of 1:2-8 at a temperature of 30°C to 60°C under stirring for a period of 2-8 hours. The hot extraction mixture so obtained is cooled and filtered. The solid mass is squeezed to get the liquid separated therefrom. ;The extract so obtained is distilled under vacuum at a temperature of 40°C-60°C to remove the solvent. The residual mass is collected. The solid mass obtained after filtration is triturated with methanol in the ratio of 1:2-8 at a temperature of 40-100°C under stirring for a period of 2-8 hours. The solution is cooled and filtered. The residue is squeezed to remove the liquid contents therefrom. The extract so obtained is distilled in the vacuum to remove the methanol therefrom. The solid mass obtained after the above step is again treated with water in the ratio of 1:2-10 at a temperature of 40-100°C for a period of 2-8 hours and filtered in the hot condition. The residue is squeezed to remove the liquid therefrom. The solution is distilled and the residual mass is collected. The water solution so obtained is distilled under vacuum at a temperature of 40-80°C to remove water therefrom and the residual mass is collected. The residual masses obtained after processing of calotropis, oleander and hydro carpus separately are dissolved in diethylene glycol or polyethylene glycol and is filtered and the filtrate is collected. The filtrate obtained from the above materials are mixed in the range of 40-60% Calotropis extract, 20-30% Hydrocarpus extract, 20-30% Oleander extract with each other to prepare formulation. The above formulation is taken into a glass beaker and 30% hydrochloric acid with or without zinc chloride (anhydrous) is added thereto. The solution is stirred for a period of 1-3 hours at a temperature of 15-50°C and cooled. Non ionic emulsifier for example tween 80 and nonyl phenol ethylene oxide 9-12 mole is added therein and mixed well. Antioxidants for example butylated hydroxy anisole ordibutyl hydroquinon alongwith para amino-benzoic acid is added and mixed well. The resultant clear A process for the preparation of a pesticide according to a preferred embodiment is herein described and illustrated in detail. STEP 1 Calotropis gigantean and/or Calotropis procera A) Leaves, flowers and tender stems 1-1.5 kg of calotropis gigantea and/or calotropis procera are cut to small pieces and crushed and first extracted with 3-8 litres of dichloroethane (EDC) at 30-60°C by stirring for 2-5 hrs. the mass so as filtered and squeezed to remove liquid. The solution was distilled under vacuum (20-50 mm Hg) at a temperature between 40°C-60°C to remove solvent. The residual syrupy mass (10-20 gm) was collected. B) The solid mass from above process was triturated with 2-7 litres of methanol at 40-75°C for 2-6 hrs and cooled and filtered. The solid mass was squeezed to remove liquid contents. The extract was distilled under vacuum (10-60 mm Hg) to remove methanol. Residual resinous mass 10-30 g was collected. C) The solid residue was again treated with 2-10 litres of water at 50-100°C under stirring for 2-6 hours and filtered hot. Liquids were squeezed out collected and mixed with water extract. The water solution was distilled under vacuum (10-50 mm Hg) at temperature between 40-75°C to remove water. The residual mass (10-25g) was collected. STEP II NERIUM Oleander A) Leaves and tender stems of Nerium oleander were cut into small pieces and gently crushed to break the epidermus. The crushed mass 1.5 kg-3kg was triturated with 2-7 litres of Dichloro ethane at a temperature between 30-60°C for 2-8 hours, cooled and filtered and the solvent was further collected by squeezing. The dichloroethane was distilled off under vacuum (10-60 mm Hg) at a temperature between 40-60°C. The residual resinous was collected. B) The solid mass from Step II-A was triturated was methanol 3-8 litres at 40-60°C for 2-8 hours and cooled and filtered. The solid mass was further squeezed to collect remaining liquid and mixed with above. The extract was distilled under vacuum (10-50 mm Hg) to remove methanol. The residual resinous mass (10-30 gm) was collected. C) The solid mass from Step II B was triturated with water 2-6 litres at 40-100°C for 2-8 hours and filtered hot (40-50°C) and mass is squeezed to collect remaining liquid and the same was added to water extract. The water solution was distilled under vacuum (10-60 mm Hg) at a temperature between 50-80°C to remove water. The residual mass (10-25g) collected. STEP III A) Fruits of Hydrocarpus are broken and soft pulp was removed. The seed 1-1.5 kg and shell 500 gm to 1 kg are crushed and boiled with methanol 2-8 litres for 2-5 hours and cooled. The reaction mass was filtered and squeezed to collect methanol extract. Methanol extraction was repeated as above. The combined extract was distilled under vacuum (10-50 mm Hg) at a temperature between 40-60°C to remove solvent. The residual mass of oil alkaloids glycosides etc. (100-250 g) was collected. B) The solid mass from Steep III A was triturated with water 2-8 litre at temperature between 40-100°C for 2-8 hours and filtered hot at (40-50°C) and the mass is squeezed to collect further liquids. The combined water mixture was allowed to settle. The oil layer was separated and added to the extract of Step III A. The water extract was distilled under vacuum (10-50 mm Hg) at a temperature between 40-75°C to remove water. The residue a semisolid mass (20-50g) was collected. STEP IV The residual masses from Step-I A, B and C were dissolved in 200 ml to 1000 ml of Diethylene glycol (DEG) or polyethylene glycol (Pely-300-600) and filtered. Similarly the residual masses from Step II A, B and C were dissolved in Diethylene glycol or polyethylene glycol (PE-300-600) 200 ml-1000 ml and filtered. The filtered was collected. The residual masses from step III A and B were dissolved in Diethylene glycol or polyethylene glycol 500 ml-2000 ml and filtered. The filtered was collected. The above three filtrates were mixed in the range of 40-60% Calotropis extract, 20-30% Hydrocarpus extract, 20-30% Oleander extract to form pesticide formulation. STEPV 1000 g. of above formulation was taken into a glass beaker and hydrochloric acid (30%) 1-100 ml alone or with 1-50 g of zinc chloride (anhydrous) was added stirred for 1-3 hrs at 15 to 50°C and cooled. Non ionic emulsifier between 80 and nonyl phenol ethylene oxide (9-12 mole) 5g -50g each was added and mixed well. Antioxidant butylated hydroxy anisole or dibutyl hydroquinone alongwith para aminobenzoic acid lg to 50g. each was added and mixed well. The resultant clear amber liquid or turbid liquid with suspended particles was bottled. I CLAIM: 1. A process for preparation of pesticide comprising treating cut and crushed leaves, flowers, fruits and tender stem of calotropis, gigantean and/or calotropis procera, nerium oleander and hydrocarpus each separately with dichloro ethane to get the extract and solid parts thereof, the residual masses obtained after treatments of the above cut and crushed leaves, flower, tender stem, fruits and/or stems, each of which is dissolved in diethylene glycols or polyethylene glycol separately and filtered, the filtrates so obtained are mixed in the range of 40-60% Calotropis extract, 20-30% Hydrocarpus extract, 20-30% Oleander extract in order to prepare the pesticide formulation, taking the said formulation in a glass beaker separately and adding 30% hydrochloric acid with or without zinc chloride thereof, stirring said beaker for a period of 1-3 hours at a temperature of 15-50°C and cooled, an ionic emulsifier and nonyl phenol ethylene oxide is then added therein and mixed well, to which antioxidants alongwith para amino benzoic acid is mixed in order to obtain amber liquid or turbid liquid for use as a pesticide. 2. A process as claimed in claim 1 wherein said cut leaves, flowers and tender stem of calotropis are treated with dichloroethane in the ratio of 1:2-8 for a period of 2-8 hours, filtering said solution and squeezing the treated residual mass to remove liquid therefrom, distilling the solution under stirring at a temperature of 40-60°C to collect residual mass, said residual mass collected after filtration is triturated with methanol in the ratio of 1:2-8 for a period of 2-8 hours and the solution is cooled and filtered, the extract so obtained is distilled, the residue is again treated with water and filtered to obtain residual mass. 3. A process as claimed in claim 1 wherein said cut leaves, flowers and tender stem of nerium oleander are treated with dichloroethane in the ratio of 1:2-8 for a period of 2-8 hours at a temperature of 30-60°C, cooling and filtering said mixture and squeezing the residual mass to obtain the liquid therefrom, distilling the solution under vaccum at a temperature of 40-60°C, to collect the residual mass, said residual mass collected after filtration is triturated with methanol in the ratio of 1:2-8 for a period of 2-8 hours, the solution is cooled and filtered, the extract so obtained is distilled, the residue is again treated with water and filtered to obtain residual mass. 4. A process as claimed in claim 1 wherein said cut and crushed fruit of hydrocarpus is treated with methanol in the ratio of 1:2-8 for a period of 2-5 hours and cooled, filtering the reaction mass and squeezing the residual mass to get the liquid extract therefrom, repeating the above step to get the extract, distilling the combined extract in the vacuum at a temperature of 40-60°C to remove the methanol therefrom, the residual mass is collected, the solid mass obtained after squeezing is triturated with water at a temperature of 40- 100°C for a period of 2-8 hours is filtered in the hot condition (40-50°C), the residual mass is squeezed to remove the liquid therefrom, the combined filtrates are allowed to settle and the oil layer is separated therefrom and is added to said extract, the water extract is'distilled under vacuum at a temperature of 40-75°C to remove water therefrom, the residual semi solid mass is collected. 5. A process as claimed in claim 1 wherein said steps of treatment with dichloroethane is carried on at a temperature of30-60°C. 6. A process for the preparation of natural pesticide substantially as herein described.

Documents:

0663-mas-2002 abstract-granded.pdf

0663-mas-2002 claims-granded.pdf

0663-mas-2002 description (complete)-granded.pdf

663-mas-2002-abstract.pdf

663-mas-2002-claims.pdf

663-mas-2002-correspondence others.pdf

663-mas-2002-correspondence po.pdf

663-mas-2002-description complete.pdf

663-mas-2002-form 1.pdf

663-mas-2002-form 18.pdf

663-mas-2002-form 26.pdf

663-mas-2002-form 3.pdf