DESC:FIELD OF INVENTION:

The present invention relates to process of making oil in water emulsion, more particularly relates to process for making Triclopyr Butoxy Ethyl Ester 20% EW to 60% EW, oil in water emulsion concentrate with improved weed control and field application.

BACKGROUND OF INVENTION:

The process invention relates to an improved process for preparing TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW an oil in water emulsion concentrate with improved weed control and for personal safety during manufacture, handling and field application.

The TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW is produced by mixing Triclopyr technical ( 94% active ingredient ) with gum solution, defoamer ethoxylated vegetable oil, emulsifier and water in a mixer with high speed disperser in a prescribed addition sequence at a controlled temperature to get oil in water emulsion concentrate with a high stability on storage.

SUMMARY OF INVENTION:

TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW is a systemic oil in water emulsion concentrate herbicide for the control of mixed weeds in plantations area such as oil palm and rubber plantation.

Many agrochemical industry are currently switching to, green revolution friendly herbicide formulation that offers less phytotoxicity to plants, are safer to people/operators for handling and field application.
The novel process invention relates to a process for making oil in water emulsion concentrate containing TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW is a new approach to maximize the coverage of weed control and to minimize the

problems of handling and field application by operators. The oil in water emulsion ( EW ) formulation is stabilized by surfactants, plant vegetable oil based solvents that are green adjuvant in the formulation. Due to interest in green formulations, plant based oil is suitable to replace petroleum solvent based adjuvant to improve the quality and performance of agricultural products. The vegetable oil phase in emulsion system could enhance the deposition,, penetration and translocation of the herbicides active ingredient through the waxy and cuticle layers of the leaves to reach target site of metabolic reaction.

Triclopyr butoxy ethyl ester 32.1 % EC is a petroleum solvent based formulation and could control grassy and certain broadleaf weeds. The petroleum based solvent may cause health problem to skin , eyes and easily absorbed by skin of human and animals. The petroleum solvents are flammable, less biodegradable and toxic to aquatic organisms and is not environment friendly. The solvents can cause rubber gaskets, pump parts surfaces and plastic parts of application equipment to deteriorate.

EFFICACY STUDY:

Chemical weed control is recognized to be an economical practice in oil palm plantations as it can reduce reliance on manpower for hand weeding.

The percentage of weed growth reduction and duration of effective weed plays an important role in the evaluation of herbicide efficacy.

A study was conducted on oil palm plantations to evaluate the efficacy of Triclopyr butoxy ethyl ester 32.1 % EW (water emulsion) with that of Triclopyr butoxy ethyl ester 32.1 EC (emulsifiable concentrate) an approved herbicide in the foreign market on a plot planted with 2 year old oil palm trees.

The treatment consisted on untreated plot, with different doses of Triclopyr butoxy ethyl ester 32.1%EW at 0.8 L/ha, 1.0 L/ha, 1.2 L/ha, 1/5 L/ha and Triclopyr butoxy ethyl ester 32.1% EC at 1.5L/ha (L/ha – litre per hectare)

Result showed that application of Triclopyr butoxy ethyl ester 32.1% EW at different doses significantly reduced the weed growth and increased vegetative growth of oil palm trees.

The effect of Triclopyr butoxy ethyl ester 32.1% EW in controlling weeds on oil palm tree was comparable with that of Triclopyr butoxy ethyl ester 32.1% EC, the recommended Triclopyr butoxy ethyl ester herbicide.

Herbicide efficacy of Triclopyr butoxy ethyl ester 32.1% EW at1.2 L/ha was higher than Triclopyr butoxy ethyl ester 32.1% EC at 1.5 L/ha for grasses and broadleaves.

Both Triclopyr butoxy ethyl ester 32.1% EW and Triclopyr butoxy ethyl ester 32.1% EC reduced dry weight of weeds significantly and 4 WAT (Weeks after treatment) is the optimum period to observe high weed mortality. The efficacy of Triclopyr butoxy ethyl ester of EW and EC at 4 WAT was ranked as follows. Triclopyr butoxy ethyl ester 32.1% EW doses at 1.5 L/ha >EW at 1.2L/ha, >EC at 1.5 L/ha> EW at 1.0L/ha.

Triclopyr butoxy ethyl ester 32.1% EW is effective in controlling both broad leaves and grasses even though the effect on broadleaves weed is higher. Triclopyr butoxy ethyl ester 32.1 % EW did not adversely affect the vegetative growth of oil palm trees and significantly improved the vegetative parameters by reducing competition with weedsfor nutrients and other growth resources.

Triclopyr butoxy ethyl ester 32.1% EW can be applied at 1.5 L/ha as its effect was comparable to Triclopyr butoxy ethyl ester 32.1% EC at 4 WAT.

Triclopyr butoxy ethyl ester 32.1% EWcould be applied at 1.2 L/hato 1.5L/ha and may therefore be recommended for the control of broad spectrum of weeds.

RAW MATERIALS:

The novel process for making TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW is an oil in water emulsion concentrate is green and user friendly and make the product more safe for handling, transfer and field application by human people, and is expected to cause less health problems to end users handling this product. They are also easy to handleand apply and does not deteriorate parts of application equipment, and less phytotoxic to non-targeted plants and less toxic to end user and aquatic organism.

The different plant ethoxylated vegetable oils defoamer used for oil in water TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW are as under;

a. Ethoxylated soyabean oil (CAS NO: 61791-23-9),
b. Ethoxylated Coconut oil (CAS NO: 67762-35-0),
c. Ethoxylated Olive oil (CAS NO:103819-46-1),
d. Ethoxylated Sunflower oil (CAS NO:186511-05-7).

From all above ethoxylated vegetable oil, soyabean oil, olive oil and sunflower oil are chiefly used for making oil in water emulsion concentrate.

The water used for oil in water emulsion concentrate is as under;
a. Distilled water ( CAS NO; 7732-18-5)
The different gumsused for oil in water emulsion concentrate are as under:

A Xanthan gum(CAS NO; 11138-66-2)
a. Gum acacia ( CAS NO; 9000-01-5 )
b. Neem gum

The different blend of nonionic alkoxy phosphate emulsifiers used for oil in water emulsion concentrate are as under:
1 Nonionic ethoxy phosphate esters
2 Nonionic butoxy phosphate esters
3 Nonionic propoxy phosphate esters

APPLICATION:

TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW - a oil in water emulsion concentrate Is diluted with required quantity of water in a mixing vessel and stirred to get an uniform mix and applied with hand directed equipment such as high volume spraying equipment, knapsack sprayers and knapsack misting machine.

PACKAGING:

TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW being water in oil emulsion can be safely packed and stored in HDPE and regular PET bottle and the end user will get quality product at fairly low price, unlike the petroleum solvent base formulation Triclopyr butoxy ethyl ester EC requires packing in aluminium and lacquered tin cans or coex multilayer bottles and are more expensive.

DESCRIPTION OF SPECIFIC EMBODIMENTS:

The invention relates to a process of making oil in water emulsion concentrate for TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW.

In carrying out the present invention the mixer is fitted with high speed disperser and charged with required quantity of distilled water followed by xanthan gum ( 2 % solution in water ). The agitation started and mixing continued for 0.5 hr.

To this mass , required quantity of Triclopyr butoxy ethyl ester technical (94% active ingredient) is charged at a controlled rate in 1.0 hr. After all the Triclopyr butoxy ethyl ester technical addition is completed, and a known weight of emulsifier nonionic alkoxy phosphate ester is charged during high speed mixing at controlled rate in 1.5 hr maintaining the temperature 20°C – 54°C of mixing mass. When all the addition of emulsifier nonionic alkoxy phosphate ester is complete, the mixer is further charged with defoamer ethoxylated vegetable oil during high speed mixing in 0.5 hr and the total mass is kept under stirring for further 0.5 hr .The agitation is stopped and allowed to settle in the mixer for 1.0 hr.

The sample of oil in water emulsion of TRICLOPYR BUTOXY ETHYL ESTER 20% EW TO 60% EW is drawn from the mixer and checked for the Triclopyr butoxy ethyl ester content and emulsification. The total time taken for oil in water emulsion concentrate of Triclopyr butoxy ethyl ester 20% EW to 60% EW takes around 6.0 hr.

The total mass of the mixer vessel is filtered through silica bed under pressure and collected in measuring tank and taken to packing line for suitable packaging.
The following examples illustrate the invention.

EXAMPLE 1:

To make 100 parts by weight of TRICLOPYRBUTOXY ETHYL ESTER 32.1% EW
A steel mixing vessel with high speed disperser is charged with 64.15 parts by weight of distilled water followed by 0.30 parts by weight of xanthan gum ( 2% solution in water ) and the agitation started. The mixing is continued for 0.5 hr.

To this mass , 34.05 parts by weight of Triclopyr butoxy ethyl ester technical (94% active ingredient) is charged at a controlled rate in 2.0 hr. While stirring is on.

After all the Triclopyr butoxy ethyl ester technical addition is complete, 0.50 parts by weight of emulsifier nonionic ethoxy phosphate ester is charged during high speed mixing at controlled rate in 1.5 hr maintaining the temperature 30°C – 32°C of mass.

When all the addition of emulsifier nonionic ethoxy phosphate ester is complete, the vessel is further charged with 1.00 parts by weight of ethoxylated vegetable soyabean oil l (as defoamer ) during high speed mixing within 1.00 hr and the total mass is kept under stirring for further 1.00 hr.

The high speed agitation is stopped and the content of the mass is allowed to settle in the mixer for further 0.30 hr.

The sample of oil in water emulsion of TRICLOPYR BUTOXY ETHYL ESTER 32.1 % EW is drawn from the mixer and checked for the Triclopyr butoxy ethyl ester content and emulsification. The total time taken for oil in water emulsion concentrate of TRICLOPYR BUTOXY ETHYL ESTER 32.1 % EW takes around 6.0 hr.

The total 100 parts by weight of formulated mass from the mixer is filtered through silica bed under pressure and collected in intermediate measuring tank and taken to packing line for suitable packaging.

EXAMPLE 2:

To make 100 parts by weight of TRICLOPYRBUTOXY ETHYL ESTER 20 % EW.

A steel mixing vessel with high speed disperser is charged with 76.80 parts by weight of distilled water followed by 0.50 parts by weight of gum acacia ( 2% solution in water ) and the agitation started. The mixing is continued for 0.5 hr.

To this mass, 21.30 parts by weight of Triclopyr butoxy ethyl ester technical (94% active ingredient) is charged at a controlled rate in 2.0 hr. While stirring is on. After all the Triclopyr butoxy ethyl ester technical addition is complete, 0.60 parts by weight of emulsifier nonionic butoxy phosphate ester is charged during high speed mixing at controlled rate in 1.5 hr maintaining the temperature 20°C – 22°C of mass.

When all the addition of emulsifier nonionic butoxy phosphate ester is complete, the mixer is further charged with 0.80 parts by weight of ethoxylated vegetable soyabean oil (as defoamer ) during high speed mixing within 1.00 hr and the total mass is kept under stirring for further 1.00 hr.

The high speed agitation is stopped and the content of the mass is allowed to settle in the mixer for further 0.50 hr.
The sample of oil in water emulsion of TRICLOPYR BUTOXY ETHYL ESTER 20% EW is drawn from the mixer and checked for the Triclopyr butoxy ethyl ester content and emulsification. The total time taken for oil in water emulsion concentrate of Triclopyr butoxy ethyl ester 20 % EW takes around 5.50 hr.

The total 100 parts by weight of formulated mass from the mixer is filtered through silica bed under pressure and collected in intermediate measuring tank and taken to packing line for suitable packaging.

EXAMPLE 3:

To make 100 parts by weight of TRICLOPYRBUTOXY ETHYL ESTER 60 % EW.

A steel mixing vessel with high speed disperser is charged with 33.95 parts by weight of distilled water followed by 0.40 parts by weight of xanthan gum ( 2% solution in water ) and the agitation started. The mixing is continued for 0.5 hr.

To this mass, 63.85 parts by weight of Triclopyr butoxy ethyl ester technical (94% active ingredient) is charged at a controlled rate in 2.0 hr. While stirring is on. After all the Triclopyr butoxy ethyl estertechnical addition is complete, 0.70 parts by weight of emulsifier nonionic propoxy phosphate ester is charged during high speed mixing at controlled rate in 1.5 hr maintaining the temperature 50°C – 52°C of mass.

When all the addition of emulsifier nonionic propoxy phosphate ester is complete, the mixer is further charged with 1.10 parts by weight of ethoxylated vegetable sunflower oil (as defoamer ) during high speed mixing within 1.00 hr and the total mass is kept under stirring for further 1.00 hr.

The high speed agitation is stopped and the content of the mass is allowed to settle in the mixer for further 0.50 hr.
The sample of oil in water emulsion of TRICLOPYR BUTOXY ETHYL ESTER 60% EW is drawn from the mixer and checked for the Triclopyr butoxy ethyl ester content and emulsification. The total time taken for oil in water emulsion concentrate of Triclopyr butoxy ethyl ester 60 % EW takes around 5.0 hr.

The total 100 parts by weight of formulated mass from the mixer is filtered through silica bed under pressure and collected in intermediate measuring tank and taken to packing line for suitable packaging. ,CLAIMS:WE CLAIM:

1. A process of making 100 parts by weight of oil in water emulsion concentrate to get TRICLOPYR BUTOXY ETHYL ESTER 20% EW to 60 % EW formulation by mixing distilled water, gum solution followed by addition of Triclopyr butoxy ethyl ester technical, emulsifier nonionic alkoxy phosphate ester and defoamer ethoxylated vegetable oil in a prescribed addition sequence in a mixing vessel.

2. The process of claim 1 where in the mixing temperature is kept at/between 20°C – 54°C .

3. The process of claim 1 where in the distilled water is added is between 33.00 to 78.00 parts by weight to the mixer. (For 100 parts product).

4. The process of claim 1 where in the gum used are xanthan gum, gum acacia and neem gum (2 % solution in water) is added between 0.30 to 0.50 parts by weight to the mixer ( 100 parts product).

5. The process of claim 1 where in the Triclopyr butoxy ethyl ester technical (94%) is added between 21.00 – 65.00 parts by weight to the mixer ( 100 parts product ).

6. The process of claim 1 where in the emulsifier used are non-ionic alkoxy phosphate ester mainly ethoxy phosphate ester, butoxy phosphate ester and propoxy phosphate ester and is added between 0.30 to 0.50 parts by weight to the mixer at a controlled rate maintaining the temperature ( 100 parts product).

7. The process of claim 1 where in the ethoxylated vegetable oil defoamer is added to mixer between 0.80 to 1.10 parts by weight ( 100 part product ). The vegetable oil used isethoxylated soyabean oil, ethoxylated sunflower oil and ethoxylated olive oil.

8. The process of claim 1 where in oil in water emulsion of Triclopyr butoxy ethyl ester 20% EW TO Triclopyr butoxy ethyl ester 60% EW is safely applied for control of broad spectrum weeds and improve the vegetative growth of young oil palm plantations.

9. The processof claim 1 where in efficacy of Triclopyr butoxy ethyl ester 32.1% EW in controlling weeds and the doses in the range of 1.2 L/ha to 1.5 L/ha.

10. The process of claim 11 where in the efficacy of Triclopyr butoxy ethyl ester 20% EW in controlling the weeds, the dose will be greater than 1.5 L/ha and for Triclopyr butoxy ethyl ester 60% EW, the dose will be less than 1.2 L/ha.