Gel formulations for hazardous products.

PROCESS FOR PREPARING GEL FORMULATIONS FOR HAZARDOUS SUBSTANCES

BACKGROUND OF THE INVENTION

I. SCOPE OF THE INVENTION

The present invention relates to novel buildings that contain hazardous products and yet are environmentally safe and safe to handle.

II. Prior Art Discussion

At present most of the harmful liquids are stored in metal drums or, if only smaller quantities are required, in plastic containers.

Hazardous compounds, especially agrochemicals, are formulated in various compositions.

Liquid compositions are conveniently intended for farmers because of the relative ease with which they can be handled. However, there are some difficulties in handling such liquid compositions. There is a danger of leaking or leaking if perforations are present in previously used containers or if dropped. Safe shock-resistant containers can be used. However, in the event of an accident, for example during transport, there is still a risk of leakage or rapid loss of liquid,

<img file="PT98352A_D0001.tif" />

* eg spill into soil.

It has been difficult to provide a formulation and containment and packaging system that protects food handlers, including farmers and transporters, and protects the environment.

SUMMARY OF THE INVENTION

The present invention provides formulations or compositions which are especially suitable to be contained in a water-soluble or water-dispersible bag containing a water-dispersible organic gel.

It is an object of the present invention to provide a novel formulation system which contains agrochemicals and is safe for everyone and the environment.

It is another object of the present invention to provide a novel agrochemical formulation system which is practical, quick and easily soluble and / or dispersible in water.

It is another object of the present invention to provide a new formulation system for agro-chemicals which is as compensated as possible, taking up as little space as possible.

It is another object of the present invention to provide a novel formulation system for containing hazardous compounds, for example agrochemicals, which reduces the risk of pollution.

H

It is also known that liquid agrochemicals may be contained in soluble bags or sachets made of films. However, such films may rupture and tear. This causes spillage of the agrochemicals they contain and causes contamination problems. In fact, there are a variety of defects that can be found in the films which cause the film to become brittle and therefore a potential source of spillage. The presence of air bubbles or dust particles or foreign bodies or gel particles or the presence of finer points on or within the film are potential weaknesses. If a film having such weaknesses is subjected to various handling or physical shocks, it is likely to break at these points. This is especially a problem in the agrochemical industry where containers may be carelessly or improperly handled by distributors or farmers.

Another object of the present invention is to prevent spillage through small perforations when using a bag containing the agrochemical product. These small perforations are rare, but just a small perforation among thousands of bags is enough to cause a great deal of trouble, as the liquid escaping from this small perforation contaminates the entire surrounding environment.

It is another object of the present invention to prevent rupture of the container containing an agrochemical formulation.

If the container is rigid there is a possibility

<img file="PT98352A_D0002.tif" />

Considerable of simple breakage. With a liquid in a bag this possibility is somewhat reduced but the liquid is still

Jf transmits the shocks and there is the problem of the hydraulic hammer effect. Another object of the present invention is to prevent or at least partially reduce this hydraulic hammer effect. It has already been proposed to reduce the possibility of breakage by means of a pneumatic space within the bag, but this represents some loss of storage space.

It is another object of the present invention to provide a formulation or composition for hazardous compounds which dissipates as much as possible the energy of a shock from a container from outside.

It is a further object of the present invention to provide a shock absorbing formulation system for containing agrochemicals, for example pesticides or plant protection agents or plant growth regulators.

The use of pharmaceutical or cosmetic gel formulations is known and there is virtually no risk of pollution or environmental contamination when handling such products, in contrast to pesticides and agrochemicals. In addition, gels used for pharmaceutical or cosmetic purposes are generally water based. Thus, it is not evident to obtain gels which are suitable for water-soluble bags or sachets, for water-soluble bags or sachets intended to contain pesticides, or for such bags with the object of

<img file="PT98352A_D0003.tif" />

I have to absorb the shocks.

Another possibility is to dispose of the agrochemicals in the form of wettable powders contained in a bag which may be water soluble. However, not all agrochemicals can be used in wettable powder form. Although these powders are wettable, the length of time before the powder becomes wet (wetting time) may give rise to some technical problems.

As stated above, other pesticide container systems have already been suggested in the past which are environmentally safe, especially those containing liquids in soluble bags or sachets. However, it may be the case that the bags have small perforations; Under these conditions, the liquid contained therein spills out and pollutes the environment.

Although thixotropic liquids may be used, this possibility of spillage through small perforations still exists during transport as displacement creates a movement that makes the thixotropic liquid become more fluid.

In addition, even if the non-aqueous liquid contained in the known water-soluble bags has a low but not zero water content, it is likely that, even if low, it may cause the bags to rupture under freezing conditions,

The present invention is intended to provide a novel formulation system for agrochemicals which dissolves rapidly when introduced into water and is not impaired under normal freezing conditions.

<img file="PT98352A_D0004.tif" />

It is yet another object of the present invention to provide a formulation system wherein less solvent is required in the pesticide formulation, which will provide a reduction in transportation and manufacturing costs.

On the other hand, the present invention aims to provide a new formulation system for agrochemicals which reduces the risk of clogging of spray nozzles or spray tank filters.

There are other objects and advantages of the present invention which will become more apparent from the following description. The objects of the present invention may be achieved wholly or partially in accordance with the invention.

DETAILED DESCRIPTION OF THE INVENTION

The present invention provides formulations or compositions which are especially suitable to be contained in a water-soluble or water-dispersible bag containing a water-dispersible organic gel which constitutes a continuous system containing effective amounts of:

a hazardous product;

optionally an organic solvent;

a water-soluble or water-dispersible surfactant which contains:

a nonionic surfactant and optionally an anionic or amphoteric surfactant; ec

* which is capable of forming a liquid phase with the active ingredient at a temperature above 70 ° C, preferably above 50 ° C; a gelling agent which may be liquid or solid at a temperature of 23 ° C and which is at least 10% soluble in the liquid mixture of the active ingredient and the surfactant at a temperature above 50 ° C, this gelling agent having a particle size of less than 100 microns, preferably less than 20 microns, being a solid mi cra, less than 3% by weight of water, preferably less than

%.

The above defined gel may optionally contain other components as follows:

an organic solvent (the term solvent encompasses a mixture of individual solvents) in which the active ingredient is completely soluble at certain concentration values, a dispersant;

a secondary thickener; and / or other additives such as stabilizing agents, defoamers, buffers and antifreeze agents.

Among the previously defined gels of the present invention, some particular gels are preferred, especially those incorporating (percentages are by weight / weight):

^The Most preferably 25 to 8.0 active ingredient, three

<img file="PT98352A_D0005.tif" />

at 50, more preferably 2 to 15 surfactant,

0.1 to 50%&gt; more preferably 2 to 10% gelling agents,

0.1 to 30, more preferably 1 to 2% secondary thickener, 80% solvent, more preferably 3 to 20% of other additives (as defined above), preferably 0.1 to 10%.

If the gels of the present invention contain a dispersant, the amount of this component may preferably be from 1 to 25% and more preferably from 2 to 8%.

According to a particular aspect of the present invention, the components of the compositions are chosen such that the gels of the invention have a viscosity of from 600 to 3θ,000 centipoises, more preferably from 1,000 and 12,000 centipoises. These Brookfield viscosities are measured with a flat plate viscometer rotating at 20 revolutions per minute.

The term continuous system means a material which is visually homogeneous, ie whose visual appearance suggests that it has only one physical phase. This does not exclude the possibility of small solid particles dispersed therein as long as these particles are small enough not to constitute a separate visible physical phase.

It is known that a gel is generally a colloid in which _The

<img file="PT98352A_D0006.tif" />

* the dispersed phase is combined with the continuous phase to provide a viscous jelly-like product; It is also a dispersed system typically consisting of a high molecular weight compound or small particle aggregate in close association with a liquid. In the gels of the present invention, the hazardous product (or active ingredient) may be in soluble or dispersed form, such as a suspension.

According to a particular aspect of the present invention, the components of the compositions are selected such that the gels of the present invention have a working density greater than 1, preferably greater than 1.05.

According to another particular aspect of the present invention, the components of the compositions are chosen such that the inventive gels contained in the bags of the present invention preferably have a spontaneity (hereinafter defined) of less than 75, preferably less than 25.

Spontaneity is assessed according to the following method; In a 150 ml glass tube a mixture of 1 ml gel and 99 ml water is capped and the vial is capped and inverted by rotating it 180 ° (top down). Spontaneity is the number of times required to completely disperse the gel.

The term surfactant means an organic material capable of substantially reducing the surface tension of water, which is 73 dynes / cm at a temperature of 20 ° C.

Surfactants which are particularly suitable for the present invention are defined in the following test: according to this test, the liquid active ingredient (50 g) and the surfactant adjuvant (5 g) are added to an amount of water at 50 ° C sufficient to adjust the volume of the mixture to 100 ml; the mixture is stirred to give a homogeneous emulsion and then allowed to stand for 30 minutes at 50 ° C in a graduated cylinder; the amount of oily layer which may eventually separate (and thus form a distinct liquid phase) should therefore be less than 20 ml.

surfactant which may be used in the present invention may be selected from the following (but not limited to) list:

nonionic surfactants: alkanolamides, polyethylene oxide polycondensates with fatty alcohols, fatty esters or fatty amines, or substituted phenols (particularly alkylphenols or arylphenols; block copolymers with ethoxy and propoxy groups; fatty acid esters) with polyols such as glycerol or glycol; polysaccharides; organopolysiloxanes; sorbitan derivatives; sucrose or glycol ethers or esters;

anionic and amphoteric surfactants: lignosulphonic acid salts, phenylsulphonic or naphthalenesulphonic acid salts, diphenyl sulphonates; alkylaryl sulfonates;

Sulfonated amines or fatty alcohols or amines; polycondensates of ethylene oxide with fatty acids and their sulphate or sulphonate derivatives; salts of esters of sulfosuccinic or sulfosuccinamic acids; taurine derivatives (particularly alkyl laurates); betaine derivatives; phosphoric esters of

<img file="PT98352A_D0007.tif" />

* alcohols or polyethylene oxide polycondensates with phenols; and the sulfate, sulfonate and phosphate functional derivatives of_fprevious compounds ..

The term gelling agent means a material corresponding to the active ingredient such that when mixed at a rate of 5 ° / 50 (w / w) θ at a temperature of 25 ° C with (and optionally triturated with) an organic solvent in which If the active ingredient is soluble, a gel is obtained. According to the present invention a gel is essentially a material having a phase difference between the controlled shear stress and the shear stress resulting such that tg (0O is less than or equal to 1.5, preferably less than or equal to a 1,2 The function tg ((X) is the tangent of angle 0 '.' (or phase difference). The measurement is carried out by means of a rheometer having a fixed flat plate and a rotating cone on the plate such that the angle between them is less than 10 °, preferably 4 °. The cone is required to rotate by means of a speed controlled motor; The rotation is sinusoidal, ie the torque and angular displacement vary according to a sinusoidal function over time. This angular displacement corresponds to the aforementioned shear force; the speed controlled motor torque (giving rise to angular displacement) corresponds to the previously mentioned controlled cutting voltage.

The gelling agents which may be used in the present invention are tetramethyl decino diol, ethoxylated dialkyl phenol, methylated clay, propylene carbonate, hypoglycated castor oil, ethoxylated vegetable oils, diatomaceous earths.

<img file="PT98352A_D0008.tif" />

* mixture of dioctyl sodium sulfosuccinate and sodium benzoate, mixtures of hexanediol and hexynediol. *

The term hazardous product used herein means a product that may cause damage to the environment or may be harmful to the person handling it.

According to a principal and preferred aspect of the present invention, the hazardous product is an active ingredient, namely an agrochemical and more precisely a pesticide or a plant protection agent (including Gregpladóreè plant growth agents and plant nutrients). ).

The present invention is not limited to certain specific agrochemicals; The following is a list of many agrochemicals which may be used in accordance with the present invention;

Fungicides such as Triadimefon, Tebuconazole, Prochloraz, Triforine, Tridemorph, Propiconazole, Pirimicarb, Iprodione, Metalaxyl, Bitertanol, Iprobenfos, Fluzilazole,

Fosetyl, Propyzamide, Chlorothalonil, Dichlone, Mancozeb, Anthraquinone, Maneb, Vinclozolin, Fenarimol, Bendiocarb, Captafol, Benalaxyl, Thiram;

Herbicides (or defoliants) such as quizalofop and its derivatives, Acetochlor, Metolachlor, Imazapur and Imazapyr, Glyphosate and Gluphosinate, Butachlor, Acifluorfen, Qxifluorfen, Butralin, Fluazifop-butyl, Bifenox, Bromoxynil, Iufynyl, Oxenylpropyl, Oxydiphenyl, Oxygen MCPA, MCPB, MGPP, Linuron, Isoproturon, Flamprop and its derivatives, Ethofumesate, Diallate, Carbetamide, Alachlor, Metsulfuron, Chlorsulfuron,

<img file="PT98352A_D0009.tif" />

'Chlorpyralid, 2h-d, Tribufos, Trichlorpyr, Diclofop-methyl, Sethoxydim, Pendimethalin, Trifluralin, Ametryn, Chloramben_rAmitrole, Asulam, Dicamba, Bentazone, Atrazine, Cyanazine, Thiobencarb, Prometryn, S - ^ - Chlorobenzyl ^^ - dimethyl-1'-oxazolidin-3-one, Fluometuron, Napropamide, Paraquat, Bentazole, Molinate, Propachlor, Imazaquin, Imazaquin, Imazaquin , Tebuthiuron and Oryzalin;

Insecticides or nematocides such as Ebufos, Carbosulfan, Amitraz, Vamidothion, Ethion, Triazophos, Propoxur, Phosalonc, Permethrin, Cypermetrin, Parathion, Methylparathion, Diazinon, Methomyl, Malathion, Lindane, Fenvalerate, Ethinethrate, Dimethrophenate, Ethopropylate Dicrotophos, Dichlorprop, Dichlorvos, Aziphos and their derivatives, Aldrin, Cyfluthrin, Deltamethrin, Disulfoton, Chlordimeform, Chlorpyrifos, Carbaryl, Dicofol, Thiodicarb, Propargite, Demeton, and Phosalone;

Plant growth regulators such as Gibernic acid, Ethrel or ethephon, Cycocel, Chlormequat, Ethephon, and Mepiquat.

In order to assess whether a surfactant adjuvant has dispersing properties and may be a Dispersant according to the present invention, the following test is performed: an aqueous suspension (100 ml) containing kaolin or atrazine (50 g) is prepared, solid particles of a size between 1 and 10 microns and containing the adjuvant surfactant (5 a) and allowed to stand at 20 ° C for 3 minutes in a graduated cylinder (use

<img file="PT98352A_D0010.tif" />

- kaolin whenever the dispersing agent can disperse a hydrophilic solid; atrazine is used whenever the dispersing agent can disperse a hydrophobic solid). Once the rest period has ceased, 9/10 (nine tenths) of the suspension volume at the top of the suspension is removed without agitation and the solids content (residue after evaporation of water) is measured. of the tenth remaining; This solids content shall not exceed 12% by weight of the 100 ml solids content of the suspension under test.

The dispersant which may be used in the present invention may be selected from the following list (which is not limiting): salts of lignosulphonic acids, such as calcium lignosulphonate, salts of phenyl acids sulphonic or naphthalene sulphonic acid condensed with naphthalene sulphonic acid; polycondensates of ethylene oxide with alcohols or fatty acids or with fatty esters or with fatty amines or substituted phenols (particularly alkyl phenols or aryl phenols); salts of sulfosuccinic acid esters, such as sodium sulfosuccinate; taurine derivatives (particularly alkyl taurates); phosphoric esters of alcohols or polycondensates of ethylene oxide with phenols; esters of polyols and fatty acids or sulfuric acid or sulfonic acids or phosphoric acids; glyceryl esters, especially fatty acid esters such as glyceryl stearate; ethylene glycols; and the like.

<img file="PT98352A_D0011.tif" />

Secondary thickener is a compound that increases the viscosity of a gel or liquid.

Secondary thickener which may be used in the present invention may be selected from the following list (which is not limiting): fused silica; hydroxyethylcellulose, carboxymethylcellulose; organically modified attapulgite or montmorillonite clay; hardened castor oil; cetyl and stearyl alcohols or esters; polyethylene glycols; glyceryl hydroxy stearate, polyvinyl alcohol; ester salts of sulfosuccinic acid such as dioctyl sodium sulfosuccinate; salts of benzoic acid, such as sodium benzoate; and alkyl sulfates.

The preparation or production of the gels of the present invention may be carried out by any known method. A convenient process is to mix the different constituents of the mixture / composition together and stir them, optionally by grinding or grinding and / or heating them. It is often easier to work by slowly adding components of the composition. It may eventually be useful to add the gelling agent last.

The present invention also encompasses water soluble or water dispersible bag containing containment systems containing the above defined gel formulations.

The chemical nature of the envelope film constituting bags containing the composition / gels of the present invention may vary widely. Suitable materials are water soluble (or possibly water dispersible) materials *

, which are insoluble in the organic solvents used to dissolve or disperse the agrochemical active ingredient. Suitable specific materials include polyethylene oxide, such as polyethylene glycol; starch and modified starch; alkyl and hydroxyalkylcellulose, such as hydroxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose; carboxyethyl cellulose; polyvinyl ethers, such as polymethyl vinyl ether; poly (S-dimethyl-triazol-ethylene), poly (vinyl sulfonic acid); polyanhydrides; low molecular weight formaldehyde / urea resins; low molecular weight formaldehyde / melamine resins; 2-hydroxyethyl polymethacrylate); poly acrylic acid and its counterparts; but preferably the surrounding film is comprised of or made of polyvinyl alcohol (APV).

Preferred material for producing bags for the materials of the present invention are polyethylene oxides or methylcellulose or polyvinyl alcohol. Where polyvinyl alcohol is used, a 4-0-100% alcoholized or hydrolyzed polyvinyl acetate film and preferably 80-99% water soluble films used to make water soluble bags are advantageously used. known. To make a bag it is necessary to give the film a configuration (possibly partially) and then fill it with the gel. Generally, the gels are able to drip even at a low speed due to their high viscosity. A container used to contain gels cannot easily be emptied due to this high viscosity of the gel (one of the reasons why gels have not been used in agriculture so far).

<img file="PT98352A_D0012.tif" />

„After filling, the sealing should be sealed, usually hot, to close it. ,

Further information is provided in the following co-pending patent applications, which are incorporated herein by reference: Leonard E. Hodakowski, Chi-Yu R. Chem. Samuel T. Gouge. Paul J. Weber for Gel Formulations for Use in Toxic or Hazardous Product Containerization Systems filed April 4, 1991; David Edwards and William McCarthy patent application for Laminated Bags for Containerization of Toxic or Hazardous Materials filed April 4, 1991; Leonard's patent application

E. Hodakowski, Chi-Yu R. Chen, Samuel T. Gouge and Paul J. Weber for Water Dispersible gel Formulations filed April 4, 1991; Leonard's patent application Ξ. Hodakowski, Ricky W. Couch, Samuel T. Gouge and Robert C. Lign for Gel Formulations filed April 4, 1991; and Samuel T. Gouge's patent application, David P. Downing, Spencer B. Cohen, Allan J. Luke, Robert D. McLaughlin, and James E. Shue to Bag In A. Bag for Containerization of Toxic or Hazardous Material filed April 4, 1991.

The following examples are for illustrative purposes and should not be considered as any restriction of the present invention.

Example 1

A gel was prepared by stirring at 5 ° C a mixture of:

<img file="PT98352A_D0013.tif" />

64,8$ «

Active Ingredient: 2,4-D — Phenoxy-benzoic acid isooctyl ester:

Solvent: Aromatic solvent whose flash point is 65 ° C. :

Surfactant: a nonionic mixed emulsifier / sulfonate mixture:

and calcium alkylbenzenesulfonate:

Gelling agent: a mixture of dioctyl sulfosuccinate salt and sodium benzoate:

24,2 %

Stir the mixture and stir until each component is dissolved or dispersed.

During stirring, the phenomenon of dissolution occurs and then that of gelling. Gelation increases during cooling to room temperature (20 ° C).

The viscosity of the gel is 3,000 centipoises.

Emulsion stability is good according to the test described above.

1,100 g of this gel is filled into a 1 liter bag made of an APV film (88% hydrolyzed polyvinyl acetate; cold water soluble; thickness:

micron). Under these conditions, the bag is practically full (about 95% v / v) and then heat sealed. The specific mass of the gel and the bag containing it together is 1,1 g / cm3.

The bag is then dropped 10 times from 1.2 m above the ground. There is no rupture or

S?

<img file="PT98352A_D0014.tif" />

spill.

The bag is then placed in a water tank under gentle agitation (i.e., agitation equivalent to that obtained with a recirculation pump). It is dispersed within x 3 minutes. There is no clogging of the filter consisting of a 100 mesh screen.

Another bag is tested by the same process as the previous bag for protection against small punctures. A needle is passed through the bag (diameter: 0.6 mm). There is a small droplet that forms where the needle has passed. However, this droplet is small enough not to drip from the bag and not to drip along the bag.

Example 2

The procedure of Example 1 is repeated except that a mixture containing the following adjuvants is used:

Surfactant: nonionic mixed emulsifier / sulfonate: 5,2%

Gelling agent: Tetramethyl Decino diol: 30%

The Brookfield viscosity of the gel is 3000 centipoises.

Emulsion stability is good according to the test described above.

1,100 g of this gel is filled into a 1 liter bag made of a cold water soluble hydrolysed polyvinyl acetate (APV) film of 88 thickness;

micron). Under these conditions, the bag is practically full.

<img file="PT98352A_D0015.tif" />

* »(About 95% v / v) θ then heat sealed. The specific mass of the gel and the bag containing it together is

1.1 g / cm3.

The bag is then dropped 10 times from a height of 1.2 m to the ground. No breakage or spillage is observed.

The bag is then placed in a water tank under gentle agitation (ie agitation equivalent to that obtained with a recirculation pump). It is dispersed within 3 minutes. There is no clogging of the filter, consisting of a 100 mesh screen.

Example 3

The procedure of Example 1 is repeated except that a mixture containing the following adjuvants is used:

Surfactant: non-ionic mixed emulsifier / sulfonate: 21.5% and calcium alkylbenzene sulfonate: 3&gt; 7%

Gelling agent: ethoxylated dialkyl phenol: 10%

The Brookfield viscosity of the gel is 3000 centipoises.

Emulsion stability is good according to the test described above.

1,100 g of this gel is introduced into a 1 liter capacity bag made of a cold water-soluble polyvinyl acetate (APV) film of 88 thickness;

• ί · » ^s 21.55 microns). Under these conditions the bag is practically full (about 95% v / v) θ then sealed hot. The specific mass of the gel and the bag containing it together is

1.1 g / cm3.

The bag is then dropped 10 times from 1.2 m above the ground. No breakage or spillage is observed.

The bag is then placed in a water tank under gentle agitation (ie equivalent ^if get with a recirculation pump.). Its dispersion was found within 3 minutes. There is no clogging of the filter consisting of a 100 mesh screen.

Example 1+

A gel is made by stirring at 50 ° C a mixture of:

Active Ingredient:

bromoxynylic acid octanoate ester: 18.65% bromoxynylic acid heptanoate ester: 13.85% methyl chloropropionic acid isooctyl ester: 37 Λ%

Solvent; aromatic solvent with a flash point of 3θ ° 0: 11,1%

Surfactant: non-ionic mixed emulsifier / sulfonate _; 13 %

Mixture of gelling agents:

hydrogenated castor oil: 3% ethoxylated vegetable oil

<img file="PT98352A_D0016.tif" />

*

The ingredients are mixed together under violent agitation with an Atritor mixer ”. The product begins to gel after a few minutes.

The Brookfield viscosity of the gel is 3 10 cetipoises.

Emulsion stability is good according to the test described above.

Spontaneity has the value 20.

1,100 g of this gel is introduced into a 1 liter bag made of an APV film (88 X hydrolyzed polyvinyl acetate; cold water soluble; thickness:

micron). Under these conditions, the bag is practically full (about 95% v / v) and then heat sealed. The specific mass of the gel and the bag containing it together is 1,1 l / cm3.

The bag is then dropped 10 times from 1.2 m above the ground. No breakage or spillage is observed.

The bag is then placed in a water tank under gentle agitation (ie agitation equivalent to that obtained with a recirculation pump). It is dispersed within 10 minutes. There is no clogging of the filter consisting of a 50 mesh screen.

Example 5

The procedure of Example h is repeated except that a mixture containing the following components was used.

Yes

<img file="PT98352A_D0017.tif" />

%

Active Ingredient; bromoxynyl oethaneate: 18.4 bromoxynyl heptanoate: 1.0% isooctyl isfeet of aceto-methylchloropropionic acid; 36.6%

Surfactant mixture;

mixed nonionic emulsifier / sulfonate. ; 9.0%

Gelling agent; diatomaceous earths; 17.0% dioctyl sodium sulfate succinic acid dal ester and sodium benzoate: 2.0%

Dispersant sodium sulfonate from naphthalene condensate with formaldehyde; 3.0%

Mix these ingredients together while stirring violently there. ubl Atritor mixer. The product begins to look like a soft paste such as a gel after a few minutes.

The Brookfield viscosity of the gel is 9,000 centipolises.

Emulsion stability is good according to the test described above.

Spontaneity has a value of 9 ·

1,100 g of this gel is filled into a 1 liter capacity bag made of an APV film (88% hydrolyzed polyvinyl acetate; cold water soluble; thickness:

micron). Under these conditions the bag is practically full (about 95 v / v) ® and then heat sealed. The specific mass of the gel and the bag containing it together is 1,1 g / cm3.

<img file="PT98352A_D0018.tif" />

*

The bag is then dropped 10 times from a height of 1,2 m · on the ground. No breakage or spillage is observed.

The bag is then placed in a water tank under gentle agitation (ie agitation equivalent to that obtained with a recirculation pump). It was dispersed within a 1 minute interval. There is no clogging of the filter consisting of a 50 mesh screen.

Example 6

The procedure of Example 5 is repeated except that a mixture containing the following components is used:

Active Ingredient: Bromoxynyl octanoate Bromoxynyl heptanoate 'atrazine

Solvent: Same as Example 1 Gelling agent: a mixture of dioctyl ester of the sodium acid of sodium sulphate?

phosphate and sodium benzoate Stabilizer: alkyl sulfate Surfactants:

ethoxylated / propoxylated block copolymer with an alkyl amine alkylphenyl sulfonate of an amine Freezing agent: polyethylene glycol Anti-caking agent: polyorganosilane

31,5 $ 31,5 $

23,25 %

1,5 % 2,15$

3.6 f 5% 1 $ 0.5%

<img file="PT98352A_D0019.tif" />

Mix these ingredients together and pass the mixture through a bead mill. The product looks like a gelatinous mixture and after about 5 hours becomes much more viscous.

The Brookfield viscosity of the gel is 9 100 centipoise and 5,200 centipoise after stirring for minutes.

Emulsion stability is good according to the test described above.

Spontaneity has the value of 11 ..

1,100 g of this gel is filled into a 1 liter opacity bag made of an APV film (88% hydrolysed polyvinyl acetate in cold water; thickness:

micron). Under these conditions the bag is practically full (about 95 v / v) and then heat sealed. The specific mass of the gel and the bag containing it together is 1 · g / cm3.

The bag is then dropped 10 times from a height of 1,2 m to the ground. No breakage or spillage is observed.

The bag is then placed in a water tank under gentle agitation (ie agitation equivalent to that obtained with a recirculation pump). It is dispersed within 5 minutes. There is no clogging of the filter, consisting of a 100 mesh screen.

Example 7

The procedure of Example 6 is repeated except that a mixture containing the following components is used:

Active Ingredient:

Bromoxynyl octanoate: 33.7 Z Acetomethylchloropropionic acid isooctyl ester: 36.2 Z

Solvent: Aromatic solvent with a flash point of 65 ° C: 3.0 Z

Surfactant:

nonionic mixed emulsifier / sulfonate: 8.5 Z and calcium dodecylbenzenesulfonate: 1.0 Z

Gelling Agent: Tetramethyl Decino Diol: 17.6 Z

The ingredients are mixed together under violent agitation with an Atritor mixer. The product begins to look like a soft paste and gels after a few minutes.

The Brookfield viscosity of the gel is 2,200 centipoises.

Emulsion stability is good according to the test described above.

Spontaneity has a value of 14.

1,100 g of this gel is introduced into a 1 liter capacity bag made of an APV film (88 Z hydrolyzed polyvinyl acetate; cold water soluble; thickness:

micron). Under these conditions, the bag is practically full (about 95 Z v / v) and then heat sealed. The specific mass of the gel and the bag containing it together is

1.1 g / cm3.

Then the bag is dropped 10 times from one

<img file="PT98352A_D0020.tif" />

* height of 1.2 m above the ground. No breakage or spillage is observed.

^T - The bag is then placed in a water tank under gentle agitation (ie agitation equivalent to that obtained with a recirculation pump). Verify your disper are within a 5 minute interval. There is no clogging of the filter consisting of a 100 mesh screen.

Example 8

The procedure of Example 7 is repeated except that a mixture containing the following components is used:

The active ingredient and solvent are the same as those used in Example 7 as the amount of active ingredient is the same, the solvent being the same but being the amount of 10.6%.

Surfactant Mixture:

ethoxylated polyarylphenol: 6, $, · and calcium dodecylbenzenesulfonate: 2%

Gelling agent: mixture of hexane diol and hexino diol: 11.5%

The ingredients are mixed together at 90 ° C under violent agitation with an Atritor mixer ”. The product begins to look like a soft paste and gels after a few minutes.

The Brookfield viscosity of the gel is 2,500 centipoises.

The emulsion stability is good in accordance with the

<img file="PT98352A_D0021.tif" />

• test previously described.

Spontaneity has a value of 5 ·

1,100 g of this gel is introduced into a 1 liter bag made of an APV film (88 cold-water-soluble hydrolysed polyvinyl acetate; thickness 55 microns). Under these conditions the bag is practically full (about 95 v / v) © and then heat sealed. The specific mass of the gel and the bag containing it together is

1.1 g / cm3.

The bag is then dropped 10 times from a height of 1,2 m to the ground. No breakage or spillage is observed.

The bag is then placed in a water tank under gentle agitation (i.e. agitation equivalent to that obtained with a recirculation pump). It disperses after 5 minutes. There was no clogging of the filter, consisting of a 100 mesh screen.

Example 9

The procedure of Example 4 is repeated except that a mixture containing the following components is used:

Active Ingredient:

Bromoxynyl octanoate: 33.5% Bromoxynyl heptanoate: 33.5 X

Solvent: Aromatic solvent with a _and 65 ° C: 17.5%

Surfactant:

nonionic mixed emulsifier / sulfonate: 4.5% and calcium dodecylbenzenesulfonate: 1.0%

Gelling Agent:

mixture of sodium sulfosuccinate dioctyl ester and sodium benzoate: 4.25%

Defoaming Agent:

tetramethyl decino diol: 0.5%

These ingredients are mixed together at 50 ° C under violent stirring with an Atritor mixer. The product starts to look like a soft paste and gels after a few minutes.

Brookfield's viscosity of gel is 4 150 centipoises.

Emulsion stability is good according to the test described above.

Spontaneity has a value of 10.

1,100 g of this gel is placed in a 1 liter bag made of an APV film (88% hydrolysed polyvinyl acetate; cold water soluble; thickness:

micron). Under these conditions, the bag is practically full (about 95% v / v) and then heat sealed. The specific mass of the gel and the bag containing it together is 1,1 g / cm3.

The bag is then dropped 10 times from a height of 1,2 m to the ground. No breakage or spillage is observed.

The bag is then placed in a water tank under gentle agitation (ie, agitation equivalent to that obtained with a recirculation pump). Its dispersion was found within 3 minutes. There is no clogging of the filter consisting of a 10Q mesh screen.