CS218596B2 - Liquid herbicide means - Google Patents

Abstract

1. Liquid, herbicidal agents in the form of aqueous suspension concentrates containing, as the active compound, isoproturon or mixtures of isoproturon with ioxynil, bromoxynil, mecoprop or salts of the last three active compounds and also formulating auxiliaries, which contain, as the formulating auxiliary, an alkali metal salt, preferably the sodium salt, of a condensation product containing sulfo groups and formed from a phenol and formaldehyde, and also alkali metal salts, ammonium salts or amine salts, preferably sodium salts, of alkyl polyglykol etherphosphate partial esters, in particular mono-(alkyl polyglycol ether)-phosphates or di-(alkyl polyglycol ether)-phosphates, the alkyl polyglykol ether radical of which consist of optionally substituted alkyl groups which can also contain double bonds and have preferably 6 to 24 and in particular 12 to 18 C atoms, and polyglycol ether groups having preferably up to 20 and in particular 4 to 12 ethylene oxide units (= EO units) per radical, the suspension concentrates having a temperature/viscosity coefficient of about 0.6 to 0.95, calculated on temperature increases in 20 degrees C intervals, within the temperature range from 10 to 70 degrees C, in particular 20 to 60 degrees C.

Description

BACKGROUND OF THE INVENTION The present invention relates to liquid herbicidal compositions in the form of faulty storage-stable suspension concentrates which remain well flowable at elevated temperatures and which contain isopreturon or mixtures of isoprcituron with ioxynil, brcmoxynil, mecoprop or salts of the last three active ingredients. as formulation auxiliaries they comprise the alkali salts of the condensation product of sulfol-containing phenol and formaldehyde or of phenol, alkali sulfite and formaldehyde, and alkali salts or optionally ammonium salts or ammonium salts of the partial esters of alkyl polyglycol ether phosphates, the latter of which confer suspension suspensions in temperature range from 10 to 70 degrees Celsius temperature viscosity coefficient from about 0.6 to 0.95, based on temperature increase at 20 ° C intervals, so that the viscosities of the suspension concentrates they are reversibly decreasing as the temperature rises.

Isoiproturon [3- (4-isopropylphenyl) -1,1-dimethylurea] is a known herbicide that is used to combat harmful grasses having small seeds (field feather grass, clrundelka) as well as chickweed and chamomile at an early stage of development. In order to broaden the spectrum of herbicidal activity, the known active ingredients ioxynil [4-hydroxy-3,5-diiodobenzonitrile], bromoxynil [3,5-dibcm-4-hydroxybenzonitrile] and mecoprop [2- ( 4-chloro-2-methylphenoxy) propionic acid].

This allows more weeds to be combated with only one application at a time. By adding ioxynil and bromoxynil to isopreturon, it is also possible to kill the dead-nettle, speedwell and three-color violet. Mixed formulations containing isoproturoin and mecoprop can also be used to control bedstraw. The herbicidal effect of such active compound combinations is known (see, eg, DOS 23 43 985; furthermore, Cole and Hcrsnail, Proceedings 1976, ον. 1, British Crop Protection Gonference — Weeds, pp. 111–113).

Generally, pesticidal active substances are used in the form of emulsifiable concentrates, sprayable powders and suspension concentrates, for example. Active substances which are difficult to dissolve in technical solvents, such as isoproturon, are usually used, for example, in the form of sprayable powders. However, expensive grinding and filter devices and often expensive synthetic silicas as carriers are required for the preparation of sprayable powders.

However, sprayable powders have the disadvantage of being heavily metered or dosed and dusted with manual handling. The user can easily contaminate these detergent preparations and cause damage. In addition, the active substances which are present in the form of soluble alkali or ammonium salts in the sprayable pigs are often highly corrosive. In addition, the spray slurries of the sprayable powders are unstable. homogeneity of dilute aqueous suspensions. Part of the active substance and solids settle relatively quickly. After half an hour often only half of the active ingredient is present in the suspension. This causes mostly uneven distribution of the active substances on the plants.

Liquid, storage-stable, aqueous suspensions which contain, for example, 20 to 50% by weight of the finely divided solid, do not exhibit these disadvantages of sprayable powder. They are prepared by grinding coarse aqueous suspensions of the active compound in a friction ball mill or sand mill. Since there is no need for a filter device in this case, the cost of the device is not particularly large. Therefore, the development of efficient storage concentrates that are stable in storage and suitable for practice is much more difficult than sprayable powders and emulsifiable concentrates.

Emulsifiable concentrates and dispersible powders exist practically as single-phase systems and can be stored, for example, in the form of a solution or a powdered product relatively easily. They only need to be able to form emulsions or suspensions at the time of use, and according to international testing regulations, for example, for sprayable powders, 50% by weight of the particles must be suspended in the sprayable powder after standing for half an hour. substances. On the other hand, aqueous suspension solids concentrates are biphasic solid-liquid systems in which solid particles of the active agent constantly exert forces such as thermal movement of molecules, sedimentation force and mutual attraction. However, if the suspension concentrates are to be used in practice, they must be stable on storage for more than two years, i.e. the fine distribution of the active ingredient particles is maintained and guaranteed at least for this period. The dispersions must remain liquid. Suspension thickening, sediments that are not spontaneously frayable, must be avoided. By nature, these two-phase systems are unstable and tend to be agitated, which increases with increasing storage time and storage temperature.

In many cases the dispersions thicken to form viscous sediments which can no longer be redispersed to liquids. Often the dispersed active agent particles suddenly flocculate when the suspension concentrates are mixed with other pesticidal formulations. This is particularly the case when the admixed compositions contain salts, or when the active substances themselves are in the form of salts, for example in the form of carboxylic acid salts or when added as phenolates. Such flocculation may occur, for example, when the pesticidal compositions are admixed with dilute spraying of the slurry of the pesticide -suspension concentrates ready for use, but also, possibly more or less slowly, already upon storage of the suspension concentrates of the solid active ingredients to which they have been admixed. substances in the form of salts or phenolates. This is particularly true of the suspension concentrates described above by combining the active ingredients isoproturon with mecoprop, -benoxynil and ioxynil, for which there is considerable demand in practice.

Processes that affect product quality can take place at suspension concentrations depending on time and temperature. According to theoretical ideas, a suspension should be stable even if it can be prepared from a plurality of dispersing, wetting and viscosity-altering agents which are suitable for the particular purpose of use, at the correct concentration, and these are smeared with particles which They are to be dispersed, and which are electrostatically -optimally charged to the same charge, so that the mutual repulsive forces thus generated can overcome very vigorously and with increasing particle fineness the increasing Van-Waals attractive forces.

The increasing fineness of the particles can in turn counteract the correspondingly increasing thermal mobility of the sedimentation force. Increasing the same electrostatic charge of the particles results in enhanced polarization of the surrounding water molecules. As a result, an increasingly dense hydrate coating of polarized water molecules is deposited onto the particles of the active ingredient, causing the viscosity of the suspension to decrease and the product to be more readily flowable. If suitable surfactants cause the hydrate coating to remain at an increasing storage temperature, the attractive forces acting between the particles are further constrained despite increasing mobility. If, on the other hand, the particles are not exactly charged or have already partially lost their charge due to surfactants, they may become stable at normal temperature at a higher storage temperature over time or may form viscous, non-dispersible sediments. The increasing mobility of the active substance particles with the increasing energy temperature of the particles is sufficient to ensure that the dispersions become so viscous because of the less well-developed hydrate coating that their attractive forces can act. There is a thixotropic effect and a hydrate coating overlaps with time, making the dispersion unstable. These are the theoretical assumptions to help these time-dependent processes explain, in fact, these processes are unequal in multiple layers and measurement methods such as zeta-potenoial measurements to determine the optimal charge of a particle are not applicable to concentrated dispersions. Similarly, this also applies to the preparation of very low viscosity dispersions. For, as practice has shown, it is difficult to select from a large number of formulation ingredients that are suitable for the heterogeneous criteria used. addition in other long-term stability tests.

Furthermore, it is known that in the development of storage-stable liquid dispersion formulations using active ingredients of technical quality, it is by no means possible to rely solely on the content of individual batches of product in suspension, since slight changes in the proportions of byproducts in the individual batches dispersions thus prepared. It is therefore preferable to test the reproducibility of the final opimal composition by numerous trials of the preparations also with respect to the various technical batches of the active substances, and if necessary, the preparations are modified and if necessary reworked.

The preparation of suspension concentrates of isoproturion is an example of this. Thus, on a large scale, isoproturon prepared on a large scale can contain, for example, according to the preparation process and purification methods used, either 97% by weight of the pure active ingredient in addition to about 2% by weight of the ortoisomer and 1% by weight of metaisomer; up to 3% by weight of the metaisomer and up to 1% by weight of the orthoisomer.

The finding of a storage-stable dispersion composition makes it extremely difficult to achieve this slight variation in the isoprcituron quality. These difficulties are exacerbated by the combination of isoprotunoin with ioxynil, bromoxynil, mecoprop, or salts thereof, such as alkali or amine salts, respectively. use of these other active substances also in technical quality.

It has been shown that the composition of the dispersions and the bio-processes for their preparation, as described in the literature, when used in the preparation of suspension concentrates of isoproturon or in combinations of isoproturon with ioxynil, bromoxynil and mecoprop do not result in storage-stable products. Thus, the foamability of isoproturon cannot be improved by the addition of partially hydrolyzed polyvinyl acetates, for example according to U.S. Pat. No. 4,071,617. In addition, it appears that the formation of viscous sediments which are not redispersible increases in stored dispersions. The same applies in the case of the use of non-ionic emulsifiers, vegetable gums and anionic surfactants in preparations, for example according to U.S. Patent No. 3,948,636 or British Patent No. 1,480,110.

In addition, non-ionic emulsifiers containing polyglykelether groups, and used, for example, in amounts up to about 2% by weight, may cause crystal growth with relatively low solubility of isoproituron in water. The use of block polymers of polyether glycols, obtained, for example, by adding ethylene oxide to the condensation product of propylene oxide and propylene glycol, in addition to dispersants and also with the addition of silicas, for example according to DOS 2,547,968 or DOS 2,651,046, leads to dispersions which solidify - on products that - are difficult to cut. In addition, the polyether glycol block polymers cause some recrystallization of the suspended active ingredient particles to form coarser particles. Viscous sediments are separated from the suspension concentrates of isoproturioin containing polycarboxylate vinyl polymers, such as polymethacrylate, for example in the processing of isoproturon according to U.S. Pat. 3,060,084.

If isoproturon is formulated into a formulation, for example according to DOS 2 651046, unusable storage concentrates which are unstable are also obtained, which thicken when stored at high temperatures, for example at 50 ° C. Also dispersions which, for example, according to -amer, patent no. 3,157,486 contain as formulation auxiliary; The ligninsuf tomates, and which, according to the examples therein, contain no other wetting agents, are unstable for storage.

Said suspension concentrates are often not sufficiently capable of grinding in friction ball mills or sand mills to be used in their preparation. This is particularly the case for those formulations whose viscosity is strongly temperature-dependent, so that these suspensions gradually thicken at temperatures between about 35 and 55 ° C. Such temperatures, however, are readily achieved in milling equipment even when the cooling jacket is water-cooled. Heat . releasing the grinding of the milled product causes an increase in the viscosity of the said preparations, which in turn leads to a deteriorated heat transfer from the milled product to the water flowing in the cooling jacket, so that the temperature of the milled product rapidly rises and easily reaches 90 ° C. whereby the dispersions often solidify completely or - even the melting point of the low melting active substances can even be reached or exceeded.

Such isopraturon dispersions that densify as the temperature rises or which, in the storage stability test at 50 ° C, densify over days or weeks, and form non-dispersible sediments, are obtained even when used in their use. the preparation of a conventional dispersant, such as sodium salts of ligninsulfonic acid, sodium salts of the condensation products of formaldehyde with sodium sulfite and phenol, optionally nonylphenol, optionally naphthol or naphthalenesulfonic acids; or alkylsulfuric acids or butylnaphthalenesulfoic acids, fatty alcohol polyglycol ethers or polyether glycol block polymers.

It has now been found that liquid herbicidal compositions can be prepared in the form of storage-stable aqueous suspension concentrates which remain well flowable even at higher temperatures and which contain isioproturon or mixtures of isoproturon with ioxym, bromoxynil, mecoprop or salts of the last The three active ingredients further comprise formulation auxiliaries such that an alkali salt, preferably sodium salt, of a condensation product of a sulfone-containing phenol and formaldehyde or phenol, an alkali sulfite and formaldehyde, as well as an alkali salt, is used as the formulation auxiliary. ammonium salts or ammonium salts, preferably sodium salts, of partial esters of alkyl polyglycol ether phosphates, in particular mono- or di-alkyl polyglycol ether) phosphates, the alkyl polyglycol ether radicals of which are optionally substituted alkyl groups, which may also containing double bonds, preferably having from 6 to 24, in particular 12 to 18 carbon atoms, and a polyglycidlethenoid group preferably from up to 20, in particular 4 to 12, ethylene oxide units per residue, the salts of partial phosphoric acid esters confer suspension concentrates in the temperature range of 10 to 70 ° C, in particular from 20 to 00 ° C, a temperature viscosity coefficient of about 0.6 to 0.95 based on the temperature increase at 20 ° C intervals, the viscosity of the suspension concentrates decreasing reversibly as the temperature rises.

Accordingly, the present invention relates to a liquid herbicidal composition in the form of an aqueous suspension concentrate comprising 4-isopropyl-ethylenedimethylurea, optionally in admixture with 4-hydroxy-3,5-diiodobenzonitrile, 3,5-dibromo-4-hydroxybenzonitrile, 2- [eta] chloro-Z-methylphenoxy J proponic acid or salts thereof; an alkali salt of the phenol-formaldehyde condensation product, said condensation product containing sulfo groups; and another polyethylene glycol ether derivative auxiliary formulation, characterized in that it contains an alkali derivative of polyethylene glycol ethers. , an ammonium or ammonium salt of a partial phosphoric acid ester of the general formula

= ¾ - ^O-, _m -PO _{(OCH3. M} wherein alkyl contains 6-24 carbon atoms and optionally contains a double bond, n is 4-20 and GMG 1 second

The herbicidal composition has a temperature viscosity coefficient of about 0.6 to 0.95, based on the temperature increase at 20 ° C intervals, in the temperature range of 10 to 70 ° C, in particular 20 to 60 ° C.

Preferred salts of the partial esters of alkyl polyglycol ether phosphates are salts of mono- or diesters of ortho-sulfonic acid, in particular mixtures of the two salts of partial esters. Preferred are alkali salts, especially sodium salts. The preparation of the salts of the partial esters of alkyl polyglycol ether phosphates used according to the present invention, which are known, can be carried out by known methods.

Possible ammonium salts are, for example, salts with mono-, di- or. trialkylamines wherein the alkyls contain 1 to 4 carbon atoms or mono-, di- or trialkanolamines with 1 to 4 carbon atoms in alkanols.

Preference is given, for example, to alkali salts, in particular sodium salts, for example mono- or diesters of orthophosphoric acid with polyglycote ^, thers of higher alcohols or fatty alcohols, such as, for example, coconut alcohol. fatty alcohols, wax alcohols or synthetic alcohols having polyglycol ether groups having up to 20, preferably 2 to 20, in particular 4 to 12, ethylene oxide units. In many cases, it is also preferred to use salts of the partial phosphoric acid esters with alkylpiperazines of unsaturated higher alcohols or unsaturated fatty alcohols. The alkyl groups may also be subselated, for example by alkoxy or; halogen atoms. However, unsubstituted alkyl groups are preferred. Mixtures of different salts of partial esters of phosphoric acid may also be used.

The amount of the phosphoric acid partial ester salts used according to the invention is preferably about 0.5 to 8% by weight, based on the finished suspension concentrate. However, it is also possible to use amounts which are greater or less than the amounts indicated herein, but generally do not bring any particular advantages.

Salts of partial phosphoric acid esters of the above type are commercially available under the tradenames Forlamt P and Forlanon (Henkel KGaA).

The salts of the partial phosphoric acid esters used according to the invention impart to suspension concentrates comprising said herbicides and isoproturon in a temperature range of from 10 to 70 ° C, in particular from 20 to 60 ° C, a temperature viscosity coefficient of about 0.6 to 0.95 based on to a temperature interval of 20 degrees Celsius.

The term temperature viscosity coefficient is understood to be a factor that indicates the measured viscosity of the suspension concentrate at an increasing temperature of 20 ° C. This factor is the quotient of the observed viscosity number at a higher temperature compared to the measured viscosity number of the suspension concentrate at 20 ° C lower. If the temperature viscosity coefficient is less than 1, then the viscosity of each suspension concentrate decreases with increasing temperature, and if it is greater than 1, the viscosity increases.

Comparable formulations show that, for example, replacement of an alkylpolyglycol ether phosphate partial ester salt with a corresponding proportion of a partial ester salt of a comparable alkyl phosphate whose alkyl residues contain no polyglycol ether groups (cf. Comparative Example 1j) or a comparable tris- (alkylpolyglycol ether) phosphate salt (cf. Comparative Example 2) leads to a complete loss of surprising and advantageous properties of the suspension concentrates according to the present synalyse, such as storage stability, flowability and a temperature viscosity coefficient of less than 1.

The alkali salts of the condensation products of the phenol and formaldehyde-containing sulfosuccins are also known and are described together with their preparation in DOS 1 945 100.

They can be obtained, for example, both by reaction of the phenolic components with formaldehyde and an alkali sulphite or an alkali bisulfite in an alkaline medium, and by the corresponding reaction of the phenolic components honed in the core. with formaldehyde. The strongly alkaline condensation products thus obtained can advantageously be rendered neutral by treatment with an acid, for example sulfuric acid, which is of importance due to the sensitivity of many biocidal active substances to alkali. The M-molar ratio of phenolic component to formaldehyde in condensation products is preferably about 1: 1.3 to 1: 2.5. In the condensation reaction, for example, phenols with single-core sulfosubstituted phenols, in particular lower alkylsubstituted phenols, or binucleated, non-condensed mono- or difunctional phenol-containing phenols or mixtures thereof and formaldehyde, or corresponding non-phenol-containing phenols, are used as phenolic components. sulfo groups, formaldehyde and alkali sulfite, optionally bisulfite. Preferred alkali salts are sodium salts. Preferred phenolic components are, for example, sulfonated on the nucleus and lower alkyl groups on the nucleosubstituted phenols, in particular nucleosubstituted cresols, or the corresponding alkylphenols or sulfonate-free cresols. Mixtures of these phenolic components may also be used.

The amount of alkali salt of the condensation product phenol and formaldehyde containing sulfosuipes in the composition according to the invention is preferably with about 1 to 10% by weight, based on the finished suspension concentrate. However, smaller or larger amounts may be used, but generally do not bring any particular advantages.

The present invention therefore relates in particular to a liquid herbicidal composition in the form of an aqueous suspension concentrate containing, as active ingredient, isoproturon or mixtures of isoprotunon with ioxynil, bromoxynil, mecoprop or salts of the latter three, as well as formulation auxiliaries which are characterized by: containing from 15 to 60% by weight of isoprone, up to 42% by weight of ioxynil, bromoxynil, mecoprop or salts thereof, up to 10% by weight, of an alkali salt of the phenol-formaldehyde condensation product containing phosphorus salts,

0.5 to 8% by weight of the alkali salt of a partial ester of an alkyl polyglycol ether phosphate -with 6 to 24 carbon atoms in -alkyl -and -with 2 to 20 ethylene oxide units,

0 to 0.4% by weight of aluminum silicate r with leaf structure,

0.2 to 2 wt. antifoam agent ·,

0 to 10% by weight of an antifreeze agent and the remainder up to 100% by weight; water.

As the foliar-structured aluminum silicate, conventional products used as suspending aids such as montmorillonites or bentonites can be used.

Conventional products based on -tributyl phosphate or silicone-based are used as antifoams, and silicones are preferred.

Suitable antifreeze agents are the customary freezing point-reducing agents, such as eithyleinglycol, propylene glycol, glycerol. Ethylene glycol is preferred.

The water used in the preparation of the suspension concentrates can be, for example, conventional drinking water or process water, preferably water having a 20 ° hardness (German hardness), but it is also possible to use desalinated water.

The suspension concentrates of the present invention are low viscous and well liquid, especially if they contain up to 50% by weight of the active ingredient or active ingredient mixture. They retain their low viscosity not only when heated, but are also surprisingly reversibia low viscosity when the temperature rises, without causing loss of suspending and dilution properties, which is particularly important, for example, in storage and use. hot climates.

The multicomponent formulations of the present invention can be well milled, despite their relatively low viscosity, surprisingly excellent storage stability, have a good wettability and dilutability when diluting concentrated spray slurries with water, and exhibit surprising compatibility with combination formulations, which often used to extend the spectrum of biological activity in the preparation of ready-to-use diluted slurry slurries.

The active ingredient content of the suspension concentrate is preferably 15 to 60% by weight, in particular 20 to 50% by weight, of which at least 18% by weight isioiproturon, if the composition additionally contains ioxynil, bromoxynil, mecoprop or salts thereof. Suitable salts of the latter three active substances are preferably water-soluble salts, in particular alkali or ammonium salts, for example of amines with lower alkyl or alkanol groups.

The preparation of the suspension concentrates is carried out, for example, by mixing isoproturon and the other active compounds used according to the invention in an aqueous solution or suspension of a co-formulation agent, and this coarse suspension is pre-grinded to a fineness of about 200 microns. finally, it is finely ground in a ball or sand mill, with the particles of isoproturon and other active substances being in the range of 0.1 to 15 microns, the major part being below 5 microns. The fineness measurement is performed using a disk centrifuge or a Coulter-Counter measuring instrument.

The application of the composition, for example in agriculture or in fields, is carried out in a simple manner by adding dilution water to the isoproturon-containing suspension concentrates in an appropriate prescribed amount, stirring briefly and applying n.a. plants in effective amounts. Dilute aqueous spray suspensions are distinguished from comparable spray tips prepared from sprayable powders or emulsifiable concentrates, in particular by containing the active ingredient almost uniformly distributed after 24 hours of standing. Sprayable powder suspensions, on the other hand, are very quickly dispersed; after half an hour, half the active ingredient is very often settled. Likewise, oily and creamy portions are separated from the emulsions of the emulsified concentrates after 1 to 4 hours of standing.

The isoproturon-containing suspension concentrates of the present invention exhibit surprisingly excellent physical compatibility with known insecticidal and fuingicidal compositions which are admixed as ready-to-use sprayable powders or emulsifiable concentrates as compared to ready-to-use spray slurries.

The present invention is illustrated by the following examples.

Example 1

By grinding all ingredients in a ball mill with 2 mm glass beads in diameter, a liquid aqueous suspension concentrate of the following composition is prepared:

50.0% by weight of isoproturon,

6.0% w / w, salts of condensation product cresol, formaldehyde and sodium sulphite,

3.0% by weight, sodium salt of an alkylpolyglycol ether phosphate mono - / - diester wherein the alkyl has 12 to 18 carbon atoms (Forlanit P, Henkel KGaA),

0,2% m / m, powdered aluminum silicate (montmori llonite),

1.0% by weight, silicone antifoam (SE2, Wacker GmbH),

4.0 wt%, ethylene glycol and

35.8% wt. water.

This dispersion is ground to a particle size such that 90% by weight of the suspended particles have a diameter below 5 microns, as measured by a Coulter-Counter measuring instrument.

When 2 ml of this suspension concentrate is poured into 99 ml of water, a spontaneously forming dilute suspension is obtained which has a surface tension of 36 to 42 dynes / cm ^-1 at 20 degrees Celsius, in which only traces are visible after 12 hours sedimented particles. In comparison to a comparable sprayable powder, there is a susceptibility of approximately 100% measured according to the CIPAC test methods.

This dispersion is easily pourable and remains stable after 3 months of storage at 0 and 50 ° C. According to the storage test, only 0.3% by volume of dispersion can be found in the form of a precipitate at the bottom, which, however, is spontaneously redispersible by shaking twice. Crystal growth of the isoproturon particles was not observed. With an increasing storage temperature of 20 ° C to 20 ° C and 60 ° C each, the dispersion is reversibly low viscous without suffering from stability.

The temperature viscosity coefficient is determined by measuring the viscosity of the suspension concentrate using a Brooikfield and viscometer at 20, 40 and 60 ° C. In this case, the suspension is first freed of the closed air bubbles by shaking in a round-bottomed flask on a vibration apparatus for 30 minutes under reduced pressure of a 20 mm water column. The dispersion is then filled into a Bnookfield viscometer meter and heated to 20, 40 and 60 ° C in a thermostat. Viscosity measurements are made with hydrometer 2 at 2.5 and 10 revolutions per minute. The results are summarized in the following table.

Measuring conditions

Brookfield viscometer hydrometer 2 hydrometer 2

2.5 rpm at 20 ° C

2.5 rpm at 40 ° C

2.5 rpm at 60 ° C rpm at 20 ° C rpm at 40 ° C rpm at 60 ° C

The viscosity of the suspension concentrate decreases with increasing temperature. The temperature viscosity coefficient-barely equals water. Thus, the coefficient found provides evidence that the hydrate coating with which the individual particles are surrounded is surprisingly stable, even at increasing temperatures. Otherwise, viscosity increases with increasing attraction between suspended particles.

Example 2

Analogously to Example 1, all components are ground to a particle size of about 5 microns in a 2 mm glass ball mill to obtain a suspension concentrate of the following composition:

20.0% by weight, isoproturon,

40.0% mecoprop sodium (U 46 KV — Pulver, BASF AG),

Briookfield viscosity tr density meter 2 density meter 2

Example 3

Measuring conditions

2.5 ct / min at 20 ° C

2.5 rpm at 40 ° C

2.5 rpm at 60 ° C ct / min at 20 ° C rpm at 40 Ό rpm at 60 ° C

Analogously to Example 1, all components are ground to a particle size of about 5 microns in a 2 mm glass ball mill to obtain a suspension concentrate of the following composition:

30.0% by weight, isoproturon,

10.0% w / w, ioxynil,

3.0% by weight, sodium salt of the condensation product of phenol and formaldehyde containing sultogroups,

6.0% wt. miono - / - dllaurylpolyglycol ether phosphate in the form of the sodium salt, with 10 ethylene oxide units,

1.0% by weight of silicone antifoam (SE 2, Wacker GmbH),

0,05% by weight of powdered aluminum silicate (montmoirillonite) and

49.5 wt. water.

Viscosity Temperature viscosity coefficient (mPas) with increasing temperature at 20 ° C intervals (calculated)

63200,675

4272

2736) 0.640

19240,748

1440

920 J0,633

2.0% by weight, sodium salt of the condensation product cresol, formaldehyde and sodium sulphite,

4.0% by weight, sodium salt of inono - / - diester of C12-18 alkylpolyglycol etherfoate (Foir.lanit P., Henkel KGaA),

1.0% by weight, silicone antifoam (SE 2, Wacker GmbH),

0.05% w / w, aluminum silicate powder (bentonite);

32.95% wt. water.

The resulting suspension concentrate has excellent storage stability, even when stored for long periods at 50 ° C. It is easily spillable. Its viscosity decreases with increasing temperature. The results of the viscosity measurements at 20 ° C temperature intervals performed according to Example 1 are summarized in the following table:

Viscosity Temperature viscosity coefficient (mPas) with increasing temperature at 20 ° C intervals (calculated)

42240.90

3805 j

3492 J0.91

13260.89

1178 j

1020 J0,87 3 months at 50 ° C virtually no sediments.

The temperature viscosity coefficients measured according to Example 1 at 20 ° C intervals are between 0.8 and 0.92.

Example 4

Analogously to Example 1, all components are ground to a fineness of about 5 microns in a 2 mm glass ball ball mill to obtain a suspension concentrate of the following composition:

35.00% palpation, isoproturonium,

10.00% by weight, sodium bromoxynil, 2.00% by weight, sodium salt of cresol condensate, formaldehyde and sodium sulfite,

3.00% wt. mono-/ dialkylpolyglycoil ether phosphate in the form of a sodium salt having from 12 to 18 carbon atoms in alkyl and from 4 to 12 ethylene oxide units,

1.00% by weight, silicone antifoam (SE 2, Wacker GmbH),

The resulting suspension concentrate is low viscous and easy to spill and has no glass218596

0,05% by weight of powdered aluminum silicate (bentonite);

48,95% touch. water.

The resulting suspension concentrate is well pourable and shows virtually no sedimentation after storage for 3 months at 50 ° C.

The temperature viscosity coefficients, measured at 20 ° C intervals according to Example 1, are between 0.78 and 0.93.

Comparative Example 1

Reduction formulation as described in Example 1 but containing, instead of the sodium salt of C12-18 alkylpolyglycol ether phosphate [Forlanit P], 3.0% by weight of C12-18 alkyl mono7-diester (Forlanit G) 452, Henkel KGaA), was milled to a suspension concentrate having a particle size of about 5 microns in a glass bead mill of 2 mm diameter using the procedure of Example 1. During the milling process, the mixture is sucked more viscous by the heat released during milling, which causes the temperature to rise to about 50 ° C, and which cannot also be removed during the milling process by cooling with water 15 ° C. After the grinding process is completed, the mixture is cooled to room temperature, the glass beads are sieved and the suspension concentrate is tested as described in Example 1. The temperature viscosity coefficient is 1.1 to 1.2. The storage test at 50 ° C showed that the product was separated after 1 month into an aqueous layer and a viscous sediment containing the active substance, which was no longer redispersible.

Comparative Example 2

A preparation analogous to Comparative Example 1, but containing instead of C12-18 alkyl monosodium dialkyl phosphate (Forlanit F 452) 3.0% by weight of trisphdoidecyltetraglycol ether phosphate is ground and processed as described in Comparative Example 1 The temperature during the grinding process also rises to about 50 ° C and cannot be reduced by cooling with water 15 ° C because the viscosity of the mixture increases strongly.

The temperature viscosity coefficient of the suspension concentrate is 1.2 to 1.4. The storage test at 50 ° C showed that the product solidified after 1 month to a viscous gel-like mass which could no longer be diluted with water.

Claims (1)

Liquid herbicidal composition in the form of an aqueous suspension concentrate containing 4-isopropinylphenyldimethylurea, optionally in admixture with 4-hydroxy-3,5-diiodobenzonitrile, 3,5-dibromo-4-hydroxybenzonitiril, 2- (4-chloro-2-methylphenoxy) propionic acid or salts thereof, an alkali salt of the phenol-photrmaldehyde condensation product, said condensation product containing sulfo groups, and another co-formulation agent based on derivatives of poilyethylene glycol ethers, characterized in that it contains an alkali, ammonium or ammonium salt of a partial phosphorus ester acids of the general formula C1-4 alkyl ------ (wherein the alkyl contains 6 to 24 carbon atoms and optionally contains double bonds, n is 4 to 20 and 1 gm 2.