MXPA98007698A - Concentrates of non-aqueous suspension of highly soluble solids in a - Google Patents

Abstract

The present invention relates to preparing stable concentrated non-aqueous suspensions of water-soluble solids using liquid organic carriers miscible with water, preferably lower alkadiols with a specific three-component surfactant system, i.e., a system comprising an enhancing surfactant of non-ionic polymeric viscosity, an anionic surfactant, and a non-ionic surfactant having a volubino hydrophobic substituent group

Description

CONCENTRATES OF NON-AQUEOUS SUSPENSION OF SOLIDS HIGHLY SOLUBLE IN WATER DESCRIPTION OF THE INVENTION The present invention relates to a method for preparing concentrated suspensions of water soluble solids with an excellent storage stability and the concentrate thus formed. The method comprises suspending the solids in a water-soluble organic liquid such as a low molar mass glycol in the presence of a three-component surfactant system. Many management problems can arise when one is forced to prepare aqueous end-use formulations and / or sludges from solids, especially active solids, for example, wettable bioactive powders since this is usually the situation in the agricultural industry . Farmers who prepare tank mixtures of herbicides, insecticides and / or other bioactives from solids for applications to grains and soils are exposed to certain dangerous safety and inconveniences due to the generation of harmful dusts, which may be irritable to the skin and dangerous when breathing. In addition, finely ground powders, still called wettable powders of many water-soluble bioactives when prepared as tank mixes do not disperse well; they have a spontaneity of "fluorescence"; they have a low suspension capacity, have a poor redispersibility and are more incompatible with other bioactives when compared with liquid bioactive concentrates. In this way, the final formulators, such as farmers, when preparing dilute aqueous active compositions find that the handling and application of solid materials such as fertilizers, are much easier if the material can be supplied in a fluid instead. in solid form. Then, the economy dictates that the active material will be supplied in a highly concentrated fluid to the final formulator. The saturation solubility in water of many water-soluble active constituents, such as potassium chloride, is too low to be economical to be supplied to the end user, simply in the form of a solution.

Alternatively, highly concentrated suspensions of water-soluble compounds, both in water and in Organic liquids, have a very poor storage; freezing / thawing; and heat / cold stability. As a result of the dissolution-recrystallization procedure of spontaneous glass, a progressive increase in the size of the active material in particle occurs. This increase in particle size results in sedimentation, shifting and changes in visco-elastic properties and thus severely limits the concentrate loading levels. The present invention relates to a unique formulation which, to a greater degree, addresses and overcomes the above problems. The particle size stability of solids in water soluble particles is obtained in a double form. First, through the proper selection of the organic carrier used as the continuous phase, the temperature coefficient of the solubility can be controlled, thus stabilizing the particle size of the solids through the commercial storage types and cycle times. temperature. The main component of the carrier liquid is non-aqueous, although small amounts of water can be used to modify the operation. Secondly, the recognition that a small number of large particles has a total surface area smaller than a large number of small particles without considering the morphology, the surface free energy of the active solid material is reduced through adsorption of surfactant on the surface of the particle, thus reducing activation to obtain a minimization of the surface area that promotes the growth of the particles.

The stability of the particle size and other desirable characteristics of the concentrate such as low "Viscosity, minimal syneresis and high fluorescence are mainly controlled through the use of a three-component surfactant system.The first component, a non-ionic viscosity improving material, preferably a polymeric material and more preferably a block copolymer of Ethylene oxide-propylene oxide, is mainly used, though through rheology control, to create a stable dispersion and secondarily to soften crystal growth.The second component, an anionic surfactant, preferably a sulfonate, although having an increase syneresis influence is mainly used to synergistically reduce the viscosity improving effect of the first polymeric component and secondly, as a result of its affinity for the surface of the solids, to assist in the dispersibility of the solid particles. The third component, which is a bulky nonionic surfactant, which contains a large hydrophobic group, preferably an ethoxylated tristyrylphenol, is mainly used to reduce the packing of the particles, that is, to reduce syneresis or sedimentation and with good luck to improve the florescence or dispersibility that occurs when the concentrate composition is diluted by emptying it in an aqueous medium to obtain the final concentration of final formulation. This third component also tends to increase the viscosity of concentrate. Optionally, a smaller amount of water can be added to the concentrate, mainly to help adjust the temperature coefficient of solubility, which ultimately minimizes changes in particle size. Palgrave, et al., (U.S. Patent 4,265,406) describe the use of an additive such as a polysaccharide to at least partially inhibit further growth on the glass surfaces, when grinding the concentrated solid material such as an explosive. soluble in water or fertilizer salts in saturated solutions. Through the use of organic carrier and agent systems t < > Surfactant of this invention, excop- cionally high fillers are prepared, ie, from about 40 to 85% by weight of the total composition of slurries of solu solids in water, which exhibit minimal changes in particle size and are characterized by the visco-elastic sedimentation and property that the suspensions perform, which are extremely stable under long-term storage conditions. The formulations of the present invention are suitable for suspending solvents or removing any water-soluble material which, in the charge, which is considered as a concentrate, exists as a separate solid phase in the Fully formulated concentrate Many of these materials find application in the areas of explosives and agricultural, especially in fertile fields.Example of such water-soluble materials include salts such as potassium nitrate, diacid ammonium phosphate, ammonium nitrate, sodium nitrate, calcium nitrate, potassium chloride, sodium chloride, ammonium phosphate, ammonium polyphosphate, potassium l acid phosphate, disodium hydrogen phosphate and the like, and similar compounds without salts such as urea. water-soluble "means any material that has a solubility in water greater than one '() (1) percent by weight, based on the total weight of the material and from 1 ° to 24 ° C. The concentration or loading of the solid material in the formulations of this invention may be: from 40 to: I percent - I weight; LO-HO weight percent reference; and more preferably 55-70 weight percent based on the total weight of the concentrate. The average volume diameter particle size of the water soluble solid material can be 0.5 to 500 microns; preferably 30 to 200 microns and more preferably about 80 to about 120 microns. The carrier can be any low molecular weight organic fluid that is miscible in water, which is liquid at room temperature. The term "miscible in water" means that organic liquids are miscible with water in all proportions, that is, they will form an individual phase with water. When the water soluble solids are In the case of bioactive agents, it is preferred that the carrier be inert or at least acceptable for the intended end use of the diluted concentrate. For example, if the solids are pesticidally active, the carrier must be agronomically acceptable. 20 All water-miscible organic liquid carriers do not work with equal effectiveness and it is generally preferred that the organic liquid has liidroxide functionality and a relatively low molecular weight; in this way, lower alcohols with mono- or poly- ']' • > Functionality are particularly effective along with their ethers or esters. Among these are the lower alkanols or alkadiols. A capacity to be miscible in maximum water was obtained with C.-C] alcohols (methanol, ethanol, isopropyl alcohol, etc.). Of the glycols 5 (alkadiols, alcatriols, etc., for example, ethylene glycol and propylene glycol), diethylene glycol is particularly preferred. Carriers of this invention also include ketones miscible in water, such as acetone, Methyl ethyl ketone, methyl isobutyl ketone and cyclohexanone; and ethers. Water-soluble or strongly polar solvents such as formamide, dimethylformamide, dimethyl sulfoxide or N-methylpyrrolidone and the like are acceptable. Partially miscible liquids such as Turfural LL and furfuryl alcohol are also useful as carriers in this invention. Mixtures of different liquids are usually adequate. The carrier concentration in the suspension concentrate should be from 11 to 58 percent by weight based on in the total weight of the concentrate; preferably from 20 to 45 percent by weight, more preferably from 22 to 35 percent by weight. The stabilization zone properties of concentrated water soluble solids compositions / The carrier: they achieve mainly through the use of a three-component surfactant system, which is from 4 to L5 percent by weight of the total weight of the concentrate. The first component, which is a viscosity or ionic improving material preferably a polymeric material with a mass by volume of less than 15,000 is used to control the rheology of the concentrate and thus mainly create a stable dispersion and secondarily soften the crystal growth of solid particles. Examples of acceptable non-ionic viscosity improvers are polyacrylic acids and their sodium salts; the polyglycol ethers of fatty alcohols and condensation products of polyethylene oxide or polypropylene oxide; and their mixtures and include ethoxylated alkylphenols (also referred to in the art as alkylaryl polyether alcohols); aliphatic alcohols ethoxylated or polyether alcohols alkyl); ethoxylated fatty acids (or esters of polyoxyethylene fatty acid); anhydrosorbitol ethoxylated esters (or polyethylene sorbitan fatty acid esters), long chain amine and cyclic amine oxides, which are nonionic in basic solutions; long chain tertiary phosphine oxides; and long chain dialkyl sulfoxides.

Licitly, the enhancers u > non-viscosity • polymeric sori lys, polyoxypropylene ethoxylated polyoxypropylene glycols (polyalkylene oxide block copolymers); ethoxylated polyoxypropylene monohydric alcohols (polyalkylene oxide block copolymers of monohydric alcohols); and ethoxylated polyoxypropylene alkylphenols (polyalkylene oxide block copolymers of alkylphenols). More preferably, the viscosity improvers are ethylene oxide-propylene oxide block copolymers of the formula: CH 3 I HO (CH 2 CH 30) M (CH 3 CHO) m (CH 2 CH 20) p H where o and p are moles of ethylene oxide; in the range where o is from 2 to 128 and p is from 2 to 128 and m are moles of propylene oxide in the range of 16 to 67. The viscosity improver is present in the concentrate from 2 to 20 weight percent; preferably from 2 to 7 weight percent; and more preferably from 2 to 6 weight percent; such percentage based on the total weight of the concentrate. The second component of the surfactant stabilizer system is an anionic surfactant whose primary function is to synergistically control the increase in viscosity caused by the first component that inhibits crystal growth. Second, its affinity for adhesion to the surface of the particulate solids aids in the dispersibility of the particles. Anionic surfactants useful herein include alkyl and alkyl ether sulphates. These materials have the respective formulas ROS0M and RO (C2H40) x SOM, wherein R is an alkyl, alkenyl or alkylaryl group of about 8 to about 22 carbon atoms, x is 1 to 10, preferably 1 to 4, and M is a water-soluble cation such as ammonium, sodium, potassium, magnesium, triethanolamine (TEA), etc. The alkyl ether sulphates useful in the present invention are condensation products of ethylene oxide and monohydric alcohols having from about 8 to about 22 carbon atoms. Specific examples of the above sulfates include ammonium lauryl sulfate, magnesium lauryl sulfate, sodium 2-ethyl-hexyl sulfate, sodium actyl sulfate, sodium oleyl sulfate, sodium tridecyl sulfate, triethanolamine lauryl sulfate, linear ammonium alcohol, nonyl phenol ether ammonium sulfate ether. sulfate, and monoxinol-4-ammonium sulfate. or the appropriate class of mionic surfactants with the water-soluble salts of the general formula: Ri-SO.-M wherein Ri is selected from the group consisting of: i) a straight-chain hydrocarbon radical or branched, saturated aliphatic having from 8 to 24, preferably from 12 to 18 carbon atoms; ii) an aryl substituted with mono-, di- or tri-C 1 -C 6 alkyl, wherein the aryl is preferably a phenyl-naphthyl group; iii) alpha-olefins having from 12 to 24 carbon atoms, preferably from 14 to 16 straight-chain carbon atoms, more preferably 1-dodecene, 1-tetradecene, 1-hexadecene, 1-octadecene, 1-eicosene, and 1-tetracosine; and iv) condensation products of naphthalene formaldehyde. Additional examples of synthetic anionic surfactants, which are within the terms of the present invention are: i) isethionates, ie the reaction products of fatty acids esterified with isethionic acid and neutralized with sodium hydroxide, wherein , for example, fatty acids are lerivan of coconut oil; and ii) the n-rnetyltaurates, that is, the sodium or potassium salts of acid methyl amide degrees of methyltauride wherein the fatty acids, for example, are derived from coconut oil. Other synthetic anionic surfactants of this variety are set forth in U.S. Patent Nos. 2,486,921; 2,486,922; and 2,396,278. Still other synthetic anionic surfactants include the classes designated as the sulfosuccinates and sulfosuccinamates. These are from the general formulas: OR II R, -0 • or CKj-CH-C-O-Na (i) so, Na Na (ii) respectively, wherein R2 is a C2-C20 alkyl or alkylamido.

These classes include surfactants such as disodium N-octadecylsulfo-succinamate; N- (1,2-dicarboxyethyl) - tetrasodium N-octadecylsulfo-succinamate; diamyl ester of sodium sulfosuccinic acid; dihexyl ester of sulphosuccinium acid. of sodium; and dioctyl esters of sodium sulphosuccinic acid. Another class of anionic organic surfactants are the B-alkoxyalkanesulfonates. These compounds have the following formula: wherein Ri is a straight chain alkyl group having from 6 to 20 carbon atoms, R is a lower alkyl group having from 1 to 3 carbon atoms and M is a water soluble cation as described above. Specific examples of B-alkoxy-alkane-1-sulfonates, or alternatively 2-alkyloxy-alkane-1-sulfonates include: potassium B-methoxidecansulfonate, sodium 2-methoxy tridecansulfonate, potassium 2-ethoxytetradecylsulfonate, 2-isopropoxyhexadecylsulphonate of sodium, lithium 2-t-butoxytetradecyl sulfonate, sodium B-methoxyoctade-cyl sulphonate, and ammonium B-propoxydecylsulfonate.

Also included in the class of anionic surfactants are the disulfonates of the general formula: wherein R5 is an alkyl group of Cq-C2o and M is a water-soluble cation as described above. Preferred anionic agents of the disulfonate class are disodium diphenyl oxide dodecyl disulfonate and ethoxylated ammonium nonylphenyl disulfonate. All of the anionic surfactants described above and their mixtures may or may not be ethoxylated with from about 1 to about 10 ethylene oxide units per unit "R". The anionic surfactant is present in the concentrate from 1 to 20 weight percent; preferably from 1 to 7 weight percent; and more preferably from 1 to 5 weight percent; such percentage is based on the total weight of the concentrate. The third component of the surfactant stabilizer system is a bulky nonionic surfactant containing a large hydrophobic group. These third components are of the formula R, 0 (CUH.:QO),: R - wherein Rr is selected from the group consisting of phenyl; mono- or trisubstituted phenyl; phenylalkyl of Ci-C.; and mono-, di- or trisubstituted Ci-Cß-alkyl, wherein the phenyl substituent group (s) each has a total of 1 to 30 carbon atoms, and wherein each substitution can be a straight or branched carbon chain , saturated or unsaturated, a phenyl, enylalkyl, alkylphenyl, or alkylphenylalkyl group, wherein r. is from 2 to 4 or may be the same or different for each alkylene oxide unit; wherein R7 is a hydrogen, phosphate or sulfate entity; and wherein X is from 2 to 100. Preferably, this component is a dinonylphenol or a tristyrylphenol, more preferably an ethoxylated dinonylphenol or tristyrylphenol and / or any ester thereof. These ethoxylated tristyrylphenols and their derivatives can be described as comprising at least one polyoxy ethylenated and / or oxypropylene (1-phenylethyl) phenolic or phenyl ester of the formula: where: m e 2 or 3; (OXi is an oxy etilenada unit and / or exi-propilenada Recurrence; n is 12 to 35; preferably 16 to 30;. And R is an entity hydrogen, phosphate or sulfate The bulky nonionic surfactant is present in the concentrate of 1 to 20 weight percent, preferably 1 to 7 weight percent and more preferably 1 to 5 weight percent, such percentage is based on the total weight of the concentrate. added to the concentrate from 0 to 30 percent by weight.The water acts mainly to control the temperature coefficient of the solubility and thus helps to minimize changes in particle size.Preferably, the water is added 0 at 20 weight percent, and more preferably from 1 to 8 weight percent, approximately, such water percentages are based on the total weight of the concentrate.While the method for preparing the concentrates of this invention is not critical, a first aspect is prep plowing first a mixture of the nonionic surfactant with the bulky hydrophobic group; the anionic surfactant; the organic liquid carrier; and water (if any) and loading that mixture into a mill or grinder such as an "Eiger" mill. The polymeric viscosity improver does not ionize then it is milled into the mixture. The material soluble in solid water that is going to be concentrated in the suspension is added to the end and ground until the desired particle size and distribution is obtained. The particle size should not be so fine that the initial viscosity (24 hours) exceeds 30,000 cps at room temperature. Although the (Amano particle volume mean diameter of the soluble solid material in water may be from about 0.5 microns to about 500 microns, preferably from about 30 to about 200 microns, still more preferably from about 80 microns to about 120 microns. To determine the stability of the concentrates of this invention, a storage stability program is conducted on numerous samples of suspension concentrate over time, the samples are initially measured for viscosity and syneresis after 24 hours. duplicate in storage at room temperature (approximately 24 ° C) and 50 ° C during evaluations of 2, 3 and 4 weeks The percentage of syneresis and the vertical "T-bar" viscosity profiles were measured at each interval. was measured at three-week intervals, and measurements of viscosity were made using a Brookfield rheometer (Model DV III) and a Brookfield LV spindle kit. The viscometer was operated for 120 seconds at each selected speed; the readings were recorded every ten seconds; and the twelve digital readings were averaged. The initial viscosities were measured at 24 hours, plus or minus 4 hours, preferably ± 2 hours. An acceptable initial viscosity scale at room temperature is about 100 to 3C, 000 cps. The vertical viscosity profile was conducted on each sample using a Brookfield Heliopath T-bar spindle set, with the tips cut, at 12 rpm or less. The container is a pitcher of 56.7 grams (two ounces) having a diameter of four centimeters and a height of eight centimeters. The vertical profile runs from the surface of the liquid to the bottom and a scale of 0 to 100 is set representing the depth of the liquid. A suspension is within the invention that after two weeks of the initial preparation and at room temperature (24 ° C), the Heliopath viscosity, at 5. Oi-i cm (inch) below the surface of the • • center, < < exceeds 400,000 cps. After completing the viscosity profile, a small glass rod was carefully dipped towards the center of the bottom of the jar. The resistance of the glass rod in the penetration through the sample was evaluated sub-ethically for the degree of compaction. Any cake formation or clay formation was detected by simply inverting the sample container and observing the presence of material that did not leave the bottom of the container in thirty (30) seconds. The syneresis was determined by measuring the respective depths in the sample jar of 226.8 g (eight ounces) of the type used in the Helipath viscosity measurements. The liquid was measured in millimeters with a ruler from the bottom of the liquid to the top surface. The upper layer separation (if any) was also measured and that layer was calculated as a percentage of the total height of the sample. An acceptable result was obtained if the percentage of syneresis is equal to or less than thirty (30) percent after twenty-four (24) hours of storage at 24 ° C and then less than five percent is visible after thirty (30) investments.

The capacity to measure was determined using a Lnostometer Bostwick No. 24925-00. Approximately fifty (50) milliliters of concentrate at 24 ° C were placed in the Consistometer apparatus. The gate opened, while simultaneously a stop clock is started. The amount of time necessary for the material to reach the LO centimeter mark was observed or the time at which the material stopped flowing was observed; what happened first. An acceptable result was obtained if the material reaches the 10 cm mark at, or in less than one minute. The emptying capacity was determined qualitatively using the 226.8 g sample jar mentioned above (eight ounces), turning it upside down; and observing the movement of the suspension. The flow was determined subjectively as "difficult" if a high flotation appeared; "moderately difficult" if a flow of ketchup-type sauce was observed; "slightly difficult", if a type of creamy dressing flow was observed; and "easy" if it flows like a latex paint, thin. The particle size was measured using a particle size analyzer Galai Instruments Model CIS-100 and following the manufacturer's instructions. The measurements were made before starting the storage tests and after they finished. An acceptable result was obtained if the particle size does not change by more than fifty (50) percent at the end of the four week storage tests. Typically, less than twenty (20) percent increase in particle size was found after three weeks of storage or after three freeze / thaw cycles using the concentrate suspensions of this invention. The methods of the present invention are demonstrated in detail in the following non-limiting working examples, wherein all parts and percentages are by weight unless otherwise indicated. Example I A mixture of 3.3 weight percent of tristyrylphenol ethoxylate (16), (Soprophor SSU, a trademark for a bulky nonionic surfactant from Rhone-Poulenc); 3.3 weight percent of ethoxylated-propoxylated block copolymer (Antarox F-88, (97 EO 39 PO 97 EO) polymeric viscosity improver trademark of Rhone-Poulenc); 3.3 weight percent of RHODACAL DSB, which is a trademark of Rhone-Poulenc for an anionic surfactant mixture of 50% water / 50% disodium diphenyloxide dodecyldisulfonate; and 25% ethylene glycol (reagent grade) was mixed in an Eiqer mill to effect a uniform mixture. Then, sixty-five percent by weight of potassium nitrate (grade of fertilizer) was added to the mixture and ground until all the particles were essentially less than 600 microns in average volume diameter and at least 85% were found between 50 microns and 600 microns. This lot was identified as "coarse" milling. All percentages are based on the total weight of the concentrate in the mixture. The above procedures were carried out with a second mixture of the second material and were ground until essentially all the particles had a mean volume diameter of less than 600 microns and at least 35% of the material had a volume average diameter of less than 50. mieras This lot was identified as "fine" milling. The batches prepared above of 65L of potassium nitrate, 25% of diethylene glycol and 10% of the surfactant system (plus water) were designated as samples A-1C and A-1F, respectively. The other two samples were prepared in a similar manner. In the first, the total level of surfactant (plus water) was reduced to 7 weight percent using only 2.3 weight percent of tristyrylphenol ethoxylate; 1.2 weight percent disodium diphenyloxide dodecylsulfonate; 1.2 percent by weight of water; and 2.3 weight percent of the ethoxylated-propoxy block copolymer side. Diethylene glycol was increased by 28 percent, weight to make the difference of these lots, that is, the coarse and fine lots of this sample were identified as A-LC and A-2F, respectively. In the next sample, the total level of surfactant (plus water) was reduced to 4 weight percent using only 1.3 weight percent of tristyrylphenol ethoxylate; 0.7 weight percent disodium dodecyl disulfonate diphenyloxide; 0.7 percent by weight of water; and 1.3 weight percent of the ethoxylated-propoxylated block copolymer. Diethylene glycol was again increased to 31 percent by weight to make a difference. These lots, ie, the coarse and fine lots of this sample were identified as A-3C and A-3F, respectively. The samples were stored at room temperature (24 ° C) and 50 ° C for four weeks. Measurements of syneresis were made at intervals of the second, third and fourth weeks, and the qualitative voiding capacity of the samples was determined at the end of the fourth week. The results of these tests are set forth in Table I below. Table I Syntheresis Cap, of emptying Thickness to: Vpi | .. Ambi n '< . Sample Concern _ ._;? On 2 weeks 3 s m.ir is 4 semari i 'n-- 1"1" 18.1 _ -. 23. "i. R -. -. - 2C i 25.3 1 '. I" 1. : t- L A-3C 4 13.4 Ib. 16. Filo to Temp. Ambient. Sample Concentration 2 weeks 3 weeks 4 weeks 4 weeks A- 1F 10 6. 7 6. "- 3. üit. Il --5F 4 7.4 5. - 14. - Difficult Difficult 50 °" Master Concentration 2 weeks 3 weeks 4 weeks 4 weeks A-1C 10 12.9 21.0 24.6 raod-Qir: - ? l A-LC 7 4.6 9.4 4.8 mod-di f icil A-3C 4 5.5 7.8 1.5 lig. dipcile Fine 50DC Sample Concentration 2 weeks 3 weeks 4 weeks 4 weeks A-1F 10 4.5 6.7 6.7 difficult A-2F 7 0.0 4.0 1.0 difficult A-3F 4- 0.0 2.0 4.2 easy The above results demonstrate the excellent control of syneresis achieved through of the use of the teachings of the present invention. Even under long-term storage conditions at both high temperature and ambient temperature conditions, a highly concentrated water-soluble suspension (65 KNO) can be drained and continue to exhibit extremely low syneresis. Examples 2- A number of samples of type A-1F was prepared as in Example 1, that is, having 10 percent of the surfactant system (plus water) using the same surfactants as in A-1F where in the ratios in percentage by weight between the surfactants were varied. Syneresis results were obtained 24 hours after the initial preparation.

Viscosity measurements were also taken after 24 hours and after the suspension was thoroughly shaken until no obvious syneresis layer was left. The results of the tests at room temperature described above are established in the Table II below. Table II Twenty-four hour assessments Percentage by weight BSU samples: DSB: FBS 'Syneresis (%) Viscosity (cps) A 3.3: 3.3: 3.3 2.7 12406 B 3.3: 2.2: 4.4 0.0 12858 C 1.0: 3.0: 6.0 4.1 15472 D 3.0: 1.0: 6.0 0.0 76831 E 2.0: 4.0: 4.0 1 3 17397 F 5.0: 1.0: 4.0 0 0 51237 e 5.0: 2.0: 3.0 1 5 14175 4.0: 2.0: 4.0 0 0 9831 With the exception of samples D and F, which exhibit unacceptably high initial viscosity, all samples using the system of the present invention demonstrate exceptional stability ! syneresis! and an initial full viscosity. Examples 10-17 A second series of samples prepared as in Examples 2-9 was subjected to room temperature (24 ° C) and 50 ° C, to evaluations of syneresis at the end of storage for two weeks and storage for four weeks. The results are set forth in Tables III and IV below.

Table III Two Week Storage Evaluation. Weight ratio BSU samples: DSB: FBS Syneresis 17 \ (%) Viscosity 50 ° C (%) A 3.3: 3.3: 3.3 6.1 5.6 B 3.3: 2.2: 4.4 0.0 0.8 C 1.0: 3.0: 6.0 6.1 7.0 D 3.0: 1.0: 6.0 0.0 0.0 1.0 4 0 4 0 < 1 5.3 '.0 1 0 4 0 0. no, .. 0 2 0 3 c 3. 0.8 4.0 2 0 4 0 4. / 1.3 Table IV Four Week Storage Evaluation Percent by weight Sample -, e BSU: DSB: FBS Syneresis TA () Viscosity 50 - -f] A 3.3: 3.3: 3.3 6.2 2.9 B 3.3: 2.2: 4.4 0.0 0.0 C 1.0: 3.0: 6.0 8.3 7.7 D 3.0: 1.0: 6.0 0.0 0.0 E 2.0: 4.0: 4.0 0.9 4.3 F 5.0: 1.0: 4.0 0.0 0.0 G 5.0 : 2.0: 3.0 3.9 1.5 H 4.0: 2.0: 4.0 3.7 1.5 The above results again illustrate the excellent syneresis results that were obtained using the system of the present invention. Examples 18-25 A third series of samples prepared as in Examples 2-9 was subjected to a viscosity evaluation of Heliopath after storage at room temperature (24 ° C) for two weeks. The results are presented in Figure 1. omc was previously indicated at the initial total viscosity levels, samples D and F have unacceptably high viscosity levels just below the surface of the concentrate after two weeks of storage at room temperature. Sample G also showed a large increase in viscosity with depth, which suggests that significant sedimentation of the suspension also occurred. However, the rest of the samples showed the relative uniformity with the depth that can be achieved using the teachings of the present invention. Examples 26-33 The following samples were prepared according to the procedures of Example 1, with, i) diacid ammonium phosphate ((NH4) H2P0) as the water-soluble solid in place of potassium nitrate and ii) propylene glycol in place of diethylene glycol. Other ingredients in their respective weight percentages (all based on the percentage by weight of the total concentrate) are as indicated in Table V below. Table V 26 27 28 * 2 9 * * 30 31 32 33 (NH) PO 4, 50 50 50 50 50 50 50 50 Propylene Glycol 44 44 44 44 44 45 9 45.5 44 Meiorador viscosity 2 2 _ _ _ _ _ 2 > c to XB Lstircno 2 2 - - 2 2 oprophor BSU Al pal CON 436 Nrml phenol sulfate 2 of air (4E0j; Antarcx F-108 ** "- 2 2 - - - - .. Igepal DM-710 P r. or. lphenol < ~ i EO '; - - - - 2 c-. ± cide 245D - - - - - ..1 1.5 Cal ae = oaio pcl ^ apl ca Molecular weight 50u * Coarse snack + * Fine grinding *' * Copolymers of ethoxylated-propylated block (128 EO 54 PO 128? O) Measurements of syneresis at room temperature and viscosity were made in each of the samples at a storage time of 24 hours and 3 weeks. of Bostwick emptying, at the end of the 3-week storage tests The results are reported in Table VI.

Table VI Results Storage Room Temperature Di H Phosphate pear Ammonium Layer vaciad liad l ^ S esis nte (%) Viscosidaa íustwick lseg; Eighty-first 24 hours / 1 week 24 hours / 3 weeks weeks .3,12.5 3739/1698 16 1844/1540 28 4.5 10.5 3513/2487 29 0.0 / 3.4 8916/5047 Detainee ^ 0 3.0 ^ .8 3833/2006 32 6.5 / 19.6 2579/1774 33 4.0 / 15.7 3661/3783 Comparisons A-1F - From A to 2F - A-3F Stopped - Vertical viscosity profiles (24 ° C) at room temperature at 3 weeks were also determined on similar samples prepared from Examples 26 to 33 and the results are presented in Figure 2. It can be seen in Figure 2 (and Figure 1) that one can easily determine if compaction or sedimentation occurs in a sample through a profile of •, Iscosidase IL-lipath. With the exception, of Samples n • A and -i ÍA, viscosities through the depth of the highly concentrated suspensions of this invention, are remarkably uniform. Other applications of this invention, wherein a product is required in the form of a highly concentrated suspension of water soluble solids, including concentrates for the production of agricultural spray formulations, sodium chloride sludges for road thaw, bulky supply to through a pipe or inorganic salts, as well as the transportation of explosive compositions in mud. While the invention has been described in conjunction with specific embodiments, it is evident that many alternatives and variations will be apparent to those skilled in the art in light of the following description above. Accordingly, the invention is intended to encompass all alternatives and variations that fall within the spirit and scope of the appended claims.

Claims (8)

1. CLAIMS 1. A non-aquase suspension concentrate, characterized in that it comprises: a) from 40 to 85 percent by weight of a compound having a solubility in water greater than one percent based on the weight of the compies and water at 24 ° C, the particles of such concentrate have an average volume diameter of 0.5 microns at 500 microns; b) from 11 to 58 weight percent of an organic liquid carrier, miscible in water; c) a surfactant system comprising: i) from 2 to 20 weight percent of the nonionic polymeric viscosity improver; ii) from 1 to 20 weight percent of an anionic surfactant; and iii) from 1 to 20 weight percent of a bulky anionic active surfactant of the formula Rβ-O- (CnH 2nO) γ-RT wherein R 6 is selected from the group consisting of a phenyl; a mono- or trisubstituted phenyl; a phenylalkyl of C? -C6; a C 1 -C 6 mono-di-or trisubstituted phenylalkyl, wherein the phenyl substituent groups each have a total of 1 to 30 carbon atoms, and wherein each substitution may be a straight or branched, saturated carbon chain or unsaturated, a phenyl group, an alkylphenyl group, a t-phenylalkyl group or a -phenyl-phenyl-lower alkyl group; where n is n 2 to d and can be the same or different for each alkylene oxide unit; wherein R7 is a hydrogen, phosphate or sulfate entity; and where X is from 2 to 100; and d) from 0 to 30 weight percent water; with the proviso that the properties of the suspension concentrate at 24 ° "are within the limitations of the stabilization zone of: 1) an initial Brookfield viscosity of 100 to 30,000 cps; 2) a Helipath viscosity of minus 400,000 cps at two weeks after the initial preparation and at 5,8 cm (two inches) below the surface of the concentrate, 3) a Bostwick consistometer time of 10 cm equal to or less than one minute, and 4) a syneresis at 24 hours less than 30% with less than 5% after thirty inversions, all previous percentages by weight are based on the total weight of the concentrate, except where indicated 2. The non-aqueous suspension concentrate in accordance with claim 1, characterized in that: the active agent system comprises: i).> 2 to 7 percent «- weight of the improver of polymeric, non-ionizing, iL from 1 to 7 percent by weight of the nonionic surfactant and iii) from 1 to 7 weight percent of the bulky nonionic surfactant. 3. The non-aqueous suspension concentrate according to claim 2, characterized in that: i) the polymeric non-ionic viscosity improver is selected from the group consisting of: a) polyacrylic acids and their sodium salts; b) pclialkylene oxide block copolymers; and c) their mixtures; ii) the anionic surfactant is selected from the group consisting of: a) alkyl or alkyl ether sulphates of the formulas: RO-SO3M or R-0- (C2H40) x-S03-M respectively wherein R is an alkyl, alkenyl or alkaryl of about 8 to about 22 carbon atoms, x is 1 to 10, and M is a water-soluble cation; b) water-soluble salts of the formula R.-LO -M where Ri is selected from the group consisting of 1) a saturated straight or branched chain aliphatic hydrocarbon radical having from 8 to 24 carbon atoms; 2) a substituted aryl mono-, di or trialkyl of C.-Cβ, wherein the aryl is a phenyl or naphthyl group; 3) -ylfa-olefin having from 12 to 24 carbon atoms; and 4) condensation products of naphthalene formaldehyde; c) isethionates; d) n-methyl taurates; e) sulfosuccinates; f) sulfosuccinamates; g) B-alkyloxy alcansulfonates; h) disulfonates; and i) their mixtures; and üi) the bulky nonionic surfactant comprises at least one poly (l-phenyl-ethyl) phenolic or phenyl polyoxy ethylated and / or oxy propylene ester of the formula: where m is 2 or 3; (OX) is an oxyethylenated and / or oxypropylene repeat unit; n is from 12 to 35; preferably from 16 to 30; and R7 is a hydrogen, phosphate or sulfate entity. 4. The non-aqueous suspension concentrate according to claim 3, characterized in that: i) the nonionic polymeric viscosity improver is an ethoxylated-propoxylated block copolymer; ii) the anionic surfactant is dodecyl diphenydiioxide disodium isolate; and iii the bulky nonionic surfactant is ethoxylated with tristyrylphenol. 5. The non-aqueous suspension concentrate according to claim 1, characterized in that the water-soluble solid is a fertilizer. 6. The non-aqueous suspension concentrate according to claim 5, characterized in that the water-soluble fertilizer is potassium nitrate or ammonium dihydrophosphate. /. The nonaqueous suspension concentrate according to claim 1, characterized in that the organic liquid carrier, miscible with water, is selected from the group consisting of alkanoles of C.-C4; C] -C alkadiols and their mixtures. 8. The non-aqueous suspension concentrate according to claim 7, characterized in that the carrier is diethylene glycol.