MXPA97009428A - Preparation of ammonium glyphosate through a solid reaction system-gase - Google Patents

Preparation of ammonium glyphosate through a solid reaction system-gase

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Publication number
MXPA97009428A
MXPA97009428A MXPA/A/1997/009428A MX9709428A MXPA97009428A MX PA97009428 A MXPA97009428 A MX PA97009428A MX 9709428 A MX9709428 A MX 9709428A MX PA97009428 A MXPA97009428 A MX PA97009428A
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Mexico
Prior art keywords
reaction
acid
clause
reactor
product
Prior art date
Application number
MXPA/A/1997/009428A
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Spanish (es)
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MX9709428A (en
Inventor
Mccabe Day Thomas
Laura Gillespie Jane
Melvyn Kramer Richard
Original Assignee
Monsanto Company
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Publication date
Priority claimed from US08/485,316 external-priority patent/US5633397A/en
Application filed by Monsanto Company filed Critical Monsanto Company
Publication of MX9709428A publication Critical patent/MX9709428A/en
Publication of MXPA97009428A publication Critical patent/MXPA97009428A/en

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Abstract

The present invention relates to a method for preparing phytoactive ammonium glyphosate characterized in that it comprises the step of: introducing anhydrous gaseous ammonia into a glyphosate acid medium to cause a reaction therebetween in a manner such that said gas is uniformly dispersed with the acid and such that the heat transfer to the outside of said reaction is optimized

Description

PREPARATION OF AMMONIUM GLIFOSATE THROUGH A SQLIDQ-GUNSEOUS REACTION SYSTEM BACKGROUND OF THE INVENTION The present invention relates to a dry herbicidal composition, which is not grouped, and to a method for manufacturing said composition. The products were prepared with the method for the preparation of an ammonium glyphosate by reacting directly gaseous ammonia with g-phosphate acid. completely in water and can be used to prepare * compositions of glofoam + or solids and dried with a high content of coajuvates., ñ DESCRIPTION OF THE STATE OF THE ART The N - fo s f or norne 111 g L i c i na? HOOCCH2 NH Ohfc PO (OH) 2], which is commonly known as glyphosate acid or simply 20 gl phosate, is widely known in the art as a highly effective herbicide. It is also known that glyphosate, an organic acid, has a relatively high water solubility. Therefore, the phosphate + o is typically formulated in the form of a water soluble salt, particularly as a monoisoprop laminate.
'? (IPñ) pair-to fight * or control herbs or plants. The glyphosate is offered commercially in the IPA salt shop by Ilonsan-to Coinpany of ', t, Louis, Missouri, UJ.'L.n.J bnjo la rnar * care st \ \ da ound ?? R,. The Patents of the Urudos States I, the 3,799,758 and the .405"granted by John E. Iranz, 26 of 1974, and the 2U < In September 1903, various salts of glyphosate, methods to prepare glyphosate salts, glyphosate formulations and methods of api A fall to combat and control herbs and plants were revealed. Other United States patents that scale out phytosede salts include United States Patent No. 4,315.7h5 issued to George D. Large on February 16, 1982, United States Patent No. 4,507,250 issued to Izal-- Bal-el on March 26, 1985, United States Patent No. 4,397,676 issued to Izal-Bal-el on August 9, 1983, United States Patent No. 4,481 issued to Michael R. Ppsbylla on November 1, 1984 and United States Patent No. 4,140,513 issued to Erhard 3. April 20, 1979. All of the above-mentioned patents are incorporated in all of the present application. as a reference. The Roundu ™ R brand herbicide is sold as a water soluble liquid concentrate, however, efforts have recently been made in the relevant technical field to develop a formulation of water-soluble solid and dry glyphosate having an efficiency equivalent to that of RoundupR. The conventional reasons for these efforts are those of economy of costs related to the packaging, shipping and storage of a solid investment with respect to a liquid. As can be seen, aqueous solutions include a significant amount of solvent that increases the volume and deposit of container containers and increases the costs associated with distribution after the product is manufactured on the market. A less obvious benefit lies in the ability to manufacture dry glyphosate, soluble in water. Specifically, it is believed that the formulated granular ions offer superior handling characteristics (ie, controlled losses) and are substantially lighter and less uncomfortable to transport (and often to handle *) making the product better suited to use in locations remote geographical However, the manufacture of a granulated glyphosate formulation involves overcoming inherent disadvantages related to higher production costs and comparative complexity of composing a solid product from a combination of liquid and solid reagents instead of manufacturing a product. in solution with the same reagents. Various methods are known for making a composition containing 20 μl of water-soluble solid glyphosate. For example, U.S. Patent No. 5,047,079 issued September 10, 1991 in the name of I) jatar, discloses a method for preparing a phytotoxic composition comprising mixing isopropyl sheet with a molten surfactant to form a matrix, the surfactant being a smell of tempera ur atmosphere. In United States Patent No. 5,070,197, granted on December 3, 1991 to Chin, and others, an x-trusion period is revealed in which a Bronsted acid is mixed. , for example, N-phosphonornetium, with sodium hydroxides in an oxtruser to produce a granular exudate * that has a residual moisture content of not more than 10%. Another method that includes the production of a dry sodium glycoside composition, but not including10 extrusion, is described in the PCT application of Publication No. UO 07/04595. In U.S. Patent No. 5,266,553, issued on November 30, 1993 to Champion et al., A method for preparing a bentazon salt or a salt is disclosed.
L5 herbicide containing a carboxylic acid functionality including repeated treatments of the salt with a neutralizing base selected from the group consisting of ammonia, an alkylamine, a hydroxalkyl amine, an alkali metal salt of an alkali metal and combinations thereof. In French Patent Publication No. 2,692,439 which was filed on May 19, 1993 and has been assigned to Productos Osa SAOTFIA, a phytotoxic preparation comprising N-phosphonornet l-glycine in the N-phosphonornet lysine is described in general. powder form or granules in combination 5 with a wetting agent, surfactant and / or a powdery additive. As exemplified in the reference, the onoainonium salt is derived from making glycolate acid with ammonium bicarbonate. United States Patent No. 5.J24.7UÜ, issued June 28, 1994 to Moreno, et al., Discloses a composition and related methods for making and using a non-hygroscopic glyphosate ammonium salt such as the mono- isopropy lainonium salt of N- (phosphono-met il) -glycine and the mono-isopropyl salt of the acid (3-arn? no- -carboxy-propyl) -methane phosphonic acid in the form of dry powder [sicl. In the publication of PCT Application No. WO 94/10044, published on May 26, 1994, a dry glycol composition is disclosed in which N-phosphonoethylglycine is mixed with, among others, a non-caustic, inorganic or organic basic material, such such as di ammonium phosphate or a basic guanidine salt such as guamdmo acetate. In the publication of the FPO Application No. 0 394 211, published on October 7, 1990, an invention is disclosed comprising a dry pesticidal composition and related methods for using and producing them. More particularly, the invention is related to a greater solubility of the pesticidal composition that is achieved by adding an effective amount of a flake! organosil cona block number or a uorocarbon wetting agent. In the publication of the FPO Patent Application No. UO 90/072775 to be published on July 12, 1990, an invention is disclosed by means of which soluble granulated flAíosato compositions are manufactured in water by means of the steps of mixing, granulating, drying, spraying and oxtruding. In the publication of the application d '* - PCÍ Patent No. UO' 12712637, which was published on August 6, 1992, an invention is disclosed that relates to water soluble dry phosphate including a composition comprising Substantially unreacted phytose, an acid acceptor such as sodium acetate and a liquid surfactant or sol i o. All prior patents and publications are incorporated herein by way of reference. In the related art, as described, it is appreciated that considerable efforts have been made towards the formulation of related compositions and methods for making and using dry glyphosates. However, none of the aforementioned references discloses a direct and practical method for producing a dry, water-dispersible, water-soluble and appreciably non-hygroscopic composition capable of absorbing and absorbing water. an exceptionally high level of adjuvants by reacting solid N-phosphonornet with the relatively inexpensive and abundant ammonia A gaseous. Therefore, there is an unmet need for current technology by the present invention that meets these and other objectives. BRIEF DESCRIPTION OF THE INVENTION The unresolved needs of current technology are met by the present invention which provides a composition of dry ammonium glycolate-based plant regulator and herbicide and a new method for producing the composition, with which the disadvantages related to the known dry compositions and the related methods that have been described are overcome by limitations hitherto unknown and undisclosed. According to the present invention, gaseous phosphate acid is charged in the form of "cake mold" with a moisture content of up to about 20% by weight (ie; loss of weight on drying * or LOD), in a suitable reactor system *, for example in a conventional mixer. Or as the mixer agitates the wet cake, it is neutralized by an equivalent amount of anhydrous gaseous ammonia which is fed directly to the mixer for reaction with the wet cake. As the reaction is exothermic, it is desirable that means be employed to facilitate the transfer of heat * from the reactor system such as a water jacket fixed around the mixer or other conventional means that dissipates the heat produced by the reaction of that mode partially controls the temperature of the reaction. Furthermore, in this aspect, it has been found that the configuration of the mixer / reaction vessel and, par- ticularly, the unitary characteristics and the location of the gaseous ammonia inlet are impor- tant variables of the process. In addition, the internal temperature of the reactor is monitored and controlled in such a way that a temperature of approximately hU ° C must not be exceeded. In addition, and in combination with the above, the relative humidity content of the wet cake and the speed at which the gaseous ammonia is added to the reaction, among other things, are also factors that influence the ease of handling of the reaction mass. Therefore, an important aspect of the present invention is the manner in which all these variables are handled so that the thermal balance can be controlled and a desirable product obtained. The ammonium glyphosate composition produced in accordance with the process of the present invention is powder-form and is suitable for final use as a herbicide or as a plant growth regulator. However, perhaps in a more important aspect, the reaction product in the form of powder - because of its highly absorbent and adsorbent character, can be formulated additionally to absorb / adsorb an exceptionally high level of a coadyuvate such as a wetting agent, an anti-foam agent and particularly a surfactant composition. Therefore, when formulated in this way, a highly desirable product loaded with coadjuvants is formed, which in all its aspects is as good and effective as the comparable products obtained by the p? ocosos dol previous art that require raw materials as expensive. Optionally, the product of the reaction in powder form or the product loaded with adjuvants can be granulated to provide an herbicide and / or plant growth regulator of ammonium gil phosphate that slides freely (ie, does not clump) , soluble in water and subscially in 111 > re of dust. It is also possible to carry out other optional procedures using the reaction product as a powder. For example, the powder can be ground additionally or dried before packaging. The significant advantages achieved by the present invention lie in its relative simplicity, and in the low comparative costs of its reagents. In addition, the process of the present invention is very strong. Fs < or this is because the gaseous ammonia is reacted directly with the solid glycolate acid to produce a powder and therefore the significant problem of isolating the ammonium glyphosate in solid form from a solution is eliminated.
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a new method for reacting N-fos fonorneti l gl i cma (áci do gil fosato) ron ainoru tu? gaseous anhydrous to produce ammonium phytate powder, a prune material that can be used in the production of gaseous phosphate compositions in granular form or loaded with tessi-active. Until now a comparatively economical, efficient and practical method of producing dried ammonium glyphosate powder capable of being formulated to absorb / adsorb an exceptionally high level of an adjuvant by reacting glycolate acid with ammonia or gas has not been known. On the other hand, several less advantageous alternative methods have been developed by means of which ammonium glyphosate as well as alkaline metal glyphosates such as sodium glyphosate have been passed as dry powder. For example, sodium glucoside has been produced by reacting glycolate acid with sodium acetate or by extruding the acid with sodium hydroxide as described in PCT Patent Application Publication Mo. UO 92/12637 and U.S. Patent No. 5,070,197 respectively. Up to now, granules and powders of sodium glyphosate have been used to produce satisfactory compositions of dry glycolate. However, when compared to ammonium glyphosate compositions, the alkali metal of sodium is much more hygroscopic, which means that it is not as 1 'resistant to ambient humidity. Therefore, sodium alkali metal glyphosate is considered more difficult and costly to process as a dry composition and, once conformed < Or, l, has a greater tendency to agglutinate with what is p? oducon Undesirable "cakes" of the finished material. In addition, due to the relative molecular weight * of the ammonia and sodium, the sodium glycolate salt compositions have a lower concentration of the active gyl phiosate than the equivalent salt compositions of the ammonium phylate.
In addition, the cost per pound of the sodium cation is much more expensive than the cost of obtaining the ammonium cation. The comparative disadvantages of the sodium phiosate compositions are, therefore, obvious. As noted above, some solid / solid reaction methods are known for making dry ammonium glyphosate. For example, it is believed that by reacting ammonium bicarbonate with g-phosate acid, as described in French Publication No. 2,692,439, a dry ammonium gil phosphate composition is obtained. The invention described herein, however, constitutes an advance in the art of making dry ammonium glyphosate even with respect to other known methods using ammonium bicarbonate. For example, in the practice of the present invention, which includes reacting anhydrous gaseous ammonia with solid N-phosphonornetylglycine, it has been observed that the cost per pound to obtain the ammonium cation derived from ammonium bicarbonate is several times more. It is expensive to obtain an equivalent amount of the same catalyst from gaseous ammonia. If large-scale pipelining of the ammonium phosphate is made, this difference in costs alone is a strong argument in favor of an effective method, such as of the present invention, to produce a solid ammonium gil phosphate using anhydrous gaseous ammonia as the source of the ammonium cation. As used in this documentation, the terms "solid" and / or "dry" refer to the physical state in which the formulation has a specific shape and volume and resists deformation. The solid can turn the form of pellets, flakes, granules, dust or similar. It is understood that the solid formulation can be subsequently dissolved in a suitable diluent, generally and preferably water, and applied to the site in which regulation or eradication of the plants is desired either by spraying or by other means. conventional From a technical perspective, there is very little known about the use of gaseous ammonia in processes such as the one disclosed here. When this is considered in combination with the safe, cost-effective and technically simple process of the gaseous ammonia of the present invention, the results obtained are unexpected. The reaction of gaseous ammonia with glyphosate acid to produce ammonium glyphosate is, perhaps, the least costly and most effective chemical approach possible. This is because the reaction includes the most fundamental reagents that include gaseous ammonia that is abundant and comparatively inexpensive, which is reacted by the gaseous acid in an addition reaction. Furthermore, as the chemistry of the reaction is so simple, no byproducts are produced as water which would complicate the reaction and would require removal as is the case when reacting ammonium hydroxide with acid gil fosato. In spite of the obvious advantages of the process of the present invention, however, it has been observed that the reaction that occurs between N-phosphonornet-il-y-i-ma and anhydrous gaseous ammonia is typically highly exothermic. Therefore, in the implementation of the present invention, an important factor * that must be considered is the transfer of heat to the exterior * of the reaction vessel ,, When the heat transfer of the reaction system is reduced and not is administered, the reaction product that is formed is a mass of solid leacción "glassy" that can hinder the continuity of the reaction. Furthermore, said product is not suitable for use as a finished product and is incompatible with conventional formulation equipment used in further processing. Since heat transfer plays such an important role in the reaction of gaseous ammonia with gaseous acid, it is very important that the reaction vessel in which the reaction takes place be designed in such a way as to ensure a high degree of transfer. In this regard, it is considered desirable that the mixing reactor / apparatus have tolerances between the edges of the components (i.e., the impellers) and the temperatures of the non-repressed heat towards the outside. inner walls of the reactor *. This is because, as the reaction occurs, there is a tendency in the reaction / product handle to adhere the inner walls of the reaction vessel. When the tolerances between the impellers and the walls are not narrow enough to allow the impellers to detach the product from the walls, the reaction mass / product forms a solid glassy coating on the inner walls of the reactor. Although said glassy product is formed only in a thin layer on the walls of the reactor, it can act as a thermal insulation bar inside the reactor * which reduces the heat transfer and imp of the heat transfer sensors. existing heat fulfill their function adequately. These conditions and the solid glassy product which is formed in relation thereto are totally different in the process of the present invention, which allows the formation of a highly desirable free sliding powder product, which is particularly suitable for its later formulation. Therefore, the strict monitoring of the process of the present invention and the extent to which the reaction between the gaseous phitosate and the gaseous ammonia of agreement are the process, are very important, to ensure the creation n of a solid product of soluble ammonium glyphosate / di water-soluble in the form of a book slip powder (ie, which does not form cake) which is characteristic of the present invention. According to the process of the present invention, the reactants are combined in such a way as to ensure a substantial dispersion of the gaseous ammonia within the moist cake of gaseous phosphate. Tempera The reaction is monitored and controlled carefully by means of various process variables including the addition of gaseous ammonia using suitable heat transfer means * well known to those skilled in the art such as adapting * a circulating water jacket around the reactor and / or the reactor impellers to generate a fluid sliding powder product. To strictly follow the process of the present invention, it is not only possible to use conventional equipment that is slightly adapted., but a powder of ammonium phylate is produced which can be * used to manufacture * products of dry phylate, highly loaded with adjuvants. The inventors have determined that, among other factors, the moisture content in the acid raw material is a critical aspect of the present invention. The amount of gaseous ammonia that is required for the practice of the invention is equivalent to the amount that is required [to achieve a neutralization of approximately 95-105% of the acid that can be * determined by * analogous methods. conventional ones known to those of ordinary skill in the art, such as by pH measurement. According to the process of the present invention, a quantity of wet cake of glycosate acid is charged with a moisture content of approximately 12% by weight and not less than approximately 3% by weight in a suitable reactor system. as a conventional suitable mixer, preferably with internal mixing impellers designed with a narrow tolerance with respect to the internal walls of the reactor / mixer. A gaseous phosphate composition with a higher moisture content can also be used in the process of the invention, although it is preferred that said composition first be dried to reduce the moisture content to the preferred range. Alternatively, it can be added a predetermined amount of sodium sulfite to prevent * the possible formation of rntrosarnins. Although the addition of sulphite of sodium is not necessary for the practice of the invention and does not affect the reaction between glyphosate acid and gaseous ammonia, some governmental regulations require that the levels of mtrosarnin in products of this nature be less than 1. ppm. Experience indicates that, when added, the effective range of sodium or sodium that must be added to ensure against the presence of unacceptable levels of nitrogen in 0.2 and 1.0 percent by weight of dry product. and ends »it. Once the wet cake of glycolate and the optional sodium sulfate have been charged to the reactor / mixer, a stoichiometric equivalent of anhydrous ammonia gas is directly fed to the reactor while the wet cake is stirred and mixed. Since the reaction is exothermic, an appropriate device must be adapted to the reactor system. rans heat exchange *, such as a circulating cold water jacket or other device known to those skilled in the art, to facilitate the transfer of heat and from that ear provide some control over the reaction temperature inside the reactor. During the gaseous ammonia addition step, various process variables are controlled, including the gaseous ammonia feed rate and the reaction temperature, so as to form a product of highly absorbent ammonium glyphosate powder. adsorbent and easy handling. As can be seen, the new process can be easily implemented using conventional equipment that is preferably designed to be substantially self-implants. In addition, however, they can also be used 'I- other equipment without such design features, in which case some measure must be incorporated, such as scraping 10 manual pepodico? untr, ron ol p? ocoso to keep * clean reactor heat transfer surfaces and product accumulation books. If this measurement is provided, the reaction / production mass, with the continuous process, forms a thermally insulating layer on the internal walls of the reactor, which frustrates heat transfer * and produces overheating of the reactor. product, destroying your face *? sti cas deseb les. The inventors have discovered that the manner in which the gaseous ammonia is introduced into the mixer for reaction with the gaseous acid is a very ignative aspect of the invention. According to the invention, the gaseous ammonia must be introduced into the reactor in such a way as to ensure * substantially a broad and uniform dispersion of the gas with the glyphosate acid. This precept is fulfilled in the invention when the feed gate (s) through which the gaseous ammonia is introduced into the reactor are located in such a way as to ensure that sufficient amounts of the acid are contacted with the gas as the The acid is stirred and the gas is introduced, to form a reaction mass / product which is the re-reaction of a reaction in which the ammonia gas has been reacted with the glycolate acid. The inadequate location of the gaseous ammonia inlets will possibly result in the deterioration of the gaseous ammonia and / or the formation of a doughy mass or a solid glassy product. For example, if an entry only allows the gaseous ammonia to react with a localized amount of the plant's phosphate buffer *, it is possible that a "hot spot" was formed in which the localized reaction mass overheated because of the accumulation 5 of excessive localized heat of the exothermic reaction. This phenomenon could not only contaminate * all the product that is produced at the moment, but also possibly plug the gas inlet (s) and thus increase the physical changes' *, in the processing equipment and create the possibility of an ammonia leak < ? asooso. In addition to the various variables of the process that have been identified, it has been determined that the temperature of the reaction mass is, at least partially, a function of the feed rate of the gaseous ammonia in the reaction.
In this regard, it has been determined that it is desirable to maintain * a temperature in the reaction mass of about 60 ° C or less to inactivate the production of a valuable product. tíajo the process conditions that have been revealed and described, the direct reaction of gaseous ammonia with acid Glitosate results in the production of a highly desirable ammonium glyphosate product capable of being formulated adi conally to absorb / adsorb an exceptionally high level of adjuvants. These conditions, including the configuration of the mixer / reactor *, the content '• > R of relative humidity of the initial glyphosate acid, the speed and form in which the gaseous ammonia is added to the reaction and various methods? to facilitate * the heat transfer to the outside of the reaction vessel, so fixed that, to your voice, you ensure that you obtain an adequate product of safe powder for further processing, There are a number of process variables that fall outside the scope of the requirements of the present invention and that negatively affect the advantages achieved by it. For example, if the temperature in the reaction mass is allowed to rise above approx. 60 ° C, the quality of the mass / pr? Duet or reaction can be substantially stopped. The following example illustrates the production of the composition of the invention according to the process described here., All percentages They are based on weight, unless clearly stated otherwise.
EXAMPLE 1 In an industrial-scale reactor system comprising a Liter 300 mixer / reactor equipped with cross flow mixing tools, a high-speed chopper and a water jacket containing cold water in circulation, 94.6 pounds (42.9 Kg) were added. ) of standard grade "N-fostomethyl glycine" "wet cake" with a moisture content of about 7.4 weight percent to the mixer / reactor, where it was mixed immediately. one go that all the wet toita had been placed in the tank, 0.4 lbs. (0.10 kg) of anhydrous ammonium sulfide, optionally 1 l, were also charged to the mixer, and mixed with the wet cake. The combination of wet cake and sulfate was then circulated within the mixer / reactor for a sufficient time to obtain a uniform mixture "Through the centrally arranged inlet into the mixer / reactor, in which the If the volume of the mixture could be contacted, 0.65 pounds (3.92 kg) of gaseous ammonia was introduced into the reactor at a flow rate of approximately 0.2 pounds (0.09 g) /? n? n and it was reacted directly with the acid mixture. glLfosato. A probe was placed inside the reactor to monitor the temperature of the exothermic acid-base reaction. A temperature not higher than 60 ° C was maintained in the reaction mass partially due to the feed flow of the gaseous ammonia that was fixed. Once the final product is obtained, it is dried in an oven at 50 ° C. The dried product was milled in a hammer mill equipped with a 40 mesh. The resulting finished product had a moisture content of not more than 1.0 weight percent. From the original reagents that included 94.6 pounds (42.9 Kg) of glyphosate acid (ie *, "wet cake" with a LOI) of 7.4%) and B.65 pounds (3.92 1-g) "Je ammonia gas, It can obtain a standard product of 97 pounds (44.03 Kgj of dry ammonium glyphosate with a moisture content of approximately 1.0% by weight.) The product obtained in relation to the preceding example. In the erect state, under suitable storage conditions, such as tightly closed polyethylene bags, the product did not degrade or form groups after 6 months of actual storage. moreover lethally, the powder reaction product / mass produced in accordance with the present invention is particularly well adapted for its additional formulation by absorption / adsorption of high levels of adjuvants. Further, the relative simplicity of the present invention, its ability to be practiced using conventional equipment and the comparatively reduced costs of the ammonium cation provided by the gaseous ammonia make the ability of the product / reaction mass in powder to absorb / adsorb high levels of adjuvants is very significant. Although the selection of a particular adjuvant or a combination of adjuvants can easily be carried out by those who are trained in the art without too much experimentation in Example 2, the exceptional absorption and adsorption capacity of the product is illustrated. / mass of i oncr on on po lvo when it is < a i ga with a training agent EXAMPLE 2 The powdered reaction product / process formed by the process described in example 1 can be used to make a dry formulation of ammonium glyphosate containing a high level of surfactant of at least approx. 20% by weight, In order to manufacture said highly charged product, 16 kilograms of the powder reaction product or mixture are mixed with 4 kilograms < A qualifying agent is the polymer and the alkaline and 1.4 kilograms of water in a mixer by lotus, for example, a Fuji Pa? Dl, for approximately 10 minutes with water at a temperature of about H0 ° C circulating in Shirt. The mass that is formed is then extruded, for example in a Fu i Paudal twin-screw extruder, equipped with meshes with 1-in. Diameter holes. The obtained extrudate consists of short, "tagliatelle" cylinders, which did not stick together and dried easily, for example in a fluid bed dryer E? Tz ~ A? Re, without forming undesirable lumps. . The dry ammonium glyphosate herbicide of the present invention retains its effectiveness after dissolution or dispersion in a suitable diluent, preferably water, and its application in the locus of the plant which is intended by spraying or by other means conventional

Claims (7)

7 \ NOVELTY OF THE INVENTION CLAIMS
1. - Method for preparing phytoactive ammonium phylatogen characterized by the step of: introducing anhydrous gaseous ammonia into an acid medium phosphate to cause a reaction between them in such a way that said gas < -e is dispersed uniformly with said acid and in such a way that the transference of heat * towards it. The exterior of said reaction is opti.
2. The method of clause 1, characterized in that said gaseous acid has a moisture content up to about 12% by weight.
3. The method of the clause, characterized in that said glyphosate acid can have a "Je hurne" Jad content of up to about 20% by weight but, in such case, it is first dried to reduce said moisture content to ca. 12% by weight before reacting with said gaseous ammonia.
4. The method of clause 1, characterized in that said glyphosate acid has a moisture content of not less than about 3% by weight.
5. The method of clause 1, characterized in that said phytose acid has a moisture content of approximately 12% by weight but not less than approximately 3% by weight. b, The method of clause 1, characterized in that said reaction is carried out in a conventional manner subst anely to an irnpLant e. ., - The method of clause 1, c rac ri ed, because the temperature of the mass / product of the reaction generated by said reaction is maintained at about the same time as C and is controlled, at least partially, by adjusting the speed at which said gaseous ammonia is reacted with said aci o., 8.- The method of clause 1, characterized by "said reaction being effected in a substantially autolol. implant and the temperature of the mass / reaction product generated by said reaction is maintained at about 60 ° C and controlled, at least partially, by ensuring < μ,? e the inner walls of said reactor are free of accumulations of product. 9. The method of clause 1, characterized in that said reaction is carried out in a substantially self-cleaning mixer / reactor and the temperature of the mass / reaction product generated by said reaction is maintained at about 60 ° C and is controlled, by at least partially, by a combination of two or more process variables that include adapting a water circulation jacket or other conventional means of facilitating the transfer of heat from said mixer / reactor, adjusting the speed at which said ammonia gaseous is reacted with said acid to maintain said temperature and ensure that the < -, inner walls of said reactor are free of accumulations of product. 10.- The method < The J1-C1 is assigned to 1, which is affected by the fact that the gaseous ammonia and said acid are reacted in amounts <That they are substi- tially and «important» are equitable. The method of clause 1, characterizing the required amount of said gaseous ammonia is equivalent to a sufficient quantity to neutralize between 95% and 105% of said acid. 12. The method of clause 6, characterized in that said gaseous acid has a moisture content of up to about 12% by weight, but not less than about 3% by weight and the temperature of the mass / reaction product. n generated by said reaction is maintained at about 60"C and is controlled, at least partially, to" just < the speed at which said gaseous ammonia is reacted * with said acid. 13. The method of clause 6, characterized in that said glyphosate acid has a moisture content of up to about 12% by weight, but not less than about 3% by weight and the temperature of the mass / reaction product generated by said reaction is maintained at about 60 ° C and is controlled, at least partially, ensuring that the inner walls of said reactor are free of? accumulations «the product. 14. The motive of clause 9, characterized in that said < ombination of process variables also includes adapting to said mixer / reactor a water or other conventional or circulation jacket to facilitate heat transfer. 15. Method of preparing a dry ammonium glyphosate capable of being highly charged with adjuvants, characterized in that it comprises the steps of: (a) charging a substantially constant mixer / reactor with a quantity of "cake" humid acid gliyosate; (b) introducing an amount of anhydrous gaseous ammonia into said reactor to cause a reaction between said gas and said acid; and (c) controlling the temperature of the mass / product or reaction generated in such a way as to maintain said temperature at a desired level of up to about h ° C. 1
6. The method of clause 15, characterized in that said glycolate acid has a moisture content of up to about 12% by weight, but not less than about 3% by weight and said gas and said acid are reacted in quantities that are substantially equivalent, they are equiomething rich. 1
7. The method of clause 15, characterized in that the step of controlling said temperature of the mass / reaction product includes adjusting the speed at which said ammonia gas is introduced to maintain said temperature at said level. wanted. 10. The method of clause 15, characterized by a niche step with the temperature of said mass / product. The reaction includes adornments to adapt to said inezcladora / reactor or a shirt of the circulation of water or other means. Conventional to facilitate * the transfer «Heat of said mixer / roactor. 19. The method of clause 1, characterized in that said step of controlling the temperature of said mass / reaction product includes, in any combination of two or more, adapting to said mixer / reactor a jacket and water circulation u another conventional means for facilitating * the heat transfer of said mixer / reactor, adjusting the speed at which said gaseous ammonia is introduced to maintain said temperature at said desired level and / or ensuring that the walls of said reactor are free «Product accumulations. 20. The method of section 15, characterized by the fact that the step of introducing the said gaseous ammonia also includes devices that ensure that said gas disperses uniformly in said acid at the time of the reaction.
MXPA/A/1997/009428A 1995-06-07 1997-12-02 Preparation of ammonium glyphosate through a solid reaction system-gase MXPA97009428A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US485,316 1995-06-07
US08/485,316 US5633397A (en) 1995-06-07 1995-06-07 Preparation of ammonium glyphosate via a gas-solid reaction system
US485316 1995-06-07

Publications (2)

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MX9709428A MX9709428A (en) 1998-07-31
MXPA97009428A true MXPA97009428A (en) 1998-11-09

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