IL121496A

IL121496A - Controlled-release encapsulated fertilizers

Info

Publication number: IL121496A
Application number: IL12149697A
Authority: IL
Inventors: Arie Markus; Zeev Wiesman; David Wolf
Original assignee: Univ Ben Gurion
Priority date: 1997-08-07
Filing date: 1997-08-07
Publication date: 2001-06-14
Also published as: NZ502497A; EP1012129A1; IL121496A0; AU8239098A; CA2299334A1; AU741233B2; WO1999007654A1

Abstract

A controlled-release encapsulated fertilizer comprising a core containing at least one fertilizer and a polymeric envelope containing at least one hormone selected from the group consisting of Auxin; indole alkyl acid; indole acetic acid (IAA); indole propionic acid (IPA); indole butyric acid (IBA); 2, 4 dichlorophenoxy acetic acid; 2, 4 chlorophenoxy propionic acid; 2, 4 dichloro phenoxyacetic acid propyl ester; and naphthalene acetic acid encapsulating said fertilzer.

Description

121,496/3 CONTROLLED-RLEASE ENCAPSULATED FERTILIZERS n iiD -mnw o vy -w>i nmn The present invention relates to control led-release encapsulated fertilizer.

More particularly, the present invention relates to a controlled-release encapsulated fertilizer comprising a core containing at least one fertilizer and a polymeric envelope containing at least one hormone encapsulating said fertilizer The encapsulating of various chemical reagents, pharmaceuticals, pesticides and herbicides in general have been proposed and described in the prior art.

As described e.g. in U. S. Patent 4,417,916, aqueous dispersions of pesticide and herbicide micro-capsules are particularly useful in controlled release pesticidal and herbicidal formulations because they can be diluted with water or liquid fertilizer and sprayed using conventional equipment, thereby producing uniform field coverage of the pesticide or herbicide/additives such as film forming agents can be added directly to the finished formulation to improve the adhesion of micro-capsules to foliage. In some cases, reduced toxicity and extended activity of encapsulated herbicides and pesticides have been noted.

A variety of techniques have heretofore been used or proposed for encapsulation purposes. In one such process, known as "simple co-acervation", a polymer separates from a solvent solution of the polymer by the action of a precipitating agent that reduces the solubility of the polymer in the solvent (e.g., a salt or a non-solvent for the polymer). Patents describing such processes and their shell wall material includes U. S. Patent Nos. 2,800,458 (hydrophilic colloids); 3,069,370 and 3,116,216 (polymers); 3,137,631 (denatured proteins); 3,4 8,250 (hydrophobic thermoplastic resins); and others.

Another method involves micro-encapsulation based on in situ interfacial condensation polymerization. British Patent No. 1 ,371 ,179 discloses a process which consists of dispersing an organic pesticide phase containing a polymethylene polyphenylisocyanate or toluylene diisocyanate monomer into an aqueous phase. The wall forming reaction is initiated by heating the batch to an elevated temperature at which point the isocyanate monomers are hydrolyzed at the interface to form amines, which in turn react with unhydrolyzed isocyanate monomers to form the polyurea micro-capsulate wall. One difficulty with this method is the possibility of continued reaction of monomer after packaging. Unless all monomer is reacted during the preparation, there will be continued hydrolysis of the isocyanate monomer with evolution of C02, resulting in the development of pressure when the formulation is packaged.

Various methods of encapsulation by interfacial condensation between direct-acting, complimentary reactions are known. Within these methods are reactions for producing various types of polymers as the capsule walls. Many of such reactions to reproduce the coating substance occur between an amine, which must be of at least di-functional character and a second reactant intermediate, which for producing a polyurea is a di-functional or polyfunctional isocyanate. The amines chiefly used or proposed in these methods are typified by ethylene diamine, having at least two primary amino groups. U. S. Patent No. 3,429,827 and U. S. Patent No. 3,577,515 are illustrative of encapsulation by interfacial condensation.

For example, U. S. Patent No. 3,577,515 describes a continuous or batch method which requires a first reactant and a second reactant complimentary to the first reactant, with each reactant in separate phases, such that the first and second reactants react at the interface between the droplets to form encapsulated droplets. The process is applicable to a large variety of polycondensation reactions, i.e., to many different pairs of reactants capable of interfacial condensation from respective carrier liquids to yield solid film at the liquid interface. The resulting capsule skin may be produced as a polyamide, polysulfonamide, polyester, polycarbonate, polyurethane, polyurea or mixtures of reactants in one or both phases so as to yield corresponding condensation copolymers. The reference describes the formation of a polyurea skin when diamines or polyamines (e.g. ethylene diamine, phenylene diamine, toluylene diamine, hexamethylene diamine and the like) are present in the water phase and di-isocyanates or polyisocyanates (e.g., toluene diisocyanate, hexamethylene diisocyanate and polymethylene polyphenylisocyanate) are present in the organic/oil phase.

Several methods for coating fertilizers of such as KN03 and NPK have been known. Until 1981 one patent by "Sierra" disclosed the coating of osmocote (NPK). After 1981 Japanese patents Nos. 84-146,053 and 54-840,716 disclosed coated fertilizers, said fertilizers were coated with urea formaldehyde.

JP 63-162,593 discloses a fertilizer envelope. Said envelope is produced by spraying a solution of polyethylene and eva (ethyl vinyl acetate) in CC12=CC12 on fertilizer granules.

The world's nursery industry utilizes numerous products and techniques in order to maintain and produce millions of ornamental plants and fruit trees. The nursery industry uses sophisticated agrotechnologies and consumes large quantities of rooting stimulators. There is an ongoing need for novel products that could increase rooting percentages of difficult-to-root (mainly woody or 4 121,496/3 A common procedure in a nursery entails the sporadic addition of fertilizers and hormones to the roots of new cuttings. The present inventors have found that the addition of a controlled-reiease encapsulated fertilizer can maintain the presence of the necessary compounds for the entire period of rooting and development of rooted plants.

With this state of the art in mind, there has now been found, according to the present invention, a controlled-reiease encapsulated fertilizer comprising a core containing at least one fertilizer and a polymeric envelope containing at least one hormone selected from the group consisting of Auxin; indole alkyl acid; indole acetic acid(lAA); indole propionic acid(IPA); indole butyric acid(lBA); 2,4 dichlorophenoxy acetic acid; 2,4 chlorophenoxy propionic acid; 2,4 dichloro phenoxyacetic acid propyl ester; and, Naphthalene acetic acid encapsulating said fertilizer.

In another embodiment of the present invention there is provided a process for encapsulating a fertilizer comprising: a) coating a fertilizer with a mixture of a first monomer and a hormone; b) adding a mixture of a second monomer and additional a hormone; and, c) heating said mixtures to induce the polymerization of said first and second monomers to form a polymeric envelope incorporating said hormone and encapsulating said fertilizer. wherein said envelope contains at least one hormone selected from the group consisting of Auxin; indole alkyl acid; indole acetic acid(IAA); indole propionic acid(IPA); indole butiric acid(IBA); 2,4 dichlorophenoxy acetic acid; 2,4 dichloro phenoxyacetic acid propyl ester; and, Naphtalene acetic acid. wherein said polymeric envelope is formed by a polymer selected from the group consisting of polyurethane; polyurea; and, polyolefins.

While the invention will now be described in connection with certain preferred embodiments in the following examples so that aspects thereof may be more fully understood and appreciated, it is not intended to limit the invention to these particular embodiments. On the contrary, it is intended to cover all alternatives, modifications and equivalents as may be included within the scope of the invention as defined by the appended claims. Thus, the following examples which include preferred embodiments will serve to illustrate the practice of this invention, it being understood that the particulars shown are by way of example and for purposes of illustrative discussion of preferred embodiments of the present invention only and are presented in the cause of providing what is believed to be the most useful and readily understood description of formulation procedures, as well as of the principles and conceptual aspects of the invention.

Examples: A series of formulations were prepared according to the present invention. As stated, according to the invention the fertilizer is the core of the formulation and the hormone is incorporated in the envelope. The hormones that were incorporated in the slow release formulations were from the following families: • Auxin- Indole alkyl acid IAA (Indole alkyl acid) , IPA (Indole Propionic Acid) and IBA (Indole Butinic Acid) - 2,4 Dichlorophenoxy acetic acid 2,4 Dichlorophenoxy acetic propionic acid 2,4 Dichloro phenoxyacetic acetic acid propyl ester Naphtalene acetic acid (NAA) auxin stimulated root regeneration and development • Triazole - Paclobutrazole (growth retardant that has an anti- gibberllin-enhanching effect on stimulation of root formation and increasing survival of rooted pland grown in stress conditions.

• Cytokinine - Benzoyladenine (plant hormone that stimulates development and branching of shoots) The coating consists of the following families of polymers: • polyurethane • polyurea • polyolefis (like polyethylene) etc Carbohydrates such as sucrose, starch, etc. that are enhancing auxin effect on stimulation of root regeneration and development are added to the envelope. Other materials that are added to the formulation are to increase the nutritional content (micro elements such as: Fe, B, Mg, Zn, Mn, Ca, Mo, etc.), to increase biotic tolerance (Benedate), Falpane, Merpan, Prochloraz, propionazol, diazinone, nephorex, etc), and to increase a biotic tolernace of the plants (triazole compounds such as majic that increase drought resistance by stimulation of wax cover of the leaves).

The above mentioned hormones increase the rate of cell division and differentiation and the result of said increased rate is a stimulation of root regeneration and development.

Growth retardants such as Triazole e.g. paclobutrazole can also be added. Said retardant has an anti-gibberllin-enhancing auxin effect on stimulation of root formation. Other materials that are added to the formulation are to increase biotic (pathogens) and abiotic (drought) tolerance of plants.

Hormones can also be added to the core if desired Procedure: The granules of fertilizer were put in a coating pan and one monomer with part of the hormone was added. The coating pan rotated until the granules were covered with one monomer containing part of the hormones, then a second monomer with the rest of the hormones and catalyst were added. The coating pan rotated and the mixture was heated up to 50 °C. When the condensation polymerization ended, and when the granules are not sticky, talcum was added followed by melted wax. The coating pan was rotated continuously. The formulation is then put in bags.

The formulations are summarized in Table 1: Table 1 Envelop formulation on fertilizer (K 03, MKP) Example No. Amount Amount Glycols Hormones NO3, g Voranate M580, g Type Amount, type amount Talc, g 1 (A1 ) 100 10 PEG-600 10 2-4 DP 1 5 . (A12) 100 10 PEG-600 10 2-4 DP 0.5 5 . (A2) 100 10 PEG-600 10 2-4D 1 5 . (A22) 100 10 PEG-600 10 2-4 D 0.5 5 . (Bl) 100 10 PEG-1000 10 2-4DP 1 5 . (B12) 100 10 PEG-1000 10 2-4DP 10.5 . (B2) 100 10 PEG-1000 10 2-4 D 1 5 . (B22) 100 10 PEG-1000 10 2-4 D 0.5 5 . (CI) 100 5 PEG-6000 15 0. (C2) 100 5 PEG-6000 15 2-4 D 1 10 1. (C22) 100 5 PEG-6000 15 2-4D 0.5 10 2. (Dl) 100 5 PEg-12000 15 2-4 DP 1 10 3 (D2) 100 5 PEG-12000 15 2-4D 1 10 4. (E03) - - - - - '-5 (Ell) - - - - 2-4 DP 1 -6. (E12) - - - - 2-4DP 1 -7. (E42) - - - - I BA 0.5 -8 (E112) - - - - 2-4DP 0.5 -9. (E512) 25g+25g - - - 2-4 DP 0.5 MKP 0. (E532) 25g - - - I BA 0.5 25g MKP 1. (I) 100 5 EDA+DETA 0.8+0.7 I B A 0.1 15 2. (II) 100 4 EDA+DETA 1 +1 2-4D 1 - Table 1 (cont) Example No. Amount Amount Glycols Hormones NO3, g Voranate Type Amount, type amount Talc, g 23. (Ill) 100 10 EDA+DETA 0.8+0.7 PB-zol 0.5 - 24. (IV) 100 5 EDA+DETA 1+1 KP 0.1 - 5. (V) 100 4 EDA+DETA 1+1 2-4-DP 0.1 - 6. (VI) 100 10 EDA+DETA 1+1 2-4-DP 0.5 - 7. (VII) 100 10 EDA+DETA 1+1 2-4-D+PB-zot 0.5+0.5 - 8. (GSK-1) 100 10 EDA+DETA 1+1 2.4D 1 5 9. (GSK-2) 100 10 EDA+DETA 1 +1 2-4D 1 5 0. (GS -3) 100 10 EDA+DETA 1+1 PB-zol 1 5 1. (GS -5) 100 10 EDA+DETA 1+1 2-4 D 1 5 2. (GS -6) 100 10 EDA+DETA 1+1 2-4DP+PB-ZOI 0.5+0.5 5 3. (GSK-7) 100 10 EDA+DETA 1+1 2-4D+PB-Z01 0.5+0.5 5 4. (GSK-8) 100 10 EDA+DETA 1+1 2-4DP+PB-Z01 + IBA 0.5+0.5+0.5 5 5. (GSK-10) 100 10 EDA+DETA 1+1 PB-zol+IBA 0.5+0.5 5 6. (GSK-9) 100 10 EDA+DETA 1+1 PB-zol 0.5 -7. (GSK-11) 100 10 EDA+DETA 1+1 PB-Z01+I BA+2-4D 0.5+0.5+0.5 -8. (GSK-12) 250 25 EDA+DETA 2.5+2.5 PB-Z0I+IBA+2DP 1.25+1.25+1.25 9. GSK-13) 250 25 EDA+DETA 2.5+2.5 PB-Z01+IBA+2DP 1.25+1.25+1.25 0. (GSK-14) 250 30 EDA+DETA 3+3 IBA+PB-Z01+2DP 1.25+1.25+1.25 -1. (GSK-15) 250 25 EDA+DETA 2.5+2.5 IBA+PB-zol 0.6+0.6 -2. (GSK-16) 250 30 EDTA+EDA 3+3 IBA+PB-Z01+2DP 0.6+0.6+0.6 -3. (GSK-17) 250 30 DETA+EDA 3+3 IBA+PB-ZOL+2DP 0.6+0.6+0.6 -4. (GSK-18) 100 10 EDA+DETA 0.5+0.5 GA3 0.5 5 5. (GSK-19) 100 10 EDA+DETA 1 +1 PB-ZOL+IBA 0.5+0.5 5 6. (GSK-20) 100 10 EDA+DETA 1+1 IBA+PB-zol 0.5+0.5 5 7. (GSK-21) 100 10 EDA+DETA 1+1 IBA+PB-zol 0.5+0.5 5 8. (GSK-22) 100 10 EDA+DETA 1+1 IBA=PB-zol 0.5+0.5 5 Table 1 (cont.) Example No. Amount Amount Glycols Hormones KNO3, g Voranate 580, g Type Amount, type amount Talc, g Wax 49. (GSK-23) 100 10 EDA+DETA 1+1 IBA+PB-zol 0.5+0.5 5 5 50. (GS -24) 100 10 EDA+DETA 0.5+0.5 - 5 5 51. (GS -25) 100 10 EDA+DETA 0.5+0.5 5 5 2. (GS -26) 100 10 EDA+DETA 0.5+0.5 5 5 3. (GSK-27) 100 10 EDA+DETA 0.5+0.5 5 5 4. (GS -28 100 10 EDA+DETA 0.5+0.5 5 5 5. (GS -29) 100 10 EDA+DETA 0.5+0.5 PB-zol 1 5 5 6. (GSK-30) 100 10 EDA+DETA 0.5+0.5 - 5 5 7. (GS -31) 100 10 EDA+DETA 0.5+0.5 - 5 5 8. (1) 100 10 EDA+DETA 1+1 - 5 5 9. (2) 100 10 EDA+DETA 1 +1 - 5 5 0. (3) 100 10 EDA+DETA 1+1 - 5 5 1. (4) 100 10 EDA+DETA 1+1 - 5 5 2. (5) 100 10 EDA+DETA 1+1 5 5 3. (6) 100 10 EDA+DETA 1+1 - 5 5 100 10 ED+DETA 1+1 - 5 5 Biological methods: Each cutting was put in a vessel with special earth and with 3 granules, the cuttings were put in green houses. The amount of roots and the length of the roots were measured.

The plants utilized included were Phelargonium: roses, melloloica, olives from different clutivars, eucalyptus of different kinds and many others. The biological tests were carried out with up to 7,000 cuttings for each plant. These tests consisted of various soft cuttings easy-to-root, semi-woody cuttings medium-to-root, difficult-to-root cuttings and grasses.

Select formulations were tested.

The biological results on several kinds of plants are summarized in tables 2-7.

TABLE 2 BIOASSAY BASED ON MUNG-BEAN CUTTINGS TO TEST EFFECT OF ENCAPSULATED FERTILIZERS Treatment Average No. Average Root Length CM Roots 6 Days 10 days after treatment Control (¾ 0) 2.5 0.4 0.9 IBA 21.7 0.2 0.4 GSK-10 39.9 0.6 1.1 GSK-30 42.2 0.5 1.0 TABLE 3 EFFECT OF ENCAPSULATED FERTILIZERS GSK10 ON ROOTING CUTTINGS OF OLIVE CULTIVARS Cultivar Percent of Average No. Root Average Root Rooting Length (cm) Control Manzanillo 26 2.3 7.6 Barnea 49 4.0 5.0 Nab ali 31 3.5 6.3 Chimlali 19 3.7 4.5 Maalot 22 1.6 5.9 T-8 (Conventional Treatment) Manzanillo 48 3.6 4.2 Barnea 73 4.8 3.4 Nabali 52 4.4 5.2 Chimlali 46 5.1 4.0 Maalot 54 3.8 4.7 GSK-10 Manzanillo 52 5.3 8.8 Barnea 89 6.1 9.6 Nabali 61 5.8 7.2 Chimlali 58 5.6 6.6 Maalot 76 4.5 7.9 Table 4 EFFECT OF GSK-10 ON ROOTING OF VARIOUS PLANT SPECIES. THE TRAIL WAS DONE WITH 7000 CUTTINGS AT "GAT" COMMERCIAL NURSERY Plant name % rooting Picus Natasha 71 Solanum blue 82 Copea shrub 94 Picus Thailand 82 Hibicus 78 Juniper espanicum 93 Juniper galwcos 55 Huniper Ramat Hnandiv 85 Cypress lemon 55 Bougainvillea Glabra (purple) 94 Bougainvillea smooth 0 Cestrum 80 Rosa indica 98 Ethrog yaman 60 Pandorea Jasmin 89 Solanum White 98 Olive-K18 84 Olive-Nab ali 50 Miaforum 80 Malloloika dwarfish 95 Kles Tamun 36 Tchaltsporum jasmine 0 alive Cypress Tota 0 with Cypress cazoica 0 callus Table 5 EFFECT OF GSK-10 ON DEVELOPMENT OF ROOT SYSTEM OF CUTTINGS OF EUCALYPTUS Root system development ladder: + Roots distributed in less than 25% of the pot medium ++ Roots distributed in about 50% of the pot medium +++ Roots distribution in morethan 75% of the pot medium Treatment Clone control T-8 GSK-10 Anulata ++ + ++++ Gillii + + +++ Ficifolia - + +++ Kruseana - + + + Popolnea + + +++ TABLE 6 EFFECT OF ENCAPSULATED FERTILIZERS ON SHOOT DEVELOPMENT OF OLIVE ROOTED PLANTS Treatment Average Shoot Elongation (cm) 30 Days 60 days after treatment T-8 2.2 4.3 (Conventional treatment) Ax 1.8 4.1 A2 4.0 7.3 Ci 2.7 6.5 TABLE 7 EFFECT OF ENCAPSULATED FERTILIZERS GSK-10 ON VEGETATIVE AND REPRODUCTIVE DEVELOPMENT OF SOLANUM BLUE ROOTED PLANTS Treatment Transplanting date Average Root Average Number of height CM flowers/plants Conventional (T-8) March 10 43 9 GSK-10 April 17 87 26 The release rate was determined by the following method, one gram of the granules were placed in a dissolution system. Samples were taken from the vessels and the amount released was determined in the following way: the amount of the fertilizer by conductometeric method and the amount of the hormone by HPLC.

Very promising results concerning the rate of root formation, length of roots, survival of plants and ease of high mass plant production were clearly observed.

The formulations were found to be most effective in: accelerating root formation, increasing rooting percentage, improving the quality of root system, and stimulation of young plant (vegetative and reproductive) development in comparison to untreated control and IBA talc powder (the common substance used at present for rooting in all nurseries).

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative examples and that the present invention may be embodied in other specific forms without departing from the essential attributes thereof, and it is therefore desired that the present embodiments and examples be considered in all respects as illustrative and not restrictive, reference being made to the appended claims, rather than to the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Claims

19 121 ,496/3 What is claimed is:

1. A controlled-reiease encapsulated fertilizer comprising a core containing at least one fertilizer and a polymeric envelope containing at least one hormone selected from the group consisting of Auxin; indole alkyi acid; indole acetic acid(IAA); indole propionic acid(IPA); indole butyric acid(IBA); 2,4 dichlorophenoxy acetic acid; 2,4 chlorophenoxy propionic acid; 2,4 dichloro phenoxyacetic acid propyl ester; and, Naphthalene acetic acid encapsulating said fertilizer.

2. A controlled-reiease encapsulated fertilizer according to claim 1r wherein said polymeric envelope is fomned by a polymer selected from the group consisting of polyurethane; polyurea; and, poiyoiefins.

3. A controlled-reiease encapsulated fertilizer according to claim 1 , further comprising a triazole incorporated therein.

4. A controlled-reiease encapsulated fertilizer according to claim 3, wherein said triazole is paciobutrazoie.

5. A contrplled-reieased encapsulated fertilizer according to claim 1, further comprising a cytokinine incorporated therein.

6. A controlled-re!eased encapsulated fertilizer according to claim 5, wherein said cytokinine is benzoyladenine.

7. A controlled-released encapsulated fertilizer according to claim 1, further comprising a carbohydrate incorporated therein. 20 121 ,496/3

8. A controiled-reieased encapsulated fertilizer according to claim 7, wherein said carbohydrate is selected from the group consisting of glucose, sucrose and starch.

9. A controiled-reieased encapsulated fertilizer according to claim 1, further comprising a fungicide incorporated therein.

10. A controiled-reieased encapsulated fertilizer according to claim 9, wherein said fungicide is selected from the group consisting of Benelate, folpane, merpan and propionazal.

11. 1. A controiled-reieased encapsulated fertilizer according to claim 1, furhter comprising an insecticide incorporated therein.

12. A controiled-reieased encapsulated fertilizer according to claim 11, wherein said insecticide is diazinone or nephorex.

13. A process for encapsulating a fertilizer according to claim 1 comprising: a) coating a fertilizer with a mixture of a first monomer and a hormone; b) adding a mixture of a second monomer and an additional hormone; and, c) heating said mixtures to induce the polymerization of said first and second monomers to form a polymeric envelope incorporating said homnone and encapsulating said fertilizer.

14. A process for encapsulating a fertilizer according to claim 13, wherein said envelope contains at least one hormone selected from the group consisting of Auxin; indole alkyi acid; indole acetic acid(!AA); indole propionic 21 121 ,486 3 acid(IPA); indole butyric acid(IBA); 2,4 dichlorophenoxy acetic acid; 2,4 dichloro phenoxyacetic acid propyl ester; and, Naphthalene acetic acid.

15. 5. A process for encapsulating a fertilizer according to claim 13, wherein said polymeric envelope is formed by a polymer selected from the group consisting of polyurethane; polyurea; and, polyolefins.

16. A process for encapsulating a fertilizer according to claim 13, wherein said envelope contains at least one honnone selected from the group consisting of Auxin; indole alkyi acid; indole acetic acid(IAA); indole propionic acid(IPA); indole butyric acid(IBA); 2*4 dichlorophenoxy acetic acid; 2,4 dichloro phenoxyacetic acid propyl ester; and, Naphthalene acetic acid, and further optionally comprising at least one further component selected from the group consisting of a growth retardant, a cytokinine, a carbohydrate, a fungicide and an insecticide. For the Applicant WOLFF, BREGMAN AND GOLLER by: ^ ^