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WO2018122682A1 - Engrais à libération contrôlée et son procédé de fabrication - Google Patents

Engrais à libération contrôlée et son procédé de fabrication Download PDF

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Publication number
WO2018122682A1
WO2018122682A1 PCT/IB2017/058152 IB2017058152W WO2018122682A1 WO 2018122682 A1 WO2018122682 A1 WO 2018122682A1 IB 2017058152 W IB2017058152 W IB 2017058152W WO 2018122682 A1 WO2018122682 A1 WO 2018122682A1
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WO
WIPO (PCT)
Prior art keywords
hydrogel
cellulose
controlled release
solution
mixing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/IB2017/058152
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English (en)
Spanish (es)
Inventor
Pedro ARAQUE MARÍN
Octavio Augusto GONZÁLEZ MURILLO
Marybel MONTOYA ÁLVAREZ
Adriana María QUINCHÍA FIGUEROA
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Soluciones Biotecnologicas Y Agroambientales (sobiotech)
Universidad EIA
Original Assignee
Soluciones Biotecnologicas Y Agroambientales (sobiotech)
Universidad EIA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Soluciones Biotecnologicas Y Agroambientales (sobiotech), Universidad EIA filed Critical Soluciones Biotecnologicas Y Agroambientales (sobiotech)
Publication of WO2018122682A1 publication Critical patent/WO2018122682A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/10—Crosslinking of cellulose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
    • C08F261/02—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
    • C08F261/04—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075—Macromolecular gels
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/011—Crosslinking or vulcanising agents, e.g. accelerators
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/015—Biocides

Definitions

  • the present invention can be used in agribusiness, particularly in the production of controlled release fertilizers and in the controlled release of organic pesticides.
  • a possible solution that paves the way to this problem is the use of systems that allow controlled release of nutrients in the soil, so that their availability can be optimized, minimum losses are achieved and help alleviate ecosystems from a considerable burden of disturbing elements.
  • Controlled release fertilizers are in the state of the art, as is the case of document CN102351608 which discloses a controlled release particle fertilizer consisting of a granular shaped double layer core. Particularly it comprises a first interface layer that covers a core, and a controlled release layer as a coating of the interface layer, controlling the dissolution of pesticides and fertilizers.
  • CN 100457694 discloses a biodegradable slow release fertilizer, which comprises a fertilizer within a surface composed of a coating of a water soluble polymer, which includes the formation of a polymer emulsion where they are mixed: cellulose, starch oxidized, polyvinyl alcohol, prepolymer polyurethane, epoxy resin, curing agents, crosslinking agent and emulsifier, which is subsequently applied to the fertilizer to control its release capacity.
  • the coating material is composed of starch, cellulose, polyvinyl alcohol, a crosslinking agent, a modifying compound and a powder filling.
  • the preparation method comprises: adding starch, cellulose, polyvinyl alcohol, water and stirring; add crosslinkers and gradually heat the mixture; then add the modifying compound and stir the added powder filling.
  • a spray-based emulsion is obtained, which is used as a coating material on the surface of controlled release granulated fertilizers.
  • Hydrogels have also been designed as systems capable of retaining substances that will then be released in a controlled manner in the environment in which they are available.
  • solid polymer matrices based on Chitosan and Xantane for controlled fertilizer release (Melaj, M., & Daraio, ME (2012).
  • Solid polymer matrices based on Chitosan and Xantane for controlled fertilizer release (Advances in Science E Ingenier ⁇ a, 3 ( ⁇ ), 1-9.)
  • Other fertilizers are directed at the root of the plants with a carboxymethylcellulose matrix manufactured by ionic crosslinking (Davidson, DW, Verma, MS, & Gu, FX (2013).
  • Controlled root targeted delivery of fertilizer using an ionically crosslinked carboxymethyl cellulose hydrogel matrix shows a wheat straw cellulose-based hydrogel with semi-penetrated polymer networks with retained water integration, for controlled release of fertilizers; this process requires a pretreatment to obtain cellulose, where wheat straw is milled and immersed in ammonia for 48 hours, Wash several times with distilled water and dry, then immerse in nitric acid at 100 ° C for 45 minutes, to finally wash with distilled water and dry (Li, X., Li, Q., Su, Y., Yue, Q., Gao, B., & Su, Y. (2015).
  • a novel wheat straw cellulose-based semi-IPNs superabsorbent with integration of water-retaining and controlled-release fertilizers (Journal of the Taiwan Institute of Chemical Engineers, 0, 1-10.).
  • a controlled fertilizer release system can also be found using straw graft copolymers in which requires that nutrients be loaded into the hydrogel by swelling from a solution with K2HPO4 + K2S2O8 + ((NH4) 2Ce (N03) 6), which is very different from the inclusion of the nutrient in the same conformation of the hydrogel (Li, Q. , Ma, Z., Yue, Q., Gao, B., Li, W., & Xu, X. (2012). Synthesis, characterization and swelling behavior of superabsorbent wheat straw graft copolymers. Bioresource Technology, 118, 204- 9.).
  • the present development proposes another alternative in the design of nutrient controlled release systems, particularly in hydrogels manufactured from cellulosic residues that can be disposed in soils, which is presented as an environmental solution against loss. of nutrients, as well as an innovation in the agricultural sector and in the development of new materials.
  • the present invention relates to a controlled release hydrogel, manufactured from cellulosic waste, and its manufacturing process.
  • the controlled release hydrogel comprises a crosslinker, cellulose, a hydrogel-forming polymer and a composition, wherein the composition is nutritious or biocide.
  • the manufacturing process comprises mixing a polymer in water with cellulose, mixing a crosslinking solution and an active composition, and finally mixing the solution of step (b) with the mixture step (a) under constant stirring until a hydrogel is formed. Form and dry the product obtained.
  • FIG. 1 Behavior of the degradation of the hydrogel over time, with different amounts of residual cellulose.
  • FIG. 2 Comparison between controlled release fertilizer and a commercial fertilizer, regarding the release of nitrogen in soil. Detailed description of the invention
  • the process for the manufacture of a controlled release hydrogel of the present invention comprises: a) mixing a polymer in water with cellulose; b) mixing a crosslinking solution and an active composition;
  • step (b) mixing the solution of step (b) with the mixture step (a) under constant stirring, until a hydrogel is formed; d) form and dry the controlled release hydrogel.
  • the controlled release hydrogel and its manufacturing process involve the following materials: polymer, water, cellulose, crosslinker and an active composition.
  • active composition can refer to a composition that can be nutritious, biocide, pesticide or an organic pesticide (of botanical origin), depending on the production requirement. By active composition it can also refer to a nutritional element, nutritional compound, nutritional composition, biocide, etc.
  • a) Mix a polymer in water with cellulose (Prepared 1)
  • the polymer mixture is formed from a hydrogel-forming polymer that dissolves in water in a proportion between 5 and 10%, under a temperature between 30 and 80 ° C and stirring 100 and 300 rpm or what is necessary until dilution. complete.
  • the present invention comprises a hydrogel-forming polymer that is selected from the group of polyvinyl alcohol (PVA), cellulose, residual cellulose, lignin, chitosan, xanthan gum, carboxymethyl cellulose, polylactic acid, acrylic acid, acrylamide, sodium alginate, alginate calcium, hydroxymethyl cellulose, carrageenan and possible combinations of the above.
  • PVA polyvinyl alcohol
  • cellulose residual cellulose
  • lignin lignin
  • chitosan chitosan
  • xanthan gum carboxymethyl cellulose
  • polylactic acid acrylic acid
  • acrylamide sodium alginate
  • alginate calcium hydroxymethyl cellulose
  • carrageenan carrageenan
  • cellulose is added in a proportion of between 5 and 20%.
  • Cellulose may or may not involve pretreatment; In one modality it is residual, so that it can be obtained from organic waste rich in this biopolymer, which can come from both the agribusiness sector (for example banana and banana, cotton, sugar cane, coconut and rice among others) , as of the industrial sector or others known by a moderately versed person.
  • a sludge containing more than 60% residual cellulose and the remaining percentage composed of carbonated and siliceous materials are used. The sludge is dried at room temperature until it reaches approximately 30% humidity, is ground and sieved.
  • an active composition is optionally added which can be a nutrient (source of nitrogen, potassium, calcium, magnesium, iron or manganese) or a biocide (fungicide, herbicide, bactericide, insecticide, acaricide, among others) or possible combinations of the previous ones, in a proportion between 0.5 and 30%. It is mixed under stirring between 100 and 300 rpm at room temperature or until properly mixed with the polymer solution in water with cellulose. b) Mix a crosslinking solution and an active composition (Prepared 2)
  • the crosslinking solution is obtained from a crosslinking substance that dissolves in water.
  • crosslinking is meant a compound that forms bridges between polymeric molecules, converting thermoplastic polymers into thermosetting.
  • the crosslinker of the present invention should be at least one, which is selected from the group of sodium tetraborate, carboxymethyl cellulose (CMC), phosphates, hydroxymethyl cellulose and possible combinations of the foregoing. It dissolves in a proportion between approximately 1 and 15%, between 30 and 50 ° C and constant agitation between 100 and 300 rpm or until its complete dilution.
  • an active composition is added.
  • the active composition can be nutritious, pesticide, herbicide, fungicide, among others.
  • the pesticides are organic pesticides of botanical origin such as nicotine, terpenes, azaridactin, caffeine, eucalyptol, saponins and sapogenins.
  • the active composition is nutritious and is composed of an anionic nutrient that is added in a proportion between 0.5 and 23% in constant agitation between 100 and 300 rpm or until a homogeneous paste is formed and even moisture loss between 30 - 60% c) Mix the solution of step (b) with the mixture step (a) under constant stirring until a hydrogel forms
  • the mixture obtained in step (b) is added on the mixture of the water-soluble hydrogel-forming polymer with residual cellulose obtained in step (a), under stirring between 100 and 200 rpm for about 2 and 10 minutes or until the crosslinkable moldable hydrogel forms. d) form and dry the controlled release hydrogel.
  • modules are prepared comprising combinations of the preparations (1 and 2), depending on the nutritional requirement.
  • a module is understood as a single element consisting of several layers, each of which is a hydrogel formed with a specific composition or substance required (nutrient or biocide). Thus they can be formed: tablets, encapsulated, granulated, powders from a single preparation, or with combinations of both in multilayer tablets that meet the specific requirements.
  • the step of step (b) can be carried out before that of step (a).
  • a controlled release hydrogel of a composition obtained by the above process comprising at least one crosslinker, residual cellulose, hydrogel-forming polymer and a nutrient or biocide composition.
  • Borax 0.5 g was dissolved in 8 mL of water and brought to a temperature of 60 ° C for 3 minutes with stirring of 90 rpm.
  • the Borax solution is added to the homogeneous potassium phosphate paste and CMC, under stirring of 200 rpm for 2 minutes or until the crosslinkable moldable hydrogel is formed.
  • the mixture is placed on a flat surface and a 5 mm thick sheet is formed, from which, before losing moisture, it is stamped to remove tablets of 9.5 mm in diameter and approximately 5 mm thick.
  • a tablet of preparation 1 was taken and placed in the middle of two tablets of preparation 2 to form a three-layer controlled release element.
  • the hydrogel formed under the preparation 2 of Example 1 was subjected to a water degradation test, for which square samples of lxl cm of the hydrogel were taken, dried at room temperature for 48 hours and its initial weight recorded, subsequently deposited in 15 mL containers of unsterilized water with pH 6.8 contained in containers with a lid. At 5, 10, 15, 20, 25 and 30 days the samples were removed, dried for 24 hours at room temperature and their degradation percentage was determined.
  • FIG. 1 the degradation behavior of the material is presented with the minimum (0, lg) and the maximum (3.5 g) residual cellulose content (CR), for a total amount of hydrogel of 30 g, finding that the maximum amount of CR that the device can contain without losing its properties with a minimum of degradation in a period of 30 days is 3.5 g.
  • Example 3 Encapsulation for controlled release of aqueous tobacco extracts with repellent and insecticidal activity
  • Borax 0.5 g was dissolved in 8 mL of water and brought to a temperature of 60 ° C for 3 minutes with stirring of 90 rpm.
  • the Borax solution is added to the homogeneous paste of PVA and Residual Cellulose, under stirring of 200 rpm for 2 minutes or until the crosslinkable moldable hydrogel is formed; a 5 mm thick sheet is formed, from which, before losing moisture, it is punched out to remove tablets of 9.5 mm diameter and approximately 5 mm thick.
  • Borax 0.5 g was dissolved in 5.5 mL of water and brought to a temperature of 60 ° C for 3 minutes with stirring of 90 rpm.
  • the Borax solution is added to the homogeneous paste of PVA and Residual Cellulose, under agitation of 350 rpm for 2 minutes or until the crosslinkable moldable hydrogel is formed; a 5 mm thick sheet is formed, from which, before losing 100% moisture, it is cut to take out tablets of 9.5 mm diameter and approximately 5 mm thick.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Fertilizers (AREA)

Abstract

La présente invention concerne un hydrogel à libération contrôlée et son procédé de fabrication, en particulier un hydrogel à libération contrôlée comprenant un agent réticulant, de la cellulose, un polymère précurseur d'hydrogel et une composition active, ladite composition pouvant être nutritive ou biocide. Le procédé de fabrication comprend (a) le mélange d'un polymère en solution aqueuse avec de la cellulose, (b) le mélange d'une solution réticulante et d'une composition et, pour finir, le mélange de la solution obtenue à l'étape (b) au mélange obtenu à l'étape (a) sous agitation constante jusqu'à formation d'un hydrogel. L'hydrogel obtenu est ensuite formé et séché.
PCT/IB2017/058152 2016-12-26 2017-12-19 Engrais à libération contrôlée et son procédé de fabrication Ceased WO2018122682A1 (fr)

Applications Claiming Priority (2)

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CONC2016/0005753 2016-12-26
CONC2016/0005753A CO2016005753A1 (es) 2016-12-26 2016-12-26 Fertilizante de liberación controlada y proceso de fabricación

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WO2018122682A1 true WO2018122682A1 (fr) 2018-07-05

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109517205A (zh) * 2018-09-29 2019-03-26 华南农业大学 一种双网络木质素水凝胶及其制备方法与应用
CN109988343A (zh) * 2019-03-18 2019-07-09 浙江大学 一种具有形状记忆功能的碱溶壳聚糖-海藻酸钠水凝胶材料及其制备方法
CN110117371A (zh) * 2019-05-23 2019-08-13 梧州渺渺科技有限公司 凝胶材料及其制备方法、可塑型制品和应用
CN110183689A (zh) * 2019-06-04 2019-08-30 重庆工商大学 一种接枝插层制备功能型木质素基水凝胶的方法
CN113603528A (zh) * 2021-08-05 2021-11-05 四川大学 一种利用制革牛毛制备角蛋白基水凝胶缓释肥料的方法

Citations (1)

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WO2016041997A1 (fr) * 2014-09-15 2016-03-24 Novioponics B.V. Composition comprenant un hydrogel et des pesticides

Patent Citations (1)

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WO2016041997A1 (fr) * 2014-09-15 2016-03-24 Novioponics B.V. Composition comprenant un hydrogel et des pesticides

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ABED M.A. ET AL.: "Preparation and evaluation of new hydrogels as new fertilizer delivery system", BASRAH JOURNAL OF SCIENCE, vol. 24, no. 1, 2006, pages 103 - 114, XP055512678, ISSN: 1814-0343 *
ALVAREZ-LORENZO C. ET AL.: "Crosslinked ionic polysaccahrides for stimuli-sensitive drug delivery", ADVANCE DRUG DELIVERY REVIEWS, vol. 65, no. 9, 2013, pages 1121 - 1282, XP028720010, ISSN: 0169-409X *
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109517205A (zh) * 2018-09-29 2019-03-26 华南农业大学 一种双网络木质素水凝胶及其制备方法与应用
CN109988343A (zh) * 2019-03-18 2019-07-09 浙江大学 一种具有形状记忆功能的碱溶壳聚糖-海藻酸钠水凝胶材料及其制备方法
CN109988343B (zh) * 2019-03-18 2020-11-13 浙江大学 一种具有形状记忆功能的碱溶壳聚糖-海藻酸钠水凝胶材料及其制备方法
CN110117371A (zh) * 2019-05-23 2019-08-13 梧州渺渺科技有限公司 凝胶材料及其制备方法、可塑型制品和应用
CN110117371B (zh) * 2019-05-23 2022-05-03 梧州渺渺科技有限公司 凝胶材料及其制备方法、可塑型制品和应用
CN110183689A (zh) * 2019-06-04 2019-08-30 重庆工商大学 一种接枝插层制备功能型木质素基水凝胶的方法
CN110183689B (zh) * 2019-06-04 2022-06-21 重庆工商大学 一种接枝插层制备功能型木质素基水凝胶的方法
CN113603528A (zh) * 2021-08-05 2021-11-05 四川大学 一种利用制革牛毛制备角蛋白基水凝胶缓释肥料的方法

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