WO2018220462A1 - Composition pour l'adsorption de phosphore et/ou d'azote d'effluents ou de déchets liquides, procédés, produits et utilisations - Google Patents

Composition pour l'adsorption de phosphore et/ou d'azote d'effluents ou de déchets liquides, procédés, produits et utilisations Download PDF

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WO2018220462A1
WO2018220462A1 PCT/IB2018/053426 IB2018053426W WO2018220462A1 WO 2018220462 A1 WO2018220462 A1 WO 2018220462A1 IB 2018053426 W IB2018053426 W IB 2018053426W WO 2018220462 A1 WO2018220462 A1 WO 2018220462A1
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composition
phosphorus
phosphate
effluent
serpentinite
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PCT/IB2018/053426
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English (en)
Portuguese (pt)
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Arthur Gabriel DA SILVA
Natália Gabriela SILVA PINHEIRO
Hamilton P. DA ROCHA JÚNIOR
Raphael CAPRUNI ANDRADE VAZ
Rochel MONTERO LAGO
Fernando Augusto MOREIRA
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Universidade Federal De Minas Gerais - Ufmg
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption

Definitions

  • the present invention is a composition for phosphorus and / or nitrogen adsorption of effluent or liquid waste comprising at least one support material, preferably serpentinite, vermiculite, charcoals (modified by oxidative or non-oxidative treatments) and / or phosphate-rich effluent treatment plant sludge; such support material being impregnated with calcium, zinc, copper, manganese, molybdenum, boron, cobalt and / or nickel; and calcined. It also addresses the use of the composition, the process for preparing the composition, the process for producing soil conditioning and nutrient release additives, phosphorus and / or nitrogen recovery devices and the additives produced.
  • Phosphorus (usually in the form of phosphate) and nitrogen (present in various forms, such as ammonium, nitrate and urea), present in industrial and domestic effluents and waste, are an environmental problem as they cause eutrophication of rivers and lakes when discarded.
  • a phosphorus concentration from 0.03 mg / L is already sufficient to cause cyanobacterial blooms (WANG, R. et al. Flickering gives early warning signals of a critical transition to a eutrophic lake state. Nature, v. 492, No. 7429, pp. 419-422, 12/20/2014 print. ISSN 0028-0836).
  • Nitrogen also contributes to eutrophication, but to a lesser extent, since phosphorus is a limiting element for flowering (ROWE, EC et al. Vegetation Type Affects the Relationship Between Soil Carbon and Nitrogen Leaching. Water, Air, and Soil Pollution, v. 177, no. 1, pp. 335-347, 2006 // 2006. ISSN 1573-2932.).
  • phosphorus and nitrogen are extremely important nutrients for agriculture.
  • Agriculture, the food and detergent industry are the main consumers of phosphorus (COOPER, J. et al., The Future Distribution and Production of Global Phosphate Rock Reserves. Resources, Conservation and Recycling, v. 57, p. 78-86,12,201.
  • Phosphorus and / or nitrogen can be removed from effluents in two ways: biological or physicochemical.
  • biological treatment organisms capable of absorbing nutrients in the form of phosphate / nitrates are used. After absorption, the generated sludge is removed and digested anaerobically, which causes the absorbed compounds to return to the aqueous phase. This nutrient-rich liquid returns to the beginning of treatment.
  • the physicochemical treatment uses iron, aluminum, magnesium or calcium ions to precipitate phosphorus in the form of phosphate, which is removed together with the sludge.
  • struvite ammonium phosphate and magnesium hexahydrate
  • Struvite has a slow nutrient release rate, allowing lower frequency of fertilizer application (LUZ, E .; BASHAN, Y. Recent advances in removing phosphorus from wastewater and its future use as fertilizer (1997 “ 2003). V. 38 , p. 4222 "4246, 2004).
  • Coals, vermiculite and serpentinites are commonly applied as additives for agriculture. Coals are very interesting both for their porous structures and high surface area, as well as their ability to increase soil organic matter content and cation exchange capacity, improving the efficiency of fertilizer use, promoting the development of beneficial microorganisms. plant growth, among other agronomically desirable characteristics (SANTALLA, M. et al. Effectiveness of wood ash containing charcoal as a fertilizer for a forest plantation in a temperate region. Plant and Soil, v. 346, no. 1, p. 63 -78,201 / 201 / 2011. ISSN 1573-5036).
  • SANTALLA M. et al. Effectiveness of wood ash containing charcoal as a fertilizer for a forest plantation in a temperate region. Plant and Soil, v. 346, no. 1, p. 63 -78,201 / 201 / 2011. ISSN 1573-5036).
  • Vermiculite is a mica-like mineral formed by hydration of certain basaltic minerals, with formula (MgFe, AI) 3 (AI, Si) 4O 10 (OH) 2 .4H 2 O. It has expansion capacity, when subjected to temperatures close to 900 ° C its volume may increase from 10 to 30 times. After this process gets the name of expanded vermiculite, where each flake trap air cells, giving the material insulating capacity. This expanded material, in addition to its insulating capabilities, is non-irritating to skin or lung, has low electrical conductivity, does not decompose and does not attract insects. Expanded vermiculite can absorb up to five times its mass in water, is a good lubricant and filter material.
  • vermiculite in agriculture is wide due to its characteristics such as high cation exchange capacity, good water retention, low mass and chemical reactivity, absence of toxicity, thermal insulation and good particle size.
  • it can be used in the production of agricultural substrates, in the cover of seeds and seedlings, as soil conditioner, nutrient and herbicide / insecticide / fungicide container, sandy soil water retainer, grassy field antifreeze agent, manufacturing load.
  • pesticides and hydroponic agriculture WU, N. et al. Organic intercalation of structure modified vermiculite. Journal of Colloid and Interface Science, v. 457, p. 264-271, 11/1/2015. ISSN 0021 -9797
  • Serpentinites comprise a class of ultrabasic magnesian metamorphic rocks composed mainly of calcium, magnesium and silicon oxides.
  • Part of the serpentine mineralogical group are magnesium silicate materials derived from changes in the hydration of olivines, which may be in nature in the form of lizardite, antagonist or chrysotile.
  • Serpentinite composition and arrangement vary from region to region due to metamorphism, which can shift silicate to carbonate phases (PEREIRA, D .; PEINADO, M. Serpentinite. Geology Today, v. 28, no. 4, p. 152- 156, 2012. ISSN 1365-2451).
  • the serpentinite reserves are distributed in the following states: Bahia, Ceará, Goiás, Minas Gerais, Mato Grosso do Sul, Para, Paraiba, Paraná, Rio Grande do Sul, Sergipe and Sao Paulo.
  • rocking or remineralization rock dust is used to correct acidity and replenish soil nutrients.
  • the water acts by slowly leaching nutrients from the rock, thus obtaining a natural soil conditioner with gradual release of nutrients.
  • One of the advantages of this technique is the decrease in the consumption of industrial fertilizers (ANDEF - National Association of Plant Protection. Phytosanitary application technology manual. 2004).
  • a problem with this technique is uncontrolled application, which can lead to nutritional imbalance and / or accumulation of heavy metals in the soil.
  • the sludge produced by the phosphating industry has a very high phosphorus and urea adsorption capacity.
  • immersion phosphating stands out.
  • a residue called phosphate sludge or phosphate sludge is formed, formed from the reaction of Fe 3+ ions (originated by the oxidation of Fe 2+ ions present in solution) with phosphate ion (P0 4 3 ), forming , iron phosphate (FeP0 4 ).
  • Characterization studies by Giffoni & Lange (2005) show that the main constituents of sludge are iron, zinc, nickel and sodium due to the attack on the metal surface and the acid mixture formation of the phosphating tank.
  • Patent document CN102229506 entitled Ivlethod for recovering phosphorus and potassium from effluent and producing slow-release composite fertilizer of phosphorus and potassium, describes a method of recovering urine phosphorus by adding magnesium to precipitate struvite producing a slow release fertilizer. Formation of the desired composite is done by first analyzing the urine composition and then adding magnesium and phosphate salts to maintain some specific proportions of magnesium, potassium and phosphate in solution, following a pH adjustment of the solution. Under such established conditions and constant agitation, the desired salt precipitates as granules.
  • the patent document CN 102167434, titled Ivlethod for recovering nitrogen and phosphorous from urine ⁇ discloses a method of separating sources of sewage and chemical method for treatment of urine recovery of nutrients, particularly nitrogen and phosphorus. Fresh urine is used to further measure the pH. The phosphorus and nitrogen concentration of the solution is adjusted by adding Na 2 HPO 4 and MgCl 2 at the required concentrations. In this process struvite is obtained, with phosphorus and nitrogen recovery of about 95%.
  • This document differs from the present invention in that it does not use the proposed composition.
  • Patent document JP201417739 entitled Hecovery phosphorus ⁇ describes a process of phosphorus recovery in effluents using a material made of a metal oxide capable of adsorbing the phosphorus contained in the solution.
  • the desorption process is done by placing the material in an alkaline solution.
  • a precipitation process is then made by adding calcium to the solution.
  • Patent Document PI 0204877-9 Titled ⁇ Sanitary Granulate used in the treatment and handling of pet waste, and the process of preparing it, utilizes the functioning vermiculite. as a sponge for the retention of animal waste that will later be used directly in agriculture.
  • the present invention proposes a composition for phosphorus and / or nitrogen adsorption of effluents or liquid waste, comprising at least one support material, preferably serpentinite, vermiculite, charcoals (modified by oxidative or non-oxidative treatments) and / or phosphate-rich effluent treatment plant sludge; such support material being impregnated with calcium, zinc, copper, manganese, molybdenum, boron, cobalt and / or nickel; and calcined.
  • This technology also addresses the use of the composition, the process for preparing the composition, the process for producing additives for soil conditioning and nutrient release, phosphorus and / or nitrogen recovery devices, the additives produced and their uses.
  • the proposed composition allows phosphorus and nitrogen adsorption directly from the effluent and can subsequently be used as an agricultural input without the need for any treatment other than decontamination.
  • Figure 1 depicts the phosphate adsorption isotherm using TEE sludge as adsorbent.
  • the present invention is a phosphorus and / or nitrogen adsorption composition of effluent or liquid waste comprising at least one support material, preferably serpentinite, vermiculite, charcoals (modified by oxidative or non-oxidative treatments) and / or phosphate-rich effluent treatment plant sludge; such support material being impregnated with calcium, zinc, copper, manganese, molybdenum, boron, cobalt and / or nickel; and calcined. It also addresses the use of the composition, the process for preparing the composition, the process for producing soil conditioning and nutrient release additives, phosphorus and / or nitrogen recovery devices and the additives produced.
  • the proposed process for preparing the phosphorus and / or nitrogen adsorption composition of effluent or liquid waste comprises the following steps:
  • The. Add the support material to an aqueous solution of 0.5 to 50% (w / w) Ca, Zn, Cu, Mn, Mo, B, Co and / or Ni salts / oxides;
  • the support material should preferably be serpentinite, vermiculite, activated or non-activated charcoals (modified by oxidative treatments or not) and / or phosphate-rich effluent treatment plant sludge.
  • Serpentinite Mg 3 Si 2 0 5 (OH) 4
  • the particle vermiculite is preferably present from 0.3 "0.6 cm and approximate composition of (Al 0. 30 Fe 0 .o4 Ti 0 .63 Mg 2. 0 o) (Si 3. Al 2 i 0. 79) (OK (OH) 2 , Mg 0. 0 i 3 In. 02 K 0. i 0 (H 2 0) n).
  • Activated or non-activated charcoals may undergo oxidative processes for the insertion of acidic groups on their surface by reaction with hot concentrated HN0 3 (80 to 100 ° C) for 5 to 30 minutes.
  • the process for producing soil conditioning additives and nutrient release from effluent and / or liquid waste comprises the following steps:
  • the effluent may be selected from the group comprising industrial effluent and / or domestic effluent free of heavy metals or toxic organic molecules and shall contain phosphate concentrations greater than 10 mg / l or 0.03 ppm.
  • the liquid residues are preferably human or animal urine, free of heavy metals or toxic organic molecules, with phosphate concentrations between 100-1000 mg / l and urea on the order of 1-20 g / l, wherein the adsorbent material may be contained in a wrapper, such as sachets or cases.
  • the decontamination of the adsorbent material can be carried out by using NaCIO, 0 3 , H 2 0 2 , artificial (Hg lamp) or natural (sun) UV light, combined or not.
  • the invention also relates to a device for phosphorus and / or nitrogen adsorption of effluents or liquid waste and production of soil conditioning and nutrient release additives, comprising the phosphorus and / or nitrogen adsorption composition defined in
  • the present invention is contained in a casing, such as sachets or cases, which allows effluent or liquid waste to pass through and retains the composition for reuse.
  • Shells shall have sufficient mechanical and chemical resistance not to degrade and / or rupture when in contact with effluent / liquid waste. Provided that the permeability and resistance characteristics (both chemical and mechanical) are observed, the malleability of the enclosures will depend on their use.
  • the present technology addresses the additive for soil conditioning and nutrient release obtained by the proposed process.
  • the proposed composition may be used for phosphorus and / or nitrogen adsorption for treatment of phosphorus and / or nitrogen rich industrial and / or domestic effluents; or for the production of additives for soil conditioning and nutrient release.
  • the material may also be used as a bed for poultry tailings storage bed.
  • poultry manure comes into contact with the composition of the present invention and the nutrients from such manure are adsorbed / retained on the material, which may later be used as an additive for soil conditioning and nutrient release.
  • the phosphorus and / or nitrogen adsorption composition of effluent and / or liquid waste comprises at least one support material selected from the serpentinite, vermiculite, charcoal and phosphate-rich effluent treatment plant sludge group; the support materials being impregnated with calcium, zinc, copper, manganese, molybdenum, boron, cobalt and / or nickel; and calcined.
  • Equation (1) 3Ca 2+ (aq) + ⁇ 0 4 3 " ⁇ 3 ⁇ ) 3 ⁇ 4 Ca 3 (P0 4 ) 2 (s) .
  • vermiculite For preparation of the composition using vermiculite as a support material, previously expanded commercial vermiculite was used.
  • the vermiculite used had particles between 0.3 " 0.6 cm and approximate composition of (Al 0. 3 o Ti 0. 0 4 Fe 0. 6 3 Mg 2. 00 ) (Si 3. 2 i Al 0. 79 ) (O 10 ( OH) 2 , Mg 0. at 0 i 3. O.10 2 0 (H 2 0) n).
  • impregnations were carried out, whether or not combined, in concentrations ranging from 0.5 to 50% (w / w) Ca, Zn, Cu, Mn, Mo, B, Co and Ni
  • the salts / oxides of the metals were solubilized in water, the vermiculite was added to the suspension and the system was kept under heating and stirring to dryness. After this step, the material was bake for 3 hours at 300 ° C, 500 ° C and 700 ° C. Another procedure used was impregnation without further calcination.
  • Serpentinite rock samples of the general formula Mg 3 Si 2 0 5 (OH) 4 were extracted in a mine and had Mg and Fe contents of 12-17% m / m and 2-3% m / m, respectively. .
  • Serpentinite powder was used, with particle size ranging from 1 to 5 mm.
  • Serpentinite samples were sprayed and retained on 200 mesh sieves.
  • the composition containing the serpentinite as support was prepared in the same manner as with vermiculite. The metal ions were dispersed in water, the serpentinite was added and the system was left under heating and stirring until complete drying.
  • the materials were calcined for 3 hours at temperatures of 300 ° C, 500 ° C and 700 ° C. These materials can be prepared without the impregnation step, with only calcination for three hours at 500 ° C, 700 ° C and 900 ° C for powdered material and calcination at 700 ° C for three hours for material with particle size ranging from 1 to 5 mm.
  • Activated or not activated charcoals are subjected or not to oxidative processes for insertion of acidic groups on their surface by reaction with hot concentrated HN0 3 (80 to 100 ° C) for 5 to 30 minutes.
  • the metal impregnation step Ca 2+ , Zn 2+ , Cu 2+ , Mn x + , Mo 6+ , B + , Co 2+ and ⁇ , are carried out at concentrations between 0.5 " 50% (The activated carbon used in this example was produced from coconut shell and activated using water vapor at 800 ° C, with a surface area between 600-800 m 2 / g and ash content of the order of 5%.
  • the base material was calcined, accompanied by surface calcium impregnation with CaO (lime) or CaCl 2 in aqueous medium. with constant heating and stirring for water evaporation and calcium impregnation on the material surface.
  • ETE automobile effluent treatment plant
  • Equation (2) P0 4 3 " + 12Mo0 4 2" + 27H + "H 3 P0 4 (Mo0 3 ) i 2 + 12H 2 0
  • Equation (3) H 3 P0 4 (Mo0 3) + C 12 H 8 0 6 6 "molybdenum blue
  • compositions for use in chemical toilets and in the form of urinal cases.
  • the sachet and case should allow liquid waste to pass through and prevent solid material from entering. In addition, they must retain the composition and allow its recovery to prepare additives for soil conditioning and nutrient release.
  • Capture assays were performed using a standard mass of 80 mg of the material synthesized in 40 mL of the standard phosphate solution, where the material remains in contact with the solution for about 8 hours, with constant stirring at 100 to 180 rpm. All initial standard solutions had an initial concentration of 300 mg / L, with percentage removals calculated from this concentration.
  • WWTP sludge from metal surface treatment processes may have a high phosphorus content as well as its capture materials due to the metal surface process used in the metallurgical industry, called diphosphating. This consists in creating on the metallic surface, after the removal of impurities, phosphate crystals of the metal, converting it from metallic to non-metallic. As a result, phosphating improves paint adhesion and makes the metal surface up to 700 times stronger.
  • the adsorption isotherm was made by repeating the material mass and volume, 200 mg and 20 mL, respectively, with the gradual increase of phosphorus concentration in the medium. The material was in contact with the solution for about 8 hours to ensure phosphorus adsorption and desorption equilibrium on its surface.
  • Solubility in citric acid simulates nutrient availability when associated with roots with mycorrhizae, ie, in this condition the available phosphorus is absorbed by the plant, obtaining greater use of it, so this feature is extremely favorable for fertilizer production.

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  • Inorganic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
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  • Environmental & Geological Engineering (AREA)
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  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

La présente invention concerne une composition pour l'adsorption de phosphore et/ou d'azote d'effluents ou de déchets liquides, comprenant au moins un matériau de support, de préférence de la serpentinite, de la vermiculite, des charbons végétaux (modifiés par traitements oxydatifs ou non) et/ou des boues de station de traitement d'effluents riches en phosphate, ledit matériau de support étant imprégné de calcium, de zinc, de cuivre, de manganèse, de molybdène, de bore, de cobalt et/ou de nickel, et calciné. L'invention concerne également l'utilisation de cette composition, le procédé de préparation de cette composition, le procédé de production d'additifs pour le conditionnement de sol et la libération nutriments, des dispositifs de récupération de phosphore et/ou d'azote et des additifs produits.
PCT/IB2018/053426 2017-06-01 2018-05-16 Composition pour l'adsorption de phosphore et/ou d'azote d'effluents ou de déchets liquides, procédés, produits et utilisations WO2018220462A1 (fr)

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Publication number Priority date Publication date Assignee Title
CN114832774A (zh) * 2022-04-07 2022-08-02 吉林农业大学 一种从生活污水生物处理系统中回收磷并直接资源化的方法

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