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WO2010010569A1 - Procédé de formation d’une composition de cendres de téguments de riz - Google Patents

Procédé de formation d’une composition de cendres de téguments de riz Download PDF

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Publication number
WO2010010569A1
WO2010010569A1 PCT/IN2008/000811 IN2008000811W WO2010010569A1 WO 2010010569 A1 WO2010010569 A1 WO 2010010569A1 IN 2008000811 W IN2008000811 W IN 2008000811W WO 2010010569 A1 WO2010010569 A1 WO 2010010569A1
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WO
WIPO (PCT)
Prior art keywords
rice husk
silver
husk ash
nanoparticles
silver nanoparticles
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/IN2008/000811
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English (en)
Inventor
Debabrata Rautaray
Murali Sastry
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Tata Chemicals Ltd
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Tata Chemicals Ltd
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Filing date
Publication date
Application filed by Tata Chemicals Ltd filed Critical Tata Chemicals Ltd
Priority to AP2011005588A priority Critical patent/AP2011005588A0/xx
Publication of WO2010010569A1 publication Critical patent/WO2010010569A1/fr
Anticipated expiration legal-status Critical
Priority to ZA2011/01305A priority patent/ZA201101305B/en
Ceased legal-status Critical Current

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Classifications

    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3291—Characterised by the shape of the carrier, the coating or the obtained coated product
    • B01J20/3295—Coatings made of particles, nanoparticles, fibers, nanofibers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes

Definitions

  • the invention relates to a process for binding metal nanoparticles to rice husk ash. More particularly the invention relates to a process for binding silver nanoparticles to rice husk ash. DESCRIPTION OF RELATED ART
  • Clean potable water is a basic human requirement. However, a large portion of the world's population, especially those living in developing countries do not have access to clean potable water.
  • Rice husk ash has been used as a water purifier but the results obtained are not consistent over time, the rice husk ash is not able to remove all bacteria, and the filter devices required for adequate filtration tend to be bulky. Moreover as the rice husk ash has a potential to trap water born bacteria due to the small size of its pores, trapped bacteria may survive on the rice husk ash and may even seep into the water that is filtered through the rice husk ash. In order to use rice husk ash as an effective water filtration medium, there is a need for a process that would impart antimicrobial properties to rice husk ash, so that the rice husk ash is also able to destroy microbes that are present in water. There is also a need for a water purification composition that is inexpensive, easy to use and effective in removing bacterial contamination from drinking water.
  • the invention relates to a process comprising binding silver nanoparticles to rice husk ash.
  • Silver nanoparticles are synthesized by the reduction of silver precursor using a reducing agent in the presence of a stabilizing agent. Thereafter, rice husk ash is soaked in the as synthesized silver nanoparticles solution for suitable time to obtain rice husk ash bonded to silver nanoparticles.
  • Fig 1(A) Transmission electron micrograph of silver nanoparticles synthesized using chitosan as a stabilizing agent and ascorbic acid as a reducing agent.
  • Fig 1 (B) Selected area electron diffraction pattern of silver nanoparticles synthesized using chitosan as a stabilizing agent and ascorbic acid as a reducing agent.
  • Fig l(C) UV- Vis spectra of silver nanoparticles synthesized using chitosan as a stabilizing agent and ascorbic acid as a reducing agent.
  • Rice husk is a perennially renewable agro-waste available at virtually no cost wherever rice paddy is grown.
  • the rice husk ash residue contains 85-95% silica, 4-12% carbon and the rest comprises of various metal oxides such as alkali, alkali earth metal and ion oxides.
  • the BET Brunauer Emmett Teller
  • surface area of rice husk ash can be as high as 80-100 square meters per gram, depending on the conditions employed for the combustion of rice husk. Its high surface area and porosity make rice husk ash an effective filtration medium that removes particulate matter as well as color and odor from water.
  • the rice husk ash used for the process may be any rice husk ash that is produced by burning rice husk.
  • the rice husk may be produced by burning rice husk in heaps, in a step grate furnace, fluidized bed furnace or tube-in-basket (TiB) burner.
  • the rice husk ash may also be obtained from boilers and brick kiln, provided it is free of uriburned husk and wood tar, grit, stone, and fused lumps of silica.
  • the rice husk ash should have high silica content.
  • the rice husk ash should have silica content of 60 to 90%.
  • Silver is a safe and effective antimicrobial agent that is lethal to single cell microorganism but is harmless to human cells.
  • Silver's antimicrobial property stems from its extremely slow release of silver ions. These silver ions bind to the cellular components of microorganisms, disrupting the normal reproduction and growth cycle resulting in the death of the microbial cell. When made into particles only a few nanometers in size silver releases a lot more ions and therefore becomes an even stronger antimicrobial agent.
  • elemental silver (Ag 0 ) is not deactivated by chloride or organic matter that may be present in water. These qualities make nano silver a suitable anti microbial agent that may be bound to rice husk ash to impart antimicrobial properties to the rice husk ash.
  • a process for binding silver nanoparticles to rice husk ash is described.
  • the process effectively binds silver nanoparticles to rice husk ash such that minimum leaching of silver occurs when water is passed through the rice husk ash.
  • the rice husk ash with bonded silver nanoparticles is a useful composition for water purification and the bactericidal qualities of rice husk ash and silver work together in making the composition very effective.
  • the process involves preparing silver nanoparticles in the presence of a stabilising agent and adding to the rice husk ash the silver nanoparticles to obtain rice husk ash with bonded silver nanoparticles.
  • the process involves the preparation of silver nanoparticles in the presence of a stabilising agent.
  • the silver nanoparticles may be prepared in the presence of a stabilising agent by any known method.
  • the stabilizing agent prevents the aggregation of nanoparticles during their formation by capping the silver nanoparticles that are formed.
  • the stabilizing agent also facilitates in binding of silver nanoparticles to rice husk ash due to associated charge.
  • the silver nanoparticles formed are then added to rice husk ash to obtain rice husk ash with bonded silver nanoparticles.
  • the silver nanoparticles are prepared in an aqueous medium.
  • the silver nanoparticles are prepared in the presence of a stabilizing agent and stored to avoid aggregation of the prepared nanoparticles.
  • the rice husk ash is added to the solution of capped silver nanoparticles to obtain rice husk ash with bonded nanoparticles.
  • the rice husk ash is soaked with the silver nanoparticles for a predetermined period of time.
  • the rice husk ash is soaked with the silver nanoparticles for a period ranging from 10 minutes to 24 hours and preferably for a period of 12 hours.
  • the rice husk ash to which silver nanoparticles are bonded is separated and washed with water.
  • the rice husk ash with bound silver nanoparticles may be separated by any means including but not limited to filtration or centrifugation, and preferably filtration.
  • the separated rice husk ash to which nano silver is bonded is washed with copious amount of water and the water used for washing the rice husk ash with bound nano silver may be removed by any method including but not limited to filtration or vacuum filtration, preferably filtration.
  • the rice husk ash to which silver nanoparticles are bound is dried by any method including but not limited to air drying or drying in a vacuum oven.
  • the amount of silver nanoparticles should be at least 0.001% by weight for bonding with the rice husk ash.
  • the size of silver nanoparticles used are in the range of 5 nm to 100 nm.
  • the process comprises, preparing silver nanoparticles comprising adding to a silver precursor a stabilizing agent and reducing the silver precursor to obtain silver nanoparticles, and adding the silver nanoparticles to rice husk ash to obtain rice husk ash with bonded silver nanoparticles.
  • the process comprises, preparing silver nanoparticles by adding to a solution of silver nitrate, a solution of chitosan to obtain a silver nitrate chitosan solution and reducing the silver nitrate by adding tri-sodium citrate dihydrate to obtain capped silver nanoparticles; and adding to the rice husk ash the silver nanoparticles to obtain a rice husk ash bonded with silver nanoparticles.
  • the silver nitrate chitosan solution is heated to a boiling temperature while stirring.
  • the solution of tri-sodium citrate is added to the boiling silver nitrate chitosan solution.
  • the solution of tri-sodium citrate is not added as a dumping action but is added slowly.
  • the silver nitrate chitosan solution is boiled further after the addition of the reducing agent. Boiling assists in reducing the silver nitrate to silver nanoparticles.
  • the process comprises preparing silver nanoparticles by forming a silver precursor solution, mixing a stabilising agent with a reducing agent and adding the stabilising agent and reducing agent solution to the silver precursor solution to obtain a solution of capped silver nanoparticles; and adding to rice husk ash the silver nanoparticle solution to obtain rice husk ash with bonded silver nanoparticles.
  • the process comprises, preparing silver nanoparticles by adding to a solution of ascorbic acid a solution of chitosan to obtain an ascorbic acid-chitosan solution and adding the ascorbic acid chitosan solution a silver nitrate solution to obtain capped silver nanoparticles; and adding to the rice husk ash the silver nanoparticles to obtain a rice husk ash bonded with silver nanoparticles.
  • the silver nanoparticles obtained by this process are triangular in shape.
  • FIG. 1(A) shows a transmission electron micrograph of silver nanoparticles synthesized using chitosan as a stabilizing agent and ascorbic acid as a reducing agent.
  • Figure 1(B) shows a selected area electron diffraction pattern of silver nanoparticles synthesized using chitosan as a stabilizing agent and ascorbic acid as a reducing agent.
  • Figure l(C) shows UV- Vis spectra of silver nanoparticles synthesized using chitosan as a stabilizing agent and ascorbic acid as a reducing agent.
  • the silver precursor may be any base metal salts including but not limited to AgNO 3 , AgBF 4 , AgPF 6 , Ag 2 O, CH 3 COOAg 5 AgCF 3 SO 3 , AgClO 4 , AgCl, Ag 2 SO 4 ,.
  • the silver precursor is silver nitrate (AgNO 3 ).
  • the concentration of silver salt may range between 0.001M and IM.
  • the stabilising agent includes but is not limited to chitosan, tri-sodium citrate dihydrate, L-lysine, tyrosine, sodium bis(2-ethylhexyl) sulfosuccinate, sodium dodecyl sulphate, cetyl trimethyl ammonium bromide, polyvinyl pyrrolidone, polyvinyl alcohol or oleylamine used alone or in combination with one another, hi accordance with an embodiment the stabilizing agent is chitosan.
  • chitosan is dissolved in 5% citric acid. The citric acid is required to dissolve the chitosan and it also helps in maintaining mild acidic conditions during reduction.
  • the reducing agent used may be any reducing agent that is capable of converting Ag + ions to Ag 0 including but not limited to tri-sodium citrate, ascorbic acid, sodium borohydride, hydrazine hydrate, tyrosine or D-Glucose and preferably the reducing agent is tri-sodium citrate dihydrate.
  • the amount of reducing agents ranges from 0.1 to 10 wt % and preferably the amount of reducing agent is 2 wt %. hi accordance with an aspect the nanoparticles obtained by this process are of spherical or triangular or flat structure.
  • the process comprises, preparing silver nanoparticles by adding to a solution of silver nitrate, a solution of sodium bis(2-ethylhexyl) sulfosuccinate (AOT) to obtain a silver nitrate AOT solution and reducing the silver nitrate by adding sodium borohydride to obtain capped silver nanoparticles; and adding to the rice husk ash the silver nanoparticles to obtain rice husk ash bonded with silver nanoparticles.
  • transmission electron microscopy selected area electron diffraction and UV- Visible spectroscopy of silver nanoparticles was carried out.
  • Figure 2 shows the UV- Vis spectra of silver nanoparticles synthesized using sodium bis(2-ethylhexyl) sulfosuccinate as a stabilizing agent and sodium borohydride as a reducing agent.
  • the silver nanoparticles are prepared in an aqueous medium by dissolving a surfactant in ethanol or an ethanol- water mixture to obtain a first solution, adding the first solution to a solution of a silver precursor in water and reducing the solution so obtained by adding a reducing agent in a predetermined manner to form silver nanoparticles.
  • the surfactant in this process stabilizes the silver nanoparticles by preventing their aggregation in the aqueous medium.
  • Rice husk ash is then added to the silver nanoparticle solution to obtain rice husk ash with bound silver nanoparticles.
  • silver nanoparticles are prepared by mixing an aqueous silver sulfate solution with aqueous solution of tyrosine to obtain a silver sulfate tyrosine solution, adding to the silver sulfate tyrosine solution a solution of KOH and boiling the said solution to form silver nanoparticles.
  • Silver nanoparticles obtained by this method are highly stable by the capping nature of tyrosine molecules on the nanoparticle surface ⁇ preventing any aggregation.
  • Rice husk ash is then added to the silver nanoparticle solution to obtain rice husk ash with bound silver nanoparticles.
  • the process as described may also be used to bind other metal nanoparticles to rice husk ash.
  • the process comprises of preparing metal nanoparticles in the presence of a stabilising agent and adding to the rice husk ash the metal nanoparticles to obtain rice husk ash with bonded metal nanoparticles.
  • the metal nanoparticles may be nanoparticles of any metal including copper, zinc, magnesium, titanium or alloys.
  • the metal nanoparticle is a bactericidal agent.
  • the rice husk ash with bonded silver nanoparticles obtained by this process may be used as a composition for removal of bacterial content from water in a water purification system.
  • Example 1 The following examples are provided to explain and illustrate certain preferred embodiments of the process of the invention.
  • 0.008 M silver nitrate (AgNO3) and 1% Chitosan [dissolved in 5% citric acid (C 6 H 8 O 7 )] aqueous solutions are prepared.
  • 14 ml of (1%) chitosan solution is added to 1386 ml of AgNC ⁇ solution and stirred for 5mins.
  • the silver nitrate- chitosan solution is heated up to boiling temperature while stirring.
  • 56 ml of 5% sodium citrate solution is added slowly to the above solution while stirring. The boiling is continued for another 15 mins after addition of sodium citrate solution.
  • 0.008 M silver nitrate (AgNO3) and 0.001 M sodium bis(2-ethylhexyl) sulfosuccinate (AOT; C20H37NaO7S) aqueous solutions are prepared.
  • 0.001 M AOT is dissolved in 1400 ml of distilled water by stirring for 15 minutes.
  • 1.9357 g Of AgNO 3 is added to the above solution and stirred for uniform mixing.
  • 51.2 ml of freshly prepared 0.01 M sodium borohydride (NaBH4) solution is added slowly to the above mixture while stirring.
  • the reduction of Ag + ions to Ag 0 occurs during the reaction of silver nitrate with sodium borohydride in the presence of AOT as a stabilizing agent.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L’invention concerne un procédé qui comprend la préparation de nanoparticules d’argent en présence d’un agent stabilisateur et l’ajout des nanoparticules d’argent à des cendres de téguments de riz pour obtenir des cendres de téguments de riz avec des nanoparticules d’argent liées.
PCT/IN2008/000811 2008-07-24 2008-12-05 Procédé de formation d’une composition de cendres de téguments de riz Ceased WO2010010569A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AP2011005588A AP2011005588A0 (en) 2008-07-24 2008-12-05 A process for forming a rice husk ash composition.
ZA2011/01305A ZA201101305B (en) 2008-07-24 2011-02-18 A process for forming a rice husk ash composition

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN1571MU2008 2008-07-24
IN1571/MUM/2008 2008-07-24

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WO2010010569A1 true WO2010010569A1 (fr) 2010-01-28

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AP (1) AP2011005588A0 (fr)
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ZA (1) ZA201101305B (fr)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012073252A1 (fr) * 2010-11-29 2012-06-07 Tata Chemicals Limited Compositions antimicrobiennes à base de cendre d'écorce de riz
WO2012095863A3 (fr) * 2011-01-11 2012-11-29 Tata Chemicals Limited Procédé de préparation de nouvelles nanoparticules de platine et nanoparticules de platine
WO2013046213A3 (fr) * 2011-07-28 2013-05-23 Tata Consultancy Services Limited Dispositif de purification de l'eau
WO2014188443A3 (fr) * 2013-04-12 2015-01-29 Tata Chemicals Limited Composition de purification d'eau
US9233863B2 (en) 2011-04-13 2016-01-12 Molycorp Minerals, Llc Rare earth removal of hydrated and hydroxyl species
WO2016005928A1 (fr) * 2014-07-09 2016-01-14 Tata Chemicals Limited Composition de purification d'eau
US9975787B2 (en) 2014-03-07 2018-05-22 Secure Natural Resources Llc Removal of arsenic from aqueous streams with cerium (IV) oxide compositions
US10081060B2 (en) 2016-03-09 2018-09-25 King Abdulaziz University Method of forming silver nanoparticles and a use thereof
CN111348793A (zh) * 2018-12-24 2020-06-30 荆门市格林美新材料有限公司 一种水合肼液相还原银粉废液的处理方法
CN112871142A (zh) * 2021-01-21 2021-06-01 广州市环境保护技术设备有限公司 一种柠檬酸接枝壳聚糖小球的制备方法和应用
CN115109560A (zh) * 2022-08-09 2022-09-27 东莞市金博奕印刷有限公司 一种具有抑菌效果的无痕硅胶贴

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