WO2021101394A4 - Modified nanostructured silica materials for heavy metal removal from contaminated water and the methods of production thereof - Google Patents

Modified nanostructured silica materials for heavy metal removal from contaminated water and the methods of production thereof Download PDF

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Publication number
WO2021101394A4
WO2021101394A4 PCT/PH2020/050015 PH2020050015W WO2021101394A4 WO 2021101394 A4 WO2021101394 A4 WO 2021101394A4 PH 2020050015 W PH2020050015 W PH 2020050015W WO 2021101394 A4 WO2021101394 A4 WO 2021101394A4
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WO
WIPO (PCT)
Prior art keywords
beads
cancelled
nanostructured
iron
filter
Prior art date
Application number
PCT/PH2020/050015
Other languages
French (fr)
Other versions
WO2021101394A2 (en
WO2021101394A3 (en
Inventor
Milagros PERALTA
Maritess MAGALONA
Ericson ESCOBEDO
Original Assignee
University Of The Philippines Los Baños
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Filing date
Publication date
Application filed by University Of The Philippines Los Baños filed Critical University Of The Philippines Los Baños
Publication of WO2021101394A2 publication Critical patent/WO2021101394A2/en
Publication of WO2021101394A3 publication Critical patent/WO2021101394A3/en
Publication of WO2021101394A4 publication Critical patent/WO2021101394A4/en

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Classifications

    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
    • 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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
    • 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
    • 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
    • B01J2220/42—Materials comprising a mixture of inorganic materials

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

This invention discloses the methods of preparing Iron-modified nanostructured silica beads and iron-modified nanosilica powder. The resulting composition is used as heavy metal adsorbents in the removal of arsenic from contaminated water. These materials allow the remediation of arsenic contaminated groundwater using low-cost, locally available, and sustainable nanomaterials.

Claims

AMENDED CLAIMS received by the International Bureau on 26 July 2021 (26.07.2021)
[Claim 1] [Amended] Nano structured filter beads and nano structured filter powder comprising of a nanosilica component with block copoly merization characteristics uniformly modified and incorporated with iron as ferric sulfate or ferric chloride, wherein: the nano structured filter beads have a particle size of 8.0 nm, pore radius of 17.0 angstroms, surface area of 349 m2/g, dry bulk density of 0.78-0.81 g/cm3, hardness of 1.02-1.71 kg/g; and the nano structured filter powder has a particle size of 36.0 nm, pore radius of 91.0 angstroms, and surface area of 110 m2/g.
[Claim 2] [Cancelled]
[Claim 3] [Cancelled]
[Claim 4] [Unchanged] A method of preparing nanostructured powder according to Claim 1 comprising the steps of: a. dissolving the nanosilica in 2.5 N NaOH at a ratio of 1:4 (wt. of nanosilica: vol. of base to obtain the silica sol); b. filtering the silica sol to remove the undissolved particles; c. dissolving the iron source (ferric sulfate or ferric chloride) in 2.5 N NaOH; d. filtering the excess iron using a funnel; e. adding the purified nanosilica to the alkaline solution of the iron salt; f. stirring the sol for ten hours; g. titrating the sol with 5 N H2S04 to reduce the pH to 7.5-8.5; h. washing the residue with deionized water; i. air-drying the residue; and j. oven drying the residue at 120-150 °C for three to twelve hours.
[Claim 5] [Unchanged] A method of preparing nanostructured beads according to Claim 1 comprising the steps of: a. dissolving the nanosilica powder in 2.5 N NaOH solution; b. titrating the resulting sodium silicate to glacial acetic acid with stirring until pH 3.5-4.0; c. adding the iron source to the solution and aging the resulting solution for 2-4 hours until a viscosity of 2750 to 3250 cP is achieved; d. dropping the solution of iron modified silica sol slowly to form beads in a column containing ammonium hydroxide with surfactant as the aqueous layer and hexane as the organic layer; e. aging the beads in ammonium hydroxide for at least two hours; f. collecting the iron modified silica beads; g. washing the iron modified silica beads; h. washing the beads with deionized water while undergoing sonication at 50-60 Hz, then with acetone or isopropyl alcohol; i. air-drying the beads; and j. oven-drying the beads at 150-200 °C for three to six hours.
[Claim 6] [Cancelled]
[Claim 7] [Cancelled]
[Claim 8] [Cancelled]
[Claim 9] [Cancelled]
[Claim 10] [Cancelled]
[Claim 11] [Cancelled]
[Claim 12] [Amended] The nanostructured filter powder according to Claim 1, wherein the allowed flow rate is 9.0 mL/min and the adsorption capacity is 0.99-1.02 mg As(III)/g adsorbent.
[Claim 13] [Amended] The nanostructured filter beads according to Claim 1 wherein the allowed flow rate is 600 mL/min and the adsorption capacity is 0.82-0.96 mg As(III)/g adsorbent.
[Claim 14] [Cancelled] [Claim 15] [Cancelled]

STATEMENT UNDER ARTICLE 19 (1)

The amendments made in the new Claim 1 specifically indicates that the nanostructured filter beads and nanostructured filter powder comprise of a nanosilica component which has block copolymerization characteristics. The nanosilica component is uniformly modified and incorporated with iron as ferric sulfate or ferric chloride. These nanostructured filter beads and nanostructured filter powder have specific properties such as pore radius, surface area, and particle size which altogether contribute to its adsorption technical effect. Moreover, the hardness and bulk density of nanostructured filter beads also contribute to the adsorption technical effect.

The amended Claims 4 and 5 now indicate the allowable flow rates of the nanostructured filter powder and nanostructured filter beads. The prescribed flow rates contribute to the adsorption technical effect.

The combined composition, properties, process of production, and flow rates of the nanostructured filter beads and nanostructured filter powder are significant in achieving the adsorption properties of the present invention.

PCT/PH2020/050015 2019-11-20 2020-11-20 Modified nanostructured silica materials for heavy metal removal from contaminated water and the methods of production thereof WO2021101394A2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PH12019050291 2019-11-20
PH12019050291A PH12019050291A1 (en) 2019-11-20 2019-11-20 Modified Nanostructured Silica Materials for Heavy Metal Removal from Contaminated Water and the Methods of Production Thereof

Publications (3)

Publication Number Publication Date
WO2021101394A2 WO2021101394A2 (en) 2021-05-27
WO2021101394A3 WO2021101394A3 (en) 2021-07-01
WO2021101394A4 true WO2021101394A4 (en) 2021-09-23

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PCT/PH2020/050015 WO2021101394A2 (en) 2019-11-20 2020-11-20 Modified nanostructured silica materials for heavy metal removal from contaminated water and the methods of production thereof

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PH (1) PH12019050291A1 (en)
WO (1) WO2021101394A2 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114632426A (en) * 2022-02-24 2022-06-17 清华大学 Copper monatomic supported film and preparation method and application thereof

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100406851B1 (en) * 2001-08-21 2003-11-21 이종협 Production Method of Mesoporous Silica comprising Magnetite used for Heavy Metal Ion Adsorbents
US20080108497A1 (en) * 2006-11-08 2008-05-08 Holland Brian T Metal-rich siliceous compositions and methods of producing same
CN103464094B (en) * 2013-09-12 2016-01-20 同济大学 A kind of preparation method of Nanoscale Iron modified zeolite
CN104941574B (en) * 2015-06-02 2018-04-10 南京大学 A kind of inorganic ions modified zeolite composite and its application
WO2019194688A1 (en) * 2018-04-06 2019-10-10 University Of The Philippines Los Baños Methods of preparing modified biopolymer-silica nanocomposite materials for arsenic removal from contaminated water and compositions therefrom

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Publication number Publication date
WO2021101394A2 (en) 2021-05-27
PH12019050291A1 (en) 2021-08-23
WO2021101394A3 (en) 2021-07-01

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