Nanoporous Silica Polyamine Composites with Surface-Bound Zirconium (IV) and Methods of Use

a technology of nanoporous silica and composites, which is applied in the direction of water/sewage treatment by ion exchange, ion exchangers, chemistry apparatus and processes, etc., can solve the problems of large amount of sludge for ultimate disposal, arsenic cannot be recovered, and the arsenic removal process is difficult, etc., to achieve the effect of reducing selectivity and reducing uptake performan

Inactive Publication Date: 2011-09-22
UNIVERSITY OF MONTANA
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Problems solved by technology

The remediation of arsenic from contaminated surface waters is a problem worldwide (Mandal, 2002).
However, all of these technologies have the significant disadvantage of creating a large amount of sludge for ultimate disposal; also the arsenic cannot be recovered and there is the possibility of leakage / leaching of colloidal oxides into the aquifer (Rosengrant, 1990; Manning 1995; Ghosh, 2004; Shaw, 2008; Meng, 2001).
Other methods suffer from a lack of specificity, low selectivity over sulfate (ion exchange), low mass-to-volume concentrations (bio-reduction), and / or high cost (membrane technologies).
Polystyrene resins modified with oxoanion chelating ligands have also shown promise but have yet to be commercialized (Streat, 1986; Fish, 1985).
However, conventional polymeric resins suffer from shrink / swell changes depending on the pH and are not very stable at extreme conditions of pH and temperature (Zagorodni, 2002).
Comparing these polymer modified silica with chelating materials prepared by directly modifying an amino-propyl functionalized silica gel surface, it was found that these materials suffer from degradation in the presence of base, have insufficient mechanical stability, and relatively low capacities due to poor surface coverage.

Method used

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  • Nanoporous Silica Polyamine Composites with Surface-Bound Zirconium (IV) and Methods of Use
  • Nanoporous Silica Polyamine Composites with Surface-Bound Zirconium (IV) and Methods of Use
  • Nanoporous Silica Polyamine Composites with Surface-Bound Zirconium (IV) and Methods of Use

Examples

Experimental program
Comparison scheme
Effect test

example 1

Materials

[0036]Silica gel (267 A° pore diameter, 2.82 mL / g pore volume, 84.7% porosity, 422 m2 / g surface area) was obtained from INEOS enterprises Ltd., UK, and was sieved to 150-250 microns. All chemicals were reagent grade and were purchased from Sigma-Aldrich Co. Stock solutions of Zr(IV), Fe(III), Th(IV), As(III), As(V), Se(IV), and Se(VI) were prepared using zirconyl chloride (ZrOCl2.8H2O), ferric sulfate (Fe2(SO4)3.4H2O), thorium nitrate (Th(NO3)4.xH2O), sodium meta-arsenite (NaAsO2), sodium hydrogen arsenate (Na2HAsO4.7H2O), sodium selenite (Na2SeO3), and sodium selenate (Na2SeO4) respectively. Solution pH was adjusted from the intrinsic pH, where necessary, using hydrochloric acid and sodium hydroxide. Stripping and recovery of arsenic was achieved with 2M—H2SO4. Metal standards for AA and ICP analysis were obtained from Fisher Scientific Co.

[0037]Infrared characterization of modified composites was carried out with a Thermo-nicolet Nexus 670 FT-IR spectrophotometer as KBr p...

example 2

Synthesis of BPAP and BPAPM (FIG. 2a) by the Mannich Reaction (Moedritzer, 1966)

[0040]10 g of BP-1 or BP-1M was mixed with a reagent solution of 30 mL-2N—HCl and 10 g of phosphorus acid (H3PO3) in a 250 mL flask equipped with an overhead stirrer. The flask was heated to 95° C., and 9 mL of formaldehyde (CH2O) solution (37.7%) was gradually added with stirring. The reaction mixture was heated at 95° C. for 24 h. The flask was cooled and the product was filtered. The resulting composite was washed three times with 40 mL of water, once with 40 mL of 1M—NaOH, three times with 40 mL of water, once with 40 mL of 1N—H2SO4, two more times with 40 mL of water, twice with 40 mL of methanol and dried to a constant mass at 65° C. A mass gain of 20 and 22% was obtained starting with BP-1 and BP-1M respectively.

[0041]Elemental Analysis: BPAP made from BP-1: 14.20% C, 3.03% H, 3.36% N, 4.34% P

[0042]BPAP made from BP-1M: 12.08% C, 2.99% H, 2.21% N, 5.56% P

IR spectra (KBr pellet): 2650(m)cm−1(νP—OH)...

example 3

Synthesis of ZrBPAP (FIG. 2b)

[0043]10 g of the BPAP composite was mixed with a reagent solution containing 40 mL of 1N—HCl and 4.24 g of ZrOCl2.8H2O. The reaction mixture was stirred at room temperature for 24 h. After 24 h the product was filtered. The resulting composite was washed two times with 50 mL of water, once with 2N—HCl, two more times with 50 mL water, twice with 50 mL methanol and dried to a constant mass at 65° C. The zirconium loading was determined by analyzing the zirconium feed solution and the final zirconium solutions after all the washes were performed. The analysis of zirconium was done via an ICP / AES method. The zirconium loading on BPAP was found to be 1.12 mmol / g which fits well with a mass gain of 17%. Although, zirconyl chloride forms a tetramer [Zr4(OH)8(H2O)16]8+ in solution, the immobilized zirconium (IV) is thought to bind to the oxygen atom(s) of two phosphonic acid moieties. This is supported by the data obtained from the elemental analysis, ICP / AES,...

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Abstract

Silica polyamine composites (SPC) made from silanized amorphous nano-porous silica gel and poly(allylamine) (BP-1) were functionalized with phosphorus acid using the Mannich reaction, resulting in a phosphonic acid modified composite (BPAP). Zirconium (IV) was immobilized on BPAP. Arsenate anions strongly adsorbed on the ZrBPAP composite in the pH range 2 to 8, while arsenite only adsorbed well at pH 10. Regeneration of the resin was carried out successfully for As(V) and As(III) using 2M-H2SO4. Four adsorption / desorption cycles were performed for As(V) at pH 4 without significant decrease in the uptake performance. ZrBPAP capture capacity and kinetics for arsenate were tested for longevity over 1000 cycles with only a marginal loss of performance.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]This application claims the benefits of U.S. Provisional Application No. 61 / 316,344 filed Mar. 22, 2010, the disclosure of which is hereby incorporated by reference in its entirety including all figures, tables and drawings.STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT[0002]This invention was made in part with Government support under Grant No. NSF 07090738 awarded by the National Science Foundation. The government has certain rights in the invention.REFERENCE TO SEQUENCE LISTING, A TABLE, OR COMPUTER PROGRAM LISTING COMPACT DISC APPENDIX[0003]Not ApplicableBACKGROUND OF THE INVENTION[0004]The remediation of arsenic from contaminated surface waters is a problem worldwide (Mandal, 2002). In terms of acute toxicity of inorganic arsenic; As(III) is more toxic than As(V). Either arsenate or arsenite can be the dominant form in aqueous systems depending on the reduction potential of the environment. Arsenate generally is the ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C02F1/62B01J41/12
CPCC02F1/285C02F2101/103B01J20/3272C02F1/42B01J20/345B01J20/3204B01J20/3236B01J20/3433
Inventor ROSENBERG, EDWARDKAILASAM, VARADHARAJAN
Owner UNIVERSITY OF MONTANA
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