IP Library Granted Patent US 10,500,564
Granted Patent B2
US 10,500,564 · App. 15/935,398 · Granted Dec 10, 2019

Preparation of chitosan-based microporous composite material and its applications

Inventor: Shameem Hasan (Sunrise, FL)
Assignee: PERMA-FIX ENVIRONMENTAL SERVICES, INC.
B01J20/24B01D15/08B01J20/0211B01J20/2808B01J20/28026B01J20/3021B01J20/3071B01J20/3085C22B34/34C22B59/00G21F9/12
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Quick Facts
Patent No.
US 10,500,564
App. No.
15/935,398
Granted
Dec 10, 2019
Kind
B2
Abstract

Microporous glutaraldehyde-crosslinked chitosan sorbents include a plurality of nanoparticles of a high Z element. The nanoparticles are disposed in the cross-linked chitosan-gluteraldehyde composite matrix and integrated with the cross-linked chitosan-gluteraldehyde composite matrix to reduce primary impact of high radiation flux and minimize radiolytic effect on said cross-linked chitosan-gluteraldehyde composite matrix. The plurality of nanoparticles is made from the high Z element such as hafnium (Hf). Methods of making and using the microporous glutaraldehyde-crosslinked chitosan sorbents, and a generator for the radioisotope 99 Mo containing the sorbents.

Claims (28)

1. A sorbent comprising:

a microporous material including chitosan which has been crosslinked with glutaraldehyde in the presence of a catalyst to a glutaraldehyde concentration of about 2 to about 4 wt % to produce a cross-linked chitosan-gluteraldehyde composite matrix which is resistant to degradation from exposure to beta and gamma radiation and from exposure to acids; and

a plurality of nanoparticles of a high Z element disposed in said cross-linked chitosan-gluteraldehyde composite matrix and integrated with said cross-linked chitosan-gluteraldehyde composite matrix to reduce primary impact of high radiation flux and minimize radiolytic effect on said cross-linked chitosan-gluteraldehyde composite matrix.

2. The sorbent as set forth in claim 1 wherein said high Z element is hafnium (Hf).

3. The sorbent as set forth in claim 2 wherein Hf is present in said cross-linked chitosan-gluteraldehyde composite matrix between 0.15 g and 0.35 g per grams of said cross-linked chitosan-gluteraldehyde composite matrix.

4. The sorbent as set forth in claim 1 wherein the sorbent has increased selectivity for the sorption of 99 Mo with respect to 99m Tc.

5. The sorbent as set forth in claim 1 further including an additive of sodium nitrate being present at 1 g/L.

6. A method for preparing a radiation-resistant sorbent, comprising:

combining chitosan with water in the presence of an acid to form a chitosan gel;

adding glutaraldehyde to the gel to form a semi-solid mass in the presence of catalyst at 70° C., in where condensation polymerization of reaction mass occurs;

washing the semi-solid mass to remove unreacted glutaraldehyde and form a washed mass;

suspending the washed mass in aqueous base to form a neutralized crosslinked mass;

disposing a plurality of nanoparticles of a high Z element on the neutralized crosslinked mass; and

drying the neutralized crosslinked mass including the plurality of nanoparticles under vacuum to form the radiation-resistant sorbent.

7. The method as set forth in claim 6 wherein said step of depositing is further defined as dispersing the plurality of nanoparticles made from hafnium (Hf) on the neutralized crosslinked mass.

8. The method as set forth in claim 7 wherein said step of depositing is further defined as dispersing the plurality of nanoparticles made from hafnium (Hf) between 0.15 g and 0.35 per grams of the neutralized crosslinked mass on the neutralized crosslinked mass.

9. A method of separating isotopes from mixtures thereof, comprising:

contacting a mixture of at least two isotopes with a radiation resistant sorbent according to claim 1 that preferentially sorbs at least one of said isotopes;

sorbing at least one of said isotopes onto or into said sorbent while one or more of the remaining isotopes are not significantly sorbed by the sorbent;

removing said one or more remaining isotopes from said sorbent.

10. The method according to claim 9 , wherein said at least two isotopes comprise 99 Mo and 99m Tc.

11. The method according to claim 10 , wherein said sorbent preferentially sorbs said 90 Mo and wherein said 99m Tc is not significantly sorbed by said sorbent.

12. The method according to claim 9 , wherein one of said isotopes is a cesium isotope.

13. The method according to claim 12 , wherein said one or more remaining isotopes comprise one or more isotopes present in a radioactive waste stream.

14. The method according to claim 9 , wherein the removing of the one or more remaining isotopes from the sorbent comprises contacting the sorbent with an eluent solution.

15. The method according to claim 14 , wherein the eluent solution comprises one or more oxidizers selected from the group consisting of a chlorite, a hypochlorite, a dichromate, and a metal oxide.

16. A generator for 99 Mo/ 99m Tc, comprising the sorbent of claim 1 .

17. A method for separating or concentrating or both one or more heavy metals from a liquid stream, comprising contacting a liquid stream containing said one or more heavy metals with a sorbent according to claim 1 , and sorbing one or more of said heavy metals thereon.

Assignments (2)
NOTICE OF GRANT OF SECURITY INTEREST IN PATENTS Recorded Jun 23, 2020
From: PERMA-FIX ENVIRONMENTAL SERVICES, INC., AS GRANTOR
To: PNC BANK, NATIONAL ASSOCIATION, AS AGENT
Reel/Frame 053020/0495 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2018
From: HASAN, SHAMEEM
To: PERMA-FIX ENVIRONMENTAL SERVICES, INC.
Reel/Frame 045646/0883 →
Continuity (4)
Continuation In Part 14547201 · Nov 19, 2014
Continuation In Part 13424289 · Mar 19, 2012
Provisional Application 61453772 · Mar 17, 2011
Related Publication 20190105630A1 · Apr 11, 2019