# US 10,501,341 B2 · Method for removing heavy metals from wastewater

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- Number: US 10,501,341 B2
- Document ID: US10501341B2
- Status: Granted
- Kind: B2
- Application number: 16/426,503
- Filed: 2019-05-30
- Published: 2019-09-19
- Granted: 2019-12-10
- Earliest claimed: 2015-12-04
- Assignees: King Fahd University of Petroleum and Minerals
- Applicants: King Fahd University of Petroleum and Minerals
- Inventors: Othman Charles Sadeq Al Hamouz; Oluwafemi S. Akintola; Tawfik Abdo Saleh Awadh
- Web page: https://patentgrep.com/patent/US10501341B2

## CPC

- C02F 1/285: {using synthetic organic sorbents}
- B01J 20/267: {Cross-linked polymers}
- B01J 20/28014: {characterised by their form}
- B01J 20/28059: {being less than 100 m2/g}
- B01J 20/3425: {of sorbents or filter aids comprising organic materials}
- C08G 73/0266: {Polyanilines or derivatives thereof}
- C02F 2101/103: {Arsenic compounds}
- C02F 2101/20: Heavy metals or heavy metal compounds
- C02F 2103/001: {Runoff or storm water}
- C02F 2103/007: {Contaminated open waterways, rivers, lakes or ponds}
- C02F 2103/10: from quarries or from mining activities
- C02F 2103/34: from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F 2103/42: from bathing facilities, e.g. swimming pools
- C02F 2303/16: Regeneration of sorbents, filters
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS

## Abstract

Cross-linked polymeric resins from anilines linked together with polyamine alkyl chains. A process for producing the cross-linked polymeric resins by Mannich-type polycondensation of anilines and diaminoalkanes linked together by an aldehyde and subsequent basification. In addition, a method for removing heavy metals, such as Pb (II) and As (V) from aqueous solution via contacting and treatment with the cross-linked polymeric resins.

## Claims

### Claim 1

A method for removing a heavy metal from an aqueous solution, comprising:
contacting a cross-linked polymeric resin with the aqueous solution comprising at least one heavy metal;
wherein the cross-linked polymeric resin has the following formula (I)
or a salt, solvate, tautomer or stereoisomer derived from the cross-linked polymeric resin of formula (I);
wherein each R1 is independently selected from H, an alkyl, a cycloalkyl, and an aryl;
each R2 is independently selected from H, —F, —Cl, —Br, —CN, —OR3, an alkyl, a cycloalkyl, and an aryl;
each R3 is independently selected from —H, an alkyl, a cycloalkyl, and an aryl;
n is a positive whole number in the range of 2-16;
X is a positive whole number; and
A1 forms a bond to A2 of another monomer unit; and
adsorbing the heavy metal onto the cross-linked polymeric resin to form a heavy metal loaded cross-linked polymeric resin and a heavy metal depleted aqueous solution.

### Claim 2 (depends on 1)

The method of claim 1, further comprising:
desorbing the heavy metal from the heavy metal loaded cross-linked polymeric resin by treating with an acid to form a cross-linked polyamine terpolymer;
treating the cross-linked polyamine terpolymer with a base to reform the cross-linked polymeric resin; and
reusing the cross-linked polymeric resin up to 15 times without a loss in adsorption capacity.

### Claim 3 (depends on 1)

The method of claim 1, wherein the heavy metal is at least one ion selected from the group consisting of Co, Cu, Zn, As, Sr, Mo, Cd, and Pb.

### Claim 4 (depends on 1)

The method of claim 1, wherein the heavy metal is at least one selected from the group consisting of lead (II) and arsenic (V).

### Claim 5 (depends on 1)

The method of claim 1, wherein the cross-linked polymeric resin has an adsorption capacity in the range of 100-1000 μg of heavy metal per g of the cross-linked polymeric resin.

### Claim 6 (depends on 1)

The method of claim 1, wherein the aqueous solution has a pH in the range of 2 to 8.

### Claim 7 (depends on 1)

The method of claim 1, wherein the aqueous solution has an initial heavy metal concentration in the range of 50 μg L−1 to 1250 μg L−1.

### Claim 8 (depends on 1)

The method of claim 1, wherein the cross-linked polymeric resin is present at a concentration in the range of 0.05-5.0 g of resin per L of the aqueous solution during the contacting.

### Claim 9 (depends on 1)

The method of claim 1, wherein the cross-linked polymeric resin is contacted with the aqueous solution for 0.1 to 24 hours.

### Claim 10 (depends on 1)

The method of claim 1, wherein the contacting is performed at a temperature in the range of 20° C. to 60° C.

### Claim 11 (depends on 1)

The method of claim 1, wherein greater than 80% of the total mass of the heavy metal is removed from the aqueous solution.

### Claim 12 (depends on 1)

The method of claim 1, wherein formula (I) each R1, R2, and R3 is —H and n is 4; and
wherein the aqueous solution comprises lead (II) and at least one additional heavy metal selected from the group consisting of Co, Cu, Zn, As, Sr, Mo, and Cd; and
wherein greater than 90% of the total mass of lead (II) is removed from the aqueous solution.