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Biomimetic Hydrogel Composites for Soil Stabilization and Contaminant Article pubs.acs.org/est Biomimetic Hydrogel Composites for Soil Stabilization and Contaminant Mitigation † ‡ ‡ † † ‡ ‡ Zhi Zhao, , Nasser Hamdan, Li Shen, Hanqing Nan, Abdullah Almajed, Edward Kavazanjian, † ‡ § and Ximin He*, , , † School for Engineering of Matter, Transport and Energy, Arizona State University, 781 E Terrace Rd, Tempe, Arizona 85287, United States ‡ The Center for Bio-inspired and Bio-mediated Geotechnics, Arizona State University, P.O. Box 873005, Tempe, Arizona 85287-3005, United States § The Biodesign Institute, Molecular Design and Biomimetics Center, Arizona State University, 727 E. Tyler St., Tempe, Arizona 85287-5001, United States *S Supporting Information ABSTRACT: We have developed a novel method to synthesize a hyper-branched biomimetic hydrogel network across a soil matrix to improve the mechanical strength of the loose soil and simultaneously mitigate potential contamination due to excessive ammonium. This method successfully yielded a hierarchical structure that possesses the water retention, ion absorption, and soil aggregation capabilities of plant root systems in a chemically controllable manner. Inspired by the robust organic−inorganic composites found in many living organisms, we have combined this hydrogel network with a calcite biomineralization process to stabilize soil. Our experi- ments demonstrate that poly(acrylic acid) (PAA) can work synergistically with enzyme-induced carbonate precipitation (EICP) to render a versatile, high-performance soil stabilization method. PAA-enhanced EICP provides multiple benefits including lengthening of water supply time, localization of cementation reactions, reduction of harmful byproduct ammonium, and achievement of ultrahigh soil strength. Soil crusts we have obtained can sustain up to 4.8 × 103 kPa pressure, a level comparable to cementitious materials. An ammonium removal rate of 96% has also been achieved. These results demonstrate the potential for hydrogel-assisted EICP to provide effective soil improvement and ammonium mitigation for wind erosion control and other applications. ■ INTRODUCTION aggregating loose soil, increasing the mechanical strength of fi Environmental degradation, especially soil instabilities that arise soil, and mitigating soil pollutants have signi cant value. from cohesionless and polluted soil, has become an increasingly Traditional soil stabilization methods usually involve heavy important global issue.1 For example, fugitive dust emission2 machinery and energy intensive processes that result in CO2 emissions, excessive consumption of natural resources, and has caused extensive negative impacts on human health and 15,16 safety.3 Effectively aggregating loose cohesionless granular soils generation of hazardous waste. Some recently developed to improve their inherent poor mechanical strength is crucial to methods based on using organic or inorganic soil stabilizers are solving the pressing issues of wind or water erosion of earth less energy consuming, but still have various disadvan- 17−20 surface,4 earthquake-induced liquefaction,5 and many insta- tages. As organic stabilizers, natural polymers are usually bility-induced troubles in constructional projects.6,7 In addition, biodegradable, which limits the lifetime of their stabilization 21 anthropogenic activities may discharge various pollutants to the effect. Common inorganic stabilizers such as salts offer + environment, among which ammonium (NH4 ) is a major limited short-term soil stabilization that is easily reversed by 8−10 + issue. Excessive NH4 can cause eutrophication in water- rain or possibly atmospheric moisture, in addition to their courses,11,12 lead to higher levels of toxic nitrogen-containing significant negative impacts on soil quality, groundwater, compounds,13 elevate greenhouse gases generation,14 and accelerate soil acidification. Interestingly, a significant portion Received: March 15, 2016 + of NH4 in aqueous systems comes from the leachate of loose, Revised: August 29, 2016 highly permeable soils.9 As a result, efficient soil stabilization Accepted: October 20, 2016 solutions that can simultaneously fulfill the need for effectively Published: October 20, 2016 © 2016 American Chemical Society 12401 DOI: 10.1021/acs.est.6b01285 Environ. Sci. Technol. 2016, 50, 12401−12410 Environmental Science & Technology Article − vegetation, and roadway environments.22 24 Furthermore, soil conducted to examine the product. Ammonium absorption/ stabilizers are rarely able to reach a soil strength level desorption was also investigated through spectral measure- comparable to cement-treated samples, nor are they capable ments. The overall performance of the PAA-EICP composite as of mitigating soil pollutants. a soil stabilizer was compared with the effectiveness of a Nature can provide great inspiration on how to overcome the conventional EICP solution to illustrate the advantages of our challenges in soil stabilization. Many living organisms use a method. combination of inorganic and organic compounds to build stable and robust materials. For example, mussel byssal threads ■ MATERIALS AND METHODS employ Fe3+ stabilized proteinaceous glue filaments to help them withstand large cyclic strains.25 Strong biomaterials such Chemicals. Hydrochloric acid (ACS grade), sodium ≥ as bones and seashells use occlusion of macromolecules within hydroxide ( 98%), phosphoric acid (ACS grade), acrylic acid ′ individual crystals to generate superior mechanical properties.26 (AA, 99%), N,N -methylenebis(acrylamide) (Bis, 99%), 2- ′ Despite the wide presence and great benefits of this hydroxy-4 -(2-hydroxyethoxy)-2-methylpropiophenone (Igar- biochemical pathway in nature, a similarly strategy is rarely cure 2959, 98%), ammonium persulfate (APS, 98%), sodium ≥ ≥ employed in soil stabilization or remediation due to the hydroxide ( 98%), ammonium chloride ( 99.5%) and urease − difficulties in integrating organic and inorganic compounds into (15 000 50 000 units/g) from Canavalia ensiformis (Jack bean) a composite in soil. Enzyme induced carbonate precipitation were purchased from Sigma-Aldrich. Calcium chloride − (EICP)27 29 provides a controllable way to introduce inorganic dihydrate (ACS grade) and sodium phosphate, dibasic ≥ ’ crystals within soil to address concerns regarding environ- ( 98%) were purchased from G-Biosciences. Nessler s reagent mental degradation27,28,30,31 and provide suitable ground for was purchased from Fluka. civil infrastructure construction.32 Hydrogel is a promising Hydrogel Preparation. Cross-linked polyacrylate gel (x- − organic candidate for soil stabilization.33 37 Compared with PAA) was prepared by dissolving 400 mg acrylic acid, 20 mg naturally occurring polymers,38 synthetic hydrogels are more Bis and 10 mg Igarcure 2959 in 1 mL DI water (Elga Ultra fi controllable and flexible in their molecular structures and Analytic Lab Water Puri cation System). The mixture was then fl compositions, which makes it possible to chemically engineer cured under UV light (Dymax 5000-EC UV light curing ood synthetic hydrogels to render a soil stabilizer that consists of system) for 30 s. inorganic−organic composites by combining hydrogels and Cementation Localization Test. A thermally curable PAA EICP. precursor (t-AA) that could be directly injected into soil was To design a hydrogel-EICP composite with effective developed. The recipe for this precursor can be found in the structural and chemical functions, we borrowed our strategy Supporting Information. A cementation localization test was from plants that have developed an extensive network of roots conducted using centrifuge tubes filled with fine-grained silica to tightly anchor themselves in the soil.39 The hyper-branched sand (F-60 silica sand, typical engineering sand used in soil root system of plants are known to facilitate aggregation of soil stabilization studies). The EICP solution was prepared by 40,41 particles. Structurally mimicking the unique root structure mixing a CaCl2-urea solution with a urease solution in a 4:1 with hydrogel material can provide additional enhancement to volume ratio. The final concentrations of reactants in EICP · soil in terms of higher strength and a larger length scale of solution were: 1.000 M CaCl2 (2H2O), 1.500 M urea and 0.450 continuity. In addition, root systems feature high water affinity mg/mL urease. t-AA of various volume fractions (0, 20, 40, 50, and great ion absorbing ability in order to constantly provide 60, 80, and 100%) were mixed with the EICP solution and the their stems and leaves with water and dissolved minerals.41,42 mixture was poured onto soil surface immediately after mixing Realizing these properties in a chemical manner is preferred for at a dose of 3 mL/in2. Control samples treated with a solution retaining water, localizing inorganic reagents to improve the that did not contain enzyme were also prepared with the same yield in biomineralization, and enhancing the mechanical method. All the centrifuge tubes were kept at 40 °C (Fisher strength of the hydrogel-EICP composite through cation- Scientific Isotemp Premium Lab Oven) for 5 h followed by hydrogel complexation.25 Additionally, the removal of incubating at room temperature (RT) for 14 days to allow time ammonium, a byproduct in EICP, may also be achieved for the cementation reaction to take place. through mimicking the ion absorbing ability of roots with Characterization Methods. All the SEM and EDX data − proper functional groups in the hydrogel.43 45 was taken using a 15 keV Hitachi S4700 field emission scanning
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