Cryptomelane Modified Biomass Wastes for Solar Interfacial Evaporation and Stabilization of Cadmium

doi:10.21203/rs.3.rs-1647787/v1

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Cryptomelane Modified Biomass Wastes for Solar Interfacial Evaporation and Stabilization of Cadmium

https://doi.org/10.21203/rs.3.rs-1647787/v1

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In recent years, solar interfacial evaporation has received increasing attention due to its potential applications in power generation, seawater desalination, and wastewater treatment. In this work, after carbonization of two biomass wastes, rice husk and coconut husk, they were modified by hydrothermally synthesized cryptomelane manganese and prepare into a solar interfacial evaporation system to explore their evaporation performance and stabilization performance of cadmium. The results demonstrate that the cryptomelane modified biochar can obtain an evaporation rate of 1.085 kg m^− 2 h^− 1 and a photothermal conversion efficiency of 77.75% under one sun (1 kW m^− 2). Under the condition that the average solar power density is only 465.22W m^− 2, the evaporation amount reaches 4.7kg m^− 2 within six hours, and the evaporation rate reaches 0.78kg m^− 2 h^− 1. The two kinds of biomass wastes modified by cryptomelane have enhanced adsorption performance for cadmium, and can be well used for long-term stabilization and recycling of Cd. It could be verified that the cryptomelane modified biochar material is a low-cost, scalable and efficient material for interfacial evaporation and reduce wastewater pollution.

solar interfacial evaporation

cryptomelane

biomass wastes

water purification

cadmium adsorption

stabilization

Fresh water and energy shortages are critical to the humankind’s survival, as well as the economic development and social progress (Albert et al. 2021; Zhu et al. 2019a; Zhu et al. 2019c). Water supplies continue to shrink as global warming and dry spells grow. According to statistics, about 2.2 billion people worldwide do not have access to safe water (WHO/UNICEF. 2017). About 4 billion people, who make up nearly two-thirds of the world's population, experience severe water shortages for at least one month of the year (Water. 2019). Solar energy is considered as a promising renewable, low-cost, electricity-independent energy, which has been the important subject of research and industrial purposes to solve the shortage problem of clean water especially in poor countries (Cheng et al. 2021; Fillet et al. 2021; Tao et al. 2020). In recent times, solar-driven evaporation has attracted considerable interest for replenishing the fresh water supply from seawater and polluted water (Wilson et al. 2020) as well as generating electricity (Huang et al. 2021).

Evaporation is a common phenomenon in nature occurring at the liquid-gas interface. There are two ways to trigger vaporization: decreasing the air pressure and increasing the water temperature (Zhao et al. 2020). Traditional solar evaporation devices generally deliver a low photothermal conversion efficiency of 30 ~ 45% because of poor solar absorption and large heat losses (Chen et al. 2019). Recently many efforts have been done to enhance solar to heat energy conversion, thermally isolate the water-air interface from bulk water, tailor the morphology of the evaporating surface and activate water to reduce energy consumption of water evaporation (Zhao et al. 2020). With the progress of the research, many achievements have been made to improve the evaporation efficiency in the new structural design of the solar evaporator (Li et al. 2018; Li et al. 2016; Qi et al. 2020; Zhang et al. 2018). Meanwhile, photothermal conversion materials for evaporation have also attracted extensive research attention, such as metal nanoparticles (Liu et al. 2017), nanostructured semiconductors (Ishii et al. 2016), carbonaceous materials (Jiang et al. 2016; Li et al. 2016; Panagiotopoulos et al. 2012; Xu et al. 2017; Xue et al. 2017; Yang et al. 2019b) and polymers (Zhou et al. 2018). In terms of applications, natural materials, the main source of which are biomass, are used for solar evaporation by raw or carbonized processes with the advantages of low cost and low environmental impact (Fillet et al. 2021). Nowadays, more and more natural materials, such as wood (Xue et al. 2017; Yu et al. 2019; Zhu et al. 2017), plants (Fang et al. 2018; Sheng et al. 2020; Zhang et al. 2020), vegetables (Long et al. 2019), algae (Yang et al. 2019a) and other atypical biomass (Guo et al. 2019; Zhou et al. 2019), have been proposed for solar thermal conversion materials with good practical results.

Biochar (BC) is produced by the fast thermal decomposition of biomass at oxygen-limited conditions without any steam or chemical activation. The pyrolysis process with little or no oxygen can enable cost-effective biomass wastes such as rice husks, straws to have larger surface area and more porous structures (Leng et al. 2021). Furthermore, BC has been confirmed to remove and immobilize heavy metal pollutants compared with active carbon (Inyang et al. 2016). In addition, manganese oxide minerals most of which have dark black or grey color are commonly found in soil or as thin coating on the surface of rocks (Lu et al. 2019). They have been proven as “photoelectric device” to exhibit highly responsive and stable photon-to-electron conversion in solar-terrestrial system (Anhuai et al. 2019). Most of manganese oxides have been noted for high oxidization potential and high adsorption capacity because of special tunnel or layered crystal structures and large specific surface area, so that they can be effectively applied in wastewater treatment (Islam et al. 2018). It has been reported that the manganese-modified biochar particles can greatly enhance the adsorption of heavy metal ions, such as Cu²⁺, Pb²⁺ and Cd²⁺, when dispersed in water (Liu et al. 2022; Sachan and Das 2022; Tan et al. 2020). As we all know, heavy metal pollution is a serious environmental problem today, among which cadmium (Cd) pollution is the most serious. Moreover, Cd can accumulate in animals and humans for a long time, causing irreversible damage (Pehlivan et al. 2008). When a certain concentration of Cd exists in the human body for a long time, it will have serious toxic effects on the organs and immune system. In severe cases, it can lead directly to cancer (Vuković et al. 2010). In view of the adsorption effect of manganese-modified biochar on heavy metal ions, cryptomelane modified biochar (CBC) was prepared as a solar thermal conversion material, which can absorb heavy metal cadmium in contaminated water while obtaining clean water.

In the present work, we report a solar steam generator utilizing cryptomelane modified rice husk biochar (CBC-R) and coconut shell biochar (CBC-C) for the generation of freshwater and the removal of Cd (II) from aqueous solutions. The water paths are constructed to link up the solar absorber to the water body with filer-paper-PVA water pipe system. The overall preparation process of the generator is shown in Fig. 1. The objectives of the study are to determine a simple and cost-effective way for both a good photothermal evaporation efficiency and stabilize of heavy metals from the polluted water.

Materials

All the chemicals MnSO₄·H₂O, KMnO_4, CH₃COOH, Cd (NO₃)₂ and sodium hydroxymethyl cellulose of analytical grade were purchased from Sinopharm Chemical Reagent Beijing Co., Ltd.

For preparation of reaction solutions and purification of the synthesis products, deionized water was used as the solvent and scour. The rick husks were collected from the agricultural wastes in Anning city in Yunnan Province, southwest of China. The coconut shell biochar, filter paper and PVA absorbent sponge form tube were purchased from JD. com.

Fabrication of manganese oxide modified biochar

For synthesis of BC, the rice husks were placed in a ceramic pot and dried at 80℃ overnight. Pyrolysis of the air-dried rice husks was conducted in a tube furnace under flowing N₂ by ramping the temperature at a rate of 10℃ per min and holding at a peak temperature of 900℃ for 2h (Sun et al. 2020). Both of the rice husk biochar (BC-R) and coconut shell biochar (BC-C) were pulverized and ground into powder less than 80 mesh for further preparation.

Cryptomelane is prepared by hydrothermal method (McKenzie 1971): 0.035mol KMnO₄ was added into 80mL deionized water, and 0.05mol MnSO₄·H₂O was added into100ml acetic acid solution with 2mol L^− 1 concentration. The above two solutions were heated to 60℃, and then the acetic acid solution dissolved with MnSO₄ was added to the KMnO₄ solution and transferred to a 500 mL conical flask. The conical flask was heated to 100℃ on a magnetic stirrer. After refluxing, the manganese oxide solid was filtrated, washed and dried at 50 ºC for 1 day. The solid particle size to less than 80 mesh and mixed mechanically with biochar powder 2.4g unmodified biochar and manganese oxide modified biochar powder was ultrasonically dispersed in 40g water for 10 min and added into 40g 2% sodium hydroxymethyl cellulose solution for continuing dispersing for 10 min, and finally get CBC-C and CBC-R.

Preparation of solar steam generators

In the first step, the filter papers were cut into discs of 6cm diameter. The filer paper was coated evenly with above solutions using a brush, and dried in the oven at 60℃. As shown in Fig. 1, a PVA sponge rod with a diameter of 1 cm was used as a water delivery channel to transport water from the beaker to the surface of the filter paper and support the filter paper to keep it stable.

Solar-driven steam generation experiments

The solar-driven steam generation was evaluated by noting the weight change of water per unit time. The solar steam generators were placed on top of a 100mL plastic beaker containing deionized water and placed on the weighing balance (AB265-S, Mettler Toledo) with automatic counting. The vessel was illuminated by a solar simulator (PL-X500D, Beijing Precise Technology, Co. Ltd) with 1 sun intensity in the laboratory. The steam generation performances were measured for at least 3 hours for each generator. In order to obtain the real outdoor evaporation effect, the evaporator also conducted all-day evaporation experiments at an altitude of about 2200m in Anning City, Yunnan Province. All the surface temperatures of steam generators were recorded using an infrared camera (FLIR One), and the sunlight intensity was enhanced by a mobile weather monitoring station on the mountain.

Treatment of simulated Cd (II) polluted solution

200 mg L^− 1 Cd (II) solution was loaded in the 100mL breaker. The vessel was also put on the weighing balance and illuminated with 1 sun intensity by a solar simulator for the adsorption experiments. Adsorption experiments were performed for each sample for 6 hours, and the Cd solution was sampled and diluted 100-fold every hour, and the concentration was determined by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). After 4 hours of sufficient adsorption, the evaporation material was completely dried in an oven at 60°C.Each sample was randomly selected three times using Energy Dispersive Spectroscopy (EDS) to obtain elemental semi-quantitative analysis results. In order to study the salt crystallization phenomenon in the long-term solar evaporation adsorption process of the steam generator, the steam generator was put into 10g L^− 1 of high-concentration Cd(Ⅱ) solution for 24 hours and 7 days in a solar experiment.

Characterization of Materials

Figure 2 shows the SEM images of CBC-C(a) and CBC-R(b) under different magnifications. From the characterization results, it can be seen that compared with the smooth block coconut shell BC, the rice husk BC has certain ravines and holes. meanwhile, both CBC-C and CBC-R adhered well to the surface of the filter paper. The XRD patterns of CBC-C and CBC-R are shown in Fig. 2(c), the cryptomelane was well generated by the hydrothermal method. The rod-like crystals uniformly loaded on the sample are the synthetic cryptomelane (Meng et al. 2020). This indicates that more potential active adsorption sites can be generated after the modification of cryptomelane (Tao et al. 2019).

Table 1 Pore characteristic parameters of all samples

Sample	S_BET (m² g^− 1)	V_total (cm³ g^− 1)	D_avg (nm)
BC-C	35.428	0.029	3.028
CBC-C	66.052	0.318	12.088
BC-R	16.689	0.014	8.106
CBC-R	72.446	0.335	10.540

Fig. 3(a) and (b) show the N2 adsorption/desorption isotherms of CBC-R and CBC-C. According to the International Union of Pure and Applied Chemistry (IUPAC) classification corresponding to micro-macropores materials, the adsorption isotherms for both materials are a combination of type I and type II isotherms (Liu et al. 2013). Nitrogen uptake at lower relative pressures (P/P0 ≤ 0.01) indicates filling of micropores (diameter ≤ 2 nm) (Long et al. 2009). Nitrogen uptake at higher relative pressures (P/P0 = 0.40 to 0.95) and explicit hysteresis loops indicate the presence of mesopores (2 nm < diameter < 50 nm) (Tao et al. 2009). The dramatic increase in the adsorption volume in the high relative pressure region (P/P0 = 0.95 to 1) indicates the presence of larger mesopores and macropores (>50 nm in diameter) (Robertson and Mokaya 2013; Wang et al. 2012). Comparing with the pore distribution curve shown in Fig. 3(c), it can be seen that CBC-R and CBC-C have a sharp peak at 1.5 to 2 nm, indicating the existence of a certain microporous structure. And there are a large number of mesopores and a small amount of mesopores and macropores. Meanwhile, pore characteristic parameters including BET surface area (S_BET), total pore volume (V_total) and average pore diameter (D_avg) of each sample were calculated from the N2 adsorption/desorption data, and the results are shown in Table 1. It can be clearly seen from the results that the specific surface area and pore volume of BC-C and BC-R before modification are small, and there is only a small amount of micropores and mesopores. After cryptomelane modification, the specific surface area and pore volume were increased. The above results demonstrate that the modified CBC-C and CBC-R are a typical hierarchical porous structure with better adsorption performance and better ability to stabilize Cd from solution.

Solar interfacial evaporation experiment

To evaluate the evaporation performance of solar absorbers, an indoor simulated evaporation experiment was carried out under the conditions of an ambient temperature of 10°C and 25% relative humidity. During the evaporation experiment, an infrared camera was used to record the temperature of the material surface, as shown in Fig. 4. Under the irradiation of 1 sun, the top surface of each device can absorb light and convert it into heat, resulting in a rapid increase in surface temperature. As shown in Fig. 4(b), compared with the blank group, each device has a good photothermal conversion performance. The surface temperature of the device rises rapidly within 10min, and then the rising trend rapidly slows down, and then the surface of each device reaches the highest temperature at 60min. Among them, the surface temperatures of the modified CBC-C and CBC-R were higher than those before modification, respectively reaching 43.0°C and 42.3°C. It can be verified from the results that after cryptomelane modification, the photothermal conversion capability of the device has been improved to a certain extent, and more light energy can be converted into heat, so that the surface temperature is higher, which can be better used for the interface water evaporates.

As shown in the mass change curve shown in Fig. 5(a), the evaporation rate did not decay during the whole experimental process, showing good durability. To further evaluate the performance of CBC, in addition to the evaporation rate, thermal efficiency (η) is also introduced to account for the utilization of sunlight by the device. The formula for calculating η is as follows (Ghasemi et al. 2014):

$$\text{η}\text{=}\frac{\text{m(λ+ C }\text{∆}\text{T)}}{\text{Qs}}$$

where η is the efficiency (dimensionless, but more often expressed in %), m is the net evaporation rate (that is, the rate of evaporation due to light alone) in kg m^− 2 h^− 1, and λ is the latent heat of phase transition in (kJ kg^− 1), C is the specific heat capacity of water (4.2 J g^− 1 K^− 1), ΔT is the interfacial water temperature difference, and Q_s is the power density of the solar flux in kW m^− 2. The calculation results are shown in Fig. 5(b) and (c), the evaporation rate of CBC-C with the highest surface temperature reaches 1.085kg m^− 2 h^− 1, which is the highest among all samples, and is about 2.14 times of the evaporation rate of the blank device. The evaporation rates of BC-C, CBC-R and BC-R were 0.978, 1.053 and 0.904 kg m^− 2 h^− 1, respectively. In the case of high radiation energy loss caused by low ambient temperature in winter (Zhao et al. 2020), the four steam generators also showed good photothermal conversion efficiency. Among them, CBC-C had the highest evaporation efficiency, reaching 77.75%, and CBC-R, BC-C and BC-R reached 75.37%, 69.04% and 64.6%, respectively. This indicates that CBC has excellent evaporation performance, and the increase in the relative content of cryptomelane effectively improves the evaporation performance of the device.

There are two main aspects of heat loss that affect photothermal conversion: heat radiation to the environment and heat conduction to bulk water (Fillet et al. 2021). The specific calculation methods are as follows (Ni et al. 2016):

$${\text{P}}_{\text{Rad}}\text{=}\text{Aεσ}\text{(}{\text{T}}^{\text{4}}\text{-}{\text{T}}_{\text{M}}^{\text{4}}\text{)}$$

$${\text{P}}_{\text{Con}}\text{=}\text{A}\text{h}\text{(}\text{T}\text{-}{\text{T}}_{\text{M}}\text{)}$$

where P_Rad is the radiative heat loss to the environment, A is the surface area of the interface material facing the sun, ε is the reflectivity of the interface material, σ is the Stefan-Boltzmann constant (5.67×10^− 8W m^− 2 K^− 4), T is the ambient temperature, and T_M is the interface material temperature, P_Con is the heat conduction loss to the bulk water, h is the convective heat transfer coefficient. According to the formula calculation, the radiative heat loss fluxes of CBC-C and CBC-R are about 19.32W m^− 2 and 18.10W m^− 2, and their radiative heat losses are 0.053W and 0.050W, respectively. Compared with other experimental results (Wang et al. 2020), the radiative heat loss increases more. It can be seen that the low ambient temperature in winter has a greater impact on the heat loss. Similarly, it can be seen from formula (3) that the ambient temperature also has a great influence on the conduction heat loss. The lower the ambient temperature, the greater the heat conduction loss. However, according to research, as the surface area of the interface evaporated material gradually increases within a certain range, the loss caused by heat conduction is smaller (Yan et al. 2022). For the devices with good scalability in this experiment, the evaporation capacity and evaporation efficiency can be improved by designing the structure and water delivery methods.

Yunnan Province (20°8′–29°16′ N, 97°31′–106°12′ E), located in southwestern China, borders the Tibetan Plateau and the Himalayas in the west, Laos and Vietnam in the south, covering an area of About 3.83 × 105 square kilometers (Duan et al. 2016). The elevation of this area increases from 76 meters in the southeast to 6,740 meters in the northwest, with an average elevation of 2,000 meters and high solar radiation intensity (Li et al. 2019). Due to its cold zone, temperate zone and tropical climate type, Yunnan Province has relatively small annual temperature difference and long sunshine hours. The hottest month (July) averages between 19°C and 22°C, and the coldest month (January) averages over 6°C, however, the daily temperature difference in Yunnan is larger (Yunling 2019). In order to obtain a certain evaporation effect in winter, the outdoor simulated evaporation experiment was selected on a mountain about 2000m above sea level in Anning City, Yunnan Province. The experimental results are shown in Fig. 6.

The CBC-C and CBC-R with the best evaporation effect were selected for the test. The surface temperature of the device before and after the test is shown in Fig. 6(a)-(c). The ambient temperature during the experiment was 10°C-15°C, and the highest temperature reached on the surfaces of the two devices was about 33.7°C. the evaporation per day was about 4.7kg m^− 2, and the evaporation rate was 0.78kg m^− 2 h^− 1. The surface temperature of the blank group was only 12.6°C, which was lower than the ambient temperature. Assuming 12 hours of sunlight per day (6:00–18:00), the production of purified water is estimated to be 9.36 kg m^− 2 per day (higher in summer). Therefore, a solar steam generator with an area of 0.28-0.39m² can produce enough clean water to meet an adult's daily water intake (about 2.7 liters per day for women and about 3.7 liters per day for men) (Sawka et al. 2005). Figure 6(d) shows the sunlight intensity curve on the day of the experiment. It can be seen that the highest solar power density on the day of the experiment is 1070W m^− 2, and the average power density is 465.22W m^− 2. Compared with the water quality change curve in Fig. 6(e), it can be seen that during the period of 13:00–14:00 when the solar power density is high, the evaporation rate increases significantly, and in the afternoon, with the decrease of the solar power density, the evaporation rate decreases obviously, which is in line with the theoretical law. It can be seen from the experimental results that the modified CBC-C and CBC-R still have excellent evaporation performance even under the condition of low solar power density, and have good practical application prospects.

3.2 Stabilization experiment of Cadmium from Aqueous Solution

After 6 hour of adsorption experiment, the experimental results is shown in Fig. 7. Considering that the volume of the solution decreases with the evaporation of water during the experiment, the volume change is taken as an important factor for the concentration change. The variation curve of solution volume with experimental time is shown in Fig. 7(a). Corresponding to the evaporation rate, the solution volume of each device gradually decreases with the evaporation of water. The concentration obtained by ICP-MS was corrected by introducing the volume change to obtain a curve of mass versus time, as shown in Fig. 7(b). The volume change, like the adsorption of Cd by the device, leads to the change of the solution concentration. Under the combined influence of these two factors, the concentration curve is unstable and fluctuates. It can be seen from the curves that the modified CBC-C and CBC-R can better adsorb Cd in solution. Combined with the semi-quantitative analysis results obtained by EDS shown in Table 2, it can be seen that the area with more Mn element content, that is, the area with more cryptomelane loading, the more Cd element adsorbed. This proves that cryptomelanin can improve the capture ability of Cd of the device, and can better adsorpt and stabilize Cd from solution. Because cryptomelane loaded on biochar can form amphiphilic sites on the carbonaceous lattice, it may have a high immobilization potential for divalent metals and enhance the adsorption of Cd(II) on biochar (Shaheen et al. 2021). At the same time, the surface of biochar modified by cryptomelane will be enriched with functional groups such as C-O, C = O, -OH, which can be complexed with Cd(II), thereby improving the adsorption effect (Zhu et al. 2019b). At the same time, the higher specific surface area brought by the modification of the device can enhance its adsorption performance for Cd in solution.

Table 2

Elemental semi-quantitative analysis results obtained by EDS
Sample	Point	K [%] ^a)	Mn [%]	Cd [%]
CBC-R-0.8	1	0.46	1.24	0.53
	2	0.49	1.31	0.54
	3	1.17	2.64	0.7
CBC-R-2.4	1	0.12	2.74	0.05
	2	0.24	21.64	0.19
	3	2.65	36.51	0.42

^a) % represents the proportion of the atomic number, and the rest of the % in the table have the same meaning

The surface crystallization of the obtained material is shown in Fig. 8(a), and only a small amount of crystalline salt appears on the surface of the outer ring. To further illustrate the crystallization of Cd (II), the whole experimental device was placed in the natural environment for 7 days, and the obtained crystallization is shown in Fig. 8(b) and (c). It can be seen that compared with the large amount of white crystalline salt produced by the internal measurement of the filter paper, only a small amount of crystalline salt appeared on the outer ring of the material surface. This shows that the water supply at the evaporation interface close to the water delivery channel is stable for a long time in the experiment, and does not lead to supersaturation of the salt solution (Liu et al. 2020). Meanwhile, the crystalline salt is well fixed on the filter paper and the outer ring on the surface of the material, which does not affect the evaporation performance and facilitates the collection of the crystalline salt.

In this paper, cryptomelane modified biomass wastes were successfully synthesized, and its interfacial evaporation performance and the adsorption and stabilization ability of heavy metal Cd were studied. Indoor evaporation experiments showed that the two biomass wastes modified by crypto-garnet obtained better evaporation performance. The device with the best evaporation performance is CBC-C, with an evaporation rate as high as 1.085kg m^− 2 h^− 1 and an efficiency of 77.75%. In order to explore the practicality of the designed device, a real evaporation experiment was also carried out in Yunnan Province with high sunlight intensity. Under the condition of 6 hours of illumination time and an average solar power density of only 465.22 W m^− 2, the modified biochar performed well, with an evaporation rate of 4.7 kg m^− 2 and an evaporation rate of 0.78 kg m^− 2 h^− 1. In the Cd stabilization experiment, the two biomass wastes have improved the adsorption performance of Cd (II) through cryptomelane modification, and the materials have good salt tolerance, can be evaporated and adsorbed for a long time, and stabilized Crystalline salts are easy to collect. Therefore, cryptomelane modified biomass wastes can be used as a low-cost and efficient interfacial evaporation material in the future, while stabilizing Cd in wastewater and reducing wastewater pollution.

Acknowledgements

The authors wish to thank the anonymous reviewers for their comments.

Funding

We thank the following funding agencies for supporting this work: the China Geological Survey Project (Grant No. DD20190589) and the National Key Research and Development Program of China (No. 2019YFC1805005).

Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Author contribution

Baoyu Zhang: Investigation, formal analysis, writing-original draft, visualization. Chenzi FAN: Funding acquisition, supervision, conceptualization, methodology, resources, writing—review and editing. Wei Guo: Formal analysis, writing-review. Yun Zhu: Analysis, visualization. All the authors contributed to critically reading of the paper and approved the final manuscript

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Cryptomelane Modified Biomass Wastes for Solar Interfacial Evaporation and Stabilization of Cadmium

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Abstract

Figures

Introduction

Experimental

Materials

Fabrication of manganese oxide modified biochar

Preparation of solar steam generators

Solar-driven steam generation experiments

Treatment of simulated Cd (II) polluted solution

Results And Discussion

3.2 Stabilization experiment of Cadmium from Aqueous Solution

Conclusion

Declarations

References

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