Influence and its mechanism of temperature variation in a muffle furnace during calcination on the adsorption performance of rod-like MgO to Congo red

Abstract

Calcination temperature plays a crucial role in determining the surface properties of generated MgO, but the influence of temperature variation in a muffle furnace during calcination on its performance is rarely reported. Herein we observed that the temperature in a muffle furnace during calcination demonstrated a gradually increasing trend as the location changed from the furnace doorway to the most inner position. The variation in temperature had a great impact on the adsorption performance of generated rod-like MgO without and/or with involvement of Na₂SiO₃ to Congo red in aqueous solution. To get a better understanding on the detailed reasons, various techniques including actual temperature measurement via multimeter, N₂ physical adsorption, CO₂ chemical adsorption and FT-IR spectrometry have been employed to probe the correlation between the adsorption performance of generated MgO from various locations and the inner actual temperature of used muffle furnace as well as their physicochemical properties. In addition, two mechanisms were proposed to elucidate the adsorption process of Congo red over the surface of generated MgO without and/or with presence of Na₂SiO₃, respectively.

Keywords

magnesium oxide / calcination / muffle furnace / placed location / adsorption performance

References

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Acknowledgements

The authors would like to acknowledge funding support from the National Natural Science Foundation of China (Grant Nos. 21575112, 21777128 and 21705125) and Shaanxi S&T Research Development Project of China (Grant No. 2016GY-231).

Supplementary information

This section contains the details for photograph of the distribution of the samples in used muffle furnace, UV-vis spectra of initial Congo red solutions treated with MgO, contour maps of the adsorption capacities of obtained MgO particles from different temperatures, photographs of the MgO with different morphologies, and comparison of the residual concentration of Congo red solution after adsorption by generated MgO from various reaction systems.

Fig. S1 Photographic image of the distribution of the samples for calcination in used muffle furnace (20 cm width × 30 cm length).

Fig. S2 UV-vis spectra of initial Congo red solutions (2500 mg·L⁻¹ for MgO without Na₂SiO₃ and 3000 mg·L⁻¹ for MgO with Na₂SiO₃, 10 mL) treated with 10 mg of MgO particles obtained from the reaction between Mg(NO₃)₂ and Na₂CO₃ (a) in the absence and (b) in the presence of 0.1 g of Na₂SiO₃ followed by calcination at 500°C, in which #1–#12 mean the placed locations of samples in used muffle furnace as indicated in Fig. 1(a).

Fig. S3 Photographs of initial Congo red solutions (2500 mg·L⁻¹ for 400°C, 3000 mg·L⁻¹ for 500°C, 2000 mg·L⁻¹ for 600°C, and 700 mg·L⁻¹ for 700°C, 10 mL) treated with 10 mg of MgO particles obtained from the reaction between Mg(NO₃)₂ and Na₂CO₃ in the absence [(a)(c)(e)(g)] and in the presence [(b)(d)(f)(h)] of 0.1 g of Na₂SiO₃ followed by calcination at (a)(b) 400°C, (c)(d) 500°C, (e)(f) 600°C, and (g)(h) 700°C [Note: The marked numbers 1–12 mean the placed locations of samples in used muffle furnace as indicated in Fig. 1(a)].

Fig. S4 Contour maps of the adsorption capacities of obtained MgO particles from the reaction between Mg(NO₃)₂ and Na₂CO₃ in the absence [(a)(c)(e)] and in the presence [(b)(d)(f)] of 0.1 g of Na₂SiO₃ followed by placing at different locations in used muffle furnace for calcination at (a)(b) 400°C, (c)(d) 600°C and (e)(f) 700°C [Note: The adsorption capacity was evaluated by the residual concentrations of Congo red solutions (initial concentration: 2500 mg·L⁻¹ for 400°C, 2000 mg·L⁻¹ for 600°C and 700 mg·L⁻¹ for 700°C, 10 mL) treated with 10 mg of MgO particles obtained from calcination at different temperatures].

Fig. S5 Contour maps of the adsorption capacities of obtained MgO particles from the reaction between Mg(NO₃)₂ and Na₂CO₃ followed by placing at different locations in used muffle furnace for calcination at 500°C with different heating rates: (a) 10.7°C/min; (b) 5.3°C/min; (c) 2.7°C/min [Note: The adsorption capacity was evaluated by the residual concentrations of Congo red solutions (initial concentration: 3000 mg·L⁻¹, 10 mL) treated with 10 mg of obtained MgO particles].

Fig. S6 Photographs of initial Congo red solutions (10 mL) treated with 10 mg of MgO particles obtained from the following reaction systems: (a) from the reactions between Mg(NO₃)₂ and K₂CO₃, MgCl₂ and Na₂CO₃ and Mg(NO₃)₂ and (NH₄)₂CO₃ followed by placing in the positions of 1, 2 and 3 as indicated in Fig. 1(a) for calcination (initial concentration of Congo red solution: 2500 mg·L⁻¹); (b) from the reactions between Mg(NO₃)₂ and Na₂CO₃ in the presence of 0.0004 mol Fe(NO₃)₃·9H₂O, Al(NO₃)₃·9H₂O and Na₂C₂O₄ followed by placing in the positions of 1, 2 and 3 as indicated in Fig. 1(a) for calcination (initial concentration of Congo red solution: 2500 mg·L⁻¹); (c) from the reactions between Mg(NO₃)₂ and Na₂CO₃ in the presence of 0.0004 mol Na₅P₃O₁₀, Na₃PO₄·12H₂O and NaF followed by placing in the positions of 1, 2 and 3 as indicated in Fig. 1(a) for calcination (initial concentration of Congo red solution: 3000 mg·L⁻¹ for the systems with Na₅P₃O₁₀ and Na₃PO₄·12H₂O and 2700 mg·L⁻¹ for the system with NaF).

Fig. S7 Photographs of the obtained MgO with different morphologies: (a) trapezoidal MgO; (b) spherical MgO; (c) spherical-like MgO; (d) nest-like MgO. Photographs of initial Congo red solutions (300 mg·L⁻¹ for trapezoidal MgO, 700 mg·L⁻¹ for spherical MgO, 2300 mg·L⁻¹ for spherical-like and nest-like MgO, 10 mL) treated with 10 mg of MgO particles with different morphologies from the system (e) in the absence and (f) in the presence of 0.1 g of Na₂SiO₃ followed by calcination at 500°C [Note: The marked numbers 1–3 mean the placed locations of samples in used muffle furnace as indicated in Fig. 1(a)].

Fig. S8 Contour maps of measured inner actual temperatures in used muffle furnace when the controller temperatures were, respectively, set as (a) 50°C, (b) 75°C and (c) 125°C (each data point was an average of three replicates, and the deviation between them was less than 0.5°C).

Table S1 Comparison of the residual concentration of Congo red solution after adsorption by generated MgO from various reaction systems

Placed location	Residual concentration of Congo red in different systems/(mg·L−1)
	System 1			System 2			System 3
	Mg(NO3)2 + K2CO3a)	MgCl2 + Na2CO3a)	Mg(NO3)2 + (NH4)2CO3a)	Fe(NO3)3a)	Al(NO3)3a)	Na2C2O4a)	Na5P3O10 b)	Na3PO4b)	NaF c)
#1	178.60	92.99	80.15	178.98	100.00	50.58	22.95	15.17	29.96
#2	35.40	33.46	50.19	37.74	27.62	39.68	62.64	44.74	78.21
#3	27.62	24.90	31.90	19.06	12.45	31.90	38.13	32.29	59.53

^†

a) C₀ = 2500 mg·L⁻¹. b) C₀ = 3000 mg·L⁻¹. c) C₀ = 2700 mg·L⁻¹.

Table S2 Comparison of the residual concentration of Congo red solution after adsorption by generated MgO with different morphologies in the absence and/or the presence of Na₂SiO₃

Sample	Placed location	Residual concentration of Congo red in different systems/(mg· L−1)
		Trapezoidal MgO (C0 = 300 mg·L−1)	Spherical MgO (C0 = 700 mg·L−1)	Spherical-like MgO (C0 = 2300 mg·L−1)	Nest-like MgO (C0 = 2300 mg·L−1)
Without Na2SiO3	#1	37.35	24.12	28.40	34.63
	#2	184.04	165.37	277.82	322.56
	#3	56.03	75.87	75.09	61.86
With Na2SiO3	#1	16.34	16.34	16.34	17.12
	#2	43.58	44.35	44.74	47.86
	#3	28.40	23.73	24.12	28.40

^†

Note: The procedures for preparation of MgO with different morphologies are as below.

① Trapezoidal MgO: In a typical procedure, 10.26 g of Mg(NO₃)₂·6H₂O was dissolved into 50 mL of double-deionized water, and the Mg(NO₃)₂ solution was then transferred into a 250 mL three-necked flask and heated to 70°C. Under vigorous stirring (ca. 800 r/min), 100 mL of 0.4 mol/L Na₂C₂O₄ solution without and/or with involvement of 0.1 g of Na₂SiO₃ was also heated to 70°C and poured into the Mg(NO₃)₂ solution in 10 s. The mixture was further stirred for 1.5 min and then maintained at a temperature of 50°C under static conditions for 1 h. After that, a white precipitate was collected, filtered off, and washed with double-deionized water and ethanol several times. The MgO sample was prepared by calcining the collected product in air from room temperature to 500°C followed by maintaining for 3 h.

② Spherical MgO: Specifically, 10.26 g of Mg(NO₃)₂·6H₂O was dissolved into 50 mL of deionized water followed by transferring into a 250 mL three-necked flask and heating to 70°C. Under the vigorous stirring (ca. 800 r/min), 100 mL of 0.4 mol/L Na₂CO₃ solution without and/or with involvement of 0.1 g of Na₂SiO₃ was also heated to 70°C and poured into the Mg(NO₃)₂ solution in 10 s. The mixture was further stirred for 3.0 min and then maintained at a temperature of 70°C under static conditions for 1 h. After that, the procedure was similar to the above.

③ Spherical-like MgO: The procedure was similar to that for preparation of spherical MgO. The only difference between them was the stirring time. Namely, after the mixture of Mg(NO₃)₂ and Na₂CO₃ solutions, the solution was stirred for 1.5 min rather than 3.0 min.

④ Nest-like MgO: The procedure was similar to that for preparation of spherical-like MgO except the preparation temperature was controlled at 80°C rather than 70°C.

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