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Preparation of Magnesium Hydroxide from Ammonium Chloride by Circulation Method

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Preparation of Magnesium Hydroxide from Ammonium Chloride by Circulation Method Asian Journal of Chemistry; Vol. 25, No. 4 (2013), 1807-1810 http://dx.doi.org/10.14233/ajchem.2013.13155 Preparation of Magnesium Hydroxide from Ammonium Chloride by Circulation Method * YANG LI , JANMING DAN and HONGLING LI School of Chemistry and Chemical Engineering, Shihezi University, Shihezi 832003, P.R. China *Corresponding author: E-mail: [email protected] (Received: 1 December 2011; Accepted: 3 October 2012) AJC-12224 In this paper, the technological conditions for preparation of magnesium hydroxide from ammonium chloride by circulation method are presented. The ammonia gas was prepared via treating carbide residue with ammonium chloride and subsequently passed into the magnesium chloride solution to form the magnesium hydroxide and ammonium chloride. The ammonium chloride was recycled consequently with precipitation separation of the magnesium hydroxide. Key facts on the productivity of magnesium hydroxide were investigated. The best condition is as follows: the molar ratio of ammonium chloride to magnesium chloride is 4.5, the magnesium is 1.5 mol/L, the reaction time is 1 h, the reaction temperature is 25 ºC and the aging time is 2 h. The productivity of magnesium hydroxide can obtain 89.10 % with a purity of above 99.12 % and the cycling rate of ammonium chloride is 69.47 % on this condition. The XRD and SEM were used to characterize the powder products. The results indicate the sheet-shaped magnesium hydroxides with 1 µm diameter were obtained. Key Words: Carbide residue, Lake magnesium chloride, Magnesium hydroxide, Calcium chloride. INTRODUCTION green flame retardants, which can prevent it from being exported as the raw material. Consequently, we propose to Magnesium hydroxide has been widely used in fuel gas produce Mg(OH)2 via carbide residue reacts with MgCl2 of desulfurization process, waste water treatment process and the lake. On the one hand, this technique can diminish the 1, 2 food industry as an important inorganic material . It is also a excess of these two substances. On the other hand, such method necessary starting material of magnesium chloride as well as is feasible and can produce satisfactory social benefits, many other industrial magnesium compounds. Compare with economic benefits and an obvious environmental protection Al(OH)3, Mg(OH)2 has the merit of higher decomposition benefits. temperature, better thermostability and better flame retardancy. Besides, the small size of Mg(OH)2 favours its application as EXPERIMENTAL a new type of green environmental-friendly flame retardants in the polymer industry around the world recently. Experiment principle: This study shows the preparation Carbide residue is the main production waste of acetylene, of Mg(OH)2 from ammonium chloride by circulation method. which prepared through calcium carbide method and is mostly The ammonia gas was generated via carbide residue reaction composed of calcium hydroxide, as nearly above 85 wt %. It with NH4Cl and subsequently it was passed into the MgCl2 has been pointed out that 1 ton calcium carbide will yield 1.2- solution and formed the Mg(OH)2 and NH4Cl. The NH4Cl can 1.5 tons of carbide residue3,4. Generally the large amount of be recycled with precipitation separation of the Mg(OH)2. carbide residue has a rather poor reputation as its soil exhausting Moreover, the filtrate has the applicability in preparation of and low recycling ratio. A little carbide residue has been used technical grade CaCl2. in construction materials. However no one reports its application Ca(OH)2 + 2NH4Cl CaCl2 + 2NH3↑ + 2H2O in Mg(OH)2 production. MgCl2 + 2NH3 + 2H2O → Mg(OH)2↓ + 2NH4Cl As is well known, the lake/sea magnesium resources in Carbide residue is the industry waste by Xinjiang Tianye China are abundant5. But the magnesium salts have always Group which manufactures the acetylene gas. The raw material been treated as the by-product of other salts. It is urgent to was preheated at 100 ºC for 2 h. This procedure can remove find a new way for large-scale application of magnesium the H2S gas, H3P gas and residual acetylene gas from the raw resources for its low utilization ratio. One solution is producing material, keeping the purity of the NH3 gas. MgCl2 comes from Mg(OH)2 to meet the increasing requirements as the clean the byproduct of potash produced by Golmud salina in 1808 Li et al. Asian J. Chem. Qinghai. The raw material was dissolved and recrystallized concentration of MgCl2 solution, but the phenomena are not for 2-3 times. obvious. The minimum productivity of Mg(OH)2 is higher than Experiment details: The excessive carbide residue was 74 % and still has little change. Because the NH3 gas will reactive with NH4Cl at 85-95 ºC and the generated NH3 gas more produced and prompt the reaction to the positive orien- was passed into MgCl2 solution with stirring. The white tation. However the productivity of Mg(OH)2 does not change deposited material was Mg(OH)2. After centrifuging and much when the molar ratio of NH4Cl to MgCl2 is above 4.5. – washing the Cl ion was eliminated (confirmed by AgNO3 This is because most of the NH3 gas cannot take the next reac- solution). Then the Mg(OH)2 is dried at 90 ºC and grounded. tion and form the NH3 -NHCl4 buffer system in the solution at The key facts such as the molar ratio of NH4Cl to MgCl2, the higher NH4Cl to MgCl2 ratio. Besides, the NH3 -NH4Cl buffer solution concentration of MgCl2, the reaction time, the reaction is favour of dissolving for Mg(OH)2. When the dissolution temperature and the aging time on the productivity of Mg(OH)2 reaches to balance, the productivity of Mg(OH)2 keeps un- -1 were investigated. changed at a concentration of 1.5 mol L of MgCl2 solution. Then the concentration of MgCl2 solution is chosen as 1.5 RESULTS AND DISCUSSION mol L-1 in the next step. Molar ratio of NH4Cl to MgCl2: In this section, the -1 90 carbide residue is excessive, the MgCl2 is 2.0 mol L , the reaction time is 1 h, the reaction temperature is room tempe- 88 rature and the aging time is 2.5 h. The Mg(OH)2 is prepared 86 via different molar ratio of NHCl4 to MgCl2. Fig. 1 shows the ) % productivity of Mg(OH)2 under these conditions. It is found ( 84 d l the productivity of Mg(OH)2 increased with increasing the e i y 82 molar ratio of NH4Cl to MgCl2. Because the NH3 gas will more 2 ) produced and prompt the reaction to the positive orientation. H O 80 ( However the productivity of Mg(OH)2 does not change much g M 78 when the molar ratio of NHCl4 to MgCl2 is above 4.5. This is because most of the NH3 gas cannot take the next reaction and 76 form the NH3 -NH4Cl buffer system in the solution at higher 74 NH4Cl to MgCl2 ratio. Besides, the NH3 -NH4Cl buffer is favour 0.5 1.0 1.5 2.0 2.5 of dissolving for Mg(OH)2. When the dissolution reaches to –1 balance, the productivity of Mg(OH)2 keeps unchanged. So MgCl 2 concentration (mol L ) the molar ration of NH4Cl to MgCl2 is chosen of 4.5. Fig. 2. Effect of productive rate of magnesium hydroxide by the concentration of magnesium chloride 90 Reaction time: In this experiment, the carbide residue is 88 excessive, the molar ration of NH4Cl to MgCl2 is chosen of -1 86 4.5, the MgCl2 is 1.5 mol L , the reaction temperature is room 84 temperature and the aging time is 2.5 h. The productivity of ) % Mg(OH)2 is evaluated by different reaction time. Fig. 3 shows ( 82 d l that the reaction is more adequate and the productivity of e i 80 y 2 Mg(OH)2 is increased by elongation the reaction time. The ) H 78 maximum of Mg(OH)2 is produced at the reaction time of 1 h. O ( g 76 M 74 90 72 85 70 80 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 ) % Rate of ammonium chloride to magnesium chloride ( 75 d l e Fig. 1. Effect of productive rate of magnesium hydroxide by the mol ratio i y 70 of ammonium chloride and magnesium chloride 2 ) H 65 O ( Concentration of MgCl2 solution: In this case, the g M 60 carbide residue is excessive, the molar ration of NH4Cl to MgCl2 is chosen of 4.5, the reaction time is 1 h, the reaction 55 temperature is room temperature and the aging time is 2.5 h. 50 The Mg(OH)2 is prepared by different concentration of MgCl2 10 20 30 40 50 60 70 80 solution reaction with NH3 gas. Fig. 2 shows the productivity Reaction time (min) of Mg(OH)2 under these conditions. It is confirmed that the Fig. 3. Effect of productive rate of magnesium hydroxide by the reaction productivity of Mg(OH)2 is increased with increasing the time Vol. 25, No. 4 (2013) Preparation of Magnesium Hydroxide from Ammonium Chloride by Circulation Method 1809 Reaction temperature: In this study, the carbide residue reaction time of 1 h and the aging time of 2 h. The Mg(OH)2 -1 is excessive, the MgCl2 is 1.5 mol L , the reaction time is 1 h, is prepared at different reaction temperature. A replication the molar ration of NH4Cl to MgCl2 is chosen of 4.5 and the experiment result is showed in Table-1. aging time is 2.5 h.
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