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Synthesis of Phosphates via Solid-State Reaction and Study on Their Properties

Author: FanYanJin
Tutor: WuWenWei
School: Guangxi University
Course: Applied Chemistry
Keywords: Solid state reaction Titanium phosphate ammonium Esterification reaction UV-shielding Ammonium phosphate, manganese Thermal decomposition
CLC: TB383.1
Type: Master's thesis
Year: 2008
Downloads: 169
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Abstract


Solid state reaction method has no solvent, selective, high yield, low energy consumption, simple operation, and many other advantages, has become a new way of synthesis of inorganic nanomaterials. The synthesized by solid state reaction method (NH 4 ) 2 Ti (PO 4 ) 2 , Ce 1-x the Ti x P 2 the O 7 and the NH 4 MnPO 4 · H 2 O series of new inorganic nano powder. Simultaneously the (NH 4 ) 2 Ti (PO 4 ) 2 catalytic synthesis of acetate, n-butyl NH < sub> 4 MnPO 4 · H 2 O nanocrystals thermal decomposition kinetics was studied. This research paper is divided into six chapters: Chapter 1 introduces the characteristics of synthetic nanomaterials research progress. Summarized the solid phase reaction prepared synthetic nano inorganic material advantages of inorganic materials. Chapter II titanium phosphate ammonium Low Temperature Synthesis and Characterization of Ti (SO 4 ) 2 (NH 4 ) 3 PO 4 · 3H 2 O as raw materials, by solid phase reaction prepared (NH , 4 ) 2 < / sub> Ti (PO 4 ) 2 . TG / DTA, IR, XRD, UV and TEM product and its pyrolysis products were characterized. The results showed that: 80 ℃ incubated 5h amorphous (NH 4 ) 2 Ti (PO 4 ) 2 < / sub> powder, the average particle size of about 40nm; product, well crystallized after calcination at 900 ℃, space group Pa3 (205), with an average particle size of about 23nm TiP 2 O 7 crystal. Product and its thermal decomposition products have high UV absorption ability. Chapter titanium phosphate ammonium Catalytic Synthesis of n-butyl ammonium nanoscale titanium phosphate catalyst, glacial acetic acid and n-butanol for the synthesis of n-butyl acetate. By uniform design method to determine the optimal experimental conditions, the results showed that: when the molar ratio of acid to alcohol 1.92:1, reaction time 5.1h, and the amount of catalyst was 1.4g (mass%, 7.8%) when the, esterification rate up to 0.99. The catalyst preparation process is simple, reusable, almost no corrosion and pollution, is a rather a catalyst for industrial application development prospects. The the Chapter Ce 1-x the Ti x P 2 O 7 powders Low Temperature Synthesis its UV-shielding properties of Na 4 P 2 O 7 · 10H 2 O, Ti (SO 4 ) 2 , Ce (SO 4 ) 2 · 4H 2 O as raw material, the use of solid state reaction in the synthesis of Ce 1-x Ti x P 2 O 7 (x = 0, 0.2,0.5,0.7,0.9, and 1.0). By XRD, TG / DTA, UV and TEM product and its thermal decomposition products were characterized. The results show that the products are obtained in the 100 ° C for amorphous nano powder, and having a good UV light-shielding effect. , CeP 2 O 7 UV shading effect of Ce, but amorphous 0.8 Ti 0.2 < / sub> P 2 O 7 than CeP 2 O 7 stable to higher temperatures. Therefore, through to CeP 2 O 7 in Ti CeP 2 O 7 amorphous state stability. This improved stability so that these amorphous pyrophosphates can be applied not only in cosmetics and paints, the same also applies to the application of the plastic film. Chapter NH 4 MnPO 4 · H 2 O the Low Temperature Synthesis and Characterization of MnSO 4 · H 2 O and (NH 4 ) 3 PO 4 · 3H 2 O as raw materials, grinding the reaction mixture at room temperature, subjected to solid phase reaction, and then the mixture was allowed to stand at room temperature for aging for 12h, followed by water to wash away the soluble inorganic salts in the mixture, after the precipitate was dried at 60 ℃, that was NH 4 MnPO 4 · H 2 O nanocrystals. XRD, TG / DTA, IR, UV and SEM product characterization. The results show that the resulting product is well crystallized, the space group of Pmnm (59) orthogonal NH MnPO 4 4 · H 2 O The average particle size of about 45nm; the MnPO 4 4 H 2 O at 600 ° C, 900 ° C calcined NH 3h get space monoclinic group C2 / m (12) (Monclinic) Mn 2 P 2 O 7 . Their particle size of approximately 22nm and 61 nm. Chapter NH 4 MnPO 4 · H 2 O thermal decomposition kinetics study using thermogravimetric differential thermal method analysis of NH 4 the MnPO 4 · H 2 O the thermal decomposition process, the results show that: the NH 4 MnPO 4 · H 2 O below 600 ℃ thermal decomposition in two steps, the first step for the crystallization of water and ammonia desorption, the second step is MnHPO 4 < / sub> dehydrating condensing the synthetic Mn 2 P 2 O 7 . The decomposition process activation energy (E) and frequency factor (A) and thermal decomposition mechanism function: reaction (1) E = 105.7 kJ / mol and lnA = 24.9s -1 , G, (a) = (1-a) -1 -1; reaction (2) E = 113.6 kJ / mol, lnA of = 14.5s -1 , G (a) = [1 / (1-a) 1/3 -1] 2 .

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