Method for preparing manganese phosphate material

A technology of manganese phosphate and phosphate, which is applied in the field of inorganic preparation of phosphate functional materials, can solve the problems of complex process, small product quantity per batch, high energy consumption under high temperature and high pressure, and achieve simple process, less production process, single The effect of high secondary yield

Inactive Publication Date: 2010-11-24
HUAZHONG AGRI UNIV
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Problems solved by technology

The synthesis of manganese phosphate monohydrate by the reaction of trivalent manganese nitrate and phosphoric acid is complicated, and trivalent manganese nitrate must first be prepared; high-temperature pyrolysis of divalent manganese oxalate is used to obtain Mn 3 o 4 , then Mn 3 o 4 、H 3 PO 4 Manganese phosphate monohydrate (Lightfoot P, Cheetham A K, Sleight A W. Inorganic Chemistry, 1987, 26, 3544-3541) can be prepared by reacting at 200°C for 3 days. The process is complex and simple The amount of secondary products is small, and high temperature and high pressure consume a lot of energy; MnPO is synthesized by hydrothermal reaction at 150°C for 12 or 24 hours with manganese nitrate hexah

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  • Method for preparing manganese phosphate material
  • Method for preparing manganese phosphate material
  • Method for preparing manganese phosphate material

Examples

Experimental program
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Embodiment 1

[0040] Embodiment 1: Mn(H 2 PO 4 ) 2 Solution reflux reaction to prepare phosphomanite [Mn(HPO 4 ) 2 (PO 4 ) 2 (H 2 O)]

[0041] Weigh 30mmol Mn(H 2 PO 4 ) 2 2H 2 O in the Erlenmeyer flask, add 100ml distilled water and be mixed with the Mn(H of 0.3mol / L 2 PO 4 ) 2 2H 2 O solution, placed in a heat-collecting constant temperature heating magnetic stirrer (its stirring speed is 30 rpm) refluxed at 100 ° C for 12 hours, took out and filtered after natural cooling, and the reaction product was washed with de-distilled water or deionized water until the conductivity of the filtrate was Just less than 30μS / cm. The product was dried in an oven at 60°C, and its crystal structure was characterized by X-ray diffractometer (XRD) (see figure 1 ), Fourier transform infrared spectroscopy (FTIR) to analyze its main functional groups (see figure 2 ) and scanning electron microscopy to characterize its morphology (see image 3 ), the result showed that the obtained product ...

Embodiment 2

[0043] Embodiment 2: with Mn (H 2 PO 4 ) 2Synthesis of manganese phosphate monohydrate (MnPO 4 ·H 2 O)

[0044] Weigh 30mmol Mn(H 2 PO 4 ) 2 2H 2 O in the Erlenmeyer flask, add 100ml distilled water and be mixed with the Mn(H of 0.3mol / L 2 PO 4 ) 2 2H 2 O solution, further add 80 and 120mmol concentrated hydrochloric acid (concentration ≥ 36%) respectively, then add 60mmol NaClO solution, place the collector type constant temperature heating magnetic stirrer (its stirring speed is 30 rpm) at 100 ℃ Reflux for 12 hours, take out and cool naturally, then filter, and wash the reaction product with deionized water until the conductivity of the filtrate is less than 30 μS / cm. The product was dried in an oven at 60°C, and its crystal structure was characterized by XRD (see Figure 7 ), FTIR analysis of its main functional groups (see figure 2 ) and scanning electron microscopy to characterize its morphology, the results showed that the product was manganese phosphate m...

Embodiment 3

[0045] Embodiment 3: with MnCl 2 Synthesis of manganite and manganese phosphate monohydrate as sources of divalent manganese

[0046] Weigh 30mmol MnCl 2 4H 2 O and 60mmol NaClO solution in a conical flask, add 100mL distilled water to prepare a solution, add 30, 60, 90, 135 and 180mmol H 3 PO 4 Solution, placed in a heat-collecting constant temperature heating magnetic stirrer (its stirring speed is 30 rpm) at 60, 80 and 100 ° C for reflux reaction for 12 hours, took out and filtered after natural cooling, and the reaction product was washed with deionized water until the filtrate conductivity Just less than 30μS / cm. The product was dried in an oven at 60°C, its crystal structure was characterized by XRD, and its main functional groups were analyzed by FTIR. The results showed that adding 30 mmol H 3 PO 4 solution, the products obtained at the three reaction temperatures are all pyrosite, and adding H 3 PO 4 The solution amounts are 60, 90, 135 and 180 mmol, and the p...

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Abstract

The invention belongs to the technical field of compound preparation, and particularly relates to a method for preparing a manganese phosphate material. The method is characterized in that: the method can synthesize a large amount of single or doped hureaulite type phosphate and manganese phosphate monohydrate (MnPO4.H2O) with good crystallinity at one time under a normal-pressure heating reflux condition. The method comprises the following steps of: preparing Mn5(HPO4)2(PO4)2(H2O) with reflux by adopting mixed solution of bivalent manganese salt and soluble phosphate or dihydric phosphate or phosphoric acid and controlling pH, temperature and time; preparing Mn5-xMx(HPO4)2(PO4)2(H2O) with reflux by mixing other soluble bivalent transition metal salt into the bivalent manganese salt and controlling pH, temperature and time, wherein M is Co, Fe, Ni, Cu and Zn and the like and x is more than or equal to 0 and less than 5.0; and preparing MnPO4.H2O with reflux reaction by adopting mixed solution of bivalent manganese salt and soluble phosphate or dihydric phosphate or phosphoric acid, adding NaClO solution and controlling solution acidity, temperature to be 40 to 100 DEG C and time for 1 hour to 7 days. The method has the advantages of mild, simple and easily controlled conditions, low energy consumption, low pollution and high single yield, and can be used for preparation of optics, magnetics, catalysts and chemical power supply materials.

Description

technical field [0001] The invention relates to a preparation method of manganese phosphate material. Described manganese phosphate is single or doped phosphatite type phosphate and manganese phosphate monohydrate (MnPO 4 ·H 2 O). The present invention is particularly suitable for synthesizing well-crystallized single or doped strengite-type phosphate or manganese phosphate monohydrate (MnPO 4 ·H 2 O), so that a large amount of metal phosphates can be synthesized at one time under simple conditions, which belongs to the inorganic preparation method of phosphate functional materials. Background technique [0002] Transition metal phosphate pore structure compounds have rich structural chemical characteristics and excellent physical and chemical properties, showing good application prospects in the field of modern industry, and are one of the hotspots of international advanced materials research. Phosphatite structural metal phosphate has the advantages of good thermal st...

Claims

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Application Information

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IPC IPC(8): C01B25/37
Inventor 邱国红殷辉刘凡冯雄汉谭文峰刘名茗陈秀华
Owner HUAZHONG AGRI UNIV
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