CN102180455A

CN102180455A - Method for preparing sodium hydrogen zirconium phosphate powder

Info

Publication number: CN102180455A
Application number: CN 201110134080
Authority: CN
Inventors: 王晶
Original assignee: Dalian Jiaotong University
Current assignee: Dalian Jiaotong University
Priority date: 2011-05-23
Filing date: 2011-05-23
Publication date: 2011-09-14

Abstract

The invention discloses a method for preparing sodium hydrogen zirconium phosphate NaZr2(PO4)3 powder. The method is characterized by comprising the following steps: preparing 0.06mol/l zirconium oxychloride solution, adding sodium polyphosphate in the solution according to the mass ratio of zirconium oxychloride solution to sodium polyphosphate of 2:5-4:5, preparing aqueous solution according to a process formula, adding in a high-pressure reactor with compactedness of 60%-80%, heating to 140-200 DEG C while stirring, keeping heat balance at the temperature for 5 hours, cooling to room temperature after reaction is finished, and filtering and washing reactants and finally drying at low temperature. The preparation method has simple process, the synthesized NaZr2(PO4)3 powder has high purity, and uniform powder granularity and is shaped into a spherical clew. The obtained NaZr2(PO4)3 powder can be applied to the field of the preparation of novel antibacterial materials, low-expansion ceramic materials, fast ion conductors, loaded noble metal catalyst materials and the like.

Description

Sodium zirconium phosphate powder preparation method

Technical field

The present invention relates to phosphorus and compound thereof, relate in particular to the preparation of the halogenide or the oxyhalogenide of phosphorus.

Background technology

As everyone knows, early stage at phosphate industry, people prepare the sodium zirconium phosphate powder material with solid reaction process.To phase early 1990s, the more gentle synthetic methods of condition such as sol-gel method and hydrothermal method had appearred successively afterwards.After this, hydrothermal synthesis method becomes the first-selection of synthetic this type of material.When Hydrothermal Preparation sodium zirconium phosphate powder material, the raw material of employing is zirconates, phosphoric acid and sodium salt substantially, by adding mineralizer, control hydrothermal temperature, hydro-thermal synthesizing zirconium phosphate sodium powder body material at a lower temperature.It is longer that but the relevant report that just can find at present, the problem that these methods exist are that the phosphoric acid consumption reaches the used time of preparation greatly.

Summary of the invention

The objective of the invention is to study a kind of hydrothermal synthesis method, within a short period of time and the condition that does not need to add a large amount of phosphoric acid and mineralizer get off to prepare the sodium zirconium phosphate powder material.

Technical solution of the present invention is achieved in that

A kind of sodium zirconium phosphate NaZr ₂(po ₄) ₃Powder preparation method is characterized in that comprising the steps:

(1) preparation 0.06～0.12mol/l chlorine oxygen zirconium ZrOCl ₂Solution is to wherein adding sodium polyphosphate and basic zirconium chloride ZrOCl ₂Mass ratio was controlled at 2: 5～4: 5;

(2) with sodium polyphosphate, basic zirconium chloride ZrOCl ₂And water joins in the autoclave after mixing by formula rate, and the compactedness of reactor is heated to 140～200 ℃ under stirring between 60%～80%, keeps the heat balance under this temperature and is incubated more than the 5h, and reaction finishes, and is cooled to room temperature;

(3) the synthetic product is filtered, washing and cryodrying obtain sodium zirconium phosphate powder.Compared with prior art, advantage of the present invention mainly shows:

1, the sodium zirconium phosphate powder epigranular of preparing, particle diameter is little, and the pattern rule is single.

2, raw materials used cheap, wherein a kind of raw material of sodium polyphosphate is adopted in phosphorus source and sodium source.

3, preparation technology is simple, and the reaction times is short.Pollution-free, energy consumption is low, environmental friendliness.

4, by hydrothermal treatment process, can obtain size-grade distribution and concentrate between 1～10 μ m the controllable sodium zirconium phosphate powder of granularity and pattern.

Description of drawings

Drawings attached 6 width of cloth of the present invention, wherein:

Fig. 1 is the SEM figure of (a) 5h of different hydro-thermal times, (b) 12h, (c) 24h powder;

Fig. 2 is the diameter of particle distribution plan of Fig. 1 different time;

Fig. 3 is different concns (a) 0.06mol/l, (b) 0.09mol/l, (c) 0.12mol/l ZrOCl ₂The SEM figure of the powder of add-on;

Fig. 4 is Fig. 3 different concns ZrOCl ₂The diameter of particle distribution plan;

Fig. 5 is the powder SEM figure of 160 ℃ of different hydrothermal temperatures (a), (b) 180 ℃, (c) 200 ℃;

Fig. 6 is the diameter of particle distribution plan of Fig. 5 differing temps.

Embodiment

The zirconium oxychloride solution of embodiment 1, configuration 0.06mol/l, to wherein adding sodium polyphosphate, sodium polyphosphate and basic zirconium chloride mass ratio were controlled at 2: 5,180 ℃ of hydrothermal temperatures, the hydro-thermal time is respectively 5h, 12h, 24h.Can obtain powder as shown in Figure 1, 2.

The zirconium oxychloride solution of embodiment 2, configuration 0.06mol/l, to wherein adding sodium polyphosphate, sodium polyphosphate and basic zirconium chloride mass ratio were controlled at 2: 5,160 ℃ of hydrothermal temperatures, hydro-thermal time 24h.Can obtain powder shown in Fig. 3 (a).

The zirconium oxychloride solution of embodiment 3, configuration 0.09mol/l, to wherein adding sodium polyphosphate, sodium polyphosphate and basic zirconium chloride mol ratio were controlled at 3: 5,160 ℃ of hydrothermal temperatures, hydro-thermal time 24h.Can obtain powder shown in Fig. 3 (b).

The zirconium oxychloride solution of embodiment 4, configuration 0.12mol/l, to wherein adding sodium polyphosphate, sodium polyphosphate and basic zirconium chloride mol ratio were controlled at 4: 5,160 ℃ of hydrothermal temperatures, hydro-thermal time 24h.Can obtain powder shown in Fig. 3 (c).

The zirconium oxychloride solution of embodiment 5, configuration 0.06mol/l, to wherein adding sodium polyphosphate, sodium polyphosphate and zirconium oxychloride mass ratio were controlled at 2: 5, and hydrothermal temperature is respectively 160 ℃, and 180 ℃, 200 ℃, hydro-thermal time 24h.Can obtain powder shown in Fig. 5 (c).

Claims

1. sodium zirconium phosphate NaZr ₂(po ₄) ₃Powder preparation method is characterized in that comprising the steps:

(1) preparation 0.06～0.12mol/l basic zirconium chloride ZrOCl ₂Solution is to wherein adding sodium polyphosphate and basic zirconium chloride ZrOCl ₂Mass ratio was controlled at 2: 5～4: 5;

(2) with sodium polyphosphate, basic zirconium chloride ZrOCl ₂And water joins in the autoclave after mixing by formula rate, and the compactedness of reactor is being heated between 140～200 ℃ under stirring between 60%～80%, keeps the heat balance under this temperature and is incubated more than the 5h, and reaction finishes, and is cooled to room temperature;

(3) the synthetic product is filtered, washing and cryodrying obtain sodium zirconium phosphate powder.