Preparation method of titanium-doped iron phosphate
By using iron oxide to regulate acidity, the problems of complex process and high cost in the prior art are solved, and the industrial production of titanium-doped iron phosphate materials with good doping uniformity is achieved.
Patent Information
- Application Number
- CN202510518201.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-23
- Publication Date
- 2025-08-26
AI Technical Summary
The existing preparation methods of titanium-doped iron phosphate materials have problems such as complex processes, high costs, and uneven doping, which are difficult to meet the needs of industrial production.
Titanium doped iron phosphate material is prepared by mixing, precipitation, washing, drying and sintering steps.
It realizes the preparation of titanium-doped iron phosphate materials with simple process, low cost and uniform doping, which is suitable for industrial production.
Smart Images
Figure CN120534941A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to a method for preparing titanium-doped ferric phosphate, and belongs to the field of inorganic material synthesis. Background Art
[0002] Iron phosphate (FePO4) is an important inorganic material widely used in battery cathode materials, catalysts and other fields. However, the poor conductivity of pure iron phosphate limits its application in high-performance batteries and other fields. In order to improve the conductivity of iron phosphate, researchers have tried to modify iron phosphate by doping with other elements, among which titanium doping is an effective method. However, the preparation methods of existing titanium-doped iron phosphate materials have problems such as complex process, high cost, and uneven doping, which makes it difficult to meet the needs of industrial production. Summary of the Invention
[0003] The present invention provides a method for preparing titanium-doped ferric phosphate materials, using ferric oxide as a neutralizing agent to change the acidity of the reaction system and promote the reaction. This method has the advantages of simple process, low cost, and uniform doping.
[0004] A method for preparing a titanium-doped ferric phosphate material, the method comprising:
[0005] S1: mixing a titanium tetrachloride aqueous solution, a ferric chloride aqueous solution, and a phosphoric acid aqueous solution to obtain a mixed solution, adding iron oxide, and reacting to obtain a titanium-doped iron phosphate precursor mixed solution;
[0006] S2: separating the precursor mixture by precipitation to obtain a precipitate of titanium-doped ferric phosphate, washing, and drying to obtain a dry powder of titanium-doped ferric phosphate;
[0007] S3 sintering the dry powder of titanium-doped ferric phosphate to obtain titanium-doped ferric phosphate material.
[0008] Optionally, in step S1, the concentrations of the components in the mixed solution are: 0.01-0.1 mol / L for the titanium tetrachloride solution, 0.1-1.0 mol / L for the ferric chloride solution, and 0.12-1.2 mol / L for the phosphoric acid solution.
[0009] Optionally, in step S1, the volume of the mixed solution consisting of the titanium tetrachloride aqueous solution, the ferric chloride aqueous solution and the phosphoric acid aqueous solution is 1 to 100 L.
[0010] Optionally, in step S1, the molar ratio of ferric chloride to ferric oxide is 2:0.5-2.
[0011] Optionally, in step S1, the reaction temperature is 25°C to 100°C, and the reaction time is 10h to 72h.
[0012] Optionally, in step S2, the supernatant obtained by precipitation separation can be further used as the mother liquor of the reaction.
[0013] Optionally, in step S3, the sintering temperature is 400° C. to 900° C., and the sintering time is 1 hour to 20 hours.
[0014] As a preferred embodiment, the method for preparing the titanium-doped iron phosphate material comprises the following steps:
[0015] 1) Solution preparation: prepare a mixed solution of titanium tetrachloride solution, ferric chloride solution and phosphoric acid, wherein the concentration of the titanium tetrachloride solution is 0.01-0.1 mol / L, the concentration of the ferric chloride solution is 0.1-1.0 mol / L, and the concentration of the phosphoric acid solution is 0.12-1.2 mol / L.
[0016] 2) Mixing reaction: Stir the mixed solution evenly, add an appropriate amount of iron oxide, wherein the molar ratio of ferric chloride to iron oxide is 2:1, and then react at a temperature of 25° C. to 100° C. for 10 h to 72 h to obtain a titanium-doped iron phosphate precursor mixed solution.
[0017] 3) Separation by precipitation: The precursor mixture is separated by precipitation to obtain a precipitate of titanium-doped ferric phosphate. The separated supernatant can be used as the mother liquor of the reaction.
[0018] 4) Washing and drying: The precipitate is washed clean and then dried to obtain dry powder of titanium-doped ferric phosphate.
[0019] 5) Sintering treatment: sintering the dry powder at a temperature of 400° C. to 900° C. to obtain titanium-doped iron phosphate material.
[0020] The beneficial effects of this application include:
[0021] 1) The method for preparing titanium-doped ferric phosphate materials provided in this application uses titanium tetrachloride, ferric chloride, phosphoric acid, and ferric oxide as the main raw materials. The method cleverly utilizes ferric oxide as a neutralizing agent to regulate the acidity of the system and promote the formation of titanium-doped ferric phosphate. This method has the advantage of simple and readily available raw materials.
[0022] 2) The preparation method of the titanium-doped ferric phosphate material provided in this application has a simple process, does not require complex equipment and tedious steps, and is easy to industrialize and produce. It has the advantages of being simple and easy to operate.
[0023] 3) The preparation method of the titanium-doped ferric phosphate material provided in this application ensures uniform distribution of titanium ions in the ferric phosphate material by performing ion doping in the liquid phase, thereby improving the performance of the material and having the advantage of good doping uniformity. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] Figure 1 The SEM image and Fe, P, and Ti element distribution diagram of the titanium-doped ferric phosphate material obtained in Example 1 are shown.
[0025] Figure 2 This is the XRD pattern of the titanium-doped iron phosphate material obtained in Example 1. DETAILED DESCRIPTION
[0026] The present application is described in detail below with reference to embodiments, but the present application is not limited to these embodiments.
[0027] Unless otherwise specified, the raw materials in the examples of this application were purchased through commercial channels.
[0028] Unless otherwise specified, conventional methods were used for testing, and instrument settings were those recommended by the manufacturer.
[0029] The analysis method in the examples of this application is as follows:
[0030] The instrument used for XRD analysis was Miniflex 600.
[0031] The scanning electron microscope (SEM) was used as SU8010.
[0032] Example 1
[0033] 1) Prepare a mixed solution: The mixed solution components are 0.02 mol / L titanium tetrachloride, 0.5 mol / L ferric chloride, and 1.0 mol / L phosphoric acid, with a total volume of 1 L.
[0034] 2) Mixing reaction: The above mixed solution was stirred evenly, and 0.125 mol of iron oxide was added, wherein the molar ratio of ferric chloride to iron oxide was 2:1, and then reacted at 60° C. for 10 h to obtain a precursor solution of titanium-doped iron phosphate.
[0035] 3) Separation by precipitation: The precursor mixed solution is separated by precipitation to obtain a precipitate of titanium-doped iron phosphate.
[0036] 4) Washing and drying: The precipitate was washed with deionized water and then dried at 80° C. for 2 hours to obtain a dry powder of titanium-doped iron phosphate.
[0037] 5) Sintering treatment: sinter the dry powder at 400° C. for 2 hours to obtain titanium-doped iron phosphate material.
[0038] Example 2
[0039] 1) Prepare a mixed solution: The mixed solution components are 0.02 mol / L titanium tetrachloride, 0.5 mol / L ferric chloride, and 1.0 mol / L phosphoric acid, with a total volume of 1 L.
[0040] 2) Mixing reaction: The above mixed solution was stirred evenly, and 0.125 mol of iron oxide was added, wherein the molar ratio of ferric chloride to iron oxide was 2:1, and then reacted at 90° C. for 24 hours to obtain a precursor solution of titanium-doped iron phosphate.
[0041] 3) Separation by precipitation: The precursor mixed solution is separated by precipitation to obtain a precipitate of titanium-doped iron phosphate.
[0042] 4) Washing and drying: The precipitate was washed with deionized water and then dried at 80° C. for 2 hours to obtain a dry powder of titanium-doped iron phosphate.
[0043] 5) Sintering treatment: sinter the dry powder at 800° C. for 2 hours to obtain titanium-doped iron phosphate material.
[0044] The titanium-doped ferric phosphate materials prepared in the above examples were characterized and analyzed, with the titanium-doped ferric phosphate material prepared in Example 1 being used as a typical example. Figure 1 From its SEM image and Fe, P, and Ti element distribution diagram, it can be seen that the particle size is uniform and the Ti element is evenly distributed. Figure 2 From its XRD pattern, it can be seen that the structure is fully developed without other impurities.
[0045] Comparative Example 1
[0046] The operation is the same as in Example 1, except that iron oxide is not used.
[0047] When iron oxide is not used as a neutralizing agent, the solution cannot generate an iron phosphate precursor, and only titanium tetrachloride is hydrolyzed to generate amorphous titanium dioxide, and the reaction does not proceed.
[0048] Comparative Example 2
[0049] The operation is the same as in Example 1, except that calcium oxide is used instead of iron oxide, and the amount used is also 0.25 mol.
[0050] Since calcium oxide has a higher alkalinity than iron oxide, the reaction is rapid and uncontrollable, and impurity ions are introduced, making it impossible to obtain the desired target product.
[0051] The above descriptions are merely a few embodiments of the present application and do not constitute any form of limitation to the present application. Although the present application discloses the preferred embodiments as above, they are not intended to limit the present application. Any technical personnel familiar with the present profession, without departing from the scope of the technical solution of the present application, using the technical content disclosed above to make slight changes or modifications are equivalent to equivalent implementation cases and fall within the scope of the technical solution.
Claims
1. A method for preparing a titanium-doped ferric phosphate material, characterized in that: The preparation method comprises: S1: mixing a titanium tetrachloride aqueous solution, a ferric chloride aqueous solution, and a phosphoric acid aqueous solution to obtain a mixed solution, adding iron oxide, and reacting to obtain a titanium-doped iron phosphate precursor mixed solution; S2: separating the precursor mixture by precipitation to obtain a precipitate of titanium-doped ferric phosphate, washing, and drying to obtain a dry powder of titanium-doped ferric phosphate; S3 sintering the dry powder of titanium-doped ferric phosphate to obtain titanium-doped ferric phosphate material.
2. The preparation method according to claim 1, characterized in that In step S1, the concentrations of the components in the mixed solution are as follows: the concentration of the titanium tetrachloride solution is 0.01-0.1 mol / L, the concentration of the ferric chloride solution is 0.1-1.0 mol / L, and the concentration of the phosphoric acid solution is 0.12-1.2 mol / L.
3. The preparation method according to claim 1, characterized in that In step S1, the volume of the mixed solution consisting of the titanium tetrachloride aqueous solution, the ferric chloride aqueous solution and the phosphoric acid aqueous solution is 1 to 100 L.
4. The preparation method according to claim 1, characterized in that In step S1, the molar ratio of ferric chloride to ferric oxide is 2:0.5-2.
5. The preparation method according to claim 1, characterized in that In step S1, the reaction temperature is 25° C. to 100° C., and the reaction time is 10 h to 72 h.
6. The preparation method according to claim 1, characterized in that In step S2, the supernatant obtained by precipitation separation can be used as the mother liquor for the reaction.
7. The preparation method according to claim 1, characterized in that In step S3, the sintering temperature is 400° C. to 900° C., and the sintering time is 1 hour to 20 hours.