A kind of preparation method of inorganic phosphate crystal material

A technology of inorganic phosphate and crystal materials, which is applied in the direction of molecular sieves, alkali-exchanged phosphates, and molecular sieve-specific aluminum phosphates. Improve the effect of the preparation process

Active Publication Date: 2015-09-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the outstanding disadvantage of most inorganic ion exchangers is that they are very sensitive to acids and cannot be used under acidic conditions.
[0017] 1) A large amount of phosphoric acid and hydrogen fluoride are used, which are likely to cause environmental pollution, especially hydrofluoric acid, which is highly corrosive and volatile, is likely to cause environmental problems and safety problems during the amplification synthesis;
[0018] 2) Ethylenediamine is used as a template, which is toxic and volatile, and should not be used in large-scale production;
[0019] 3) It needs to be crystallized at 150-180°C for 5-7 days, the crystallization temperature is high, the time is long, and the energy consumption is large, which is not conducive to large-scale industrial production

Method used

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  • A kind of preparation method of inorganic phosphate crystal material
  • A kind of preparation method of inorganic phosphate crystal material
  • A kind of preparation method of inorganic phosphate crystal material

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preparation example Construction

[0038] The above-mentioned inorganic phosphate crystal material adopts a hydrothermal synthesis method, and the preparation method comprises the following steps:

[0039] a) Mix the aluminum source, sodium phosphate and / or lithium phosphate, fluoride, and deionized water in a molar ratio of 3-5:6-10:6-10:20-100, and fully stir to form an initial condensation glue;

[0040] b) Use sodium hydroxide solution and / or lithium hydroxide solution to adjust the pH value of the initial gel obtained in step a) to 8-9; preferably the pH value is 8-8.5, and the recommended pH value is greater than 8.5 and less than or equal to 9, The preferred pH value is greater than or equal to 8.2 and less than 8.5.

[0041] c) Crystallize the gel obtained in step b) under hydrothermal conditions to obtain the inorganic phosphate crystal material; the crystallization temperature is 120-160° C., and the crystallization time is 12-90 hours; preferably, the crystallization temperature The temperature is ...

Embodiment 1

[0059] Mix the aluminum source, sodium phosphate and / or lithium phosphate, fluoride, and deionized water in a certain proportion, stir at room temperature for 0.5 hours to form an initial gel, add dropwise sodium hydroxide solution and / or lithium hydroxide solution, adjust its pH value to a certain value in 8-9, and stir for 1 hour. The obtained gel was transferred into a stainless steel kettle equipped with polytetrafluoroethylene lining, placed in an oven for crystallization at a certain temperature for a period of time, and the obtained product was washed three times with deionized water to obtain a white crystal sample. The corresponding relationship between the sample number and the ratio of raw materials in the initial gel, the sodium hydroxide solution and / or lithium hydroxide solution used to adjust the pH value of the initial gel, the adjusted pH value, the crystallization temperature, and the crystallization time is as follows: Table 1 shows.

[0060] Table 1: Corr...

Embodiment 2

[0066] Elemental analysis of the samples NAP-1, LAP-1, LNAP-6, LNAP-7, LNAP-8, LNAP-11, LNAP-12, and LNAP-13 prepared in Example 1, elements with an atomic number greater than 8 Adopt Philips Magix X-ray fluorescence spectrometer to measure the element composition of sample, the content of Li in the sample adopts IRIS Advantage full-frequency direct-reading plasma spectrometer (ICP) to measure, and the results are shown in Table 2 and figure 1 .

[0067] Table 2: Analysis results of sample composition elements

[0068] Sample serial number

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Abstract

An inorganic phosphatic crystal material has a two-dimension electronegativity skeleton structure formed by four elements of aluminium, oxygen, phosphor and fluorine. Sodion and / or lithium ion is disposed in the interlayer and pore canals of the two-dimension electronegativity skeleton. The expression of the material is Na5-XLiXAl3(PO4)6F6. A preparation method of the material provided by the invention comprises the following steps of: mixing an aluminium source, phosphatic of sodium and / or phosphatic of lithium, fluoride and deionized water according to the mol ratio of 3-5: 6-10: 6-10: 20-100, and stirring to form an initial gel; adjusting pH value of the initial gel obtained from step a to 8-9 by the use of a sodium hydroxide solution and / or a lithium hydroxide solution; and hydrothermally crystallizing the gel obtained from step b at the crystallization temperature of 120-160 DEG C for 12-90 hours so as to obtain the inorganic phosphatic crystal material. By the adoption of the inorganic phosphatic crystal material provided by the invention, the performance of solid electrolyte and an inorganic ion exchanger is raised.

Description

technical field [0001] The invention relates to a preparation method of an inorganic phosphate crystal material. Background technique [0002] Since Wilson et al first reported the synthesis of aluminum phosphate series molecular sieves in 1982, phosphates have always been a research hotspot, especially mixed metal phosphates containing transition metals. At present, the research in this field is deepening day by day, and mixed metal phosphate inorganic materials with new composition, new structure and new properties have come out one after another. Among the many phosphate crystal compounds that have been reported, metal ions often show different valence states and coordination numbers in the crystal, and the skeleton structure unit of the crystal can be either in the form of oxide, or in the form of oxyfluoride or in the form of Both forms coexist. Therefore, mixed metal phosphate inorganic materials have rich crystallographic structures and unique physical properties, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/06C01B39/54
Inventor 刘中民张莹田鹏许磊苏雄周游樊栋
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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