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A method for batch preparation of low-cost carbon-coated titanium phosphate compounds

A technology for carbon-coated phosphoric acid and titanium compounds is applied in the field of titanium phosphate compound ceramic powder, and the high-temperature solid-phase synthesis reaction method prepares carbon-coated titanium phosphate compound powder, which can solve the problem of difficulty in realizing large-scale production and complex production process. , impure products and other problems, to achieve the effect of good application prospects, simple synthesis process and cheap raw materials

Active Publication Date: 2019-12-17
BENAN ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually compared with the traditional solid-phase synthesis method, the powder prepared by these methods has higher purity and excellent performance, but the production process is complicated and the equipment is more, it is difficult to achieve large-scale production, especially when carbon coating requires multiple heat treatments and grinding, the cost is high, and it cannot meet the requirements of reducing battery cost
The traditional solid-phase synthesis method also has its own defects, such as many side reactions caused by uneven powder mixing, impure products, etc.

Method used

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  • A method for batch preparation of low-cost carbon-coated titanium phosphate compounds
  • A method for batch preparation of low-cost carbon-coated titanium phosphate compounds
  • A method for batch preparation of low-cost carbon-coated titanium phosphate compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Sodium carbonate, ammonium dihydrogen ammonium phosphate, and titanium dioxide powder are used as raw materials, and the content of sodium, titanium, and phosphorus is added to the mixture of ethanol and water (1:10) in a molar ratio of 1:2:3. The raw material powder and ethanol The mass ratio of the mixed liquid with water is 30:70. Polyacrylic acid was selected as the dispersant, and the amount of dispersant added was 1wt.% of the powder, and a uniform slurry was obtained by ball milling at a high speed of 200 rpm for 2 hours. Continue to add the active substance graphite (20wt.%) pretreated by ethanol, further ball mill at 200 r / min for 2 h, and then pour out the slurry. The obtained slurry was spray-dried, the inlet air temperature was set at 220°C, the outlet air temperature was 110°C, and the centrifugal speed was 12000 rpm, and the obtained spherical powder precursor was collected. Put the precursor into an inert gas-filled sintering furnace, and sinter at 750°C...

Embodiment 2

[0053] Lithium carbonate, ammonium dihydrogen phosphate, and titanium dioxide powder are used as raw materials, and the contents of lithium, titanium, and phosphorus are added to the mixed solution of ethanol and water (1:10) in a molar ratio of 1:2:3. The raw material powder and ethanol The mass ratio of the mixed liquid with water is 30:70. Sodium hexametaphosphate was selected as a dispersant, and the amount of dispersant added was 1wt.% of the powder, and a uniform slurry was obtained by ball milling at a high speed of 200 rpm for 2 hours. Continue to add the active substance graphite (20wt.%) pretreated by ethanol, further ball mill at 200 r / min for 2 h, and then pour out the slurry. The obtained slurry was spray-dried, the inlet air temperature was set at 220°C, the outlet air temperature was 110°C, and the centrifugal speed was 15,000 rpm, and the obtained spherical powder precursor was collected. Put the precursor into an inert gas-filled sintering furnace, and sinter...

Embodiment 3

[0055] Sodium carbonate, ammonium dihydrogen phosphate, and titanium dioxide powder are used as raw materials, and the content of potassium, titanium, and phosphorus is added to the mixed solution of ethanol and water (1:10) in a molar ratio of 1:2:3. The raw material powder and ethanol The mass ratio of the mixed solution with water is 20:80. Castor oil was selected as the dispersant, and the amount of dispersant added was 1wt.% of the powder, and a uniform slurry was obtained by ball milling at a high speed of 200 rpm for 2 hours. Continue to add the active substance graphite (20wt.%) pretreated by ethanol, further ball mill at 200 r / min for 2 h, and then pour out the slurry. The obtained slurry was spray-dried, the inlet air temperature was set at 220°C, the outlet air temperature was 110°C, and the centrifugal speed was 17,000 rpm, and the obtained spherical powder precursor was collected. Put the precursor into an inert gas-filled sintering furnace, and sinter at 750°C f...

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Abstract

The invention relates to a batch preparation method for a low-cost carbon-clad titanium phosphate compound. The chemical formula of the titanium phosphate compound is MxTi2(PO4)3, wherein M is selected from at least one of alkali metals, and x is equal to 1-1.05. The method comprises the following steps: (1) carrying out wet-process ball milling on the raw materials of an alkali metal source, a phosphorus source, a titanium source and a carbon source in a stoichiometric ratio, so as to obtain slurry; (2) carrying out centrifugal spray drying on the slurry, so as to obtain carbon-clad titaniumphosphate compound precursor mixed powder; and (3) sintering the precursor mixed powder by virtue of a solid-phase synthesis method, so as to obtain titanium phosphate compound powder. According to the batch preparation method, the process is simple, the cost is low and the preparation method can be widely applied to the large-scale production of the titanium phosphate compounds.

Description

technical field [0001] The invention relates to a method suitable for preparing carbon-coated titanium phosphate compound ceramic powder in batches, in particular to a method of ball milling and mixing with carbon-containing precursors and precursors of various phase components, spray drying and granulation. The invention relates to preparing carbon-coated titanium phosphate compound powder through a high-temperature solid-phase synthesis reaction method, which belongs to the field of ion-conducting ceramic materials. Background technique [0002] Titanium phosphate compound is a typical NASICON structure, which has a large tunnel size to allow the free migration of alkali metal ions. It is a fast ion conductor with high ion conductivity and small electron conductivity, and has excellent thermal stability, and is an important electrode material for alkali metal ion batteries. NaTi 2 (PO 4 ) 3 For example, at 1mol / LNa 2 SO 4 In solution, NaTi 2 (PO 4 ) 3 There is a p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/447C04B35/626C04B35/628C04B35/638C04B35/64
CPCC04B35/447C04B35/6261C04B35/62655C04B35/62839C04B35/638C04B35/64C04B2235/3201C04B2235/3203C04B2235/3232C04B2235/658C04B2235/782
Inventor 曾诗蒙刘宇夏骥贺健贺诗阳张娜
Owner BENAN ENERGY
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