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Room temperature mechanical force solid phase chemical reaction preparation of antimony-doped nano stannic oxide

A nano-tin dioxide, solid-phase chemical reaction technology, applied in fibrous fillers and other directions, can solve the problems of difficult to achieve uniform mixing, hydrolysis of tin ions, slow reaction speed, etc., to achieve shortened chemical reaction time, constant concentration, and improved diffusion. effect of speed

Inactive Publication Date: 2009-04-22
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] From the content of the above Chinese patent application, it can be seen that the traditional solid-phase method is simple to operate and low in cost, but the reaction speed is slow, and it is difficult to achieve uniform mixing during doping; the cost of hydrothermal method, sol-gel method and metal alkoxide hydrolysis method Higher, the chemical co-precipitation method has strict requirements on the precipitation conditions such as pH value, and it is easy to cause the hydrolysis of antimony and tin ions, and improper control will also cause uneven doping

Method used

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  • Room temperature mechanical force solid phase chemical reaction preparation of antimony-doped nano stannic oxide

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Embodiment 1

[0027] In this embodiment, the reactants are stannous chloride and antimony trichloride, and the ligand is oxalic acid. The process flow is as follows: figure 1 As shown, there are the following steps in sequence

[0028] 1. Ingredients

[0029] The molar ratio of stannous chloride, antimony trichloride and oxalic acid is 1:2, wherein the molar ratio of stannous chloride and antimony trichloride is 10:1;

[0030] 2. Mixing

[0031] Mix the proportion of stannous chloride, antimony trichloride and oxalic acid until uniform;

[0032] 3. Preparation of precursors by mechanical solid-phase chemical reaction method

[0033] The uniformly mixed stannous chloride, antimony trichloride and oxalic acid are ball milled at room temperature and normal pressure, so that they react to form precursors under the mechanical shear force and impact force generated during the ball milling process, and the speed of the ball mill is controlled At 300 rpm, ball milling for 50 minutes can complet...

Embodiment 2

[0041] In this embodiment, the reactants are stannous sulfate and antimony trichloride, and the ligand is ammonium carbonate. The process flow is as follows: figure 1 As shown, there are the following steps in sequence:

[0042] 1. Ingredients

[0043] The molar ratio of the total amount of stannous sulfate and antimony trichloride to ammonium carbonate is 1:3, wherein the molar ratio of stannous sulfate and antimony trichloride is 15:1;

[0044] 2. Mixing

[0045] Mix the proportioned stannous sulfate, antimony trichloride and ammonium carbonate until uniform;

[0046] 3. Preparation of precursors by mechanochemical reaction method

[0047] The uniformly mixed stannous sulfate, antimony trichloride and ammonium carbonate are ball milled at room temperature and normal pressure, so that they react to form precursors under the action of mechanical shear force and impact force generated during the ball milling process. The speed of the ball mill is at 350 rpm, ball milling fo...

Embodiment 3

[0055] In this embodiment, the reactants are tin chloride and antimony sulfate, and the ligand is oxalic acid. The process flow is as follows: figure 1 As shown, there are the following steps in sequence:

[0056] 1. Ingredients

[0057] The molar ratio of tin chloride, antimony sulfate total amount and oxalic acid is 1:5, wherein the molar ratio of tin chloride, antimony sulfate is 12:1;

[0058] 2. Mixing

[0059] Mix tin chloride, antimony sulfate and oxalic acid in proportion until uniform;

[0060] 3. Preparation of precursors by mechanochemical reaction method

[0061] The uniformly mixed reaction system is ball milled at room temperature and normal pressure, so that it reacts to form a precursor under the action of mechanical shear force and impact force generated during the ball milling process. It can completely react tin chloride, antimony sulfate and oxalic acid to form precursors;

[0062] 4. Precursor removal

[0063] The precursor is removed by washing and fi...

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Abstract

The invention discloses a room-temperature mechanical force solid-phase chemical reaction method for stibium-doped nanometer tin dioxide and relates to a technology for preparing the stibium-doped nanometer tin dioxide in anti-electrostatic painting, plastic, fibre and other fields. Stanniferous inorganic salt and antimonial inorganic salt are used as reactants; and oxalic acid, ammonium carbonate, ammonium hydrogen carbonate, sodium oxalate or sodium bicarbonate and the like are used as ligands. The method comprises the following process steps: the materials are matched, are mixed and are subjected to room-temperature mechanical force solid-phase chemical reaction to prepare a precursor; the precursor is subjected to impurity removal, drying and thermal decomposition to obtain the target product. The method is characterized in that water is not introduced in the reaction process to prevent the hydrolysis of tin ions and stibium ions so as to realize even doping; simultaneously, the method utilizes shearing force and impacting force produced in the ball milling process to crush a solid-phase reaction system, increases the specific surface areas of the reactants and increases the speed of reaction to prepare the superfine and even precursor; the precursor is washed and dried; and the temperature and the time for thermal decomposition are controlled, thereby obtaining the nanometer tin dioxide doped powder body which has distribution of particle diameter of between 30 and 80 nm and a controllable pattern.

Description

1. Technical field [0001] The invention patent belongs to "nano-oxide powder preparation technology", which relates to antimony-doped nano-tin dioxide and its preparation method that can be used in antistatic coatings, plastics, fibers and other fields. 2. Background technology [0002] Antimony-doped tin dioxide (ATO) powder has been widely used due to its excellent properties such as high electrical conductivity, light color transparency, good stability and weather resistance, especially after the powder is nano-sized, due to its large specific A series of new features such as surface area have greatly improved its performance. At present, the preparation methods of nano-tin dioxide and its blends mainly include: chemical co-precipitation method, hydrothermal method, sol-gel method, metal alkoxide hydrolysis method, solid-phase method and so on. For example: the Chinese patent application number 200310107905.0 adopts tin compounds and organic substances with complexing ab...

Claims

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Application Information

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IPC IPC(8): C09C1/00
Inventor 朱达川涂铭旌
Owner SICHUAN UNIV
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