阅读说明：本技术 粉末涂料用浅色三维导电粉体及其制备方法 (Light-colored three-dimensional conductive powder for powder coating and preparation method thereof ) 是由 唐骏 姚超 左士祥 卓仲标 周铭 孟祥远 李霞章 刘文杰 钱大庆 于 2021-04-07 设计创作，主要内容包括：本发明属于无机功能材料技术领域,尤其涉及一种粉末涂料用浅色三维导电粉体及其制备方法,包括步骤(1),在去离子水中加入片状基材和棒状基材,搅拌均匀制备得到片-棒基材分散液,步骤(2),在盐酸溶液中加入五水四氯化锡、三氯化锑和氯化铌,搅拌至固体全部溶解,制得锡-铌-锑盐酸混合溶液,步骤(3),将制得的片-棒基材分散液在恒温搅拌的条件下边滴加锡-铌-锑盐酸混合溶液,抽滤,煅烧,制得三维浅色导电粉体,步骤(4),用气流粉碎三维浅色导电粉体的同时,喷洒表面处理剂干燥后,即得粉末涂料用浅色三维导电粉体。本发明的浅色导电粉体其独特的片-棒三维形态,极易构筑成导电网络,在较少的添加量下达到良好的导电效果。(The invention belongs to the technical field of inorganic functional materials, and particularly relates to light-colored three-dimensional conductive powder for powder coating and a preparation method thereof, which comprises the following steps (1), adding the flaky base material and the rod-shaped base material into deionized water, uniformly stirring to prepare a flaky-rod base material dispersion liquid, step (2), adding tin tetrachloride pentahydrate, antimony trichloride and niobium chloride into a hydrochloric acid solution, stirring until the solid is completely dissolved to prepare a tin-niobium-antimony hydrochloric acid mixed solution, step (3), dropwise adding the tin-niobium-antimony hydrochloric acid mixed solution into the prepared sheet-rod base material dispersion liquid under the condition of constant-temperature stirring, carrying out suction filtration and calcination to prepare three-dimensional light-colored conductive powder, and step (4), spraying a surface treatment agent to dry while crushing the three-dimensional light-colored conductive powder by using airflow to obtain the light-colored three-dimensional conductive powder for the powder coating. The light-colored conductive powder has a unique sheet-rod three-dimensional shape, is easy to construct a conductive network, and achieves a good conductive effect with a small addition amount.)

1. A preparation method of light-colored three-dimensional conductive powder for powder coating is characterized by comprising the following steps,

step (1), preparation of a sheet-rod base material dispersion: adding the ground flaky base material and the ground rodlike base material into deionized water in sequence, uniformly stirring to prepare a flaky-rodlike base material dispersion liquid,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding tin tetrachloride pentahydrate, antimony trichloride and niobium chloride into a hydrochloric acid solution, stirring until the solid is completely dissolved to prepare a tin-niobium-antimony hydrochloric acid mixed solution,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1), heating to 50-80 ℃, adjusting the pH value to 1.0-3.0, dropwise adding a tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, and simultaneously using an alkaline solution to keep the pH value to 1.0-3.0, wherein the mass ratio of the tin tetrachloride pentahydrate to the sheet-rod base material is 0.6-1.2: after the dropwise addition of the 1, tin-niobium-antimony hydrochloric acid mixed solution, continuously preserving heat, stirring and reacting for 0.5-1h, carrying out suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying the filter cake, calcining for 1-3h at the temperature of 500-700 ℃ to obtain three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (4) carrying out jet milling on the three-dimensional light-colored conductive powder obtained in the step (3), spraying a surface treating agent, mixing for 10-30 minutes, and drying to obtain the light-colored three-dimensional conductive powder for the powder coating.

2. A preparation method of light-colored three-dimensional conductive powder for powder coating is characterized by comprising the following steps,

step (1), preparation of a sheet-rod base material dispersion: sequentially adding the ground flaky base material and the ground rodlike base material into deionized water, and uniformly stirring to prepare a flaky-rodlike base material dispersion liquid, wherein the mass ratio of the total mass of the flaky base material and the rodlike base material to the deionized water is 1: 10-20,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding tin tetrachloride pentahydrate, antimony trichloride and niobium chloride into a 1-3mol/L hydrochloric acid solution, stirring until the solid is completely dissolved, transferring to a capacity bottle, and performing constant volume with dilute hydrochloric acid to prepare a tin-niobium-antimony hydrochloric acid mixed solution, wherein the mass ratio of the tin tetrachloride pentahydrate to the antimony trichloride to the niobium chloride is as follows: 10-15 parts of antimony trichloride: 1, tin tetrachloride pentahydrate: 15-20 parts of niobium chloride: 1,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1), heating to 50-80 ℃, adjusting the pH value to 1.0-3.0, dropwise adding a tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, and simultaneously using an alkaline solution to keep the pH value to 1.0-3.0, wherein the mass ratio of the tin tetrachloride pentahydrate to the sheet-rod base material is 0.6-1.2: after the dropwise addition of the 1, tin-niobium-antimony hydrochloric acid mixed solution, continuously preserving heat, stirring and reacting for 0.5-1h, carrying out suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying the filter cake, calcining for 1-3h at the temperature of 500-700 ℃ to obtain three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (3) carrying out jet milling on the three-dimensional light-colored conductive powder obtained in the step (3), spraying a surface treating agent, mixing for 10-30 minutes, and drying at 110 ℃ for 5 hours to obtain the light-colored three-dimensional conductive powder for the powder coating.

3. The method for preparing light-colored three-dimensional conductive powder for powder coating according to claim 1 or 2, wherein the flaky substrate in step (1) is one of flaky natural mica, flaky synthetic mica, flaky alumina, flaky silica or glass flakes, the particle size is 5-25 micrometers, and the rod-shaped substrate is one of attapulgite, rod-shaped titanium dioxide or potassium titanate, wherein the rod-shaped titanium dioxide or potassium titanate has a diameter of 0.2-0.3 micrometer and a length of 10-20 micrometers, the diameter of the attapulgite is 15-25 nanometers and the length of 0.5-5 micrometers.

4. The method for producing a light-colored three-dimensional conductive powder for powder coating according to claim 1 or 2, wherein in the step (1), the mass ratio of the flaky substrate to the rod-shaped substrate is 4: 1.

5. the method for preparing a light-colored three-dimensional conductive powder for powder coating according to claim 1 or 2, wherein the mass concentration of the tin-niobium-antimony hydrochloride mixed solution in the step (2) is 0.3 to 0.5g/mL in terms of tin tetrachloride pentahydrate.

6. The method for preparing light-colored three-dimensional conductive powder for powder coating according to claim 1 or 2, wherein the alkali solution in the step (3) is a solution of sodium hydroxide, ammonia water, potassium hydroxide or urea, wherein the concentration of the alkali solution is 2.0-4.0 mol/L.

7. The method for preparing light-colored three-dimensional conductive powder for powder coating according to claim 1 or 2, wherein the surface treatment agent in step (4) is one of titanate coupling agent, octyltriethoxysilane, polydimethylsiloxane or trimethylolpropane, and the mass ratio of the surface treatment agent to the three-dimensional light-colored conductive powder is 0.005-0.02: 1.

8. the method for preparing light-colored three-dimensional conductive powder for powder coating according to claim 7, wherein the surface treatment agent is pre-diluted with a diluent, the diluent is one of acetone, butanone, isopropanol or isooctane, and the mass ratio of the surface treatment agent to the diluent is 0.5-2: 1.

9. the method for preparing light-colored three-dimensional conductive powder for powder coating according to claim 2, wherein in the step (4), the drying temperature is 110 ℃ and the time is 5 hours, and in the step (2), the concentration of dilute hydrochloric acid for constant volume is 0.1-0.5 mol/L.

10. The light-colored three-dimensional conductive powder for powder coating, which is produced by the method for producing a light-colored three-dimensional conductive powder for powder coating according to any one of claims 1 to 9.

Technical Field

The invention belongs to the technical field of inorganic functional materials, and relates to a preparation method of coated light-colored conductive powder, in particular to light-colored three-dimensional conductive powder for powder coating and a preparation method thereof.

Background

In recent years, with the weight reduction of automobiles, the molding of automobile bodies is becoming more and more a trend, and thus the demand for high-performance conductive coating materials for automobile primers is increasing. At present, most car and enterprise manufacturers spray a layer of conductive primer on the surface of a plastic part in advance and then carry out electrostatic spraying, and in the spraying mode, the volatilization amount of solvent components is high, the uncoated paint is difficult to recycle, the effective utilization rate is about 50%, and the discharge amount of VOCs is high.

However, powder coatings have been popular with the market due to their advantages of environmental friendliness (zero VOCs), recyclability of waste powders, and excellent chemical protection, and the market share has increased year by year. At present, a great deal of research work is done at home and abroad for applying the powder coating to automobile coating, and particularly, the innovation of a spraying mode on plastic parts and the appearance of low-temperature curing powder coating enable the application of the powder coating to be more and more extensive. The powder coating can be directly coated on the surface of a coated object, a coating film is formed after baking and curing, the powder which is not coated can be recovered and then sent to a powder supply system for application, the loss of the coating in construction is greatly reduced, and the utilization rate of the powder coating is about more than 95%.

At present, the powder coating which enables the surface of a plastic part to have certain conductive performance directly determines the conductive effect of the powder coating after the powder coating is sprayed on the surface of the plastic part by adding a conductive material, the conductive performance of the conductive material and the powder coating rate of the powder coating.

Disclosure of Invention

The invention aims to solve the problems and provides a preparation method of light-colored three-dimensional conductive powder for powder coating.

Another object of the present invention is to provide a light-colored three-dimensional conductive powder for powder coating.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of light-colored three-dimensional conductive powder for powder coating comprises the following steps,

step (1), preparation of a sheet-rod base material dispersion: adding the ground flaky base material and the ground rodlike base material into deionized water in sequence, uniformly stirring to prepare a flaky-rodlike base material dispersion liquid,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding tin tetrachloride pentahydrate, antimony trichloride and niobium chloride into a hydrochloric acid solution, stirring until the solid is completely dissolved to prepare a tin-niobium-antimony hydrochloric acid mixed solution,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1), heating to 50-80 ℃, adjusting the pH value to 1.0-3.0, dropwise adding a tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, and simultaneously using an alkaline solution to keep the pH value to 1.0-3.0, wherein the mass ratio of the tin tetrachloride pentahydrate to the sheet-rod base material is 0.6-1.2: after the dropwise addition of the 1, tin-niobium-antimony hydrochloric acid mixed solution, continuously preserving heat, stirring and reacting for 0.5-1h, carrying out suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying the filter cake, calcining for 1-3h at the temperature of 500-700 ℃ to obtain three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (4) carrying out jet milling on the three-dimensional light-colored conductive powder obtained in the step (3), spraying a surface treating agent, mixing for 10-30 minutes, and drying to obtain the light-colored three-dimensional conductive powder for the powder coating.

A preparation method of light-colored three-dimensional conductive powder for powder coating comprises the following steps,

step (1), preparation of a sheet-rod base material dispersion: sequentially adding the ground flaky base material and the ground rodlike base material into deionized water, and uniformly stirring to prepare a flaky-rodlike base material dispersion liquid, wherein the mass ratio of the total mass of the flaky base material and the rodlike base material to the deionized water is 1: 10-20,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding tin tetrachloride pentahydrate, antimony trichloride and niobium chloride into a 1-3mol/L hydrochloric acid solution, stirring until the solid is completely dissolved, transferring to a capacity bottle, and performing constant volume with dilute hydrochloric acid to prepare a tin-niobium-antimony hydrochloric acid mixed solution, wherein the mass ratio of the tin tetrachloride pentahydrate to the antimony trichloride to the niobium chloride is as follows: 10-15 parts of antimony trichloride: 1, tin tetrachloride pentahydrate: 15-20 parts of niobium chloride: 1,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1), heating to 50-80 ℃, adjusting the pH value to 1.0-3.0, dropwise adding a tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, and simultaneously using an alkaline solution to keep the pH value to 1.0-3.0, wherein the mass ratio of the tin tetrachloride pentahydrate to the sheet-rod base material is 0.6-1.2: after the dropwise addition of the 1, tin-niobium-antimony hydrochloric acid mixed solution, continuously preserving heat, stirring and reacting for 0.5-1h, carrying out suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying the filter cake, calcining for 1-3h at the temperature of 500-700 ℃ to obtain three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (3) carrying out jet milling on the three-dimensional light-colored conductive powder obtained in the step (3), spraying a surface treating agent, mixing for 10-30 minutes, and drying at 110 ℃ for 5 hours to obtain the light-colored three-dimensional conductive powder for the powder coating.

In the preparation method of the light-colored three-dimensional conductive powder for the powder coating, the flaky base material in the step (1) is one of flaky natural mica, flaky synthetic mica, flaky alumina, flaky silica or glass flakes, the particle size is 5-25 micrometers, and the rod-shaped base material is one of attapulgite, rod-shaped titanium dioxide or potassium titanate, wherein the diameter of the rod-shaped titanium dioxide or potassium titanate is 0.2-0.3 micrometer, the length of the rod-shaped titanium dioxide or potassium titanate is 10-20 micrometers, the diameter of the attapulgite is 15-25 nanometers, and the length of the attapulgite is 0.5-5 micrometers.

In the above method for producing a light-colored three-dimensional conductive powder for a powder coating, in the step (1), the mass ratio of the sheet-like base material to the rod-like base material is 4: 1.

in the preparation method of the light-colored three-dimensional conductive powder for the powder coating, the mass concentration of the tin-niobium-antimony hydrochloric acid mixed solution in the step (2) is 0.3-0.5g/mL calculated by stannic chloride pentahydrate.

In the preparation method of the light-colored three-dimensional conductive powder for the powder coating, the alkali liquor in the step (3) is sodium hydroxide, ammonia water, potassium hydroxide or urea solution, wherein the concentration of the alkali liquor is 2.0-4.0 mol/L.

In the preparation method of the light-colored three-dimensional conductive powder for the powder coating, the surface treating agent in the step (4) is one of titanate coupling agent, octyl triethoxysilane, polydimethylsiloxane or trimethylolpropane, and the mass ratio of the surface treating agent to the three-dimensional light-colored conductive powder is 0.005-0.02: 1.

in the preparation method of the light-colored three-dimensional conductive powder for the powder coating, the surface treating agent is diluted by a diluent in advance, the diluent is one of acetone, butanone, isopropanol or isooctane, and the mass ratio of the surface treating agent to the diluent is 0.5-2: 1.

in the preparation method of the light-colored three-dimensional conductive powder for the powder coating, in the step (4), the drying temperature is 110 ℃, the time is 5 hours, and in the step (2), the concentration of dilute hydrochloric acid for constant volume is 0.1-0.5 mol/L.

The light-color three-dimensional conductive powder for the powder coating is prepared by the preparation method of the light-color three-dimensional conductive powder for the powder coating.

Compared with the prior art, the invention has the advantages that:

(1) in the aspect of conductivity, the light-color conductive powder has unique sheet-rod three-dimensional shape, is easy to construct a conductive network, and achieves good conductive effect with less addition amount. Meanwhile, the color is light, and the decorative effect is good.

(2) Compared with the traditional flaky conductive powder, the flaky conductive powder prepared by the coating process of the antimony-niobium co-doped tin oxide has high whiteness and good and stable conductivity, and simultaneously reduces the content of heavy metal antimony in the powder.

(3) The surface modification of the conductive powder solves the compatibility and the dispersibility of the conductive powder with resin in the powder coating, saves the binding step of the conductive powder in the powder coating, improves the powdering rate of the powder coating, simplifies the process and reduces the production cost.

Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.

Drawings

FIG. 1 is a scanning electron microscope image of a light-colored three-dimensional conductive powder for powder coating in a coating prepared in example 3.

Detailed Description

In order to make the technical solution of the present invention better understood, the technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments.

Example 1

A preparation method of light-colored three-dimensional conductive powder for powder coating comprises the following steps,

step (1), preparation of a sheet-rod base material dispersion: adding the ground flaky base material and the ground rodlike base material into deionized water in sequence, uniformly stirring to prepare a flaky-rodlike base material dispersion liquid,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding tin tetrachloride pentahydrate, antimony trichloride and niobium chloride into a hydrochloric acid solution, stirring until the solid is completely dissolved to prepare a tin-niobium-antimony hydrochloric acid mixed solution,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1), heating to 50-80 ℃, adjusting the pH value to 1.0-3.0, dropwise adding a tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, and simultaneously using an alkaline solution to keep the pH value to 1.0-3.0, wherein the mass ratio of the tin tetrachloride pentahydrate to the sheet-rod base material is 0.6-1.2: after the dropwise addition of the 1, tin-niobium-antimony hydrochloric acid mixed solution, continuously preserving heat, stirring and reacting for 0.5-1h, carrying out suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying the filter cake, calcining for 1-3h at the temperature of 500-700 ℃ to obtain three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (4) carrying out jet milling on the three-dimensional light-colored conductive powder obtained in the step (3), spraying a surface treating agent, mixing for 10-30 minutes, and drying to obtain the light-colored three-dimensional conductive powder for the powder coating.

The flaky base material in the step (1) is one of flaky natural mica, flaky synthetic mica, flaky alumina, flaky silica or glass flakes, the particle size is 5-25 micrometers, and the rodlike base material is one of attapulgite, rodlike titanium dioxide or potassium titanate, wherein the diameter of the rodlike titanium dioxide or potassium titanate is 0.2-0.3 micrometer, the length of the rodlike titanium dioxide or potassium titanate is 10-20 micrometers, the diameter of the attapulgite is 15-25 nanometers, and the length of the attapulgite is 0.5-5 micrometers.

In the step (1), the mass ratio of the sheet-shaped base material to the rod-shaped base material is 4: 1.

and (3) the mass concentration of the tin-niobium-antimony hydrochloride mixed solution in the step (2) is 0.3-0.5g/mL calculated by the tin tetrachloride pentahydrate.

And (3) the alkali liquor is sodium hydroxide, ammonia water, potassium hydroxide or urea solution, wherein the concentration of the alkali liquor is 2.0-4.0 mol/L.

The surface treating agent in the step (4) is one of titanate coupling agent, octyl triethoxysilane, polydimethylsiloxane or trimethylolpropane, and the mass ratio of the surface treating agent to the three-dimensional light-colored conductive powder is 0.005-0.02: 1.

the surface treatment agent is pre-diluted by a diluent, the diluent is one of acetone, butanone, isopropanol or isooctane, and the mass ratio of the surface treatment agent to the diluent is 0.5-2: 1.

example 2

A preparation method of light-colored three-dimensional conductive powder for powder coating comprises the following steps,

step (1), preparation of a sheet-rod base material dispersion: sequentially adding the ground flaky base material and the ground rodlike base material into deionized water, and uniformly stirring to prepare a flaky-rodlike base material dispersion liquid, wherein the mass ratio of the total mass of the flaky base material and the rodlike base material to the deionized water is 1: 10-20,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding tin tetrachloride pentahydrate, antimony trichloride and niobium chloride into a 1-3mol/L hydrochloric acid solution, stirring until the solid is completely dissolved, transferring to a capacity bottle, and performing constant volume with dilute hydrochloric acid to prepare a tin-niobium-antimony hydrochloric acid mixed solution, wherein the mass ratio of the tin tetrachloride pentahydrate to the antimony trichloride to the niobium chloride is as follows: 10-15 parts of antimony trichloride: 1, tin tetrachloride pentahydrate: 15-20 parts of niobium chloride: 1,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1), heating to 50-80 ℃, adjusting the pH value to 1.0-3.0, dropwise adding a tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, and simultaneously using an alkaline solution to keep the pH value to 1.0-3.0, wherein the mass ratio of the tin tetrachloride pentahydrate to the sheet-rod base material is 0.6-1.2: after the dropwise addition of the 1, tin-niobium-antimony hydrochloric acid mixed solution, continuously preserving heat, stirring and reacting for 0.5-1h, carrying out suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying the filter cake, calcining for 1-3h at the temperature of 500-700 ℃ to obtain three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (3) carrying out jet milling on the three-dimensional light-colored conductive powder obtained in the step (3), spraying a surface treating agent, mixing for 10-30 minutes, and drying at 110 ℃ for 5 hours to obtain the light-colored three-dimensional conductive powder for the powder coating.

The flaky base material in the step (1) is one of flaky natural mica, flaky synthetic mica, flaky alumina, flaky silica or glass flakes, the particle size is 5-25 micrometers, and the rodlike base material is one of attapulgite, rodlike titanium dioxide or potassium titanate, wherein the diameter of the rodlike titanium dioxide or potassium titanate is 0.2-0.3 micrometer, the length of the rodlike titanium dioxide or potassium titanate is 10-20 micrometers, the diameter of the attapulgite is 15-25 nanometers, and the length of the attapulgite is 0.5-5 micrometers.

In the step (1), the mass ratio of the sheet-shaped base material to the rod-shaped base material is 4: 1.

and (3) the mass concentration of the tin-niobium-antimony hydrochloride mixed solution in the step (2) is 0.3-0.5g/mL calculated by the tin tetrachloride pentahydrate.

And (3) the alkali liquor is sodium hydroxide, ammonia water, potassium hydroxide or urea solution, wherein the concentration of the alkali liquor is 2.0-4.0 mol/L.

The surface treating agent in the step (4) is one of titanate coupling agent, octyl triethoxysilane, polydimethylsiloxane or trimethylolpropane, and the mass ratio of the surface treating agent to the three-dimensional light-colored conductive powder is 0.005-0.02: 1.

the surface treatment agent is pre-diluted by a diluent, the diluent is one of acetone, butanone, isopropanol or isooctane, and the mass ratio of the surface treatment agent to the diluent is 0.5-2: 1.

in the step (4), the drying temperature is 110 ℃, the time is 5 hours, and in the step (2), the concentration of dilute hydrochloric acid for constant volume is 0.1-0.5 mol/L.

Example 3

A preparation method of light-colored three-dimensional conductive powder for powder coating comprises the following steps,

step (1), preparation of a sheet-rod base material dispersion: adding 80g of ground flaky natural mica powder with the particle size of 5-25 microns and 20g of attapulgite powder with the diameter of 15-25 nanometers and the length of 0.5-5 microns into 1000g of deionized water in sequence, uniformly stirring to prepare a sheet-rod base material dispersion liquid,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding 300g of tin tetrachloride pentahydrate, 20g of antimony trichloride and 20g of niobium chloride into 700mL of 1mol/L hydrochloric acid solution, stirring until the solid is completely dissolved, transferring the solution into a 1000mL capacity bottle, fixing the volume with 0.5mol/L hydrochloric acid solution to obtain a tin-niobium-antimony hydrochloric acid mixed solution,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1) and heating to 50-80 ℃, adjusting the pH value to 1.0-3.0 by using 1mol/L hydrochloric acid solution, dropwise adding 200mL of tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, simultaneously using 2mol/L sodium hydroxide solution to keep the pH value to 1.0-3.0, after dropwise adding the tin-niobium-antimony hydrochloric acid mixed solution, continuously keeping the temperature and stirring for reaction for 0.5-1h, performing suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying the filter cake, calcining at the temperature of 500-DEG and 700 ℃ for 1-3h to prepare three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (3) adopting a commercially available jet mill to jet mill the three-dimensional light-colored conductive powder obtained in the step (3), and spraying a surface treatment agent, wherein the surface treatment agent is a titanate coupling agent and is diluted by acetone in advance, the weight ratio of the titanate coupling agent to the acetone is 0.5:1, and the mass ratio of the titanate coupling agent to the three-dimensional light-colored conductive powder is 0.02: 1, mixing for 10-30 minutes, and drying at 110 ℃ for 5 hours to obtain the light-colored three-dimensional conductive powder for the powder coating. As can be seen from figure 1, the sheet natural mica powder and the rod-shaped attapulgite powder form a three-dimensional conductive path in the coating.

Example 4

A preparation method of light-colored three-dimensional conductive powder for powder coating comprises the following steps,

step (1), preparation of a sheet-rod base material dispersion: adding 80g of grinded flaky alumina powder with the particle size of 5-25 micrometers and 20g of rodlike titanium dioxide powder with the diameter of 0.2-0.3 micrometers and the length of 10-20 micrometers into 2000g of deionized water in sequence, uniformly stirring to prepare a sheet-rod base material dispersion liquid,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding 500g of tin tetrachloride pentahydrate, 50g of antimony trichloride and 25g of niobium chloride into 1000mL of 1mol/L hydrochloric acid solution, stirring until the solid is completely dissolved, transferring the solution into a 2000mL volumetric flask, fixing the volume with 0.1mol/L hydrochloric acid solution to obtain a tin-niobium-antimony hydrochloric acid mixed solution,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1) and heating to 60-70 ℃, adjusting the pH value to 1.0-3.0 by using 3mol/L hydrochloric acid solution, dropwise adding 480mL tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, simultaneously using 3mol/L potassium hydroxide solution to keep the pH value to 1.0-3.0, after dropwise adding the tin-niobium-antimony hydrochloric acid mixed solution, continuing to perform heat preservation stirring reaction for 0.6-8h, performing suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying a filter cake, calcining at 600-650 ℃ for 2h to prepare three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (3) adopting a commercially available jet mill to jet mill the three-dimensional light-colored conductive powder obtained in the step (3) and spraying a surface treatment agent, wherein the surface treatment agent is octyl triethoxy silane and is diluted by butanone in advance, the weight ratio of the octyl triethoxy silane to the butanone is 2:1, and the mass ratio of titanate coupling agent to the three-dimensional light-colored conductive powder is 0.005: 1, mixing for 20 minutes, and drying at 110 ℃ for 5 hours to obtain the light-colored three-dimensional conductive powder for the powder coating.

Example 5

A preparation method of light-colored three-dimensional conductive powder for powder coating comprises the following steps,

step (1), preparation of a sheet-rod base material dispersion: adding 80g of grinded flaky silicon oxide powder with the particle size of 5-25 microns and 20g of potassium titanate powder with the diameter of 0.2-0.3 micron and the length of 10-20 microns into 1000g of deionized water in sequence, uniformly stirring to prepare a sheet-rod base material dispersion liquid,

step (2), preparing a tin-niobium-antimony hydrochloric acid mixed solution: adding 300g of tin tetrachloride pentahydrate, 25g of antimony trichloride and 18g of niobium chloride into 650mL of 1mol/L hydrochloric acid solution, stirring until the solid is completely dissolved, transferring the solution into a 1000mL capacity bottle, fixing the volume with 0.2mol/L hydrochloric acid solution to obtain a tin-niobium-antimony hydrochloric acid mixed solution,

step (3), preparing three-dimensional light-colored conductive powder: stirring the sheet-rod base material dispersion liquid prepared in the step (1) and heating to 50-80 ℃, adjusting the pH value to 2.0-2.5 by using 1mol/L hydrochloric acid solution, dropwise adding 800mL of tin-niobium-antimony hydrochloric acid mixed solution under the condition of constant-temperature stirring, simultaneously using 4mol/L ammonia water solution to keep the pH value to 1.0-3.0, after dropwise adding the tin-niobium-antimony hydrochloric acid mixed solution, continuously keeping the temperature and stirring for reaction for 0.5-1h, performing suction filtration, washing with deionized water until the conductivity of the filtrate is less than or equal to 300 mu S/cm, drying a filter cake, calcining at the temperature of 500-700 ℃ for 1-3h to prepare three-dimensional light-colored conductive powder,

step (4), preparing light-colored three-dimensional conductive powder for powder coating: and (3) adopting a commercially available jet mill to jet mill the three-dimensional light-colored conductive powder obtained in the step (3), and spraying a surface treatment agent, wherein the surface treatment agent is polydimethylsiloxane, the polydimethylsiloxane is diluted by isopropanol in advance, the weight ratio of a titanate coupling agent to acetone is 1:1, and the mass ratio of the polydimethylsiloxane to the three-dimensional light-colored conductive powder is 0.01: 1, mixing for 25 minutes, and drying at 110 ℃ for 5 hours to obtain the light-colored three-dimensional conductive powder for the powder coating.

The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit of the invention.