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Method for preparing ferrous phosphide Fe3P at high temperature and high pressure

A high-temperature, high-pressure, phosphating technology, which is applied in the field of functional material synthesis, can solve problems such as long reaction time, difficult processing, and low cleanliness, and achieve the effects of improving synthesis efficiency, avoiding volatilization loss, and improving the degree of crystallization

Active Publication Date: 2018-03-20
INST OF GEOCHEM CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is: a kind of preparation under high temperature and pressure 3 P method to solve technical problems such as complex operation process of the prior art, accelerated aging of experimental equipment, long reaction time, low purity, low cleanliness, powdery and difficult post-processing of the obtained ferric iron phosphide product

Method used

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  • Method for preparing ferrous phosphide Fe3P at high temperature and high pressure
  • Method for preparing ferrous phosphide Fe3P at high temperature and high pressure
  • Method for preparing ferrous phosphide Fe3P at high temperature and high pressure

Examples

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Embodiment example 1

[0035] Use analytically pure iron nanopowder (Fe) and red phosphorus powder (P) as starting materials, grind and mix them thoroughly in an agate mortar with alcohol at a molar ratio of 3:1, and take about 0.30 g of iron-phosphorus mixed powder for use The powder tablet press will be pressed into a cylinder of φ6mm×6mm, and the boron nitride ceramic rod will be processed into a boron nitride ceramic tube with a length of 10mm, an outer diameter of 10mm, and an inner diameter of 6mm, and placed in an oven at 150°C for 2 hours. , and then put the powder cylinder sample in a boron nitride ceramic tube, and seal it with 2mm boron nitride ceramic sheets up and down to complete the high-voltage assembly block. High voltage assembly block assembly method:

[0036] ① Drill a circular through hole with a diameter of 12mm in the center of the pyrophyllite cube of 32mm×32mm×32mm;

[0037] ②The circular through hole of the pyrophyllite block is covered with a graphite sleeve heating furna...

Embodiment example 2

[0042] Use analytically pure iron nanopowder (Fe) and red phosphorus powder (P) as starting materials, grind and mix them thoroughly in an agate mortar with alcohol at a molar ratio of 3:1, and take about 0.30 g of iron-phosphorus mixed powder for use The powder tablet press will be pressed into a cylinder of φ6mm×6mm, and the boron nitride ceramic rod will be processed into a boron nitride ceramic tube with a length of 10mm, an outer diameter of 10mm, and an inner diameter of 6mm, and placed in an oven at 150°C for 2 hours. , and then put the powder cylinder sample in a boron nitride ceramic tube, and seal it with 2mm boron nitride ceramic sheets up and down to complete the high-voltage assembly block. High voltage assembly block assembly method:

[0043] ① Drill a circular through hole with a diameter of 12mm in the center of the pyrophyllite cube of 32mm×32mm×32mm;

[0044] ②The circular through hole of the pyrophyllite block is covered with a graphite sleeve heating furna...

Embodiment example 3

[0049] Use analytically pure iron nanopowder (Fe) and red phosphorus powder (P) as starting materials, grind and mix them thoroughly in an agate mortar with alcohol at a molar ratio of 3:1, and take about 0.30 g of iron-phosphorus mixed powder for use The powder tablet press will be pressed into a cylinder of φ6mm×6mm, and the boron nitride ceramic rod will be processed into a boron nitride ceramic tube with a length of 10mm, an outer diameter of 10mm, and an inner diameter of 6mm, and placed in an oven at 150°C for 2 hours. , and then put the powder cylinder sample in a boron nitride ceramic tube, and seal it with 2mm boron nitride ceramic sheets up and down to complete the high-voltage assembly block. High voltage assembly block assembly method:

[0050] ① Drill a circular through hole with a diameter of 12mm in the center of the pyrophyllite cube of 32mm×32mm×32mm;

[0051] ②The circular through hole of the pyrophyllite block is covered with a graphite sleeve heating furna...

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Abstract

The invention discloses a method for preparing ferrous phosphide at high temperature and high pressure. The method comprises the following steps of using analytically pure ferrous nanometer powder andred phosphorus powder as starting raw materials; performing sufficient grinding and mixing on the analysis pure ferrous nanometer powder and the red phosphorus powder according to a mol ratio of 3:1in an agate mortar by using alcohol; using a tabletting machine for pressing the ground mixed powder into a cylindrical sample; processing a boron nitride ceramic rod into a round tube; putting the round tube into a baking oven to be baked; putting the cylindrical sample into the boron nitride round tube; sealing the upper and lower sides by using boron nitride ceramic sheets; then, putting a whole into a six-surface-top big pressing machine to be subjected to high-temperature and high-pressure reaction; taking out the reacted samples; clearing away boron nitride outside the sample to obtain apure Fe3P blocky sample. The technical problems that in the prior art, the reaction variable cannot be easily controlled, the quartz tube is corroded, the reaction time is long, the product purity islow, the crystallinity degree is low, the product is powder and cannot realize the later-stage processing, and the like are solved.

Description

technical field [0001] The invention belongs to the field of synthesis of functional materials, and in particular relates to a method for preparing Fe3iron phosphide under high temperature and high pressure. 3 P's method. Background technique [0002] In industry, iron phosphide Fe 3 P, also known as iron phosphide and ferrophosphorus, is a by-product of phosphorus chemical industry and is widely used in metallurgy, smelting, and chemical industries. Ultra-fine ferrophosphorus powder has the characteristics of electrical conductivity, heavy anti-corrosion, anti-marine biological adsorption, and environmental protection. It is a new technology product in the paint and coating industry, especially in replacing zinc powder. corrosion advantage. Has been widely used in epoxy zinc-rich primers, conductive coatings, fillers, etc., suitable for any paint coating as anti-rust and anti-corrosion pigments. In the field of earth sciences, meteorite [(FeNi) 3 P] is a common phospho...

Claims

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Application Information

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IPC IPC(8): C04B35/515C04B35/645C04B35/65
CPCC04B35/5154C04B35/645C04B35/65C04B2235/405C04B2235/42C04B2235/656
Inventor 尹远翟双猛李泽明
Owner INST OF GEOCHEM CHINESE ACADEMY OF SCI
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