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A method for preparing high-purity ultrafine tricalcium silicate powder by wet chemical method

A technology of ultra-fine silicic acid and wet chemical method, applied in the direction of silicate, alkaline earth metal silicate, etc., can solve the problems of complicated and lengthy preparation process, repeated and cumbersome process, long holding time, etc., to achieve high purity and improve sintering. Active, the effect of reducing the holding time

Active Publication Date: 2020-01-21
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the defects of high sintering temperature, repeated and cumbersome process and long holding time in the traditional solid-state sintering method in the prior art; Larger particle size and other defects, the present invention provides a method for preparing high-purity ultrafine tricalcium silicate powder by wet chemical method, using TEOS as silicon source and CaC 2 o 4 As a calcium source, the silicon source and the calcium source are uniformly mixed on the nanoscale under wet chemical preparation conditions, and high-purity ultrafine C 3 S powder, this method simplifies the preparation process, improves the synthesis efficiency, and is easy to promote and large-scale commercial production

Method used

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  • A method for preparing high-purity ultrafine tricalcium silicate powder by wet chemical method
  • A method for preparing high-purity ultrafine tricalcium silicate powder by wet chemical method
  • A method for preparing high-purity ultrafine tricalcium silicate powder by wet chemical method

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Experimental program
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Effect test

Embodiment 1

[0033] Accurately weigh 0.2mol TEOS, 0.6mol CaC 2 o 4 , 0.8mol C 2 h 5 OH, about 90ml deionized water, add the weighed TEOS to deionized water and C 2 h 5 In the mixed solution of OH, the pH value of the solution was adjusted to 1 with nitric acid, and evenly dispersed active SiO was obtained after stirring for 1 hour. 2 Sol. CaC 2 o 4 Added in portions to the active SiO under stirring 2 sol, and set the heating temperature of the magnetic stirrer to 30 ° C to obtain SiO after stirring for 2 hours 2 and CaC 2 o 4 Uniformly mixed suspension slurry; place the above suspension slurry in a 120°C drying oven to fully dry, and then grind to obtain SiO 2 and CaC 2 o 4 Mix the powder evenly, and press it into a flake-shaped raw meal with a pressure of 10 MPa; calcinate the flake-shaped raw meal at 1400 ° C for 6 hours, and sinter the C 3 S was put into a planetary ball mill and milled at 400r / min for 3 hours to obtain high-purity ultrafine C 3 S powder.

Embodiment 2

[0035] Accurately weigh 0.2mol TEOS, 0.6mol CaC 2 o 4 , 1mol C 2 h 5 OH, about 72ml of deionized water, add the weighed TEOS to distilled water and C 2 h 5 In the mixed solution of OH, the pH value of the solution was adjusted to 1 with nitric acid, and evenly dispersed active SiO was obtained after stirring for 1 hour. 2 Sol. CaC 2 o 4 Added in portions to the active SiO under stirring 2 sol, and set the heating temperature of the magnetic stirrer to 30 ° C to obtain SiO after stirring for 4 hours 2 and CaC 2 o 4 Uniformly mixed suspension slurry; place the above suspension slurry in a 120°C drying oven to fully dry, and then grind to obtain SiO 2 and CaC 2 o 4 Mix the powder evenly, and press it into a flake-shaped raw meal with a pressure of 10MPa; calcinate the flake-shaped raw meal at 1450°C for 6 hours, and sinter the 3 S was put into a planetary ball mill and milled at 350r / min for 3 hours to obtain high-purity ultrafine C 3 S powder.

Embodiment 3

[0037] Accurately weigh 0.5mol TEOS, 1.5mol CaC 2 o 4 , 2mol C 2 h 5 OH, about 180ml deionized water, add the weighed TEOS to deionized water and C 2 h 5 In the mixed solution of OH, the pH value of the solution was adjusted to 1.5 with nitric acid, and evenly dispersed active SiO was obtained after stirring for 1 hour. 2 Sol. CaC 2 o 4 Added in portions to the active SiO under stirring 2 sol, and set the heating temperature of the magnetic stirrer to 60 ° C to obtain SiO after stirring for 2 hours 2 and CaC 2 o 4 Uniformly mixed suspension slurry; place the above suspension slurry in a 120°C drying oven to fully dry, and then grind to obtain SiO 2 and CaC 2 o 4 Mix the powder evenly, and press it into flake-shaped raw meal with a pressure of 10MPa; calcinate the flake-shaped raw meal at 1400°C for 12 hours, and sinter the 3 S was put into a planetary ball mill and milled at 300r / min for 6 hours to obtain high-purity ultrafine C 3 S powder.

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Abstract

The invention discloses a method for preparing high-purity and superfine tricalcium silicate powder by virtue of a wet chemical method, belonging to the fields of building materials and biomaterials.The method comprises the steps of by respectively adopting TEOS and CaC2O4 as a silicon source and a calcium source, TEOS as a raw material and deionized water and ethanol as solvents, adjusting the pH value by utilizing nitric acid as a catalyst, preparing uniformly scattered active SiO2 sol, adding a corresponding proportion of CaC2O4, stirring at a proper temperature to obtain uniformly mixed SiO2-CaC2O4 suspension slurry, drying, carrying out uniform pressure formation, calcining at 1400-1450 DEG C, and carrying out ball milling, so as to obtain high-purity and superfine C3S powder, wherein the content of free calcium oxide (f-CaO) in the powder can be below 0.5%, the average particle size of the powder is 2.92-4.01 microns, and the specific surface area of the powder can reach 2060m<2> / kg. Compared with a traditional solid-phase sintering method, the method has the advantage that the high-purity, fine-particle and large-specific surface area C3S powder can be obtained under the conditions of relatively low energy consumption and environmental friendliness; and compared with a traditional method, the method has the advantages of simplicity, feasibility, time conservation, convenience in production and popularization and the like.

Description

technical field [0001] The invention belongs to the field of building materials and biological materials, and relates to a preparation method of high-purity ultrafine tricalcium silicate powder, specifically a wet chemical method for preparing high-purity ultrafine tricalcium silicate (C 3 S) Powder method. Background technique [0002] With the rapid development of human architectural civilization and science and technology, people have higher and higher requirements for the strength and durability of engineering building components, and the properties of cementitious materials have an important impact on their strength and other properties. Tricalcium silicate (3CaO SiO 2 ,C 3 S) Portland cement clinker as the main hydraulic gelling component is widely used in construction, roads, tunnels and other infrastructure fields. On the other hand, the researchers found that C 3 S has good in vitro degradability, excellent bioactivity and biocompatibility, as well as arbitrary ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/24C04B7/02
CPCC01B33/24C01P2002/72C01P2004/04C01P2004/61C01P2006/12C04B7/02
Inventor 汪涛吴蒙李峰黄卫星
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS