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Preparation method of phosphate ion-based particles

A phosphate ion and particle technology, which is applied in the field of preparation of calcium phosphate and magnesium phosphate, can solve the problem that the morphology and structure of calcium phosphate particles and magnesium phosphate particles are difficult to control

Active Publication Date: 2021-04-23
SOUTHWEST JIAOTONG UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The main purpose of the present invention is to provide a method for preparing calcium phosphate spherical particles and magnesium phosphate particles and a method for improving the industrialization process of the particles, so as to solve the difficulty in controlling the morphology and structure of calcium phosphate particles and magnesium phosphate particles in the prior art The problem

Method used

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  • Preparation method of phosphate ion-based particles
  • Preparation method of phosphate ion-based particles
  • Preparation method of phosphate ion-based particles

Examples

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example 1

[0102] This example illustrates method M1. According to method 1, calcium phosphate hollow spherical particles and / or magnesium phosphate particles are synthesized by calcium / phosphate ions and magnesium / calcium in different molar ratios, specifically: the phosphate solution containing phosphate ions is directly mixed with magnesium ions and calcium The cation solution of ions is mixed to form a clear aqueous solution, and the ionic ratio in the clear aqueous solution obtained by mixing different concentrations of phosphate solution and cationic solution is also different; then the clear aqueous solution is placed in an oven at 100°C for hydrothermal reaction for 6 hours; The pH of the clear aqueous solution was adjusted to 7 prior to hydrothermal treatment.

[0103] Table 1 shows the molar ratios of calcium / phosphate ions and magnesium / calcium in the clarified aqueous solutions and the morphology and composition of the corresponding precipitates.

[0104]

[0105] Table 1...

example 2

[0127] This example illustrates M2. Specifically: prepare different concentrations of disodium phosphate solutions and different concentrations of calcium chloride and magnesium chloride solutions according to the ratio in Table 3, and then heat them to 100° C. respectively, and then mix them.

[0128] Table 3 Morphology of particles obtained by reacting calcium ions, magnesium ions and phosphate ions at different concentrations.

[0129]

[0130] The precipitates are all hollow spherical nanoparticles with a size ranging from 50nm to 200nm, wherein, Figure 19 , Figure 20 , Figure 21 with Figure 22 The morphology of the precipitates synthesized by M2-1, M2-2, M2-3 and M2-4 methods are shown respectively. Figure 23 The XRD pattern corresponding to M2-2 shows that it is amorphous and its composition is calcium phosphate substituted with magnesium. Amorphous spherical particles have a shorter degradation time compared to crystalline calcium phosphate particles.

example 3

[0132] This example is described in terms of M1-LW. Specifically: 1) the lake water is sampled from Lake Mälaren, and the molar ratio of magnesium / calcium measured by inductively coupled plasma atomic emission spectrometry is 0.35; 2) disodium phosphate is then dissolved in undiluted lake water to form a 1.4 mM clear aqueous solution of phosphate ions; 3) Adjust the clear aqueous solution to pH 7, then heat it in an oven to 100°C and keep it warm for 3 hours. This process yields calcium phosphate nanoparticles with a particle size of about 100-250 nm, see Figure 24 . Its XRD spectrum shows that it is amorphous, see Figure 26 Curve a in.

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Abstract

The invention discloses a preparation method of phosphate ion-based particles, including a preparation method of calcium phosphate particles and / or magnesium phosphate particles and a preparation method of calcium phosphate nanoparticles. The preparation method of the calcium phosphate particles and / or magnesium phosphate particles comprises the following steps: 1) forming a clear aqueous solution at room temperature by mixing a cationic solution with a phosphate solution; the initial pH value of the clear aqueous solution is 4.0-10; 2 ) making the magnesium ions, calcium ions and phosphate ions generate calcium phosphate particles and / or precipitate magnesium phosphate particles through a hydrothermal method. The preparation method of the calcium phosphate nanoparticles comprises the following steps: 1) heating the cation solution to 60-100°C; 2) heating the phosphate solution to 60-100°C; 3) directly mixing the two solutions and immediately forming calcium phosphate nanoparticles Particles settle. The method is simple to operate and can effectively adjust the morphology and structure of calcium phosphate particles and magnesium phosphate particles.

Description

technical field [0001] The present invention relates to the technical field of preparation of calcium phosphate and magnesium phosphate, in particular to two methods for preparing crystalline and amorphous calcium phosphate spherical particles and magnesium phosphate particles, and a new method for their industrialization. The invention also describes the use of these particles in biological materials. Background technique [0002] Previous literatures have studied the synthesis method and application of spherical calcium phosphate (CaP) (Bohner M et al., Biomatter.2013; 3:e25103:1-14). Current synthetic methods of calcium phosphate spherical particles focus on spraying and self-assembly using surfactants and biomolecules (U.S. Pat. No 5,702,677; U.S. Pat. No 5,858,318; Wang P et al., Mater. Lett. 2009; 63: 1207–9; Hagmeyer D et al., J Mater Chem. 2011; 21:9219-25). [0003] Using microwave-assisted rapid synthesis, creatine phosphate (CP) was successfully used as phosphat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32
Inventor 秦伟伟秦涛
Owner SOUTHWEST JIAOTONG UNIV