A method of adding surfactant-assisted ball milling to prepare β-tricalcium phosphate powder

A technology of surfactant and tricalcium phosphate powder, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problem of β-tricalcium phosphate multi-impurity phase, imbalance of calcium-phosphorus atomic ratio, wide range of particle size distribution, etc. problems, to achieve the effect of solving the imbalance of raw material ratio, sufficient solid phase reaction and improving purity

Active Publication Date: 2019-05-17
SOUTH CHINA UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solid phase synthesis method is more mature in the dry process, but the particle size of the raw material after ball milling in the traditional process is large, and the particle size distribution range is wide. At the same time, the atomic ratio of calcium and phosphorus in the raw material is often unbalanced due to the sticking of the raw material to the pot or ball during the ball milling process. , resulting in more impurity phases in the prepared β-tricalcium phosphate

Method used

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  • A method of adding surfactant-assisted ball milling to prepare β-tricalcium phosphate powder
  • A method of adding surfactant-assisted ball milling to prepare β-tricalcium phosphate powder
  • A method of adding surfactant-assisted ball milling to prepare β-tricalcium phosphate powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Measure 1% of surfactant KW-300 into ethanol and ultrasonically disperse for 10 minutes. The proportion of ethanol is 0.5% of the total weight of calcium and phosphorus raw materials. Take by weighing 49.58g calcium hydrogen phosphate (CaHPO 4 2H 2 O) and 14.42g calcium carbonate (CaCO 3 );

[0029] (2) Transfer the raw materials and ethanol containing surface activity into the ball milling tank together, and ball mill and mix them for 3 hours at a speed of 300 r / min on the planetary ball mill, and the powder raw materials after mixing will not stick to the tank and balls;

[0030] (3) place the mixed slurry in an oven to dry at a temperature of 50° C. to remove ethanol, and then pass through a 50-mesh sieve;

[0031] (4) Put the sieved powder into a muffle furnace for calcination at 850° C. for 5 hours to obtain β-tricalcium phosphate powder.

[0032] figure 1 For the TG-DSC curve of the surfactant KW-300 added in this embodiment, it can be seen from the figur...

Embodiment 2

[0035] (1) Measure 2.5% of surfactant KW-300 into ethanol and ultrasonically disperse for 30 minutes. The proportion of ethanol is 1.5% of the total weight of calcium and phosphorus raw materials. Take by weighing 49.58g calcium hydrogen phosphate (CaHPO 4 2H 2 O) and 14.42g calcium carbonate (CaCO 3 );

[0036] (2) Transfer the raw materials and ethanol containing surface activity into a ball mill tank together, and ball mill and mix them for 9 hours at a speed of 400 r / min on a multi-dimensional swing nano ball mill, and the powder will not stick to the tank after mixing;

[0037] (3) place the mixed slurry in an oven to dry at a temperature of 60° C. to remove ethanol, and then pass through a 50-mesh sieve;

[0038] (4) Put the sieved powder into a muffle furnace and calcinate at 900° C. for 3 hours to obtain β-tricalcium phosphate powder.

[0039] Figure 4 The XRD spectrum of the β-tricalcium phosphate powder prepared for this example was compared with the standard s...

Embodiment 3

[0041] (1) Measure 5% of surfactant KW-300 into ethanol and disperse it ultrasonically for 25 minutes. The ratio of ethanol is 3% of the total weight of calcium and phosphorus raw materials. Take by weighing 49.58g calcium hydrogen phosphate (CaHPO 4 2H 2 O) and 14.42g calcium carbonate (CaCO 3 );

[0042] (2) Transfer the raw materials and ethanol containing surface activity into a ball mill tank, and ball mill and mix them for 6 hours at a speed of 500 r / min on a planetary ball mill, and the powder will not stick to the tank after mixing;

[0043] (3) Place the mixed slurry in an oven to dry at a temperature of 70° C. to remove ethanol, and then pass through a 50-mesh sieve;

[0044] (4) The sieved powder was put into a muffle furnace and calcined at 950° C. for 3 hours to obtain β-tricalcium phosphate powder.

[0045] The test results of the β-tricalcium phosphate powder prepared in this example are similar to those in Example 1 and Example 2, and will not be repeated h...

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Abstract

The invention discloses a method for adding a surfactant to assist in ball milling to prepare Beta-tricalcium phosphate powder, comprising: (1) adding the surfactant, polyester macromolecular compound KW-300, into a dispersant, and ultrasonically dispersing; (2) weighing dicalcium phosphate and calcium carbonate as raw materials at calcium / phosphorus ratio of 1.40 to 1.60; (3) transferring the dispersant containing the surfactant and the raw materials into a ball milling tank for ball milling so as to obtain mixed slurry; (4) drying the mixed slurry in an oven, and removing the dispersant to obtain dried powder; (5) grinding the dried powder, screening, and calcining at 850-1000 DEG C to obtain the Beta-tricalcium phosphate powder. The Beta-tricalcium phosphate powder that is ball-milled has smaller particle size and more uniform distribution, solid-phase reaction is more sufficient, calcium-phosphorus atom ratio imbalance due to tank sticking and sphere sticking during ball milling of the raw materials is avoided, and the purity of the prepared Beta-tricalcium phosphate powder is further improved.

Description

technical field [0001] The invention relates to a preparation method of β-tricalcium phosphate, in particular to a method for preparing β-tricalcium phosphate powder by adding a surfactant to assist ball milling. Background technique [0002] β-Tricalcium phosphate is a biodegradable material with excellent biological activity and good biocompatibility, and plays a huge role in bone tissue engineering and other fields. At present, the preparation methods of β-tricalcium phosphate mainly include wet method, hydrothermal method and dry method. The process of wet method is relatively complicated, and the requirements for reaction conditions such as reactant concentration and pH value are relatively high. The hydrothermal method requires high temperature and high pressure reaction conditions, which is rarely used and is not suitable for mass production. The dry method is synthesized by solid-phase reaction of raw materials, the preparation process is simple, and the obtained p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32
CPCC01B25/321C01P2002/72C01P2002/82C01P2002/88C01P2004/52
Inventor 任力王迎军康军沛杨军忠刘卅王琳
Owner SOUTH CHINA UNIV OF TECH
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