Preparation method of high-osteoinductivity alpha-tricalcium phosphate nano-powder for 3D printing

A technology of tricalcium phosphate nanometer and 3D printing, which is applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, and can solve the instability of α-TCP and restrict the market application of α-TCP/3D printing technology and technology development, poor osteoinductive performance of α-TCP, etc., to achieve excellent osteoinductive performance, broad prospects for biomedical applications, and reduced energy costs

Pending Publication Date: 2022-03-08
ZHONGSHAN POLYTECHNIC
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0006] However, there are still some technical difficulties in the application of α-TCP to 3D printing, the most critical of which is the poor osteoinductive performance of α-TCP, which has almost no effect on promoting bone formation. This factor seriously restricts the further development of α-TCP / 3D printing technology. Market application and technology development
In addition, at present, people mainly obtain α-TCP nanopowder by high-temperature roasting and rapid cooling, but part of the α phase will still transform into β phase during the rapid cooling process, making it difficult to obtain high-purity α-TCP; and At the same time, since α-TCP is unstable at room temperature, it will transform into β phase in a small amount during storage.

Method used

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  • Preparation method of high-osteoinductivity alpha-tricalcium phosphate nano-powder for 3D printing
  • Preparation method of high-osteoinductivity alpha-tricalcium phosphate nano-powder for 3D printing

Examples

Experimental program
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Effect test

Embodiment 1

[0047] The highly osteoinductive α-tricalcium phosphate nanopowder for 3D printing described in Example 1 and its preparation method are prepared from the following raw material components in parts by mass according to the following steps:

[0048] (1) First, 1 part of Ce(NO 3 ) 3 , 0.1 part LiCl, 20 parts Ca(NO 3 ) 2 , 5 parts of sodium chloride and 500 parts of pure water were added to the hydrothermal reaction kettle and fully stirred evenly, then slowly dripped into 20 water glass with a modulus of 3.1, and the dropping time was controlled to be 15 minutes; Heat it to 150°C and keep it warm for 30 minutes; then stop the reaction and cool down to room temperature to discharge, first filter and wash the reaction liquid fully, and then roast the filter cake at 200°C for 10 minutes to prepare negatively charged phyllosilicate 1#.

[0049] (2) Then first add 0.1 part of negatively charged phyllosilicate 1# and 1000 parts of pure water prepared in the above steps (1) to the h...

Embodiment 2

[0051] The highly osteoinductive α-tricalcium phosphate nanopowder for 3D printing described in Example 2 and its preparation method are prepared from the following raw material components in parts by mass according to the following steps:

[0052] (1) First, 2.5 parts of Ce 2 (SO 4 ) 3 , 2.5 parts Dy(NO 3 ) 3 , 0.25 Li 2 SO 4 , 0.25 parts of LiOH, 25 parts of Ca(NO 3 ) 2 , 25 parts of CaCl 2 , 5 parts of sodium chloride and 500 parts of pure water were added to the hydrothermal reaction kettle and fully stirred evenly, then slowly dripped into 50 parts of water glass with a modulus of 3.4, and the dropping time was controlled to be 60 minutes; Raise the temperature to 200°C and keep it warm for 60 minutes; then stop the reaction and cool down to room temperature to discharge, first fully filter and wash the reaction solution, and then roast the filter cake at 300°C for 30 minutes to obtain negatively charged layered silicate 2# .

[0053] (2) then first add 0.5 part...

Embodiment 3

[0055] The highly osteoinductive α-tricalcium phosphate nanopowder for 3D printing described in Example 3 and its preparation method are prepared from the following raw material components in parts by mass according to the following steps:

[0056] (1) First, 1 part of CeCl 3 , 1 Dy 2 (SO 4 ) 3 , 1 part of DyCl 3 , 0.1 part LiCl, 0.1 part Li 2 SO 4 , 0.1 part of LiOH, 30 parts of Ca(NO 3 ) 2 , 30 parts of CaCl 2 , 5 parts of sodium chloride and 500 parts of pure water were added to the hydrothermal reaction kettle and fully stirred evenly, then slowly dripped into 30 parts of water glass with a modulus of 3.2, and the dropping time was controlled to be 30min; Raise the temperature to 160°C and keep it warm for 30 minutes; then stop the reaction and cool down to room temperature to discharge, first fully filter and wash the reaction solution, and then roast the filter cake at 250°C for 15 minutes to obtain negatively charged layered silicate 3# .

[0057] (2) then fir...

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Abstract

The preparation method of the high-osteoinductive alpha-tricalcium phosphate nano-powder for 3D printing comprises the following steps: S1, reactant mixing: firstly, mixing rare earth, lithium salt, calcium salt and a cosolvent in a solvent, and then slowly dropwise adding water glass; s2, hydrothermal reaction: carrying out reaction for 30 to 60 minutes at the temperature of 150 to 200 DEG C; s3, roasting: cooling the product, filtering and washing, and roasting the filter cake at 200-300 DEG C for 10-30 minutes to obtain electronegative layered silicate; s4, hydrothermal reaction: mixing reactants, heating to 100-150 DEG C, and reacting for 1-3 hours; s5, roasting: cooling a product, filtering, washing, and roasting a filter cake at 400-500 DEG C for 60-90 minutes; and S6, grinding: grinding a product to obtain the alpha-tricalcium phosphate nano powder. The problem of poor osteogenesis effect of the alpha-TCP / 3D printing bone finished product is creatively and thoroughly solved by introducing the electronegative layered lamellar crystals, the bone finished product is an ideal bone repair material, the bone induction performance of the bone finished product is excellent, and the bone induction performance of the bone finished product is far better than that of alpha-TCP similar products produced in the prior art or imported abroad, so that the bone finished product has very wide biomedical application prospects.

Description

technical field [0001] The present invention relates to the technical field of preparation of 3D printing materials, more specifically, to a method for preparing highly osteoinductive α-tricalcium phosphate nanopowder for 3D printing with high osteoinductivity, high purity and high stability. Background technique [0002] Studies have confirmed that calcium phosphate is an important component of inorganic substances in the bones of organisms. Bone repair materials with phosphates such as calcium phosphate as the main active ingredient have the advantage of biocompatibility and are a new type of bioactive material that has been widely used. . For example, the publication number is CN109650909A, which is a Chinese invention patent named a calcium phosphate osteoinductive bioceramic scaffold based on light-curing 3D printing technology and its preparation method. Growth provides space for osteoinductivity. [0003] Among them, the mixed system composed of one or several calci...

Claims

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Application Information

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IPC IPC(8): C01B25/32C01B33/20B33Y70/00B33Y70/10B33Y10/00B82Y40/00B82Y30/00A61L27/12A61L27/58A61L27/50
CPCC01B25/32C01B33/20B33Y70/00B33Y10/00B82Y40/00B82Y30/00A61L27/12A61L27/58A61L27/50C01P2006/80A61L2400/12A61L2430/02
Inventor 聂建华王俊侯勇江常胜余明君李金盛李彩凤
Owner ZHONGSHAN POLYTECHNIC
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