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A tetracalcium phosphate nano-powder with high mechanical properties for 3D printing and preparation method thereof

A 3D printing, tetracalcium phosphate technology, applied in the field of 3D printing materials, can solve the problems of failing to meet the requirements of cancellous bone, hindering TTCP, restricting technology development and medical applications, etc.

Active Publication Date: 2022-04-15
ZHONGSHAN POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) Mechanical properties are a prerequisite for the practical use of all bone repair materials, but the mechanical properties of the finished bone repair materials produced by the existing TTCP through 3D printers are poor (for example, the compressive strength is less than 10 MPa, and the bending strength is not higher than 1 MPa. ), not only far from meeting the requirements of compact bone, but even basically completely unable to meet the requirements of cancellous bone
This is the biggest key technical bottleneck of TTCP / 3D printing technology, which seriously restricts its further technical development and medical application.
[0006] (2) High-purity TTCP cannot be prepared through the existing technology, which also seriously restricts the application of TTCP / 3D printing technology in clinical medicine
Regardless of the dry process (high-temperature solid-phase method) or wet process, even if it is roasted at a high temperature of up to 1400 ° C for at least 5 hours, a series of intermediate products that hinder the formation of TTCP will still be formed during the roasting stage, resulting in many products such as triphosphate Calcium, hydroxyapatite and other by-products make the purity of TTCP very low

Method used

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  • A tetracalcium phosphate nano-powder with high mechanical properties for 3D printing and preparation method thereof
  • A tetracalcium phosphate nano-powder with high mechanical properties for 3D printing and preparation method thereof

Examples

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Effect test

Embodiment 1

[0042] A preparation method of tetracalcium phosphate nano powder with high mechanical properties for 3D printing, comprising the following steps:

[0043] (1) 1 part of lithium chloride, 20 parts of calcium nitrate, 5 parts of sodium chloride and 100 parts of water are added to the hydrothermal reaction kettle and fully stirred evenly;

[0044] (2) 0.1 part of cerium nitrate, 15 parts of water glass (modulus is 3.1) and 200 parts of water are fully mixed, and then slowly dripped into the hydrothermal reaction kettle to react with the mixture in the step (1), and the dropping time is 15min;

[0045] (3) Fully mix 10 parts of tetraisopropyl titanate and 200 parts of water, and then slowly drop them into the hydrothermal reaction kettle to react with the mixture in step (2), and the dropping time is 15 minutes;

[0046] (4) Airtightly raise the temperature to 110°C and keep it warm for 30 minutes, stop the reaction and cool down to room temperature to discharge, first filter th...

Embodiment 2

[0050] A preparation method of tetracalcium phosphate nano powder with high mechanical properties for 3D printing, comprising the following steps:

[0051] (1) 2.5 parts of lithium sulfate, 2.5 parts of lithium hydroxide, 25 parts of calcium nitrate, 25 parts of calcium chloride, 5 parts of sodium chloride and 100 parts of water are added to the hydrothermal reaction kettle and fully stirred evenly;

[0052] (2) Fully mix 0.25 parts of cerium sulfate, 0.25 parts of dysprosium nitrate, 30 parts of water glass (modulus 3.4) and 200 parts of water, then slowly drop them into the hydrothermal reaction kettle to react with the mixture in step (1) , the dropping time is 60min;

[0053] (3) Fully mix 15 parts of tetraisopropyl titanate, 15 parts of tetrabutyl titanate and 200 parts of water, and then slowly drop them into the hydrothermal reaction kettle to react with the mixture in step (2). 60min;

[0054] (4) Airtightly heat up to 130°C and keep it warm for 60 minutes, stop the ...

Embodiment 3

[0058] A preparation method of tetracalcium phosphate nano powder with high mechanical properties for 3D printing, comprising the following steps:

[0059] (1) Add 1 part of lithium chloride, 1 part of lithium sulfate, 1 part of lithium hydroxide, 15 parts of calcium nitrate, 15 parts of calcium chloride, 5 parts of sodium chloride and 100 parts of water into the hydrothermal reaction kettle and fully Stir well;

[0060] (2) Fully mix 0.1 part of cerium chloride, 0.1 part of dysprosium sulfate, 0.1 part of dysprosium chloride, 10 parts of water glass (modulus 3.2), 10 parts of water glass (modulus 3.3) and 200 parts of water, Then slowly drip into the hydrothermal reaction kettle to react with the mixture in the step (1), the dropping time is 30min;

[0061] (3) Fully mix 10 parts of tetraisopropyl titanate, 10 parts of tetrabutyl titanate and 200 parts of water, and then slowly drop them into the hydrothermal reaction kettle to react with the mixture in step (2). 30min;

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Abstract

The invention discloses a preparation method of tetracalcium phosphate nano-powder with high mechanical properties for 3D printing. The steps are as follows: (1) mixing lithium salt, calcium salt, sodium chloride and water; (2) mixing rare earth compound, water Mix the glass and water and add dropwise to the mixture in (1); (3) mix the titanium source and water and add dropwise to the mixture in (2); (4) seal the reactant prepared in (3) and heat up Insulation reaction, discharging after cooling down, filtering and washing to obtain a filter cake, roasting the filter cake to obtain a negatively charged phyllosilicate; (5) mixing the negatively charged phyllosilicate prepared in (4) with water, and then Add calcium chloride, disodium hydrogen phosphate, sodium hydroxide and calcium carbonate and mix evenly. Under airtight conditions, heat up and stir to react; (6) filter and wash the reaction solution obtained in (5) to obtain a filter cake. The cake is roasted, cooled, and ground to a particle size of no more than 200 mesh. The tetracalcium phosphate nano powder has excellent mechanical properties.

Description

technical field [0001] The invention belongs to the technical field of 3D printing materials, in particular to a tetracalcium phosphate nano-powder with high mechanical properties for 3D printing and a preparation method thereof. Background technique [0002] Human beings have been suffering from orthopedic diseases for a long time. Every year, a large number of patients suffer from orthopedic diseases and need surgical treatment such as bone defect repair and reconstruction. Therefore, bone repair biomaterials are widely used in clinical medicine, involving many fields of clinical medicine, such as orthopedic surgery, stomatology, and craniocerebral surgery. For a long time, people have gradually developed biomedical metal materials, polymer biorepair materials, etc., but these bone repair materials are not easy to shape, difficult to match the shape of bone defects, and have poor biocompatibility, large human immune rejection, and They cannot be degraded in the human body...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32B82Y40/00B33Y70/00
CPCC01B25/32B82Y40/00B33Y70/00C01P2006/80
Inventor 聂建华
Owner ZHONGSHAN POLYTECHNIC