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Method for preparing nano-hydroxyapatite with assistance of segmented pulse ultrasound

A technology of nano-hydroxyapatite and hydroxyapatite, which is applied in the direction of nanotechnology, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of high preparation cost and toxicity of organic solvents, and achieve excellent adsorption performance and large adsorption capacity , the effect of rich pores

Pending Publication Date: 2021-04-13
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main problem of this method is that the preparation cost is high, and the organic solvent used is toxic

Method used

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  • Method for preparing nano-hydroxyapatite with assistance of segmented pulse ultrasound
  • Method for preparing nano-hydroxyapatite with assistance of segmented pulse ultrasound
  • Method for preparing nano-hydroxyapatite with assistance of segmented pulse ultrasound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1 Existing ultrasonic-assisted method for preparing nano-hydroxyapatite

[0043] A. Dissolve 2.736g of dipotassium hydrogen phosphate and 0.7286g of D-sorbitol in 100ml of SBF solution to form a 0.12mol / L phosphorus source solution; dissolve 2.22g of anhydrous calcium chloride in 100ml of SBF solution Form a 0.20mol / L calcium source solution, then pour the calcium source solution directly into the phosphorus source solution and stir the suspension for 1h. After the suspension was placed in a 40 kHz, 50 W ultrasonic wave for 10-60 min, it was washed twice with water and ethanol to remove excess ions. Finally, the product was heated and dried in an oven to obtain powdered HAP.

[0044] The reaction time of the method exceeds 1 hour, and the prepared nano-hydroxyapatite has a length of 200 nm and a diameter of about 30 nm.

[0045] B. Take 0.5mol / L CaCl respectively 2 solution, 0.5mol / L NH 4 h 2 PO 4 After mixing 30 mL and 50 mL of the solution, adjust the pH...

Embodiment 2

[0050] Example 2 The method for preparing nano-hydroxyapatite assisted by segmental pulse ultrasound under different pulse ultrasound working conditions according to the present invention

[0051] In order to study the modification effect of different pulsed ultrasonic conditions, a total of 10 kinds of material preparation experiments were designed, and the specific pulsed ultrasonic conditions are shown in the table.

[0052]

[0053] * The t1 segment refers to the drug mixing and stirring segment, and the t2 segment refers to the drug reaction segment. The number represents the duration of the ultrasonic wave, and 36s / 18s represents the duration of an ultrasonic pulse.

[0054] Working condition No. 6 (t1-1s / 35s; t2-16s / 2s)

[0055] (1) (preheating cycle) Take calcium nitrate tetrahydrate solid and add ultrapure water to prepare a solution with a concentration of 0.025mol / L, then take 250ml and pour it into an ultrasonic reactor, turn on the magnetic stirring, insert a t...

Embodiment 3

[0068] Example 3 Results Analysis of Segmented Pulse Ultrasound Assisted Preparation of Nano-Hydroxyapatite under Different Pulse Conditions

[0069] Nano hydroxyapatite SEM figure prepared by this method (see figure 2 ) shows that the prepared nano-hydroxyapatite nanoparticles are rod-shaped and spherical, with a width of 9nm and a length of 40nm. 2 / g.

[0070] XRD test (see image 3 ) shows that the phase of the material is mainly Ca 10 (PO 4 ) 6 Oh 2 , while FTIR (see Figure 4 ) shows that the material has PO 4 2- group and OH - . Comparing the XRD and FTIR patterns of 10 materials, it can be found that the crystalline phase of the materials is roughly similar, and does not change with the length of the pulse ultrasound, indicating that ultrasound will not change the material changes during the material preparation process. But at 1100cm -1 Appearing on the left and right represents PO 4 2- The absorption vibration peaks of No. 4 and No. 8 are slightly large...

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Abstract

The invention discloses a method for preparing nano-hydroxyapatite with the assistance of segmented pulse ultrasound in order to overcome the defects of existing hydroxyapatite material preparation technologies. According to different energy requirements of material mixing and reaction stages, pulse ultrasound is increased in a segmented mode, cavitation of ultrasonic waves in water is utilized, the temperature and time needed by the reaction are reduced, and the method has the advantages of being simple, low in energy consumption, short in reaction time and safe in process. According to the method, the reaction time of the raw materials is only about 40 minutes, and the prepared hydroxyapatite nanoparticles are rod-shaped and spherical, have the width of 9 nm and the length of 40 nm, have the particle size of about 13.4 nm, belong to ultrafine nanoparticles, have the specific surface area of 140 m<2> / g, are rich in pores and have PO42-functional groups with strong activity. Therefore, the hydroxyapatite nanoparticles have a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and relates to a preparation method of hydroxyapatite material, in particular to a method for preparing nano-hydroxyapatite assisted by segmental pulse ultrasound. The high-quality nano-hydroxyapatite material prepared by the method can be used to control the problem of environmental heavy metal pollution. Background technique [0002] Hydroxyapatite (molecular formula: Ca 10 (PO 4 ) 6 (OH) 2 , referred to as HAP) is the main component of bones and teeth, and is a weakly alkaline calcium phosphate material with low solubility (pH=7-9). Its structure is very flexible, and all anions and cations and groups can be replaced under the condition of charge balance. In addition, such compounds exhibit good chemical stability, as well as thermal stability. These properties make hydroxyapatite have good application prospects in the fields of biomaterials, optics, radiation, environment, a...

Claims

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Application Information

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IPC IPC(8): C01B25/32B82Y40/00
CPCC01B25/325B82Y40/00C01P2004/16C01P2004/32C01P2004/64C01P2006/12
Inventor 葛仕福王玺玉周彩铃
Owner SOUTHEAST UNIV
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