Preparation method of calcium phosphate

A technology of calcium phosphate and calcium compounds, which is applied in the field of calcium phosphate, can solve problems such as unfavorable continuous chemical industry mass production, unfavorable mass production, and limited synthetic applications, so as to shorten the molecular diffusion distance, strengthen mixing kinetics, and ensure stable and reliable reproducible effect

Inactive Publication Date: 2015-04-01
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent 200610055171.X uses the water-soluble polymer compound polyvinylpyrrolidone (PVP) as a template, and uses calcium nitrate and ammonium phosphate as raw materials. It is left to stand at 25°C for 7 days at room temperature, and the resulting precipitate is washed, suction-filtered, Spherical hydroxyapatite nanocrystalline products can be obtained by drying. This method requires long-term aging, long production cycle, and cumbersome procedures, which is not conducive to the realization of continuous chemical industry mass production.
[0005] Chinese patent 03142004.4 and the journal paper "Journal of Inorganic Materials", 2004, 19 (01): 234-238. all report a kind of preparation method of amorphous nano-calcium phosphate, the synthesis temperature of this kind of method is lower range is 0~20 °C, which limits its synthetic application at room temperature or higher temperature, the energy consumption for cooling is high, and the synthesis cycle is long
[0006] Chinese patent 201110263963.7 discloses a synthesis method of amorphous calcium phosphate, which is synthesized in an ultrasonic environment at 0°C, so it cannot be synthesized at room temperature
In addition, special ultrasonic equipment needs to be added, and the synthesis time is long, which is not conducive to mass production

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 1. The raw material solution of phase A is prepared by mixing 0.2M calcium nitrate and 1M triethanolamine solution;

[0061] 2. Preparation of phase B raw material solution, which is 0.12M disodium hydrogen phosphate solution;

[0062] 3. Adjust the back pressure of the closed system to 2.2MPa, and set the flow rate F of the phase A raw material liquid delivery pump A =75mL / min, the flow rate F of the phase B raw material liquid delivery pump B =75mL / min;

[0063] 4. Run the two-phase delivery pump to simultaneously transport the two-phase raw material liquid to the microchannel continuous mixing reactor with a channel size of 105 μm for uniform mixing reaction;

[0064] 5. Pass the mixed product through a rapid heating heat exchanger to make the system temperature reach 145°C;

[0065] 6. Enter the constant temperature of 145°C for 6s, and transport it to the rapid cooling heat exchanger to reduce the system temperature to 25°C;

[0066] 7. The cooled reaction prod...

Embodiment 2

[0070] 1. The raw material solution of phase A is prepared by mixing 0.2M calcium nitrate and 1M triethanolamine solution;

[0071] 2. Preparation of phase B raw material solution, which is 0.12M disodium hydrogen phosphate solution;

[0072] 3. Set the flow rate F of the phase A raw material liquid delivery pump A =75mL / min, the flow rate F of the phase B raw material liquid delivery pump B =75mL / min, at room temperature of 25°C under normal pressure, the two-phase raw material liquid is simultaneously transported to a microchannel continuous mixing reactor with a channel size of 105μm. Form calcium phosphate aggregate sol;

[0073] 4. Transport the mixed reaction product calcium phosphate aggregate sol to a washing and dehydrating device, wash twice with water and once with ethanol, and vacuum dry at 60°C to constant weight to obtain calcium phosphate powder.

[0074] The results of X-ray powder diffraction analysis are as follows: Figure 6 , is a typical diffuse peak o...

Embodiment 3

[0076] 1. The raw material solution of phase A is prepared by mixing 0.19M calcium nitrate and 1M triethanolamine solution;

[0077] 2. Preparation of phase B raw material solution, which is 0.12M disodium hydrogen phosphate solution;

[0078] 3. Adjust the back pressure of the closed system to 2.2MPa, and set the flow rate F of the phase A raw material liquid delivery pump A =75mL / min, the flow rate F of the phase B raw material liquid delivery pump B =75mL / min;

[0079] 4. Run the two-phase delivery pump to simultaneously transport the two-phase raw material liquid to the microchannel continuous mixing reactor with a channel size of 105 μm for uniform mixing reaction;

[0080] 5. Pass the mixed product through a rapid heating heat exchanger to make the system temperature reach 100°C;

[0081] 6. Enter the constant temperature of 100°C for 6s, and transport it to the rapid cooling heat exchanger to reduce the system temperature to 25°C;

[0082] 7. The cooled reaction produ...

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Abstract

The invention provides a preparation of calcium phosphate, relates to calcium phosphate, and provides a preparation method of calcium phosphate, which has the advantages that production is continuous and high in yield stable, required raw materials are simple, reaction conditions are mild and controllable, production cycle is short and product quality is uniform and stable. The method comprises the following steps of: 1) preparing raw materials; 2) delivering clear liquid of phase A and clear liquid of phase B prepared in the step 1) to a microchannel continuous mixing system through a metering pump of a raw material delivery system so that liquid components of each phase are uniformly differentiated, and performing a continuous integral reaction to form a calcium phosphate aggregate; 3) delivering the calcium phosphate aggregate obtained in the step 2) to a heating system; 4) feeding into an insulating system; 5) feeding into a cooling system; and 6) delivering the cooled reaction product to a dehydration cleaning device, and drying the cleaned product to obtain calcium phosphate nano-particle powder.

Description

technical field [0001] The invention relates to calcium phosphate, in particular to a method for preparing calcium phosphate based on differential reaction technology. Background technique [0002] Calcium phosphate is widely used in the field of biomedical bone tissue repair because of its better biocompatibility, bioactivity, osteoinductivity and biodegradability. The latest applications also include adsorption of heavy metals in water treatment, drug release, cosmetic repair, cosmetic additives and toothpaste additives. [0003] Chinese patent 200310105951.7 uses calcium nitrate, diammonium hydrogen phosphate and urea as raw materials, uses a multi-frequency sonochemical generator to carry out sonochemical synthesis, filters the suspension, washes, and vacuum-dries to obtain nano-hydroxyapatite powder, and the obtained Hydroxyapatite powder has small particle size, uniform particle size, and no agglomeration. Because the synthesis temperature (40-80°C) is relatively low,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32
Inventor 谢容泉林亚庆关涛关栋云
Owner 关涛
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