CN102173401A

CN102173401A - Preparation method of submicron natural hydroxyapatite (HAp)

Info

Publication number: CN102173401A
Application number: CN2011100507811A
Authority: CN
Inventors: 韩凤兰; 吴澜尔
Original assignee: North Minzu University
Current assignee: North Minzu University
Priority date: 2011-03-03
Filing date: 2011-03-03
Publication date: 2011-09-07

Abstract

The invention discloses a preparation method of submicron natural hydroxyapatite (HAp). Wet grinding is adopted, and sodium hexametaphosphate ((NaPO3)6) serves as a dispersing agent; the mass ratio of the (NaPO3)6 to the HAp is 0.004; a grinding medium for the wet grinding is a corundum ball; and grinding time is 8 to 10 hours. The method is simple in process, relatively low in cost and relatively low in time consumption. A powder material of the prepared natural HAp can be used for preparing biological ceramics.

Description

The preparation method of the natural hydroxyapatite of a kind of submicron

Technical field

The present invention relates to chemical technology field, relate in particular to the preparation method of the natural hydroxyapatite of a kind of submicron, the natural hydroxy apatite powder material of preparation can be used for preparing biological ceramics.

Background technology

1972, Japanese scholar Aoki, the successful in succession synthesizing hydroxylapatite of American scholar Jarcho also sinters pottery into.1974-1975, the hydroxylapatite ceramic that discoveries such as Aoki are burnt till has good bio-compatibility.From then on, omnibearing fundamental research and clinical application research have all been carried out to hydroxyapatite material in countries in the world.80 years hydroxylapatite ceramics that begin one's study of China, units such as Wuhan Polytechnical Univ, Sichuan University, Shandong Industrial Ceramic Design Institute, Aviation Material Inst., Beijing's stomatology institute all successfully develop hydroxylapatite ceramic, and have carried out many clinical studyes.The preparation method of hydroxy apatite powder is a lot, and solid reaction process is dried preparation; Hydrothermal synthesis method; Sol-gel method; Chemical precipitation method etc.

Solid reaction process is dried preparation, is with solid-state calcium phosphate and other compound uniform mixing, have that water vapour exists, temperature is higher than the method that reaction under 1000 ℃ the condition obtains hydroxy apatite powder.

The hydroxyapatite powder that dry method is produced, no lattice shrinks, and crystal property is good, but powder grain is thick, often has impurity to exist mutually, and not only time-consuming but also easy pickup when grinding is therefore in the less employing in biological ceramics field.

Hydrothermal synthesis method is in an airtight pressurized vessel, makes reaction medium with the aqueous solution, by to reaction vessel heating, makes indissoluble or insoluble substance dissolves and recrystallization under usual conditions.

This method complex technical process is difficult to obtain the hydroxyapatite of quantitative Ca/P.

Sol-gel method is at first to dissolve alkoxide and make hydrolysis of alkoxide, polymerization by adding distilled water in organic solvent, forms colloidal sol.Then, along with the adding of water, colloidal sol changes gel into, and gel is by cryodrying under the vacuum state and height

But its cost of material height, when organic solvent toxicity and high-temperature heat treatment particle easily fast factor such as reunion restricted the application of this method.

Chemical precipitation method is that the aqueous solution of certain density calcium salt and microcosmic salt is stirred, and by control pH value chemical reaction takes place, and obtains gluey hydroxyapatite product, grinds by calcination and obtains its crystal powder.

The problem that this method exists is: grinding is consuming time longer with the granularity screening process, and gained hydroxyapatite crystal grain is easily reunited, and powder granularity control out of true and flowability are generally relatively poor.

Summary of the invention

Technical problem to be solved by this invention is the preparation method that the natural hydroxyapatite of a kind of submicron is provided at the deficiencies in the prior art.

The present invention is by the following technical solutions:

The preparation method of the natural hydroxyapatite of a kind of submicron adopts wet grinding, is dispersion agent with the Sodium hexametaphosphate 99.

Described preparation method, described Sodium hexametaphosphate 99 consumption is: m (NaPO ₃) ₆: m (HAp)=0.4%.

Described preparation method, described grinding grinding medium is the corundum ball.Milling time is 8-10h.

The inventive method technology is simple, and cost is lower, and is consuming time shorter.

Description of drawings

Fig. 1 is the process flow sheet of the inventive method;

Fig. 2 is the D50 of the embodiment of the invention 1 gained powder and the relation of Sodium hexametaphosphate 99 add-on;

Fig. 3 is the D50 of the embodiment of the invention 2 gained powders and the relation of Sodium hexametaphosphate 99 add-on;

Fig. 4 is the SEM figure of the embodiment of the invention 2 gained submicron hydroxyapatites.

Embodiment

Below in conjunction with specific embodiment, the present invention is described in detail.

Embodiment 1: with reference to figure 1, wet grinding is ground HAp powder weight 100g, Al with the small-sized stirring in laboratory ₂O ₃Mill Jie corundum ball 300g, water 100ml, rotating speed 1500r/min.Use Sodium hexametaphosphate 99 to be dispersion agent, the consumption of Sodium hexametaphosphate 99 is according to m (NaPO ₃) ₆: m (HAp) is respectively 0.5%, 1%, 2%, 3%, 4% and experimentizes, and milling time is 8h, and the HAP (white solution) that takes out in the shredder crosses 100 mesh sieves, precipitates 20 hours, oven for drying 12 hours, granularity Detection.The result as shown in Figure 2, as can be seen from Figure 2, as the dispersion agent (NaPO that adds ₃) ₆: m (HAp) is 0.5% o'clock, the D50 minimum.But can't determine that also this is (NaPO ₃) ₆Best add-on.As can be seen from Figure 1, the concentration of the dispersion agent of adding is too big, supersaturation absorption situation can occur, and the wetting ability of solid surface descends on the contrary, is unfavorable for molten wet and dispersion.

Embodiment 2: different with embodiment is, according to m (NaPO ₃) ₆: m (HAp) is respectively 0.1%, 0.2%, 0.4%, 0.6%, 0.8% and experimentizes, and milling time is 10h, measures the granularity of this group powder, its size-grade distribution such as Fig. 3.Shown in, as the dispersion agent (NaPO that adds ₃) ₆: m (HAp) is 0.4% o'clock, the D50 minimum.From electromicroscopic photograph Fig. 4 as can be seen, use Sodium hexametaphosphate 99 to be dispersion agent, the add-on of dispersion agent is 0.4% o'clock, and the granularity of superfine powder has reached submicron order, and some has reached nano level.

Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.

Claims

1. the preparation method of the natural hydroxyapatite of submicron is characterized in that, adopts wet grinding, is dispersion agent with the Sodium hexametaphosphate 99.

2. preparation method according to claim 1 is characterized in that, described Sodium hexametaphosphate 99 consumption is: m (NaPO ₃) ₆: m (HAp)=0.4%.

3. preparation method according to claim 1 is characterized in that, described grinding grinding medium is the corundum ball.Milling time is 8-10h.