CN105152151B - A kind of method that β tricalcium phosphates are prepared based on multi-D swing nano ball grinding - Google Patents
A kind of method that β tricalcium phosphates are prepared based on multi-D swing nano ball grinding Download PDFInfo
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- CN105152151B CN105152151B CN201510472440.1A CN201510472440A CN105152151B CN 105152151 B CN105152151 B CN 105152151B CN 201510472440 A CN201510472440 A CN 201510472440A CN 105152151 B CN105152151 B CN 105152151B
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Abstract
The invention belongs to biology medical material technical field, discloses a kind of method that β tricalcium phosphates are prepared based on multi-D swing nano ball grinding.Methods described includes following preparation process：Using multi-D swing nanon ball-mill by phosphorous raw material and the difference ball milling processing of calcic raw material, the raw material after processing dispensing and is then added into volatile dispersant in proportion, mixes and is uniformly dispersed under ultrasound and stirring condition, obtain slurry；Slurry is dried and removes dispersant, then high-temperature calcination carries out solid phase reaction, obtains powder；Powder is scattered in deionized water, filtered, β tricalcium phosphates are obtained after drying.The present invention use multi-D swing nano ball grinding process technology, process stabilizing, simple, is advantageous to mass production, gained β tricalcium phosphates purity height, has a good application prospect.
Description
Technical field
The invention belongs to biology medical material technical field, and in particular to one kind is prepared based on multi-D swing nano ball grinding
The method of bata-tricalcium phosphate.
Background technology
Bata-tricalcium phosphate not only has good biocompatibility, and has excellent bioactivity and biodegradable
Property, after implanting, material dissolves and absorbs the part for being converted into host freshman bone tissue self by body fluid, finally makes
The position of defect is substituted by the bone tissue of new life completely, is a kind of Biodegradable material of function admirable, in bone tissue work
Journey field plays huge effect.
In general the preparation method of bata-tricalcium phosphate mainly has wet processing, hydro-thermal method technique and dry process etc..It is wet
Method technique is synthesized by solution reaction, and small grains or amorphous powder can be made.Wet processing mainly have chemical precipitation method,
Three kinds of methods such as acid-base neutralization reaction method, alcoholic compound method.The reactant concentration of wet processing can not be too big, and rate of addition can not
Too fast, wherein chemical precipitation method also needs to use ammoniacal liquor constantly regulate pH value, and technique is complex.
Hydro-thermal method technique is in special closed reaction vessel, using the aqueous solution as reaction medium, to reaction vessel
Create a high temperature, the reaction environment of high pressure prepares a kind of method of material.Hydro-thermal method technique requires higher to reaction condition,
Using less and be unsuitable for producing in enormous quantities.
Dry process is to react to synthesize by raw material solid phase, and the preferable powder of crystallization can be made.Compare into dry process
Ripe mainly have a solid-phase synthesis, and traditional solid-phase synthesis uses planetary ball mill ball milling mixing raw material, raw material after ball milling
Particle diameter is larger, while often because raw material glues tank or slimeball makes in raw material that calcium phosphorus atoms are than unbalance in mechanical milling process, so as to cause
With the presence of impurities phase in obtained bata-tricalcium phosphate.
The content of the invention
In order to solve the shortcomings that above prior art and weak point, it is an object of the invention to provide one kind to be based on multidimensional
The method that swing type nano ball grinding prepares bata-tricalcium phosphate.
The object of the invention is achieved through the following technical solutions：
A kind of method that bata-tricalcium phosphate is prepared based on multi-D swing nano ball grinding, including following preparation process：
Phosphorous raw material and calcic raw material difference ball milling are processed using multi-D swing nanon ball-mill, after then processing
Raw material dispensing and add volatile dispersant in proportion, mix and be uniformly dispersed under ultrasound and stirring condition, obtain slurry；Will
Slurry, which is dried, removes dispersant, and then high-temperature calcination carries out solid phase reaction, obtains powder；Powder is scattered in deionized water,
Filter, bata-tricalcium phosphate is obtained after drying.
Preferably, described phosphorous raw material refers to the mixing of one or both of calcium monohydrogen phosphate and calcium pyrophosphate；It is described
Calcic raw material refer to the mixing of one or both of calcium carbonate and calcium hydroxide.
Preferably, the processing of described ball milling refers to 6~12h of ball milling under the conditions of rotating speed is 300~500r/min.
Preferably, described dispensing in proportion refers to carry out dispensing by Ca/P mol ratio for 1.50~1.64.
Preferably, described volatile dispersant refers to absolute ethyl alcohol or deionized water.
Preferably, the time of described ultrasound and stirring is 2~4h；The speed of stirring is 100~300r/min.
Preferably, described high-temperature calcination refers to calcine 2~3h under the conditions of temperature is 850~1100 DEG C.
(α represents angle of oscillation to the fundamental diagram of multi-D swing nanon ball-mill of the present invention in figure as shown in Figure 1
Degree).The ball grinding technique is moved by the multi-D swing of tank body high speed, makes irregular movement of the abrasive media in tank more acute
It is strong, the collision impact of the more intensity of multi-frequency is produced, powder stock is obtained by ball milling and more refines；Shock blind spot is reduced simultaneously,
Improve grinding efficiency.
The preparation method of the present invention has the following advantages that and beneficial effect：
(1) preparation technology of the invention is simple, less demanding to preparation condition, is advantageous to mass production；
(2) preparation technology of the invention is more stable, and it uses multi-D swing nano ball grinding process technology, makes raw material ball
Particle diameter after mill is smaller, scattered more stable in dispersant, so that solid phase reaction is more abundant；
(3) preparation method of the invention processes raw material elder generation ball milling, and then the method for dispensing avoids ball milling mistake in proportion
Calcium phosphorus atoms caused by gluing wall or slimeball in journey improve the purity of last obtained bata-tricalcium phosphate powder than unbalance.
Brief description of the drawings
Fig. 1 is the fundamental diagram of the multi-D swing nanon ball-mill of the present invention；
Fig. 2 is embodiment 1 using the calcium monohydrogen phosphate and the average grain of calcium carbonate after multi-D swing nanon ball-mill ball milling
The comparison diagram of average grain diameter behind footpath, with common planetary ball mill ball milling；
Fig. 3 is the XRD spectra of the gained bata-tricalcium phosphate powder of embodiment 1~3 and the comparison diagram of standard spectrogram；
Fig. 4 is the IR spectrograms of the gained bata-tricalcium phosphate powder of embodiment 1~3.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
Use multi-D swing nanon ball-mill that calcium monohydrogen phosphate and calcium carbonate are distinguished into ball milling with 300r/min rotating speed
6h, it is then 1.50 to weigh the calcium monohydrogen phosphate (CaHPO after ball milling according to Ca/P mol ratios4·2H2O) 37.86g and calcium carbonate
(CaCO3) 11.81g, add 70mL absolute ethyl alcohols；By above-mentioned mixed liquor under ultrasound electric stirring 3h, be sufficiently mixed it
It is uniformly dispersed, obtains slurry；Slurry is put in baking oven and dried, is then placed in Muffle furnace and calcines 3h at 900 DEG C, obtain powder
Body；Finally the powder after calcining is scattered in deionized water and filters drying, obtains bata-tricalcium phosphate powder.
The present embodiment use multi-D swing nanon ball-mill ball milling after calcium monohydrogen phosphate and calcium carbonate average grain diameter, with
Average grain diameter after common planetary ball mill ball milling is contrasted, and as a result (1# is common planetary ball mill ball in figure as shown in Figure 2
Calcium monohydrogen phosphate average grain diameter after mill, 2# are the average grain diameter of the calcium carbonate after common planetary ball mill ball milling, and 3# is this implementation
The average grain diameter of calcium monohydrogen phosphate after example multi-D swing nanon ball-mill ball milling, 4# is the present embodiment multi-D swing nanosphere
The average grain diameter of calcium carbonate after grinding machine ball milling).As seen from Figure 2, the raw material after the processing of multi-D swing nano ball grinding
Average grain diameter be significantly less than common planetary ball milling processing, the particle diameter of raw material is smaller, its mix in dispersant disperse it is more uniform,
Solid phase reaction will be more abundant, and the purity of obtained powder also can be higher.
Embodiment 2
Use multi-D swing nanon ball-mill that calcium pyrophosphate and calcium carbonate are distinguished into ball milling with 500r/min rotating speed
12h, it is then 1.50 to weigh the calcium pyrophosphate (Ca after ball milling according to Ca/P mol ratios2P2O7) 45.91g and calcium carbonate (CaCO3)
18.09g, add 100mL deionized waters；By above-mentioned mixed liquor under ultrasound electric stirring 4h, be sufficiently mixed it scattered equal
It is even, obtain slurry；Slurry is put in baking oven and dried, is then placed in Muffle furnace and calcines 2h at 1000 DEG C, obtain powder；Most
Powder after calcining is scattered in deionized water afterwards and filters drying, obtains bata-tricalcium phosphate powder.
Embodiment 3
Use multi-D swing nanon ball-mill that calcium pyrophosphate and calcium hydroxide are distinguished into ball milling with 400r/min rotating speed
9h, it is then 1.50 to weigh the calcium pyrophosphate (Ca after ball milling according to Ca/P mol ratios2P2O7) 45.91g and calcium hydroxide (Ca
(OH)2) 13.39g, add 90mL absolute ethyl alcohols；By above-mentioned mixed liquor under ultrasound electric stirring 4h, it is sufficiently mixed point
Dissipate uniformly, obtain slurry；Slurry is put in baking oven and dried, is then placed in Muffle furnace and calcines 3h at 850 DEG C, obtain powder
Body；Finally powder after calcining is scattered in deionized water and filters drying, obtains bata-tricalcium phosphate powder.
The XRD spectra of the gained bata-tricalcium phosphate powder of embodiment 1~3 and the comparison diagram of standard spectrogram are as shown in Figure 3；Its IR
Spectrogram is as shown in Figure 4.The bata-tricalcium phosphate free from admixture phase component that the present invention obtains it can be seen from Fig. 3 and Fig. 4, purity are higher.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (5)
- A kind of 1. method that bata-tricalcium phosphate is prepared based on multi-D swing nano ball grinding, it is characterised in that prepare step including following Suddenly：Phosphorous raw material and calcic raw material difference ball milling are processed using multi-D swing nanon ball-mill, then by the original after processing Expect dispensing in proportion and add volatile dispersant, mix and be uniformly dispersed under ultrasound and stirring condition, obtain slurry；By slurry Dry and remove dispersant, then high-temperature calcination carries out solid phase reaction, obtains powder；Powder is scattered in deionized water, filtered, Bata-tricalcium phosphate is obtained after drying；Described ball milling processing refers to 6~12h of ball milling under the conditions of rotating speed is 300~500r/min；Described ultrasound and stirring Time be 2~4h；The speed of stirring is 100~300r/min.
- 2. a kind of method that bata-tricalcium phosphate is prepared based on multi-D swing nano ball grinding according to claim 1, it is special Sign is：Described phosphorous raw material refers to the mixing of one or both of calcium monohydrogen phosphate and calcium pyrophosphate；Described calcic is former Material refers to the mixing of one or both of calcium carbonate and calcium hydroxide.
- 3. a kind of method that bata-tricalcium phosphate is prepared based on multi-D swing nano ball grinding according to claim 1, it is special Sign is：Described dispensing in proportion refers to carry out dispensing by Ca/P mol ratio for 1.50~1.64.
- 4. a kind of method that bata-tricalcium phosphate is prepared based on multi-D swing nano ball grinding according to claim 1, it is special Sign is：Described volatile dispersant refers to absolute ethyl alcohol or deionized water.
- 5. a kind of method that bata-tricalcium phosphate is prepared based on multi-D swing nano ball grinding according to claim 1, it is special Sign is：Described high-temperature calcination refers to calcine 2~3h under the conditions of temperature is 850~1100 DEG C.
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| CN106892414B (en) * | 2017-03-30 | 2019-05-17 | 华南理工大学 | A method of addition surfactant auxiliary ball mill prepares bata-tricalcium phosphate powder |
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| CN2437403Y (en) * | 2000-08-08 | 2001-07-04 | 吕庆 | Multi-D swing ball mill |
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| CN2437403Y (en) * | 2000-08-08 | 2001-07-04 | 吕庆 | Multi-D swing ball mill |
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| MA过程中W-Cu系纳米粉体的X射线相分析;张代东 等;《铸造设备研究》;20011231(第6期);15页第2栏倒数第18行至倒数第3行 * |
| β-磷酸三钙粉末和多孔β-磷酸三钙生物陶瓷的研制;张士华;《中国优秀博硕士学位论文全文数据库（硕士） 医药卫生科技辑》;20030615(第2期);第10页第6行至最后一行 * |
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