CN1292803C - Preparation for artificial bone-filling material with hollow ball structure - Google Patents
Preparation for artificial bone-filling material with hollow ball structure Download PDFInfo
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- CN1292803C CN1292803C CNB2005100416215A CN200510041621A CN1292803C CN 1292803 C CN1292803 C CN 1292803C CN B2005100416215 A CNB2005100416215 A CN B2005100416215A CN 200510041621 A CN200510041621 A CN 200510041621A CN 1292803 C CN1292803 C CN 1292803C
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Abstract
The present invention relates to a method for preparing artificial bone filler with a hollow ball structure. The present invention comprises the following steps that adhesive is dropped into a polyvinyl chloride ball body, and thus, a macromolecular template of the ball body is manufactured; the template is dipped in slurry after solidified, and is dried and sintered, and thus, hydroxyapatite or beta-tricalcium phosphate bioceramic with a hollow ball structure is manufactured. The granular bioceramic with the hollow ball structure prepared by the method of the present invention is used for the bone filling. The single particle uses active bioceramic as main material, has good biocompatibility and high intensity, and can provide brackets for new bones. Simultaneously, the internal surface area and the external surface area of the hollow ball body are large, which provides sufficient space for cells to grow; the hollow ball body can be used for storing or adsorbing medicaments. The present invention has double functions of filling of bone defects and drug release bodies.
Description
Technical field
The present invention relates to a kind of preparation method of artificial bone-filling material, particularly a kind of preparation method of artificial bone-filling material of hollow ball structure.
Background technology
The hydroxyapatite spherical granule is widely used as bone filler and pharmaceutical carrier at present, Chinese patent " built-in anti-tuberculosis anti-cancer anti-inflammation slow released material " (ZL92111035.9, open day on November 17th, 1993, publication number CN 1078452A) disclosed technology becomes hollow circular cylinder with mixed sinterings such as hydroxyapatite, aluminum phosphate in, utilize cavity storage medicine, but its structure is unfavorable for the cell growth, and biocompatibility is relatively poor.Document " porous devitrified glass is as the preparation and the external release research thereof of drug carrier material " (author Wang De equality, be selected from " Journal of Inorganic Materials " 2001,11 (6)) in, reported that the gauze bio active ceramic is as bone filling and preparation of drug carriers and research, this class material has better biocompatibility, but degradability is poor.Following document: " preparation of Porous Spherical Hydroxyapatite Biomaterial and structure " (author Liu Xinan, Li Wei, difficult to understand in the king, select from " applied chemistry " 2003,20 (3)), A.C.Queiroz, J.D.Santos, F.J.Monteiro, I.R.Gibson, et al.Absorption and releasestudies of sodium ampicillin from hydroxyapatite and glass-reinforcedhydroxyapatite composites[J] Biomaterials 2001, the how empty body of the block shape of the domestic and international employing of 22:1393-1400. report bioceramic preparation is as the purposes of artificial bone-filling material and thing carrier aspect.
Summary of the invention
The preparation method that the purpose of this invention is to provide a kind of artificial bone-filling material of hollow ball structure, the hollow ball structure bone of preparation is filled ceramic particle in this way, solve its structure and be unfavorable for shortcomings such as cell is grown, intensity is low, had the damaged and drug controlled-release body dual function of the bone of filling up.
The technical solution adopted in the present invention is: the preparation method of graininess artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.5～1.0g and dissolve in the carbon tetrachloride of 10～100ml, stir and make dissolving fully, make bonding agent;
Slurry is hydroxyapatite slurry or bata-tricalcium phosphate slurry,
In particle diameter is hydroxyapatite powder 10～50g of 0.1～0.5 μ m, add the dehydrated alcohol of 10～200ml, put into polyvinyl butyral resin 0.2～3ml again, stir, make the hydroxyapatite slurry;
At particle diameter is the dehydrated alcohol that adds 10～200ml among 0.1～0.5 μ m bata-tricalcium phosphate powder, 10～50g, puts into polyvinyl butyral resin 0.2～3ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200～1200 μ m places mould of plastics, the application of force contacts with each other spheroid, splash into the above-mentioned bonding agent 0.2～1.2ml for preparing subsequently in the ball junction, place air set, from mould of plastics, deviate from the spheroid template that is cured stand-by;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned hydroxyapatite slurry or bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 70～100 ℃ and made it bone dry in 5～8 hours, repeat to soak damp technology 2～5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 400～600 ℃ with the sintering rate of 3～5 ℃/min, to temperature back insulation 2～4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100～1250 ℃ with the sintering rate of 3～5 ℃/min, is incubated after 2～4 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite or the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
The preferable technical scheme of the present invention is: the preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.5g and dissolve in the carbon tetrachloride of 30ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 10ml among the hydroxyapatite powder 20g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.2ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 70 ℃ and made it bone dry in 8 hours, soak the pool repeatedly 2 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 4 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
The preferable technical scheme of the present invention is: the preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.7g and dissolve in the carbon tetrachloride of 80ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 50ml among the hydroxyapatite powder 35g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.9ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 600 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.6ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 85 ℃ and made it bone dry in 7 hours, soak the pool repeatedly 3 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 5 ℃/min, is incubated after 4 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
The preferable technical scheme of the present invention is: the preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.9g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 120ml among the hydroxyapatite powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 1.5ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1000 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1.0ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 95 ℃ and made it bone dry in 6 hours, soak the pool repeatedly 4 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 3 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
The preferable technical scheme of the present invention is: the preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 1.0g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 200ml among the hydroxyapatite powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 2.2ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 100 ℃ and made it bone dry in 5 hours, soak the pool repeatedly 5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 4 ℃/min, to temperature back insulation 3 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
The preferable technical scheme of the present invention is: the preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.5g and dissolve in the carbon tetrachloride of 30ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 20ml among the bata-tricalcium phosphate powder 20g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.3ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 70 ℃ and made it bone dry in 7.5 hours, soak the pool repeatedly 2 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
The preferable technical scheme of the present invention is: the preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.8g and dissolve in the carbon tetrachloride of 85ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 80ml among the bata-tricalcium phosphate powder 40g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 1.2ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 830 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.8ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 90 ℃ and made it bone dry in 6.5 hours, soak the pool repeatedly 4 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 600 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 3 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
The preferable technical scheme of the present invention is: the preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 1.0g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 200ml among the bata-tricalcium phosphate powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 2ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 100 ℃ and made it bone dry in 5 hours, soak the pool repeatedly 5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
The preferable technical scheme of the present invention is: the preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.6g and dissolve in the carbon tetrachloride of 40ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 60ml among the bata-tricalcium phosphate powder 30g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.7ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 500 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.5ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 80 ℃ and made it bone dry in 8 hours, soak the pool repeatedly 3 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 4 ℃/min, to temperature back insulation 3 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
The invention has the beneficial effects as follows, the bone filler particles that method of the present invention prepares, inside is the hollow ball structure, the ball controllable size, the hollow ball surface is porose, the individual particle shape bioceramic of this hollow ball structure, with the active biological ceramic is main material, has excellent biological compatibility and higher intensity, can be new bone support is provided, simultaneously the hollow ball surfaces externally and internally is long-pending bigger, for the growth of cell provides enough spaces, and can be used for depositing or adsorbing medicine, have the damaged and drug controlled-release body dual function of the bone of filling up.
Description of drawings
Fig. 1 hollow ball preparation technology flow chart;
The hollow ball granule sketch map that Fig. 2 makes.
The specific embodiment
The present invention is described in detail with drawings and Examples below.
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.5～1.0g and dissolve in the carbon tetrachloride of 10～100ml, stir and make dissolving fully, make bonding agent;
Slurry is hydroxyapatite slurry or bata-tricalcium phosphate slurry,
In particle diameter is hydroxyapatite powder 10～50g of 0.1～0.5 μ m, add the dehydrated alcohol of 10～200ml, put into polyvinyl butyral resin 0.2～3ml again, stir, make the hydroxyapatite slurry;
At particle diameter is the dehydrated alcohol that adds 10～200ml among 0.1～0.5 μ m bata-tricalcium phosphate powder, 10～50g, puts into polyvinyl butyral resin 0.2～3ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200～1200 μ m places mould of plastics, the application of force contacts with each other spheroid, splash into the above-mentioned bonding agent 0.2～1.2ml for preparing subsequently in the ball junction, place air set, from mould of plastics, deviate from the spheroid template that is cured stand-by;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned hydroxyapatite slurry or bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 70～100 ℃ and made it bone dry in 5～8 hours, repeat to soak damp technology 2～5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 400～600 ℃ with the sintering rate of 3～5 ℃/min, to temperature back insulation 2～4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100～1250 ℃ with the sintering rate of 3～5 ℃/min, is incubated after 2～4 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite or the bata-tricalcium phosphate bioceramic of hollow ball structure, referring to Fig. 1;
Then the continuous hollow spheroid is cut into one hollow ball granule, referring to Fig. 2.
Embodiment 1
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.5g and dissolve in the carbon tetrachloride of 30ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 10ml among the hydroxyapatite powder 20g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.2ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 70 ℃ and made it bone dry in 8 hours, soak the pool repeatedly 2 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 4 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
Embodiment 2
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.7g and dissolve in the carbon tetrachloride of 80ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 50ml among the hydroxyapatite powder 35g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.9ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 600 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.6ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 85 ℃ and made it bone dry in 7 hours, soak the pool repeatedly 3 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 5 ℃/min, is incubated after 4 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
Embodiment 3
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.9g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 120ml among the hydroxyapatite powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 1.5ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1000 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1.0ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 95 ℃ and made it bone dry in 6 hours, soak the pool repeatedly 4 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 3 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
Embodiment 4
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 1.0g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 200ml among the hydroxyapatite powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 2.2ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 100 ℃ and made it bone dry in 5 hours, soak the pool repeatedly 5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 4 ℃/min, to temperature back insulation 3 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
Embodiment 5
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.5g and dissolve in the carbon tetrachloride of 30ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 20ml among the bata-tricalcium phosphate powder 20g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.3ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 70 ℃ and made it bone dry in 7.5 hours, soak the pool repeatedly 2 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
Embodiment 6
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.8g and dissolve in the carbon tetrachloride of 85ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 80ml among the bata-tricalcium phosphate powder 40g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 1.2ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 830 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.8ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 90 ℃ and made it bone dry in 6.5 hours, soak the pool repeatedly 4 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 600 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 3 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
Embodiment 7
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 1.0g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 200ml among the bata-tricalcium phosphate powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 2ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 100 ℃ and made it bone dry in 5 hours, soak the pool repeatedly 5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
Embodiment 8
The preparation method of artificial bone-filling material with hollow ball structure may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.6g and dissolve in the carbon tetrachloride of 40ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 60ml among the bata-tricalcium phosphate powder 30g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.7ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 500 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.5ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 80 ℃ and made it bone dry in 8 hours, soak the pool repeatedly 3 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 4 ℃/min, to temperature back insulation 3 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
Claims (9)
1. the preparation method of an artificial bone-filling material with hollow ball structure is characterized in that, may further comprise the steps: the first step, the preparation of bonding agent and slurry
Get PS plastics 0.5～1.0g and dissolve in the carbon tetrachloride of 10～100ml, stir and make dissolving fully, make bonding agent;
Slurry is hydroxyapatite slurry or bata-tricalcium phosphate slurry,
In particle diameter is hydroxyapatite powder 10～50g of 0.1～0.5 μ m, add the dehydrated alcohol of 10～200ml, put into polyvinyl butyral resin 0.2～3ml again, stir, make the hydroxyapatite slurry;
At particle diameter is the dehydrated alcohol that adds 10～200ml among 0.1～0.5 μ m bata-tricalcium phosphate powder, 10～50g, puts into polyvinyl butyral resin 0.2～3ml again, stirs, and makes the bata-tricalcium phosphate slurry; Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200～1200 μ m places mould of plastics, the application of force contacts with each other spheroid, splash into the above-mentioned bonding agent 0.2～1.2ml for preparing subsequently in the ball junction, place air set, from mould of plastics, deviate from the spheroid template that is cured stand-by;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned hydroxyapatite slurry or bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 70～100 ℃ and made it bone dry in 5～8 hours, repeat to soak damp technology 2～5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 400～600 ℃ with the sintering rate of 3～5 ℃/min, to temperature back insulation 2～4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100～1250 ℃ with the sintering rate of 3～5 ℃/min, is incubated after 2～4 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite or the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
2. the preparation method of artificial bone-filling material with hollow ball structure according to claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.5g and dissolve in the carbon tetrachloride of 30ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 10ml among the hydroxyapatite powder 20g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.2ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 70 ℃ and made it bone dry in 8 hours, soak the pool repeatedly 2 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 4 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
3. the preparation method of artificial bone-filling material with hollow ball structure according to claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.7g and dissolve in the carbon tetrachloride of 80ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 50ml among the hydroxyapatite powder 35g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.9ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 600 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.6ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 85 ℃ and made it bone dry in 7 hours, soak the pool repeatedly 3 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 5 ℃/min, is incubated after 4 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
4. the preparation method of artificial bone-filling material with hollow ball structure according to claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.9g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 120ml among the hydroxyapatite powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 1.5ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1000 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 95 ℃ and made it bone dry in 6 hours, soak the pool repeatedly 4 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 3 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
5. the preparation method of artificial bone-filling material with hollow ball structure according to claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 1.0g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 200ml among the hydroxyapatite powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 2.2ml again, stirs, and makes the hydroxyapatite slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed the above-mentioned hydroxyapatite slurry for preparing, take out to place under the temperature that is placed in the baking oven 100 ℃ and made it bone dry in 5 hours, soak the pool repeatedly 5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 4 ℃/min, to temperature back insulation 3 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1250 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the hydroxyapatite of hollow ball structure, then the continuous hollow spheroid is cut into one hollow ball granule.
6. the preparation method of artificial bone-filling material with hollow ball structure according to claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.5g and dissolve in the carbon tetrachloride of 30ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 20ml among the bata-tricalcium phosphate powder 20g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.3ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 70 ℃ and made it bone dry in 7.5 hours, soak the pool repeatedly 2 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 3 ℃/min, to temperature back insulation 2 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
7. the preparation method of artificial bone-filling material with hollow ball structure according to claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.8g and dissolve in the carbon tetrachloride of 85ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 80ml among the bata-tricalcium phosphate powder 40g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 1.2ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 830 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.8ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 90 ℃ and made it bone dry in 6.5 hours, soak the pool repeatedly 4 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 600 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 3 ℃/min, is incubated after 2 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
8. the preparation method of artificial bone-filling material with hollow ball structure according to claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 1.0g and dissolve in the carbon tetrachloride of 100ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 200ml among the bata-tricalcium phosphate powder 50g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 2ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 1200 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 1.2ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 100 ℃ and made it bone dry in 5 hours, soak the pool repeatedly 5 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 5 ℃/min, to temperature back insulation 4 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
9. the preparation method of artificial bone-filling material with hollow ball structure according to claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation of bonding agent and slurry
Get PS plastics 0.6g and dissolve in the carbon tetrachloride of 40ml, stir and make dissolving fully, make bonding agent;
At particle diameter is the dehydrated alcohol that adds 60ml among the bata-tricalcium phosphate powder 30g of 0.1～0.5 μ m, puts into polyvinyl butyral resin 0.7ml again, stirs, and makes the bata-tricalcium phosphate slurry;
Second step, the preparation of macromolecule spheroid template
The polrvinyl chloride spheroid of getting particle diameter and be 500 μ m places mould of plastics, and the application of force contacts with each other spheroid, splashes into the above-mentioned bonding agent 0.5ml for preparing subsequently in the ball junction, places air set, deviates from the spheroid template that is cured stand-by from mould of plastics;
The 3rd step, molding
The spheroid template that is cured is immersed in the above-mentioned bata-tricalcium phosphate slurry for preparing, take out to place under the temperature that is placed in the baking oven 80 ℃ and made it bone dry in 8 hours, soak the pool repeatedly 3 times;
The 4th step, sintering
The binder removal process is heated the spheroid template of forming to 500 ℃ with the sintering rate of 4 ℃/min, to temperature back insulation 3 hours, and the macromolecule spheroid template that the burning-off heap is stamped;
Densification process continues to be warming up to 1100 ℃ with the sintering rate of 4 ℃/min, is incubated after 3 hours, cools to room temperature with the furnace, promptly gets the bata-tricalcium phosphate bioceramic of hollow ball structure;
Then the continuous hollow spheroid is cut into one hollow ball granule.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022162023A1 (en) | 2021-01-28 | 2022-08-04 | Galvita Ag | Solid pharmaceutical compositions and methods of producing the same |
| EP4311543A1 (en) | 2022-07-27 | 2024-01-31 | Galvita AG | Methods for loading template inverted carriers |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004045410A1 (en) * | 2004-09-15 | 2006-03-30 | Glatt Gmbh | Bone replacement implant for human and veterinary applications |
| CN101759169B (en) * | 2009-11-13 | 2013-01-16 | 中国科学院上海硅酸盐研究所 | Calcium phosphate nano-structure hollow microsphere and preparation method thereof |
| CN102846409A (en) * | 2011-06-29 | 2013-01-02 | 北京爱康宜诚医疗器材股份有限公司 | Spinous metal particle body |
| CN102846408B (en) * | 2011-06-29 | 2015-09-16 | 北京大学第三医院 | Metallic granular body for bone-grafting filling |
| CN103893829B (en) * | 2014-03-27 | 2015-06-24 | 西安理工大学 | Preparation method of injectable porous compound bone cement |
| CN105439619B (en) * | 2016-01-06 | 2017-07-04 | 山东理工大学 | A kind of method of utilization waste and old wood grain production light ceramic ball |
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| JPS535134A (en) * | 1976-06-30 | 1978-01-18 | Sumitomo Chem Co Ltd | Racemization of optical active 2-(4)chlorophenyl)-3-methylbutylic acid |
| JPH04224512A (en) * | 1990-12-26 | 1992-08-13 | Olympus Optical Co Ltd | Carrier for sustained release agent and its production |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS535134A (en) * | 1976-06-30 | 1978-01-18 | Sumitomo Chem Co Ltd | Racemization of optical active 2-(4)chlorophenyl)-3-methylbutylic acid |
| JPH04224512A (en) * | 1990-12-26 | 1992-08-13 | Olympus Optical Co Ltd | Carrier for sustained release agent and its production |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022162023A1 (en) | 2021-01-28 | 2022-08-04 | Galvita Ag | Solid pharmaceutical compositions and methods of producing the same |
| EP4311543A1 (en) | 2022-07-27 | 2024-01-31 | Galvita AG | Methods for loading template inverted carriers |
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