CN108114316A - A kind of ceramic base dentistry bone meal and preparation method thereof - Google Patents
A kind of ceramic base dentistry bone meal and preparation method thereof Download PDFInfo
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
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- A61L27/24—Collagen
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L27/12—Phosphorus-containing materials, e.g. apatite
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Abstract
The present invention relates to a kind of ceramic base dentistry bone meal and preparation method thereof.It prepares component and includes porous hydroxyapatite and type i collagen；The preparation component of porous hydroxyapatite include extra fine quality than hydroxyapatite, the first PMMA particles and the 2nd PMMA particles, and the grain size of the first PMMA particles is 50~100 μm, and the grain sizes of the 2nd PMMA particles is 500~1000 μm；Porous hydroxyapatite is prepared by sintering, and sintering includes such as the next stage：First stage：Heating rate is 5~10 DEG C/min, and target temperature is 500~600 DEG C, and constant temperature time is 20~30min；Second stage：Heating rate is 5~10 DEG C/min, and target temperature is 1200~1500 DEG C, and constant temperature time is 200~300min；Phase III：Stop heating, Temperature fall.The dentistry bone meal has excellent water absorbing properties, Bone Defect Repari effect and relatively low production cost.
Description
Technical field
The present invention relates to medical material tech fields more particularly to a kind of ceramic base dentistry bone meal and preparation method thereof.
Background technology
In dental operation, there are many kinds of situation patient can be caused to generate bone defect or Bone mineral change after surgery, such as
The bone defect that periodontal cyst generates after extracing, the situation of Bone mineral change caused by alveolar ridge atrophy after tooth is extracted.These situations
Often limit the effect of the postoperative knitting of patient and follow-up dental implant, it is therefore desirable to carry out bone plantation.It solves at present
Gold method mainly transplanted using autologous bone, but due to its limited source, and there is centainly postoperative in donor site
Complication, application are restricted.Allogenic bone transplantation is there are potentially antigenic property and pathophorous risk, therefore, manually
Bone renovating material because its source is sufficient, can standardized production, and avoid unnecessary transmission equivalent risk, become crowd
The research direction of more scholars, and be also widely used in clinic, obtain good therapeutic effect.
But inventor has found that the ingredient of currently used bone meal is mostly inorganic mineral material, in order to and it is natural
The performance of bone is more nearly, but there is also poor biocompatibility, hydrophily are poor, can not be provided for the growth of cell with multiplication
The problem of good environment.
The optimal dentistry bone meal material Bio-Oss of using effect is external product on the market at present, expensive, is added
The medical treatment cost of patient.
The content of the invention
(1) technical problems to be solved
It is poor for existing dentistry bone meal poor biocompatibility, hydrophily, be unfavorable for adherency of the cell on bone meal material and
The problem of multiplication, the present invention provides a kind of ceramic base dentistry bones for having both good biocompatibility and excellent hydrophilic effect
Powder improves Bone Defect Repari effect, while also has relatively low production cost, convenient for clinical practice.
(2) technical solution
In order to solve the above technical problem, the present invention provides following technical solutions：
A kind of ceramic base dentistry bone meal, the preparation component of the dentistry bone meal include：
Porous hydroxyapatite；
Type i collagen, quality are the 1%~10% of the porous hydroxyapatite quality；
Wherein, the preparation component of the porous hydroxyapatite includes hydroxyapatite, the first PMMA particles and second
PMMA particles, mass ratio 5：(2.5~3.5)：(1.5~2.5), and the grain size of the first PMMA particles be 50~100 μm, second
The grain size of PMMA particles is 500~1000 μm；With
The porous hydroxyapatite is prepared by sintering, and the sintering includes such as the next stage：
First stage：Heating rate is 5~10 DEG C/min, and target temperature is 500~600 DEG C, constant temperature time for 20~
30min；
Second stage：Heating rate is 5~10 DEG C/min, and target temperature is 1200~1500 DEG C, constant temperature time for 200~
300min；
Phase III：Stop heating, Temperature fall.
Preferably, the porous hydroxyapatite has the hole of connection；With
The porous hydroxyapatite is：The particle of 20 mesh sieves can be crossed, it is preferable that the porous hydroxyapatite is：Energy
Cross 20 mesh sieves, and the particle retained by 60 mesh sieves.
Preferably, the preparation method of the porous hydroxyapatite includes：
(a) hydroxyapatite suspension is prepared；
(b) the first PMMA particles and the 2nd PMMA particles are added in the hydroxyapatite suspension, sintering base is made
Liquid；
(c) the sintering base fluid is placed in agglomerating plant and be sintered, agglomerated material is made；
(d) agglomerated material is crushed and sieved, the porous hydroxyapatite is made.
Preferably, the step (a) carries out as follows：
15~20g hydroxyapatites with 20~35mL PBS solutions are mixed in batches, add 1.5~2.5mL concentration
It for the poly-vinyl alcohol solution of 0.05~0.1g/mL, stirs evenly, preparation obtains the hydroxyapatite suspension.
Preferably, the poly-vinyl alcohol solution is prepared as follows：
Polyvinyl alcohol and purified water are mixed, the container containing polyvinyl alcohol and purified water is then put into water bath device
In, heat while stirring, treat the solution in container become it is transparent, without layering, without caking to get to the poly-vinyl alcohol solution.
It is highly preferred that the temperature setting of the water-bath is 80~95 DEG C.
The present invention also provides a kind of preparation methods of above-mentioned dentistry bone meal, include the following steps：
(1) it is blended：The porous hydroxyapatite and the type i collagen are mixed and stirred for uniformly, obtaining with PBS solution
Mixed liquor；
(2) mould is filled：The mixed liquor is poured into mold；
(3) freeze：The mold is freezed；
(4) crush：Material disintegrating after will be lyophilized；
(5) sieve：The particle screening that will be obtained after crushed obtains ceramic base dentistry bone meal.
Preferably, in step (3), described freeze includes the following steps：
The mold is put into freeze dryer, it is after pre-freeze, the first distillation, the second distillation and cooling four-stage, i.e., complete
It is freezed into described；Wherein, first distillation and second sublimation stage vacuumize, and vacuum degree is less than -0.05MPa, is mixed
50~120Pa of gas；With
The pre-freeze carries out as follows：Rate of temperature fall is 2.0~5.0 DEG C/min, and target temperature is -15~-30
DEG C, constant temperature time is 200~350min；
First distillation includes following 4 temperature gradients：
Heating rate is 0.5~1 DEG C/min, and target temperature is -15~-10 DEG C, and constant temperature time is 200~300min；
Heating rate is 0.3~0.5 DEG C/min, and target temperature is -10~-5 DEG C, and constant temperature time is 200~300min；
Heating rate is 0.2~0.3 DEG C/min, and target temperature is -5~-2 DEG C, and constant temperature time is 100~200min；
Heating rate is 0.1~0.2 DEG C/min, and target temperature is -2~0 DEG C, and constant temperature time is 100~200min；
Second distillation includes following 5 temperature gradients：
Heating rate is 0.5~1 DEG C/min, and target temperature is 10~20 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 20~30 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 30~40 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 40~50 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 50~60 DEG C, and endpoint is carried out every 1h, until closing
Lattice；Terminal≤0.9Pa/10min；
The cooling carries out as follows：Rate of temperature fall is 2~5 DEG C/min, until preceding box temperature degree reaches 20~25
℃。
Preferably, in step (5), the screening carries out as follows：
The particle obtained after the pulverization process is first crossed into 20 mesh sieves, sieved particle is after 60 mesh sieves, by 60 mesh sieves
The particle of retention is ceramic base dentistry bone meal；With
Send the particle retained by 20 mesh sieves back to the pulverising step.
Preferably, in step (2), the thickness for filling mould is no more than 11mm, is preferably 5~10mm.
Preferably, in step (1), when the type i collagen is in terms of g, the PBS solution with mL timing, the type i collagen and
The amount ratio of the PBS solution is 1：(25~45).
(3) advantageous effect
The above-mentioned technical proposal of the present invention has the following advantages that：
(1) the PMMA particles of two kinds of different-grain diameters has been selected to be sintered pore-creating to hydroxyapatite so that porous hydroxyapatite
Apatite has larger surface area and roughness, not only improves the attachment of biological tissue and gos deep into hole, also improves product
Water absorbing properties, be conducive to doctor and operated；It ensure that the support strength of product, while simulate the three-dimensional rack knot of bone tissue
Structure provides sufficient space for growing into for osteocyte.Type i collagen is with the addition of as organic phase, bioactivity is improved, promotes bone generation
It thanks and is proliferated.
(2) dentistry bone meal production cost provided by the invention is low, and preparation method is simple, convenient for large-scale production.
Description of the drawings
Fig. 1 is that SEM schemes ceramic base dentistry bone meal in one direction；
Fig. 2 is SEM figure of the ceramic base dentistry bone meal on other direction；
Fig. 3 is picture in art, and wherein A figures, B figures show the bone defect of preparation, and what C figures were inserted is ceramic base dentistry powder, and D schemes
What is inserted is Bio-Oss bone meal；
Fig. 4 is 12 weeks after operation CBCT figures, and wherein A figures represent A1 groups, and B figures represent B1 groups, and C figures represent B2 groups, and D figures represent A2
Group；
Fig. 5 a and Fig. 5 b are pictures (× 10) under 12 weeks after operation Goldner trichrome stain microscopes, and wherein Fig. 5 a are A1 groups,
Fig. 5 b are B1 groups；
Picture (× 1.25) under Fig. 6 12 weeks after operation Goldner trichrome stain microscopes, wherein A figures to D figures are respectively A1
Group, B1 groups, B2 groups, A2 groups.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is the part of the embodiment of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
On the premise of all other embodiments obtained, belong to the scope of protection of the invention.
First, the present invention provides a kind of ceramic base dentistry bone meal, the preparation component of the dentistry bone meal includes：
Porous hydroxyapatite；
Type i collagen, quality are the 1%~10% of the porous hydroxyapatite quality, for example, can be specially 1%,
2%th, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%；
Wherein, the preparation component of the porous hydroxyapatite includes hydroxyapatite, the first PMMA particles and second
PMMA particles, mass ratio 5：(2.5~3.5)：(1.5~2.5), and the grain size of the first PMMA particles is 50~100 μm, example
Such as, can be 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, alternatively, any combination for above-mentioned grain size；
The grain size of 2nd PMMA particles be 500~1000 μm, for example, can be 500 μm, 600 μm, 700 μm, 800 μm,
900 μm, 1000 μm, alternatively, any combination for above-mentioned grain size；With
The porous hydroxyapatite is prepared by sintering, and the sintering includes such as the next stage：
First stage：Heating rate is 5~10 DEG C/min, and target temperature is 500~600 DEG C, constant temperature time for 20~
30min；
Second stage：Heating rate is 5~10 DEG C/min, and target temperature is 1200~1500 DEG C, for example, can be 1200
DEG C, 1300 DEG C, 1400 DEG C, 1500 DEG C, constant temperature time is 200~300min；
Phase III：Stop heating, Temperature fall.
The grain size of first PMMA particles is smaller, can provide stent micropore, increases porosity.And the grain of the 2nd PMMA particles
Footpath is larger, can provide support aperture structure.PMMA amount of particles is excessive, it will cause sintered hydroxyapatite structure not
Continuously, the phenomenon that easily losing powder, not being molded, without required mechanical structure and mechanical strength.Dosage is very few, then can not carry
For effective stent and pore structure.
Type i collagen dosage also has an impact the performance of material.Dosage excessively can be fully wrapped around firmly by hydroxyapatite, is formed
Fluffy solid is not easy crushing and processing, and hydroxyapatite can not have an effect.The excessively few then product water imbibition of dosage is poor, meets moisture
It dissipates, is highly detrimental to Clinical practice.
In some embodiments, the porous hydroxyapatite has the hole of connection；With
The porous hydroxyapatite is：The particle of 20 mesh sieves can be crossed, it is preferable that the porous hydroxyapatite is：Energy
Cross 20 mesh sieves, and the particle retained by 60 mesh sieves.
In some embodiments, the preparation method of the porous hydroxyapatite includes：
(a) hydroxyapatite suspension is prepared；
(b) the first PMMA particles and the 2nd PMMA particles are added in the hydroxyapatite suspension, sintering base is made
Liquid；
(c) the sintering base fluid is placed in agglomerating plant and be sintered, agglomerated material is made；
(d) agglomerated material is crushed and sieved, the porous hydroxyapatite is made.
Preferably, the step (a) carries out as follows：
By 15~20g hydroxyapatites in batches (for example, hydroxyapatite can be divided into 3~10 parts, so as to by hydroxyl
Base apatite point feeds for 3~10 times) and 20~35mL PBS solutions mixing, add 1.5~2.5mL concentration be 0.05~
The poly-vinyl alcohol solution of 0.1g/mL, stirs evenly, and preparation obtains the hydroxyapatite suspension.PBS solution herein is normal
Phosphate buffer solution, pH are 7.0~7.4, concentration 10M.
Preferably, the poly-vinyl alcohol solution is prepared as follows：
Polyvinyl alcohol and purified water are mixed, the container containing polyvinyl alcohol and purified water is then put into water bath device
In, heat while stirring, treat the solution in container become it is transparent, without layering, without caking to get to the poly-vinyl alcohol solution.
It is highly preferred that the temperature setting of the water-bath is 80~95 DEG C.
The present invention also provides a kind of preparation methods of above-mentioned dentistry bone meal, include the following steps：
(1) it is blended：The porous hydroxyapatite and the type i collagen are mixed and stirred for uniformly, obtaining with PBS solution
Mixed liquor；
(2) mould is filled：The mixed liquor is poured into mold；
(3) freeze：The mold is freezed；
(4) crush：Material disintegrating after will be lyophilized；With
(5) sieve：The particle screening that will be obtained after crushed obtains ceramic base dentistry bone meal.
In some embodiments, in step (3), described freeze includes the following steps：
The mold is put into freeze dryer, it is after pre-freeze, the first distillation, the second distillation and cooling four-stage, i.e., complete
It is freezed into described；Wherein, first distillation and second sublimation stage vacuumize, and vacuum degree is less than -0.05MPa, aeration
50~120Pa；With
The pre-freeze carries out as follows：Rate of temperature fall is 2.0~5.0 DEG C/min, and target temperature is -15~-30
DEG C, constant temperature time is 200~350min；
First distillation includes following 4 temperature gradients：
Heating rate is 0.5~1 DEG C/min, and target temperature is -15~-10 DEG C, and constant temperature time is 200~300min；
Heating rate is 0.3~0.5 DEG C/min, and target temperature is -10~-5 DEG C, and constant temperature time is 200~300min；
Heating rate is 0.2~0.3 DEG C/min, and target temperature is -5~-2 DEG C, and constant temperature time is 100~200min；
Heating rate is 0.1~0.2 DEG C/min, and target temperature is -2~0 DEG C, and constant temperature time is 100~200min；
Second distillation includes following 5 temperature gradients：
Heating rate is 0.5~1 DEG C/min, and target temperature is 10~20 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 20~30 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 30~40 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 40~50 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 50~60 DEG C, and endpoint is carried out every 1h, until closing
Lattice；Terminal≤0.9Pa/10min；
The cooling carries out as follows：Rate of temperature fall is 2~5 DEG C/min, until preceding box temperature degree reaches 20~25
℃。
In some embodiments, in step (5), the screening carries out as follows：
The particle obtained after the pulverization process is first crossed into 20 mesh sieves, sieved particle is after 60 mesh sieves, by 60 mesh sieves
The particle of retention is ceramic base dentistry bone meal；With
Send the particle retained by 20 mesh sieves back to the pulverising step.
Preferably, in step (2), the thickness for filling mould is no more than 11mm, is preferably 5~10mm.
Preferably, in step (1), when the type i collagen is in terms of g, the PBS solution with mL timing, the type i collagen and
The amount ratio of the PBS solution is 1：(25~45).
It is several embodiments that the present invention enumerates below.
Embodiment 1
A kind of ceramic base dentistry bone meal prepares component and includes：
Porous hydroxyapatite；
Type i collagen, quality are the 1% of porous hydroxyapatite quality；
Wherein, the preparation component of porous hydroxyapatite includes hydroxyapatite, the first PMMA particles and the 2nd PMMA
Grain, mass ratio 5：2.5：1.5, and the grain size of the first PMMA particles is 50 μm, the grain size of the 2nd PMMA particles is 500 μm；With
Porous hydroxyapatite is prepared by sintering, and sintering process is as shown in table 1
Table 1
Embodiment 2
A kind of ceramic base dentistry bone meal prepares component and includes：
Porous hydroxyapatite；
Type i collagen, quality are the 10% of porous hydroxyapatite quality；
Wherein, the preparation component of porous hydroxyapatite includes hydroxyapatite, the first PMMA particles and the 2nd PMMA
Grain, mass ratio 5：3.5：2.5, and the grain size of the first PMMA particles is 100 μm, the grain size of the 2nd PMMA particles is 1000 μm；
With
Porous hydroxyapatite is prepared by sintering, and sintering process is as shown in table 2：
Table 2
Embodiment 3
A kind of ceramic base dentistry bone meal prepares component and includes：
Porous hydroxyapatite；
Type i collagen, quality are the 5% of porous hydroxyapatite quality；
Wherein, the preparation component of porous hydroxyapatite includes hydroxyapatite, the first PMMA particles and the 2nd PMMA
Grain, mass ratio 5：3：2, and the grain size of the first PMMA particles is 70 μm, the grain size of the 2nd PMMA particles is 600 μm；With
Porous hydroxyapatite is prepared by sintering, and specific preparation method includes the following steps：
(a) hydroxyapatite suspension is prepared：
1g polyvinyl alcohol is weighed, is put into conical flask, is added 10mL purified waters, conical flask is put into water-bath and is heated
Dissolving, bath temperature is arranged to 80 DEG C, and is carried out at the same time stirring, treats that the solution in conical flask becomes homogeneous transparent, without caking, nothing
Layering is to get to poly-vinyl alcohol solution.
The PBS solution of 20mL pH7.0 is added in beaker, 15g hydroxyapatites are added in beaker in batches, then is added
Enter 1.5mL poly-vinyl alcohol solutions, and open magnetic agitation simultaneously, stir evenly suspended up to the hydroxyapatite of modest viscosity
Liquid.With being continuously added for hydroxyapatite, the viscosity of system becomes increasing, therefore, can be in order to stir evenly
Constantly change position of the magneton in beaker.
In this step, hydroxyapatite and the amount ratio of solvent PBS solution influence the viscosity of hydroxyapatite suspension.
Suitable viscosity can be ensured that the PMMA particles subsequently added can be evenly distributed in suspension, will not sink to the bottom.It is examined based on above-mentioned
Consider, the Optimum of hydroxyapatite is 15~20g, and the Optimum of PBS solution is 20~35mL.In the present embodiment, hydroxyl
The dosage of base apatite is 15g, and the dosage of PBS solution is 20mL.
(b) the first PMMA particles and the 2nd PMMA particles are added in hydroxyapatite suspension, stirred evenly, be made and burn
Tie base fluid；
(c) the sintering base fluid is transferred in crucible, is placed in sintering furnace and is sintered, obtain agglomerated material.Wherein,
Sintering process is as shown in table 3：
Table 3
When the temperature of sintering furnace is down to room temperature, fire door is opened, obtained agglomerated material is transferred to clean room, was shifted
Crucible cover should not be opened in journey.
(d) agglomerated material is put into micromill to crush, pulverized particles is carried out with vibrating screen or stainless steel sieve
Screening, the mesh number of upper sieve is 20 mesh, and the mesh number of lower screen is 60 mesh；The particle retained by 60 mesh sieve is collected, it is as porous
Hydroxyapatite.
It is crushed again by the particle that 20 mesh retain.
The porous hydroxyapatite as made from the above method has the hole of connection, and is：20 mesh sieves can be crossed, and by 60 mesh sieves
The particle of retention.
Embodiment 4
The preparation component that embodiment 3 is provided is prepared into ceramic base dentistry bone meal, preparation method includes the following steps：
(1) it is blended：50g porous hydroxyapatites and 5g type i collagens are mixed and stirred with the PBS solution of 45mL pH7.0
It mixes uniformly, obtains mixed liquor.
(2) mould is filled：The mixed liquor is poured into mold, is filled in mold process without vacuumizing discharge gas with water-circulating pump
Bubble selects glass/stainless steel/PTFE molds to fill mould, is struck off according to mold size, and it is 10mm to fill mould thickness.
(3) freeze：
The mold is put into freeze dryer, it is after pre-freeze, the first distillation, the second distillation and cooling four-stage, i.e., complete
It is freezed into described；Wherein, first distillation and second sublimation stage vacuumize, and vacuum degree is less than -0.05MPa, aeration
50~120Pa.
Wherein, the parameter setting of four-stage is as shown in table 4.
Table 4
(4) crush：Material after will be lyophilized, which is put into micromill, to be crushed；With
(5) sieve：The particle vibrating screen or stainless steel that obtain after crushed are sieved and sieved, is first sieved with 20 mesh sieves
Point, then retained with 60 mesh sieves, the particle retained by 60 mesh sieves is collected, is ceramic base dentistry bone meal.
Pulverising step is back to by the particle that 20 mesh retain.
Embodiment 5
The preparation component that embodiment 3 is provided is prepared into ceramic base dentistry bone meal, preparation method with embodiment 4 substantially
It is identical, the difference is that：
In step (3), the parameter setting of four-stage is as shown in table 5.
Table 5
(1) ceramic base dentistry bone meal Shape measure
As can be seen that ceramic base dentistry bone meal has larger surface area and roughness from Fig. 1 and Fig. 2, so as to favourable
In the attachment and deeply of biological tissue, the water absorbing properties of bone meal can also be improved.
(2) application effect detects
Testing program：
Animal model：2 13 months miniature pigs extract the second molar finishing bone defect in four quadrants, make near and far
Bones morphology is as far as possible consistent；
Test material：Ceramic base dentistry bone meal, Bio-Oss bone meal, Bio-gide films.
Experiment grouping：Ceramic base dentistry bone meal+Bio-gide films be A groups, Bio-Oss bone meal+Bio-gide films be B groups, A
Group includes upper jaw A1 groups (n=2, A11, A12) and lower jaw A2 groups (n=3, A21, A22, A23), and B groups include upper jaw B1 groups (n=
And lower jaw B2 groups (n=1) 1).Blank group (n=1) is without any processing for defect of maxilla.
Surgical procedure：(1) preoperative 12h fasting, water, posterior auricular muscle meat injection ketamine 0.2ml/kg and fast dormancy 0.10ml/
kg；(2) left lateral position, disinfection, drape in mouth week and mouth, puts opener；(3) frist premolar it is remote in and the 3rd premolar teeth
Nearly middle incision gum, open trapezoidal valve, divide gum, quickly loose tooth, completely extract the second premolar teeth in 4 quadrants；(4) pulling out
Tooth area cheek side grinds the bone defect of 10mm × 10mm × 5mm sizes with motor, and Bio-Oss bone meal or pottery are respectively filled according to grouping
Porcelain abutment section bone meal, then Bio-Gide collagem membranes are covered, tight suture mucous membrane is layered, as shown in Figure 3；(5) postoperative injection mould
Plain sodium 3d, 1 time a day, 400,000 U every time.
Result of the test：
(1) gross findings：All defective regions are that mucous membrane tissue is covered, and each group bone defect area Wound healing is good
It is good, no infection.
(2) imaging observation result：12 weeks after operation is swept with 16 slices spiral CTs (German Siemens, model Somatom 16)
Animal art area, A1 groups are retouched, defective region alveolar ridge top owes continuous, has portion of material to come off from defective region, single defective region quilt substantially
Area of new bone is filled up；B1 groups defective region is filled up substantially by area of new bone, area of new bone boundary visible with surrounding sclerotin；A2 and B2 groups defective region
It is filled up by area of new bone, area of new bone has been basically completed with autologous bone and has been connected, and density is without significant difference.Each group bone defect area is visible new
Raw bone, height of alveolar ridge recover, the visible continuous cortex bone (as shown in Figure 4) of alveolar ridge.Pass through medical imaging analysis software
Image-pro Plus 6.0 calculate bone defect area area of new bone and add up OD value (IOD), react different groups of defective region area of new bone
Variable density, result A1：21.73±2.23；A2:20.28±1.31；B1:22.02 ± 0.51, B2:20.56±1.08；It is empty
White is 16.66 ± 1.04.Statistical analysis shows that ceramic base dentistry bone meal repairs maxilla and mandibular with Bio-Oss bone meal
Defect is forming new bone density morning notable difference, and each group is compared with blank control, and there were significant differences.
(3) histological findings：Specimen sampling is carried out, embedding, section carry out Goldner trichrome stains and methylene
Indigo plant dyeing, optical microphotograph Microscopic observation New born formation situation.The thinly-sliced of Goldner three-color process dyeing is observed under multifunctional microscope
Piece, osteoid, new mineralising bone and mature bone boundary are apparent, Haversian system unobvious in new mineralising bone and osteoid, bone defect area
In cavity be unabsorbed bone material.A, B groups newborn bone amount no significant difference.From maxilla (Fig. 5 a and Fig. 5 b) and mandibular
(Fig. 6) finds out, mandibular skeletonization effect is good compared with maxilla.
(4) statistical analysis：Using medical imaging analysis software Imagepro P1us6.0 to the new of each group bone defect area
Skeletogenous region area is compared with non-osteogenic zone area, each group is substantially compared into bone amount, as shown in table 6.It is equal to add bone meal group
More into bone amount compared with blank group, the bone forming area of mandibular is more apparent than maxilla, and B groups are big compared with A group bone defects area bone forming area, but not
Substantially.
6 each group bone defect area area of new bone area area of table is compared with non-osteogenic zone area
The result of the test monitored according to application effect can be seen that ceramic base dentistry bone meal provided by the invention and be pulled out in reparation
The effect of tooth area bone defect is with the current best bone meal material Bio-oss of effect on the market without significant difference.But the present invention carries
For the cost of the bone meal material of confession but well below Bio-oss, preparation method is also simple.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent substitution to which part technical characteristic；
And these modification or replace, do not make appropriate technical solution essence depart from various embodiments of the present invention technical solution spirit and
Scope.
Claims (10)
1. a kind of ceramic base dentistry bone meal, which is characterized in that the preparation component of the dentistry bone meal includes：
Porous hydroxyapatite；
Type i collagen, quality are the 1%~10% of the porous hydroxyapatite quality；
Wherein, the preparation component of the porous hydroxyapatite includes hydroxyapatite, the first PMMA particles and the 2nd PMMA
Grain, mass ratio 5：(2.5~3.5)：(1.5~2.5), and the grain size of the first PMMA particles is 50~100 μm, the 2nd PMMA
The grain size of grain is 500~1000 μm；With
The porous hydroxyapatite is prepared by sintering, and the sintering includes such as the next stage：
First stage：Heating rate is 5~10 DEG C/min, and target temperature is 500~600 DEG C, and constant temperature time is 20~30min；
Second stage：Heating rate is 5~10 DEG C/min, and target temperature is 1200~1500 DEG C, constant temperature time for 200~
300min；
Phase III：Stop heating, Temperature fall.
2. dentistry bone meal according to claim 1, which is characterized in that the porous hydroxyapatite has the hole of connection；
With
The porous hydroxyapatite is：The particle of 20 mesh sieves can be crossed, it is preferable that the porous hydroxyapatite is：20 can be crossed
Mesh sieve, and the particle retained by 60 mesh sieves.
3. dentistry bone meal according to claim 1, which is characterized in that the preparation method bag of the porous hydroxyapatite
It includes：
(a) hydroxyapatite suspension is prepared；
(b) the first PMMA particles and the 2nd PMMA particles are added in the hydroxyapatite suspension, sintering base fluid is made；
(c) the sintering base fluid is placed in agglomerating plant and be sintered, agglomerated material is made；
(d) agglomerated material is crushed and sieved, the porous hydroxyapatite is made.
4. dentistry bone meal according to claim 3, which is characterized in that the step (a) carries out as follows：
15~20g hydroxyapatites are mixed in batches with 20~35mL PBS solutions, adding 1.5~2.5mL concentration is
The poly-vinyl alcohol solution of 0.05~0.1g/mL, stirs evenly, and preparation obtains the hydroxyapatite suspension.
5. the preparation method of any one of a kind of Claims 1-4 dentistry bone meal, which is characterized in that include the following steps：
(1) it is blended：The porous hydroxyapatite and the type i collagen are mixed and stirred for uniformly, being mixed with PBS solution
Liquid；
(2) mould is filled：The mixed liquor is poured into mold；
(3) freeze：The mold is freezed；
(4) crush：Material disintegrating after will be lyophilized；With
(5) sieve：The particle screening that will be obtained after crushed obtains ceramic base dentistry bone meal.
6. preparation method according to claim 5, which is characterized in that in step (3), described freeze includes the following steps：
The mold is put into freeze dryer, after pre-freeze, the first distillation, the second distillation and cooling four-stage, that is, completes institute
It states lyophilized；Wherein, it is described first distillation and second sublimation stage vacuumize, vacuum degree be less than -0.05MPa, aeration 50~
120Pa；With
The pre-freeze carries out as follows：Rate of temperature fall is 2.0~5.0 DEG C/min, and target temperature is -15~-30 DEG C, permanent
The warm time is 200~350min；
First distillation includes following 4 temperature gradients：
Heating rate is 0.5~1 DEG C/min, and target temperature is -15~-10 DEG C, and constant temperature time is 200~300min；
Heating rate is 0.3~0.5 DEG C/min, and target temperature is -10~-5 DEG C, and constant temperature time is 200~300min；
Heating rate is 0.2~0.3 DEG C/min, and target temperature is -5~-2 DEG C, and constant temperature time is 100~200min；
Heating rate is 0.1~0.2 DEG C/min, and target temperature is -2~0 DEG C, and constant temperature time is 100~200min；
Second distillation includes following 5 temperature gradients：
Heating rate is 0.5~1 DEG C/min, and target temperature is 10~20 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 20~30 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 30~40 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 40~50 DEG C, and constant temperature time is 60~150min；
Heating rate is 0.5~1 DEG C/min, and target temperature is 50~60 DEG C, and endpoint is carried out every 1h, until qualified；Eventually
Point≤0.9Pa/10min；
The cooling carries out as follows：Rate of temperature fall is 2~5 DEG C/min, until preceding box temperature degree reaches 20~25 DEG C.
7. preparation method according to claim 5, which is characterized in that in step (5), it is described screening as follows into
Row：
The particle obtained after the pulverization process is first crossed into 20 mesh sieves, sieved particle is retained after 60 mesh sieves by 60 mesh sieves
Particle be ceramic base dentistry bone meal；With
Send the particle retained by 20 mesh sieves back to the pulverising step.
8. preparation method according to claim 5, which is characterized in that in step (2), the thickness for filling mould is no more than 11mm.
9. preparation method according to claim 8, which is characterized in that in step (2), the thickness for filling mould is 5~10mm.
10. according to claim 5 to 9 any one of them preparation method, which is characterized in that in step (1), when the I types glue
Original is in terms of g, and for the PBS solution with mL timing, the amount ratio of the type i collagen and the PBS solution is 1：(25~45).
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| CN114096288A (en) * | 2019-07-26 | 2022-02-25 | 华沙整形外科股份有限公司 | Hydratable and flowable implantable compositions and methods of making and using the same |
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