CN110507862A - A kind of preparation method of high-strength composite guidance Tissue bone regeneration material - Google Patents
A kind of preparation method of high-strength composite guidance Tissue bone regeneration material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of high-strength composite guidance Tissue bone regeneration material, belong to bone-regeneration material technical field.Polylactic acid and hydroxyacetic acid polymerize by the present invention, matrix fiber is prepared using electrostatic spinning technique, collagen is coated on matrix fiber, and bone-regeneration material is processed by 3D printing technique and collagenous fiber bundle, with good mechanical strength, Human Arterial Smooth Muscle Cells can be good at adherency on the material, and grow along collagenous fiber bundle direction；Collagen is the important protein of animal connective tissue; connective tissue is other than containing 60~70% moisture; collagen accounts for about 20~30%; because there is the collagen of high-content; connective tissue is provided with certain structure and mechanical properties, such as tensile strength, pulling force, elastic force to reach the function of support, protection；Collagenous fiber bundle is that collagenous fibres arrange bunchy in loose connective tissue, is interlaced with one another identical, fibre bundle Chang You branch, and fiber has toughness, and anti-tractive force is strong.
Description
Technical field
The present invention relates to a kind of preparation methods of high-strength composite guidance Tissue bone regeneration material, belong to bone-regeneration material skill
Art field.
Background technique
In dentistry field, the reasons such as periodontosis, tip of a root lesion, wound cause the defect of periodontium, remain after extraction
The absorption of remaining alveolar ridge, and the reasons such as Bone mineral change will cause tooth supporting tissue defect in implant prostheses.Mesh
Preceding these problems, which mainly pass through, can increase bone amount in defect or improve the guided tissue regeneration (GTR) of bone mass or draw
Bone tissue regeneration art (GBR) is led to be treated.In this treatment technology, GTR film and GBR timbering material are key factors, directly
It connects and influences final repairing effect.In in the past few decades, the material for GTR/GBR is had changed a lot,
From biological stability, permanent type substitute to Bioabsorbable, temporary substitute transition, and gradually become in clinical application
Main trend.The application of absorbability GTR film and GBR timbering material avoids second operation and takes out problem, saves operation
Time and cost, reduce because operation caused by complication, therefore become current oral cavity bone impairment renovation material research
Emphasis.
The characteristics of physiologic theory of GTR/GBR and clinical application are for osteanagenesis process and generate and perfect.When
When bone defect occurs, since the speed that different tissues cell grows into defect, migrates is different, defect will be come first
It is filled, is formed soft tissue " clip pad " from the connective tissue of surrounding, and the presence of this " clip pad " will postpone the healing of bone tissue
Process.Using GTR/GBR technology, above-mentioned soft tissue is mechanically hindered first and enters bone defect position, keeps bone defect portion
There is a metastable regenerative environ-ment in position.New bone formation at bone defect be mainly by be located at periosteum occur the osteoblast of layer Lai
It undertakes, membrane material becomes the regenerated bracket of epiphysis periosteum at this time, and guidance has osteogenic cell adherence and to defect area
Migration.Timbering material at be filled in bone defect not only acts as supporting function, is able to maintain former organized shape, but also
Play template action, the place of boarding of relying, growth, differentiation and proliferation be provided for osteocyte, thus realize Guided Bone Regeneration and
Control the purpose of the structure of regenerating tissues.In addition, can constantly be dissolved in the degradation process of timbering material in vivo out calcium, phosphorus from
Son promotes mineralising deposition process, shortens healing time.
There are many type of the GTR/GBR film of studies and clinical application at present, by biodegradability be divided into Absorbable membrane and
Nonabsorable film two major classes.Nonabsorable film is primarily used for guide tissue regeneration, and this kind of material has very strong biologically inert,
Property is stablized, and does not react, but because it cannot be absorbed by tissue with tissue, needs to carry out two after 4 ~ 6 weeks after being implanted into human body
Secondary operation is taken out, and the chance of wound is increased, thus is difficult to be accepted by patients, and clinical therapeutic efficacy is also undesirable, therefore gradually
Replaced Absorbable membrane.Absorbability membrane material has good biocompatibility, nonantigenic interference, takes without second of operation
Out, degradation time can regulate and control, can directly participate in the features such as tissue repair and bootable cell growth of intrinsic reticular structure,
As ideal Guided bone regeneration membrane material.Ideal GTR/GBR film should have following characteristics:
(1) good biocompatibility and with the matched degradation rate of regeneration；
(2) good permeability also ensures the supply of nutriment and organizes metabolism while playing barrier action
It carries out；(3) suitable mechanical strength and clinical operability；
It (4) being capable of slow release active material promotion new bone formation.From materialogy angle, single material and single knot
Structure can not meet above-mentioned requirements simultaneously, therefore clinical existing guide tissue regeneration film material has been all made of multilayer and has answered
Close structure.
At present mainly using collagen or artificial macromolecule as the Absorbable membrane of main material used in clinic.Collagem membrane has
Following advantages:
(1) it is the main component of connective tissue, participates in tissue metabolism；
(2) there is higher inductivity to fibroblast；
(3) there is the characteristic for inhibiting epithelial cell mobile；
(4) poor antigen；
(5) there is anastalsis.What application was more at present is pigskin collagen film, due to the how purified processing of collagen, is generally not easy to draw
Play rejection.In addition, collagem membrane is generally gradually absorbed by organisms after implanting 8 weeks, remove the hardship of second operation from.Experiment
It confirms, collagem membrane is used on mouse nod the Guided Bone Regeneration reparation of bone defect, can not only play the role of obstructing fibr tissue,
It can also promote the regeneration of bone and participate in induced osteogenesis differentiation.
Bone tissue has very strong power of regeneration, when fracture or defect occur for bone tissue, forms hemotoncus in damaged zone first,
And then it is changed into granulation, and fibr tissue machine forms fibrocartilage, with the progress of mineral deposit and growing into for blood vessel, at
Osteocyte is also grown into therewith, and synthesis collagenous fibres are laid equal stress on the raw bone tissue of renewing, is finally completed entire regenerative process.It can be complete
It heals related with the gap size of damaged zone, if gap is excessive, osteoblast is difficult to get over gap and cannot occur normal
Agglutination is only filled by fibr tissue, in this case fracture or bone defect will be difficult to heal, need using timbering material into
Row fills the completion to assist knitting.
According to the difference of material source, osteanagenesis timbering material can be divided into autologous bone, homogeneous allogenic bone, bone- xenograft,
Decalcified bone matrix and artificial synthesis bone etc..Allograph bone is possible to cause rejection in vivo；Autologous bone meets bone tissue reparation
Requirement, but being limited source makes it be not widely deployed for clinic；And artificial synthesis bone, such as tricalcium phosphate, due to material
The characteristic for expecting itself, is difficult structure required for meeting carrying cell, these materials are difficult to meet the needs of clinical repair.With
The fast development of organizational engineering carries out Bone Defect Repari using organizational engineering principle, it has also become the hot spot studied at present.
Summary of the invention
The technical problems to be solved by the invention: aiming at the problem that existing bone-regeneration material bad mechanical strength, one is provided
The preparation method of kind high-strength composite guidance Tissue bone regeneration material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) lactic acid and hydroxyacetic acid are uniformly mixed, carry out vacuumize process to get mixture, mixture is stirred simultaneously
Stannous chloride is added to get reactant A in cooling processing in reactant A, continues 30~40min of stirring to get mixture A, incites somebody to action
Mixture A carries out vacuumizing reaction treatment, is cooled to room temperature to get presoma material；
(2) 7: 3 tetrahydrofuran and n,N-Dimethylformamide are uniformly mixed by volume to get mixed solution, in mass ratio 1
: 5 by presoma material and mixed solution after mixing, filter up to spinning solution, spinning solution be subjected to electrostatic spinning processing, i.e.,
Obtain matrix fiber；
(3) matrix fiber is immersed in mass fraction is to be protected from light stir process in 2% sodium periodate solution, is filtered up to precipitating,
Precipitating is washed with deionized 3~5 times to get washing precipitating, it is 1% glycerin solution that washing precipitating, which is immersed in mass fraction,
In after 1~2h, take out and impregnate in deionized water 20~for 24 hours, dehydration is to get pretreatment matrix fiber；Matrix will be pre-processed
It is in 80% collagen solution that fiber, which is immersed in mass fraction, and immersion treatment filters up to filter residue, and filter residue, which is placed in temperature, is
It dries in 80~90 DEG C of baking oven to constant weight, is cooled to room temperature up to semi-finished product, semi-finished product are placed in deionized water and impregnate 1
It, is dehydrated to get modified matrix fiber；
(4) modified matrix fiber, polyacrylamide, deionized water, collagenous fiber bundle are taken, by modified matrix fiber, polyacrylamide
Amine, deionized water mixing, low whipping speed are that 10~20min is stirred under 200~300r/min to get mixed slurry, are being mixed
Collagenous fiber bundle is added in slurry, continues 20~25min of stirring to get matrix slurry, matrix slurry is printed, i.e.,
It obtains high-strength composite and guides Tissue bone regeneration material.
Vacuumize process step described in step (1) are as follows: in mass ratio 9: 1 are uniformly mixed lactic acid and hydroxyacetic acid, In
Pressure is to vacuumize 5~10min under 4000~4500Pa.
Stirring described in step (1) and the processing step that cools down are as follows: by mixture in temperature be 60~65 DEG C, mixing speed is
1~2h is stirred under 500~600r/min to get reactant, and reactant is cooled to 25~27 DEG C, is passed through 5~10min of nitrogen.
The mass ratio of stannous chloride described in step (1) and reactant A is 1: 5.
Step vacuumizes reaction step described in (1) are as follows: mixture A is evacuated to 400~450Pa, temperature is 65~
8~10h is reacted at 70 DEG C.
Electrostatic spinning described in step (2) processing: by spinning solution voltage be 18~20kV, rectangular steel plates as receive dress
It sets, the reception distance of syringe needle and steel plate carries out electrostatic spinning under conditions of being 20~25cm.
Step is protected from light stir process step described in (3) are as follows: matrix fiber is immersed in mass fraction by mass ratio 1: 3 is
It is 40~50 DEG C in temperature in 2% sodium periodate solution, mixing speed is to be protected from light 30~50min of stirring under 200~300r/min.
Immersion treatment step described in step (3) are as follows: it is 80% collagen egg that pretreatment matrix fiber, which is immersed in mass fraction,
In white solution, 1~2h is impregnated in stirring at being 50~60 DEG C in temperature.
Modified matrix fiber described in step (4), polyacrylamide, deionized water, the ratio point between collagenous fiber bundle
Not are as follows: according to parts by weight, weigh respectively 30~40 parts of modified matrix fibers, 50~60 parts of polyacrylamides, 80~100 parts go
Ionized water, 20~30 parts of collagenous fiber bundles.
Print processing step described in step (4) are as follows: by matrix slurry temperature be 20~25 DEG C, platform temperature be 37~
39 DEG C of air pressures are 0.11~0.14MPa, and speed is 8~10mm/s, and printing filling spacing is 0.8~0.9mm, and printing thickness is
It is printed under 0.28~0.30mm.
The present invention is compared with other methods, and advantageous effects are:
(1) polylactic acid and hydroxyacetic acid polymerize by the present invention, prepare matrix fiber using electrostatic spinning technique, collagen is coated on
On matrix fiber, and bone-regeneration material is processed by 3D printing technique and collagenous fiber bundle, there is good mechanical strength, people
Arterial smooth muscle cell can be good at adherency on the material, and grow along collagenous fiber bundle direction；Collagen is
The important protein of object connective tissue, for connective tissue other than containing 60~70% moisture, collagen accounts for about 20~30%, because
To there is the collagen of high-content, connective tissue is provided with certain structure and mechanical properties, as tensile strength, pulling force,
Elastic force etc. is to reach the function of support, protection；Collagenous fiber bundle is that collagenous fibres arrange bunchy in loose connective tissue, each other
Interweave and coincide, fibre bundle Chang You branch, fiber has toughness, and anti-tractive force is strong；
(2) copolymer that polylactic acid and hydroxyacetic acid polymerize in the present invention is that one kind can be with biodegradable macromolecule material
Material, has excellent mechanical performance, biocompatibility and biodegradability and degradation speed is controllable, copolymer quilt in human body
It is degraded to lactic acid and light acetic acid, carbon dioxide and water are then generated by metabolism, to excrete, pair nontoxic to the human body
Effect；
(3) collagen has good biocompatibility and biodegradable in the present invention, and biocompatibility refers to collagen and place
There is good interaction between chief cell and tissue or between the matrix of cell peripheral, there is interactional coordination
Property, and collagen can become a part of cell and tissue, the physiological function brought into normal play jointly；Collagen is beaten using 3D
Print technology is coated to matrix fiber, and matrix fiber is made to have good biocompatibility；
(4) 3D printing technique is total with Clinical Computer tomoscan, magnetic as a kind of novel digital forming technique in the present invention
Vibration imaging etc. combines, and using CAD personalization implantation material, realization is precisely controlled pore structure, design with
The substantially identical bone-regeneration material of patient bone defect area is conducive to the biocompatibility for improving implantation material；By glue
The matrix resin of original coating has good mechanical strength, and matrix resin and collagenous fiber bundle mixing, collagenous fibres element are distributed in
On matrix fiber, under load effect, the collagenous fibres network across crackle may prevent crackle from expanding and propagate, and make forced section
Position crack, which glances off, generates a large amount of matrix crackles, and the matrix debris and the plane of disruption of the more voluminous life of crackle are also more, can absorb
More energy provide some strength for bone-regeneration material.
Specific embodiment
In mass ratio 9: 1 are uniformly mixed lactic acid and hydroxyacetic acid, 5 are vacuumized in the case where pressure is 4000~4500Pa~
Mixture in temperature is 60~65 DEG C to get mixture by 10min, and mixing speed is that 1~2h is stirred under 500~600r/min,
Up to reactant, reactant is cooled to 25~27 DEG C, is passed through 5~10min of nitrogen to get reactant A, in mass ratio 1: 5
Stannous chloride is added in reactant A, continues 30~40min of stirring to get mixture A, mixture A is evacuated to 400~
450Pa, temperature are that 8~10h is reacted at 65~70 DEG C, are cooled to room temperature to get presoma material；7: 3 by tetrahydro by volume
Furans and n,N-Dimethylformamide are uniformly mixed to get mixed solution, and in mass ratio 1: 5 by presoma material and mixed solution
After mixing, it filters up to spinning solution, in voltage is 18~20kV by spinning solution, rectangular steel plates are as reception device, syringe needle
Reception distance with steel plate carries out electrostatic spinning under conditions of being 20~25cm to get matrix fiber；In mass ratio 1: 3 by matrix
It is in 2% sodium periodate solution that fiber, which is immersed in mass fraction, is 40~50 DEG C in temperature, mixing speed is 200~300r/min
Under be protected from light 30~50min of stirring, filter up to precipitate, precipitating is washed with deionized 3~5 times to get washing precipitating, will wash
Precipitating be immersed in mass fraction and be in 1% glycerin solution after 1~2h take out and impregnate in deionized water 20~for 24 hours, dehydration,
Up to pretreatment matrix fiber；It is to be in temperature in 80% collagen solution that pretreatment matrix fiber, which is immersed in mass fraction,
1~2h is impregnated in stirring at 50~60 DEG C, filters up to filter residue, filter residue is placed in the baking oven that temperature is 80~90 DEG C and is dried to perseverance
Weight is cooled to room temperature up to semi-finished product, semi-finished product is placed in deionized water and are impregnated 1 day, is dehydrated to get modified matrix fiber；
According to parts by weight, 30~40 parts of modified matrix fibers, 50~60 parts of polyacrylamides, 80~100 parts of deionizations are weighed respectively
Water, 20~30 parts of collagenous fiber bundles mix modified matrix fiber, polyacrylamide, deionized water, low whipping speed 200
10~20min is stirred under~300r/min to get mixed slurry, and collagenous fiber bundle is added in mixed slurry, continues stirring 20
Matrix slurry in temperature is 20~25 DEG C, platform temperature is that 37~39 DEG C of air pressures are 0.11 to get matrix slurry by~25min
~0.14MPa, speed are 8~10mm/s, and printing filling spacing is 0.8~0.9mm, and printing thickness, which is that 0.28~0.30mm is lower, beats
Print guides Tissue bone regeneration material to get high-strength composite.
Embodiment 1
In mass ratio 9: 1 are uniformly mixed lactic acid and hydroxyacetic acid, vacuumize 5min in the case where pressure is 4000Pa to get mixing
Object, by mixture temperature be 60 DEG C, mixing speed be 500r/min under stir 1h to get reactant, reactant is cooled to
25 DEG C, nitrogen 5min is passed through to get reactant A, in mass ratio 1: 5, stannous chloride is added in reactant A, continue to stir
30min is evacuated to 400Pa to get mixture A, by mixture A, and temperature is to react 8h at 65 DEG C, is cooled to room temperature to get preceding
Drive body material；7: 3 tetrahydrofuran and n,N-Dimethylformamide are uniformly mixed by volume to get mixed solution, by quality
After mixing by presoma material and mixed solution than 1: 5, it filters up to spinning solution, in voltage is 18kV, square by spinning solution
For shape steel plate as reception device, the reception distance of syringe needle and steel plate carries out electrostatic spinning to get matrix fibre under conditions of being 20cm
Dimension；Matrix fiber is immersed in mass fraction to be 40 DEG C in temperature, stirring is fast in 2% sodium periodate solution by mass ratio 1: 3
Degree is to be protected from light to stir 30min under 200r/min, is filtered up to precipitating, and precipitating is washed with deionized 3 times and precipitates to get washing,
After washing precipitating is immersed in mass fraction as 1h in 1% glycerin solution, 20h in deionized water is taken out and is impregnated, is dehydrated,
Up to pretreatment matrix fiber；It is to be in temperature in 80% collagen solution that pretreatment matrix fiber, which is immersed in mass fraction,
1h is impregnated in stirring at 50 DEG C, filters up to filter residue, filter residue is placed in the baking oven that temperature is 80 DEG C and is dried to constant weight, room is cooled to
Semi-finished product are placed in deionized water and impregnate 1 day up to semi-finished product by temperature, are dehydrated to get modified matrix fiber；In parts by weight
Meter, weighs 30 parts of modified matrix fibers, 50 parts of polyacrylamides, 80 parts of deionized waters, 20 parts of collagenous fiber bundles respectively, will be modified
Matrix fiber, polyacrylamide, deionized water mixing, low whipping speed are that 10min is stirred under 200r/min to get mixing slurry
Material, is added collagenous fiber bundle in mixed slurry, continues to stir 20min to get matrix slurry, in temperature is 20 by matrix slurry
DEG C, platform temperature is that 37 DEG C of air pressures are 0.11MPa, speed 8mm/s, and printing filling spacing is 0.8mm, and printing thickness is
It is printed under 0.28mm and guides Tissue bone regeneration material to get high-strength composite.
Embodiment 2
In mass ratio 9: 1 are uniformly mixed lactic acid and hydroxyacetic acid, vacuumize 8min in the case where pressure is 4250Pa to get mixing
Object, by mixture temperature be 62 DEG C, mixing speed be 550r/min under stir 1h to get reactant, reactant is cooled to
26 DEG C, nitrogen 8min is passed through to get reactant A, in mass ratio 1: 5, stannous chloride is added in reactant A, continue to stir
35min is evacuated to 425Pa to get mixture A, by mixture A, and temperature is to react 9h at 68 DEG C, is cooled to room temperature to get preceding
Drive body material；7: 3 tetrahydrofuran and n,N-Dimethylformamide are uniformly mixed by volume to get mixed solution, by quality
After mixing by presoma material and mixed solution than 1: 5, it filters up to spinning solution, in voltage is 19kV, square by spinning solution
For shape steel plate as reception device, the reception distance of syringe needle and steel plate carries out electrostatic spinning to get matrix fibre under conditions of being 22cm
Dimension；Matrix fiber is immersed in mass fraction to be 45 DEG C in temperature, stirring is fast in 2% sodium periodate solution by mass ratio 1: 3
Degree is to be protected from light to stir 40min under 250r/min, is filtered up to precipitating, and precipitating is washed with deionized 4 times and precipitates to get washing,
After washing precipitating is immersed in mass fraction as 1h in 1% glycerin solution, 22h in deionized water is taken out and is impregnated, is dehydrated,
Up to pretreatment matrix fiber；It is to be in temperature in 80% collagen solution that pretreatment matrix fiber, which is immersed in mass fraction,
1h is impregnated in stirring at 55 DEG C, filters up to filter residue, filter residue is placed in the baking oven that temperature is 85 DEG C and is dried to constant weight, room is cooled to
Semi-finished product are placed in deionized water and impregnate 1 day up to semi-finished product by temperature, are dehydrated to get modified matrix fiber；In parts by weight
Meter, weighs 35 parts of modified matrix fibers, 55 parts of polyacrylamides, 90 parts of deionized waters, 25 parts of collagenous fiber bundles respectively, will be modified
Matrix fiber, polyacrylamide, deionized water mixing, low whipping speed are that 15min is stirred under 250r/min to get mixing slurry
Material, is added collagenous fiber bundle in mixed slurry, continues to stir 22min to get matrix slurry, in temperature is 22 by matrix slurry
DEG C, platform temperature is that 38 DEG C of air pressures are 0.12MPa, speed 9mm/s, and printing filling spacing is 0.8mm, and printing thickness is
It is printed under 0.29mm and guides Tissue bone regeneration material to get high-strength composite.
Embodiment 3
In mass ratio 9: 1 are uniformly mixed lactic acid and hydroxyacetic acid, vacuumize 10min in the case where pressure is 4500Pa to get mixing
Object, by mixture temperature be 65 DEG C, mixing speed be 600r/min under stir 2h to get reactant, reactant is cooled to
27 DEG C, nitrogen 10min is passed through to get reactant A, in mass ratio 1: 5, stannous chloride is added in reactant A, continue to stir
40min is evacuated to 450Pa to get mixture A, by mixture A, and temperature is to react 10h at 70 DEG C, be cooled to room temperature to get
Presoma material；7: 3 tetrahydrofuran and n,N-Dimethylformamide are uniformly mixed by volume to get mixed solution, by matter
Amount than 1: 5 by presoma material and mixed solution after mixing, filter up to spinning solution, in voltage be 20kV by spinning solution,
Rectangular steel plates carry out electrostatic spinning under conditions of being 25cm as reception device, the reception distance of syringe needle and steel plate to get matrix
Fiber；Matrix fiber is immersed in mass fraction to be 50 DEG C in temperature, stirring in 2% sodium periodate solution by mass ratio 1: 3
Speed is that stirring 50min is protected from light under 300r/min, is filtered up to precipitating, and it is heavy to get washing precipitating to be washed with deionized 5 times
It forms sediment, it is to take out and impregnate in deionized water for 24 hours in 1% glycerin solution after 2h that washing precipitating, which is immersed in mass fraction, is taken off
Water is to get pretreatment matrix fiber；It is in 80% collagen solution, in temperature that pretreatment matrix fiber, which is immersed in mass fraction,
Degree is that 2h is impregnated in stirring at 60 DEG C, filters up to filter residue, filter residue is placed in baking oven at a temperature of 90 °C and is dried to constant weight, cooling
To room temperature up to semi-finished product, semi-finished product are placed in deionized water and are impregnated 1 day, is dehydrated to get modified matrix fiber；By weight
Number meter, weighs 40 parts of modified matrix fibers, 60 parts of polyacrylamides, 100 parts of deionized waters, 30 parts of collagenous fiber bundles respectively, will
Modified matrix fiber, polyacrylamide, deionized water mixing, low whipping speed are that 20min is stirred under 300r/min to get mixing
Collagenous fiber bundle is added in slurry in mixed slurry, continues to stir 25min to get matrix slurry, is in temperature by matrix slurry
25 DEG C, platform temperature is that 39 DEG C of air pressures are 0.14MPa, speed 10mm/s, and printing filling spacing is 0.9mm, and printing thickness is
It is printed under 0.30mm and guides Tissue bone regeneration material to get high-strength composite.
Reference examples: the compound guiding Tissue bone regeneration material of Dongguan company production.
The compound guiding Tissue bone regeneration material that embodiment and reference examples are prepared is detected, specific detection is such as
Under:
Porosity: by every group of 4 cylindrical stents be cut into diameter be 6.0mm, highly be 2.5mm cylindric sample, press
ISO15901-1:2005 standard, the contact angle being arranged in test are 130 °, and equilibration time 30s utilizes mercury injection apparatus test material
Porosity.
Mechanical property: using the compression strength of material after the test sintering of electronic table universal testing machine, test speed is
0.5mm/min, every kind of material are chosen 3 samples and are tested.
Specific test result such as table 1.
1 performance characterization contrast table of table
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples |
| Porosity/% | 75.1 | 75.0 | 76.5 | 50.8 |
| Compression strength/MPa | 15.6 | 17.9 | 16.0 | 3.3 |
As shown in Table 1, compound guiding Tissue bone regeneration material prepared by the present invention has good mechanical strength and porosity.
Claims (10)
1. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material, it is characterised in that specific preparation step are as follows:
(1) lactic acid and hydroxyacetic acid are uniformly mixed, carry out vacuumize process to get mixture, mixture is stirred simultaneously
Stannous chloride is added to get reactant A in cooling processing in reactant A, continues 30~40min of stirring to get mixture A, incites somebody to action
Mixture A carries out vacuumizing reaction treatment, is cooled to room temperature to get presoma material；
(2) 7: 3 tetrahydrofuran and n,N-Dimethylformamide are uniformly mixed by volume to get mixed solution, in mass ratio 1
: 5 by presoma material and mixed solution after mixing, filter up to spinning solution, spinning solution be subjected to electrostatic spinning processing, i.e.,
Obtain matrix fiber；
(3) matrix fiber is immersed in mass fraction is to be protected from light stir process in 2% sodium periodate solution, is filtered up to precipitating,
Precipitating is washed with deionized 3~5 times to get washing precipitating, it is 1% glycerin solution that washing precipitating, which is immersed in mass fraction,
In after 1~2h, take out and impregnate in deionized water 20~for 24 hours, dehydration is to get pretreatment matrix fiber；Matrix will be pre-processed
It is in 80% collagen solution that fiber, which is immersed in mass fraction, and immersion treatment filters up to filter residue, and filter residue, which is placed in temperature, is
It dries in 80~90 DEG C of baking oven to constant weight, is cooled to room temperature up to semi-finished product, semi-finished product are placed in deionized water and impregnate 1
It, is dehydrated to get modified matrix fiber；
(4) modified matrix fiber, polyacrylamide, deionized water, collagenous fiber bundle are taken, by modified matrix fiber, polyacrylamide
Amine, deionized water mixing, low whipping speed are that 10~20min is stirred under 200~300r/min to get mixed slurry, are being mixed
Collagenous fiber bundle is added in slurry, continues 20~25min of stirring to get matrix slurry, matrix slurry is printed, i.e.,
It obtains high-strength composite and guides Tissue bone regeneration material.
2. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
In: vacuumize process step described in step (1) are as follows: in mass ratio 9: 1 are uniformly mixed lactic acid and hydroxyacetic acid, are in pressure
5~10min is vacuumized under 4000~4500Pa.
3. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
In stirring described in step (1) and the processing step that cools down are as follows: it by mixture in temperature is 60~65 DEG C, mixing speed is 500~
1~2h is stirred under 600r/min to get reactant, and reactant is cooled to 25~27 DEG C, is passed through 5~10min of nitrogen.
4. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
In: the mass ratio of stannous chloride described in step (1) and reactant A is 1: 5.
5. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
In: step vacuumizes reaction step described in (1) are as follows: mixture A is evacuated to 400~450Pa, temperature is at 65~70 DEG C
React 8~10h.
6. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
In the processing of: electrostatic spinning described in step (2): in voltage being 18~20kV by spinning solution, rectangular steel plates are as reception device, needle
The reception distance of head and steel plate carries out electrostatic spinning under conditions of being 20~25cm.
7. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
In: step is protected from light stir process step described in (3) are as follows: in mass ratio 1: 3 matrix fiber is immersed in mass fraction is 2% high
It is 40~50 DEG C in temperature in sodium iodide solution, mixing speed is to be protected from light 30~50min of stirring under 200~300r/min.
8. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
In: immersion treatment step described in step (3) are as follows: it is that 80% collagen is molten that pretreatment matrix fiber, which is immersed in mass fraction,
In liquid, 1~2h is impregnated in stirring at being 50~60 DEG C in temperature.
9. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
Ratio between: modified matrix fiber described in step (4), polyacrylamide, deionized water, collagenous fiber bundle is respectively as follows:
According to parts by weight, 30~40 parts of modified matrix fibers, 50~60 parts of polyacrylamides, 80~100 parts of deionizations are weighed respectively
Water, 20~30 parts of collagenous fiber bundles.
10. a kind of preparation method of high-strength composite guidance Tissue bone regeneration material according to claim 1, feature exist
In print processing step described in step (4) are as follows: by matrix slurry in temperature be 20~25 DEG C, platform temperature is 37~39 DEG C
Air pressure be 0.11~0.14MPa, speed be 8~10mm/s, printing filling spacing be 0.8~0.9mm, printing thickness be 0.28~
It is printed under 0.30mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113117150A (en) * | 2019-12-31 | 2021-07-16 | 广州迈普再生医学科技股份有限公司 | Guided tissue regeneration membrane and preparation method and application thereof |
| CN114288481A (en) * | 2022-01-25 | 2022-04-08 | 点云生物(杭州)有限公司 | Multilayer composite medicine-carrying guided bone regeneration membrane and preparation method thereof |
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2019
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113117150A (en) * | 2019-12-31 | 2021-07-16 | 广州迈普再生医学科技股份有限公司 | Guided tissue regeneration membrane and preparation method and application thereof |
| CN113117150B (en) * | 2019-12-31 | 2022-07-19 | 广州迈普再生医学科技股份有限公司 | Guided tissue regeneration membrane and preparation method and application thereof |
| CN114288481A (en) * | 2022-01-25 | 2022-04-08 | 点云生物(杭州)有限公司 | Multilayer composite medicine-carrying guided bone regeneration membrane and preparation method thereof |
| CN114288481B (en) * | 2022-01-25 | 2022-07-19 | 点云生物(杭州)有限公司 | Multilayer composite medicine-carrying guided bone regeneration membrane and preparation method thereof |
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