CN105288751B - A kind of multi-gradient bionic joint cartilage material preparation process based on 3D printing - Google Patents
A kind of multi-gradient bionic joint cartilage material preparation process based on 3D printing Download PDFInfo
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- CN105288751B CN105288751B CN201510752927.5A CN201510752927A CN105288751B CN 105288751 B CN105288751 B CN 105288751B CN 201510752927 A CN201510752927 A CN 201510752927A CN 105288751 B CN105288751 B CN 105288751B
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- 238000010146 3D printing Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 claims abstract description 46
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 claims abstract description 46
- CMMUKUYEPRGBFB-UHFFFAOYSA-L dichromic acid Chemical compound O[Cr](=O)(=O)O[Cr](O)(=O)=O CMMUKUYEPRGBFB-UHFFFAOYSA-L 0.000 claims abstract description 12
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- 239000000203 mixture Substances 0.000 claims description 16
- 229920002125 Sokalan® Polymers 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 15
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 12
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 12
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- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
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- 239000011521 glass Substances 0.000 claims description 6
- 229920001684 low density polyethylene Polymers 0.000 claims description 6
- 239000004702 low-density polyethylene Substances 0.000 claims description 6
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- 238000000110 selective laser sintering Methods 0.000 claims description 5
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- 239000004698 Polyethylene Substances 0.000 claims description 4
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
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- Materials For Medical Uses (AREA)
- Prostheses (AREA)
Abstract
A kind of multi-gradient bionic joint cartilage material preparation process based on 3D printing, belongs to biomimetic material preparation technology.Preparing material includes：Modified ultra-high molecular weight polyethylene material for 3D printing；Dichromic acid aoxidizes solution；Graft esterification solution；Polyglycol solution；Three kinds of bionic joint cartilage materials.Preparation technology：1) porous ultra-high molecular weight polyethylene is prepared using 3D printing technique；2) in the surface-crosslinked PVA/HA composite aquogels bionic cartilage material of the porous ultra-high molecular weight polyethylene of 3D printing；3) sample after step 2 is crosslinked PVA/HA PAA composite aquogel bionic cartilage materials again through esterification treatment；4) esterification treatment and the cross-linked PVA hydrogel bionic cartilage material again of the sample after step 3；So as to obtain the bionic joint cartilage material with multilayered and graded structure.The bionic cartilage material prepared is similar with natural cartilage structure, function phase, it is not easy to wear loosen, boundary lubrication is good, bioactivity is sufficient, instead of the effect of cartilage to a certain extent.
Description
Technical field
The present invention relates to a kind of bionic joint cartilage material preparation process, particularly a kind of multi-gradient based on 3D printing
Bionic joint cartilage material preparation process.
Background technology
Human body natural joint is made up of articular surface, articular cavity and several parts of capsular ligament, and the surface of ball and socket joint and fossa glenoid is covered
Articular cartilage is covered with, articular cartilage is a kind of hyperhydrated biological tissue, is mainly made up of cartilage cell, extracellular matrix and water.
The structure of native articular cartilage is uneven, non-linear, anisotropic, and five layers can be divided into from articular surface to deep：Superficial
Layer, intermediate layer, deep layer, calcified layer and subchondral bone, the composition, structure between each layer are totally different, and different zones have it is different
Mechanical property, and have very close dependence between each layer, the common function of exercising cartilage.In the normal life of human body
Articular cartilage can provide an excellent lubricating bearing articular surface in reason environment, can carry the weight for transmitting 7-9 times of human body,
, as a rule, being capable of proper motion more than 70 years and coefficient of friction is extremely low (0.001-0.03).
Because joint is that human body bears the maximum biological friction pair of load, therefore articular cartilage will bear to move institute in life
The abrasion to go round and begin again caused, with advancing age, and many factors such as congenital disorders, abrasion, wound, it can cause soft
The metabolic disorder of osteocyte, the proteoglycan content in cartilage greatly reduce, and articular cartilage flexibility decrease, collagenous fibres break
Split, cause articular cartilage constantly to degenerate and wear, knuckle synovia deficiency, softening, erosion occur, come off, subchondral bone exposure, bone
Directly contacted between bone, rigid friction occurs, joint the symptoms such as pain, swelling, bony crepitus occurs, ultimately results in Bones and joints
Scorching generation.At present, osteoarthritis turns into the No.1 disabling condition in the world caused by articular cartilage is worn, and the whole world there are about 4
Hundred million people endure the torment of bone and joint diseases.
Artificial joint prosthesis is that the joint assembly substitution that manually material makes the natural joint of lesion or damage occurs, right
In the secondary selection of Artificial Intervention material friction, be concentrated mainly on both at home and abroad at present ultra-high molecular weight polyethylene (UHMWPE)/metal,
Metal/metal and ceramics/ceramic articulation etc., but Artificial Intervention material does not possess the metabolism of nature vitality, prosthese
The poor compatibility of interface behavior and life medium, the abrasion of joint implant contact surface is the phenomenon certainly existed, and is worn
All continuing every year, wear particle is also being stepped up always.Substantial amounts of clinic study is it has proven convenient that the abrasion of joint prosthesis
One of major reason of joint replacement aseptic loosening, i.e., caused by wear particle localized interface bone dissolving caused by prosthese without
Bacterium loosens, and is the main reason for causing prosthetic replacement to fail.It is caused that its clinical meaning is not only in that prosthese destroys in itself
Mechanicalness failure, a large amount of particulate matters with induction Periprosthetic bone dissolving biological respinse can be produced by also residing in abrasion.
The content of the invention
The invention aims to provide a kind of multi-gradient bionic joint cartilage material preparation process based on 3D printing,
A kind of bionic joint cartilage material similar with function phase with native articular cartilage structure is obtained by this method, solves artificial close
The problem of abrasion of section and sterile loosening.
The object of the present invention is achieved like this：The material of bionic joint cartilage of the present invention has：Available for changing for 3D printing
Property superhigh molecular weight polyethylene material；Dichromic acid aoxidizes solution；Graft esterification solution；Polyglycol solution；Three kinds of bionic joints
Cartilage material.
The described specific composition of modified ultra-high molecular weight polyethylene material available for 3D printing includes：Super high molecular weight is gathered
Ethene 60.8%, low density polyethylene (LDPE) 23.7%, CNT 8.8%, talcum powder 3.4%, poly- (methyl) acrylate
2.7%th, antioxidant CA 0.3%, titanate esters 0.3%；
The dichromic acid oxidation specific composition of solution includes：Potassium bichromate 20%, the concentrated sulfuric acid 80%；
The specific composition of graft esterification solution includes：Polyvinyl alcohol 7%, the concentrated sulfuric acid 1.5%, deionized water 91.5%；
The bionic joint cartilage material is divided into three kinds, and specific composition is respectively：
(1) polyvinyl alcohol 15%, nanometer hydroxyapatite 3%, deionized water 82%；
(2) polyvinyl alcohol 14%, nanometer hydroxyapatite 3%, polyacrylic acid 3%, deionized water 80%；
(3) polyvinyl alcohol 15%, deionized water 85%；
The specific composition of described polyglycol solution includes：Polyethylene glycol 100%；
Described polyvinyl alcohol purity >=99%, potassium bichromate is analyzes pure level, and the concentrated sulfuric acid is 98% grade of mass fraction, institute
The percentage for the material stated is mass percent.
Multi-gradient bionic joint cartilage material preparation process based on 3D printing comprises the following steps：
1) the ultra-high molecular weight polyethylene model with loose structure is created using Three-dimensional Design Software, exports STL forms
File, special 3D printing software is imported, utilize fused glass pellet (FDM) or selective laser sintering (SLS) technology printing system
The standby ultra-high molecular weight polyethylene block with loose structure；
2) the ultra-high molecular weight polyethylene block with loose structure is immersed in dichromic acid oxidation solution, is placed in 75 DEG C
10min in water-bath, be then placed on 10min in 50 DEG C of salpeter solutions, except after deoxidation surface formed small-molecule substance,
Taking-up is cleaned with a large amount of deionized waters；Described dichromic acid oxidation solution is by quality percentage by potassium bichromate and the concentrated sulfuric acid
Than 1:4 configurations form；
3) polyvinyl alcohol 15%, nanometer hydroxyapatite 3% and deionized water 82% are weighed by mass percentage is placed in appearance
In device, 24h is swelled at room temperature, and container is then prepared into PVA/HA mixed solutions as in 95 DEG C of thermostat water bath；Press
Mass percent weighs polyvinyl alcohol 7%, the concentrated sulfuric acid 1.5% and deionized water 91.5% and is placed in container, is prepared by above-mentioned steps
Go out grafting solution；
4) it will aoxidize to immerse with the ultra-high molecular weight polyethylene sample with loose structure after cleaning and grafting solution be housed
Container in, be placed in 90 DEG C of thermostat water bath, stir, react 2h；
5) the PVA/HA mixed solutions prepared are added to loose structure ultra-high molecular weight polyethylene specimen surface so that
The thickness of PVA/HA mixed solutions is 1mm, and the loose structure ultra-high molecular weight polyethylene sample after handling as stated above is put
Dry at room temperature, after one week, the surface formation first layer PVA/HA of loose structure ultra-high molecular weight polyethylene sample is compound
Hydrogel bionic joint cartilage；
6) polyvinyl alcohol 14% that weighs by mass percentage, nanometer hydroxyapatite 3%, polyacrylic acid solution 3%, go
Ionized water 80%, is placed in beaker, is then gently mixed with glass bar and is sealed in a moment with preservative film, allows it to be swelled 2- at room temperature
3h；It is put into 95 DEG C of electronic thermostatic water-baths and dissolves by heating after the completion of swelling, by beaker from water-bath after solution is completely dissolved
Middle taking-up, PVA/HA-PAA mixed solutions are obtained, are placed in ultrasonic 2-3h in ultrasonic wave, and first layer is carried by what step 5 obtained
The loose structure ultra-high molecular weight polyethylene sample of PVA/HA composite aquogel bionic joint cartilages is placed in 60 DEG C of grafting solution
In, stirring, react 2h；Then PVA/HA-PAA mixed solutions are added to the loose structure super high molecular weight after step 5 is handled
Polyethylene sample surface, it is 0.5mm to make its thickness, is placed in the low temperature storage box that temperature is -20 DEG C and freezes 10-12 hours, so
Afterwards defrosting 2-3 hours at room temperature, place into low temperature storage box and freezed afterwards, so freezing, thaw 3 times；
7) sample after freeze-thaw is immersed in the beaker for filling polyglycol solution, 1-2h is dehydrated, in dehydration
In sample is weighed at regular intervals, when the weight of sample no longer changes, take out sample and be put into resistance furnace
Row annealing, annealing temperature are 120 DEG C, annealing time 1h, and sample is taken out after the completion of annealing, and with deionized water to sample
Cleaned, remove remnants polyglycol solution；Sample after cleaning is put into deionized water carry out it is rehydrated, it is rehydrated
After the completion of, the surface of loose structure ultra-high molecular weight polyethylene sample forms the bionical pass of second layer PVA/HA-PAA composite aquogels
Save cartilage；
8) polyvinyl alcohol 15% is weighed by mass percentage and deionized water 85% is placed in container, is swelled at room temperature
24h, container is then prepared into PVA solution as in 95 DEG C of thermostat water bath；Loose structure after step 7 is handled surpasses
High molecular weight polyethylene sample is placed in 60 DEG C of grafting solution, stirring, reacts 2h；It is PVA by the mass percent prepared
Solution is added to the loose structure ultra-high molecular weight polyethylene specimen surface after step 7 processing so that the thickness of PVA solution is
0.5mm, it is that 10-12 hours are freezed in -20 DEG C of low temperature storage box to be subsequently placed in temperature, then defrosting 2-3 hours at room temperature,
Place into low temperature storage box and freezed afterwards, so freezing, thaw 9 times after, loose structure ultra-high molecular weight polyethylene examination
The surface of sample forms third layer PVA hydrogel bionic joint cartilages；
9) the loose structure ultra-high molecular weight polyethylene sample with three layers of bionic joint cartilage prepared is put into Sheng
Have in the hermetic bag of deionized water and preserve.
Advantage：As a result of such scheme, the multi-gradient bionic joint cartilage material and natural joint prepared
Cartilage structure, function phase are similar, and have very strong binding ability between each layer, it is not easy to wear loosen, boundary lubrication it is good,
Bioactivity is sufficient, is truly realized instead of cartilage function, solves the problems, such as the abrasion of joint prosthesis and sterile loosening, reach
The purpose of the present invention.
Brief description of the drawings：
Fig. 1 is loose structure ultra-high molecular weight polyethylene sample schematic diagram after 3D printing of the invention.
Fig. 2 is the multi-gradient bionic joint cartilage material preparation process schematic diagram based on 3D printing of the present invention.
Embodiment
Embodiment 1：The material of bionic joint cartilage of the present invention has：Modified ultra-high molecular weight polyethylene available for 3D printing
Material；Dichromic acid aoxidizes solution；Graft esterification solution；Bionic joint cartilage material.
The described specific composition of modified ultra-high molecular weight polyethylene material available for 3D printing includes：Super high molecular weight is gathered
Ethene 60.8%, low density polyethylene (LDPE) 23.7%, CNT 8.8%, talcum powder 3.4%, poly- (methyl) acrylate
2.7%th, antioxidant CA 0.3%, titanate esters 0.3%；
The dichromic acid oxidation specific composition of solution includes：Potassium bichromate 20%, the concentrated sulfuric acid 80%；
The specific composition of graft esterification solution includes：Polyvinyl alcohol 7%, the concentrated sulfuric acid 1.5%, deionized water 91.5%；
The bionic joint cartilage material is divided into three kinds, and specific composition is respectively：
(1) polyvinyl alcohol 15%, nanometer hydroxyapatite 3%, deionized water 82%；
(2) polyvinyl alcohol 14%, nanometer hydroxyapatite 3%, polyacrylic acid 3%, deionized water 80%；
(3) polyvinyl alcohol 15%, deionized water 85%；
The specific composition of described polyglycol solution includes：Polyethylene glycol 100%；
Described polyvinyl alcohol purity >=99%, potassium bichromate is analyzes pure level, and the concentrated sulfuric acid is 98% grade of mass fraction, institute
The percentage for the material stated is mass percent.
Multi-gradient bionic joint cartilage material preparation process based on 3D printing comprises the following steps：
1) the ultra-high molecular weight polyethylene model with loose structure is created using Three-dimensional Design Software, exports STL forms
File, special 3D printing software is imported, utilize fused glass pellet (FDM) or selective laser sintering (SLS) technology printing system
The standby ultra-high molecular weight polyethylene block with loose structure；
2) the ultra-high molecular weight polyethylene block with loose structure is immersed in dichromic acid oxidation solution, is placed in 75 DEG C
10min in water-bath, be then placed on 10min in 50 DEG C of salpeter solutions, except after deoxidation surface formed small-molecule substance,
Taking-up is cleaned with a large amount of deionized waters；Described dichromic acid oxidation solution is by quality percentage by potassium bichromate and the concentrated sulfuric acid
Than 1:4 configurations form；
3) polyvinyl alcohol 15%, nanometer hydroxyapatite 3% and deionized water 82% are weighed by mass percentage is placed in appearance
In device, 24h is swelled at room temperature, and container is then prepared into PVA/HA mixed solutions as in 95 DEG C of thermostat water bath；Press
Mass percent weighs polyvinyl alcohol 7%, the concentrated sulfuric acid 1.5% and deionized water 91.5% and is placed in container, is prepared by above-mentioned steps
Go out grafting solution；
4) it will aoxidize to immerse with the ultra-high molecular weight polyethylene sample with loose structure after cleaning and grafting solution be housed
Container in, be placed in 90 DEG C of thermostat water bath, stir, react 2h；
5) the PVA/HA mixed solutions prepared are added to loose structure ultra-high molecular weight polyethylene specimen surface so that
The thickness of PVA/HA mixed solutions is 1mm, and the loose structure ultra-high molecular weight polyethylene sample after handling as stated above is put
Dry at room temperature, after one week, the surface formation first layer PVA/HA of loose structure ultra-high molecular weight polyethylene sample is compound
Hydrogel bionic joint cartilage；
6) polyvinyl alcohol 14% that weighs by mass percentage, nanometer hydroxyapatite 3%, polyacrylic acid solution 3%, go
Ionized water 80%, is placed in beaker, is then gently mixed with glass bar and is sealed in a moment with preservative film, allows it to be swelled 2- at room temperature
3h；It is put into 95 DEG C of electronic thermostatic water-baths and dissolves by heating after the completion of swelling, by beaker from water-bath after solution is completely dissolved
Middle taking-up, PVA/HA-PAA mixed solutions are obtained, are placed in ultrasonic 2-3h in ultrasonic wave, and first layer is carried by what step 5 obtained
The loose structure ultra-high molecular weight polyethylene sample of PVA/HA composite aquogel bionic joint cartilages is placed in 60 DEG C of grafting solution
In, stirring, react 2h；Then PVA/HA-PAA mixed solutions are added to the loose structure super high molecular weight after step 5 is handled
Polyethylene sample surface, it is 0.5mm to make its thickness, is placed in the low temperature storage box that temperature is -20 DEG C and freezes 10-12 hours, so
Afterwards defrosting 2-3 hours at room temperature, place into low temperature storage box and freezed afterwards, so freezing, thaw 3 times；
7) sample after freeze-thaw is immersed in the beaker for filling polyglycol solution, 1-2h is dehydrated, in dehydration
In sample is weighed at regular intervals, when the weight of sample no longer changes, take out sample and be put into resistance furnace
Row annealing, annealing temperature are 120 DEG C, annealing time 1h, and sample is taken out after the completion of annealing, and with deionized water to sample
Cleaned, remove remnants polyglycol solution；Sample after cleaning is put into deionized water carry out it is rehydrated, it is rehydrated
After the completion of, the surface of loose structure ultra-high molecular weight polyethylene sample forms the bionical pass of second layer PVA/HA-PAA composite aquogels
Save cartilage；
8) polyvinyl alcohol 15% is weighed by mass percentage and deionized water 85% is placed in container, is swelled at room temperature
24h, container is then prepared into PVA solution as in 95 DEG C of thermostat water bath；Loose structure after step 7 is handled surpasses
High molecular weight polyethylene sample is placed in 60 DEG C of grafting solution, stirring, reacts 2h；It is PVA by the mass percent prepared
Solution is added to the loose structure ultra-high molecular weight polyethylene specimen surface after step 7 processing so that the thickness of PVA solution is
0.5mm, it is that 10-12 hours are freezed in -20 DEG C of low temperature storage box to be subsequently placed in temperature, then defrosting 2-3 hours at room temperature,
Place into low temperature storage box and freezed afterwards, so freezing, thaw 9 times after, loose structure ultra-high molecular weight polyethylene examination
The surface of sample forms third layer PVA hydrogel bionic joint cartilages；
9) the loose structure ultra-high molecular weight polyethylene sample with three layers of bionic joint cartilage prepared is put into Sheng
Have in the hermetic bag of deionized water and preserve.
Claims (1)
1. a kind of preparation technology of the multi-gradient bionic joint cartilage based on 3D printing, it is characterized in that：
Preparing the multi-gradient bionic joint cartilage material requested based on 3D printing has：
Available for the modified ultra-high molecular weight polyethylene material of 3D printing, specific composition includes：Ultra-high molecular weight polyethylene
60.8%th, low density polyethylene (LDPE) 23.7%, CNT 8.8%, talcum powder 3.4%, poly-（Methyl）Acrylate 2.7%, antioxidant
CA0.3%, titanate esters 0.3%；
Dichromic acid aoxidizes solution, and specific composition includes：Potassium bichromate 20%, the concentrated sulfuric acid 80%；
Graft esterification solution, specific composition include：Polyvinyl alcohol 7%, the concentrated sulfuric acid 1.5%, deionized water 91.5%；
Bionic joint cartilage material, the material are divided into three kinds, and specific composition is respectively：
（1）Polyvinyl alcohol 15%, nanometer hydroxyapatite 3%, deionized water 82%；
（2）Polyvinyl alcohol 14%, nanometer hydroxyapatite 3%, polyacrylic acid 3%, deionized water 80%；
（3）Polyvinyl alcohol 15%, deionized water 85%；
The specific composition of polyglycol solution is polyethylene glycol 100%；
Described polyvinyl alcohol purity >=99%；Potassium bichromate is the pure level of analysis；The concentrated sulfuric acid is 98% grade of mass fraction；Described thing
The percentage of matter is mass percent；
Multi-gradient bionic joint cartilage material preparation process based on 3D printing comprises the following steps：
1）The ultra-high molecular weight polyethylene model with loose structure is created using Three-dimensional Design Software, exports STL formatted files,
Special 3D printing software is imported, utilizes fused glass pellet（FDM）Or selective laser sintering（SLS）Technology printing preparation has
The ultra-high molecular weight polyethylene block of loose structure；
2）Ultra-high molecular weight polyethylene block with loose structure is immersed in dichromic acid oxidation solution, is placed in 75 DEG C of water-baths
10min in pot, is then placed on 10min in 50 DEG C of salpeter solutions, except the small-molecule substance that surface is formed after deoxidation, takes out
Cleaned with a large amount of deionized waters；Described dichromic acid oxidation solution is by potassium bichromate and the concentrated sulfuric acid by mass percentage 1:
4 configurations form；
3）Polyvinyl alcohol 15%, nanometer hydroxyapatite 3% and deionized water 82% is weighed by mass percentage to be placed in container,
24h is swelled at room temperature, and container is then prepared into PVA/HA mixed solutions as in 95 DEG C of thermostat water bath；By quality hundred
Divide and be placed in container than weighing polyvinyl alcohol 7%, the concentrated sulfuric acid 1.5% and deionized water 91.5%, it is molten to prepare grafting by above-mentioned steps
Liquid；
4）By aoxidizing the appearance equipped with grafting solution is immersed with the ultra-high molecular weight polyethylene sample with loose structure after cleaning
In device, it is placed in 90 DEG C of thermostat water bath, stirs, reacts 2h；
5）The PVA/HA mixed solutions prepared are added to loose structure ultra-high molecular weight polyethylene specimen surface so that PVA/
The thickness of HA mixed solutions is 1mm, and the loose structure ultra-high molecular weight polyethylene sample after handling as stated above is placed in into room
The lower drying of temperature, after one week, the surface of loose structure ultra-high molecular weight polyethylene sample forms first layer PVA/HA compound water congealings
Glue bionic joint cartilage；
6）The polyvinyl alcohol 14% that weighs by mass percentage, nanometer hydroxyapatite 3%, polyacrylic acid solution 3%, deionized water
80%, it is placed in beaker, is then gently mixed with glass bar and is sealed in a moment with preservative film, allows it to be swelled 2-3h at room temperature；Swelling
After the completion of be put into 95 °C of electronic thermostatic water-baths and dissolve by heating, beaker is taken out from water-bath after solution is completely dissolved,
PVA/HA-PAA mixed solutions are obtained, are placed in ultrasonic 2-3h in ultrasonic wave, and answered what step 5 obtained with first layer PVA/HA
The loose structure ultra-high molecular weight polyethylene sample of Heshui gel bionic articular cartilage is placed in 60 DEG C of grafting solution, stirring,
React 2h；Then PVA/HA-PAA mixed solutions are added to the examination of the loose structure ultra-high molecular weight polyethylene after step 5 is handled
Sample surface, it is 0.5mm to make its thickness, is placed in the low temperature storage box that temperature is -20 DEG C and freezes 10-12 hours, then in room temperature
Lower defrosting 2-3 hours, place into low temperature storage box and freezed afterwards, so freezing, defrosting 3 times；
7）Sample after freeze-thaw is immersed in the beaker for filling polyglycol solution, be dehydrated 1-2h, it is every in dehydration
Sample is weighed every certain time, when the weight of sample no longer changes, taking-up sample, which is put into resistance furnace, to be moved back
Fire processing, annealing temperature are 120 °C, annealing time 1h, sample are taken out after the completion of annealing, and sample is carried out with deionized water
Cleaning, remove remnants polyglycol solution；Sample after cleaning is put into deionized water and carries out rehydrated, rehydrated completion
Afterwards, it is soft to form second layer PVA/HA-PAA composite aquogel bionic joints for the surface of loose structure ultra-high molecular weight polyethylene sample
Bone；
8）Polyvinyl alcohol 15% is weighed by mass percentage and deionized water 85% is placed in container, is swelled 24h at room temperature, then
By container as in 95 DEG C of thermostat water bath, PVA solution is prepared；Loose structure super high molecular weight after step 7 is handled
Polyethylene sample is placed in 60 DEG C of grafting solution, stirring, reacts 2h；The mass percent prepared is added for PVA solution
Loose structure ultra-high molecular weight polyethylene specimen surface to after step 7 processing so that the thickness of PVA solution is 0.5mm, then
It is that 10-12 hours are freezed in -20 DEG C of low temperature storage box to be placed in temperature, then defrosting 2-3 hours at room temperature, is placed into afterwards
Freezed in low temperature storage box, so freezing, thaw 9 times after, the surface shape of loose structure ultra-high molecular weight polyethylene sample
Into third layer PVA hydrogel bionic joint cartilages；
9）The loose structure ultra-high molecular weight polyethylene sample with three layers of bionic joint cartilage prepared is put into and filled
Preserved in the hermetic bag of ionized water.
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| CN106039418B (en) * | 2016-07-22 | 2019-01-22 | 胡懿郃 | A kind of preparation method of PLGA-HA-PVA bracket modification HA-PVA artificial cartilage material |
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| CN107115569B (en) * | 2017-05-03 | 2019-05-07 | 中国矿业大学 | Soft-soft contact bionic joint preparation process |
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