CN108042854A - For the production technology of the gelatin fiber guide tissue regeneration film of Dental implant surgery - Google Patents
For the production technology of the gelatin fiber guide tissue regeneration film of Dental implant surgery Download PDFInfo
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- CN108042854A CN108042854A CN201711360418.3A CN201711360418A CN108042854A CN 108042854 A CN108042854 A CN 108042854A CN 201711360418 A CN201711360418 A CN 201711360418A CN 108042854 A CN108042854 A CN 108042854A
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- gelatin
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- dental implant
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- 108010010803 Gelatin Proteins 0.000 title claims abstract description 47
- 229920000159 gelatin Polymers 0.000 title claims abstract description 47
- 239000008273 gelatin Substances 0.000 title claims abstract description 47
- 235000019322 gelatine Nutrition 0.000 title claims abstract description 47
- 235000011852 gelatine desserts Nutrition 0.000 title claims abstract description 47
- 239000000835 fiber Substances 0.000 title claims abstract description 43
- 238000005516 engineering process Methods 0.000 title claims abstract description 21
- 230000017423 tissue regeneration Effects 0.000 title claims abstract description 19
- 239000004053 dental implant Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000001356 surgical procedure Methods 0.000 title claims abstract description 18
- 238000010146 3D printing Methods 0.000 claims abstract description 29
- 102000008186 Collagen Human genes 0.000 claims abstract description 29
- 108010035532 Collagen Proteins 0.000 claims abstract description 29
- 229920001436 collagen Polymers 0.000 claims abstract description 29
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000001954 sterilising effect Effects 0.000 claims abstract description 6
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 45
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 17
- 238000003860 storage Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 150000002148 esters Chemical class 0.000 claims description 10
- 230000002045 lasting effect Effects 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000007639 printing Methods 0.000 claims description 9
- 150000007524 organic acids Chemical class 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 5
- 238000009825 accumulation Methods 0.000 claims description 5
- 238000004132 cross linking Methods 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 5
- 238000003958 fumigation Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000011112 process operation Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 150000002894 organic compounds Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- ZNZYKNKBJPZETN-WELNAUFTSA-N Dialdehyde 11678 Chemical class N1C2=CC=CC=C2C2=C1[C@H](C[C@H](/C(=C/O)C(=O)OC)[C@@H](C=C)C=O)NCC2 ZNZYKNKBJPZETN-WELNAUFTSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920001744 Polyaldehyde Chemical class 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 229930003944 flavone Chemical class 0.000 claims description 2
- 150000002213 flavones Chemical class 0.000 claims description 2
- 235000011949 flavones Nutrition 0.000 claims description 2
- 229930003935 flavonoid Chemical class 0.000 claims description 2
- 150000002215 flavonoids Chemical class 0.000 claims description 2
- 235000017173 flavonoids Nutrition 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 claims description 2
- 150000002924 oxiranes Chemical class 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 150000005846 sugar alcohols Chemical class 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 15
- 239000004615 ingredient Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000005520 cutting process Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 210000004027 cell Anatomy 0.000 description 10
- 210000001519 tissue Anatomy 0.000 description 7
- 241001465754 Metazoa Species 0.000 description 6
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical group O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 210000004379 membrane Anatomy 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 210000000988 bone and bone Anatomy 0.000 description 3
- 229940015043 glyoxal Drugs 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 210000000056 organ Anatomy 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 102000010834 Extracellular Matrix Proteins Human genes 0.000 description 2
- 108010037362 Extracellular Matrix Proteins Proteins 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 210000002744 extracellular matrix Anatomy 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 210000003491 skin Anatomy 0.000 description 2
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 102000016942 Elastin Human genes 0.000 description 1
- 108010014258 Elastin Proteins 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 210000001691 amnion Anatomy 0.000 description 1
- 210000001557 animal structure Anatomy 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 235000014103 egg white Nutrition 0.000 description 1
- 210000000969 egg white Anatomy 0.000 description 1
- 229920002549 elastin Polymers 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000003195 fascia Anatomy 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 210000004086 maxillary sinus Anatomy 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/04—Macromolecular materials
- A61L31/043—Proteins; Polypeptides; Degradation products thereof
- A61L31/045—Gelatin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/04—Macromolecular materials
- A61L31/043—Proteins; Polypeptides; Degradation products thereof
- A61L31/044—Collagen
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
Landscapes
- Health & Medical Sciences (AREA)
- Heart & Thoracic Surgery (AREA)
- Surgery (AREA)
- Vascular Medicine (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Materials For Medical Uses (AREA)
- Prostheses (AREA)
Abstract
The present invention relates to the production technologies of the gelatin fiber guide tissue regeneration film for Dental implant surgery, comprise the following steps：It prepares and main component step is added in base soln step, base soln, crosslinking agent step, 3D printing step, drying steps, cutting, packaging, sterilization steps are added in into gelatin/collagen solution.Compared with prior art, the invention has the advantages that：The gelatin fiber guide tissue regeneration film to be formed is prepared using production technology disclosed by the invention, height is understood on ingredient, is conducive to precisely be selected in clinical practice；Microstructure is less than 2 μm of fibre structure, beneficial to cell adherence；It has passed through full cross-linked inside fibre structure, between fiber, good mechanical property and clinical manipulation can be kept to experience under the thickness of 0.1mm；Gap is less than cell dia between fiber, and cell can be guided to be adhered to first in material surface and grown, and gradually gos deep into the degradation of material.
Description
Technical field
The present invention relates to a kind of production technologies of the gelatin fiber guide tissue regeneration film for Dental implant surgery, belong to group
Weaver's journey and regenerative medicine field, applied to (tooth) plantation section surgical operation, the guiding bone being particularly used in the operation of bone increment
Regenerate art, maxillary sinus defect repair etc..
Background technology
In organizational project and regenerative medicine field, being applied to material that is clinical and meeting same requirements at present mainly includes two
Class --- animal derived acellular matrix material and using large biological molecule again moulding diaphragm or spongy material, and can
Certain crosslinking agent, antimicrobial component etc. can be added on demand.
Animal derived acellular matrix material is with the membrane-like tissue of animal, organ (such as skin, fascia, amnion
Deng) by a series of physics, chemistry or enzymatic treatment, removal can cause the ingredients such as the cell of immunological rejection, be retained in
Highly conserved extracellular matrix supporting structure, main component typically contain collagen, elastin laminin etc. between species.De- cell
The main problem of host material is mass uniformity Shortcomings.Since de- cell technology core is to retain cell as far as possible
The natural structure of epimatrix, therefore the form of final products, structure, dependent on animal tissue or the spontaneous growth state of organ.Together
When, between different animals individual and the different position of the same tissue/organ of same animal individual, there are one for extracellular matrix
Fixed architectural difference causes the mass uniformity of acellular matrix material there are larger fluctuation range, and is difficult to pass through pumping
The pattern of inspection fully reflects the quality of all products；In addition, the ingredient of acellular matrix material is not accomplished to understand completely, it is actual
Certain proportion infection problems as caused by unknown cause occurred in clinical practice.It is contemplated that with medical advance and to controlling
The continuous improvement of accuracy requirement is treated, acellular matrix class material is increasingly difficult to meet the needs of precisely treating.
Using large biological molecule again moulding diaphragm or spongy material, the large biological molecule is generally collagen egg
White or gelatin is by the way that animal organ's (be often skin, bone, tendon etc.) is obtained by purifying.The large biological molecule of acquisition
General elder generation's wiring solution-forming, then by way of lyophilized it is again moulding, may add in the solution on demand crosslinking agent or it is antibacterial into
Point, to realize the optimization of material mechanical performance or bacteriostasis property etc..The main shaping method of such material is lyophilized, product
Final form largely influenced by refrigerating process.Due to refrigerated container, to be difficult to temperature height homogeneous, even if actual
With there is also differences between batch product.The spongelike structure of acquisition based on lamellar structure, is beneficial to cell on microcosmic containing part
Fibre structure below 2 μm of the diameter of adherency, therefore the cell culture experiments that such material carries out can substantially reflect that guiding cell glues
It grows nonparasitically upon another plant long scarce capacity；In addition, the material that such technology obtains is generally thicker, it is thicker in Dental implantion and related surgical
Material occupies larger space, influences the closing of surface of a wound no-station pole canopy, increases operative failure risk.If in such technical foundation obtain compared with
Thin material is difficult to form effective connection between lamella or fiber, can cause declining to a great extent for mechanical strength, can not be applied to hand
Art operates.Therefore, it should a kind of new technical solution be provided and solved the problems, such as present on.
The content of the invention
The purpose of the present invention is：For shortcoming in the prior art, one kind height on ingredient is provided and understands, be beneficial to
The production technology of the gelatin fiber guide tissue regeneration film for Dental implant surgery of cell adherence.
To achieve the above object, the technical solution adopted by the present invention is：
For the production technology of the gelatin fiber guide tissue regeneration film of Dental implant surgery, comprise the steps of：
(1) base soln step is prepared
Under 10-35 DEG C of temperature conditionss, the water, organic acid and small molecular ester of certain volume part are put into instead simultaneously
It answers in container, stirs and evenly mixs, the organic acid is volatile organic acid, and esters are the acid no more than six carbon with being no more than six carbon
Alcohol is condensed the esters to be formed, three mix postposition magnetic stirring apparatus persistently stir 0.5-50 it is small when base soln is made, stirring can
It is carried out within the temperature range of 4-35 DEG C, when stirring minimum no less than 0.5 is small, before adding in main component to next step after mixing,
The room temperature storage time is no more than 15 days, and 4-8 DEG C of storage is no more than 30 days；
(2) main component step is added in base soln
Gelatin or collagen are added in step (1) prepares the base soln formed, gelatin/collagen solution is made, it is bright
The mass concentration of glue/collagen solution is 10-22%, is stirred and evenly mixed after addition in the range of 10-30 DEG C, it is small that room temperature need to stir 1-30
When, it can store in the range of 0-30 DEG C after mixing, be raised with temperature, storable number of days is reduced, and storage at room temperature is no more than 10
My god；
(3) crosslinking agent step is added in into gelatin/collagen solution
Crosslinking agent is added in the gelatin/collagen solution prepared to step (2), the crosslinking agent is to contain 2 or more energy
The organic compound to react with the amino in gelatin/collagen or carboxyl, the mass concentration of the crosslinking agent is 0.05%-
5%, it adds in after crosslinking agent and reacts lasting in solution and occur, 4-30 DEG C of solution temperature need to be kept, and started after 1min-8h is stored
For 3D printing, and 3D printing process operation is completed in 2-30h, the beginning and ending time of 3D printing is adjusted according to solution temperature；
(4) 3D printing step
Solution will be obtained in above-mentioned steps (3), by task equipment progress 3D printing, water when basis matches somebody with somebody liquid in print procedure
Divide content different, stringent to control print area humiture, temperature is 10-35 DEG C, relative humidity 15-85%, and persistently to printing
Nozzle injecting protective gas avoids solution from curing accumulation at nozzle, controls electric field strength as cathode voltage 15-35kV, cathode
Voltage -0.01-7kV, printing distance are 3-25cm, with the diaphragm fibre diameter of acquisition uniformly or by the lasting variation of design；
(5) drying steps
The diaphragm obtained in step (4) is placed in baking oven and is further dried, strengthens cross-linking reaction, until obtaining heavily fortified point
Tough slim diaphragm structure, and the fiber that microstructure is less than 2 μm；
(6) cut, pack, sterilization steps
The diaphragm obtained in step (5) is cut into required shape and specification, is packed by medical instrument usual manner, and
It is sterilized by the way of irradiation or epoxyethane fumigation, obtains the 3D printing gelatin fiber guiding tissue available for Dental implant surgery
Regeneration membrane.
Further technical solution：
Esters described in step (1) are ethyl acetate or butyl acetate.
Organic acid described in step (1) is acetic acid, and the esters are ethyl acetate, and the adding proportion of the acetic acid and water is
9:1-5:4, the adding proportion of acetic acid and ethyl acetate is 9:2-5:7.
Organic compound described in step (3) is dialdehyde, polyaldehyde, polyalcohol, epoxides, flavones and flavonoid class
Substance.
Due to the application of above-mentioned technical proposal, the present invention has the following advantages that compared with prior art：
1st, the gelatin fiber guide tissue regeneration film to be formed is prepared using production technology disclosed by the invention, first in ingredient
Upper height is understood, is conducive to precisely be selected in clinical practice.
2nd, the gelatin fiber guide tissue regeneration film to be formed is prepared using production technology disclosed by the invention, microstructure is equal
For the fibre structure below 2 μm, beneficial to cell adherence.
3rd, the gelatin fiber guide tissue regeneration film to be formed is prepared using production technology disclosed by the invention, in fibre structure
It has passed through full cross-linked between portion, fiber, good mechanical property and clinical manipulation body can be kept under the thickness of 0.1mm
It tests.
4th, the gelatin fiber guide tissue regeneration film to be formed is prepared using production technology disclosed by the invention, gap between fiber
Less than cell dia, cell can be guided to be adhered to first in material surface and grown, and gradually goed deep into the degradation of material.
Specific embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not limited to
Following embodiments.
Embodiment one
For the production technology of the gelatin fiber guide tissue regeneration film of Dental implant surgery, comprise the steps of：
(1) base soln step is prepared
Under 10 DEG C of temperature conditionss, water, acetic acid, ethyl acetate three are put into reaction vessel simultaneously, wherein, acetic acid
Dispensing ratio with water is 9:1, the dispensing ratio of acetic acid and ethyl acetate is 9:2, it is uniformly mixed juxtaposition magnetic stirring apparatus and continues
Stir 50 it is small when be made base soln, before adding in main component to next step after mixing, the room temperature storage time is no more than 15 days, 4-
8 DEG C of storages are no more than 30 days；
(2) main component step is added in base soln
Gelatin or collagen are added in step (1) prepares the base soln formed, gelatin/collagen solution is made, it is bright
The mass concentration of glue/collagen solution be 10%, stirred and evenly mixed after addition in the range of 10-30 DEG C, room temperature need to stir 1-30 it is small when,
It can store in the range of 0-30 DEG C after mixing, be raised with temperature, storable number of days is reduced, and storage at room temperature is no more than 10 days；
(3) crosslinking agent step is added in into gelatin/collagen solution
Crosslinking agent is added in the gelatin/collagen solution prepared to step (2), and the crosslinking agent is glyoxal, additional proportion
For 50 μ l/100ml, add in and react lasting in solution after crosslinking agent and occur, 4 DEG C of solution temperature need to be kept, started after the completion of preparing
For 3D printing, and ensure most long to complete 3D printing process operation in 30h.
(4) 3D printing step
Solution will be obtained in above-mentioned steps (3), by task equipment progress 3D printing, water when basis matches somebody with somebody liquid in print procedure
Divide content different, stringent to control print area humiture, temperature is 10 DEG C, relative humidity 15%, and persistently to printing head spray
Protective gas is penetrated, solution is avoided to cure accumulation at nozzle, controls electric field strength as cathode voltage 15kV, cathode voltage-
0.01kV, printing distance are 3cm, with the diaphragm fibre diameter of acquisition uniformly or by the lasting variation of design；
(5) drying steps
The diaphragm obtained in step (4) is placed in baking oven and is further dried, strengthens cross-linking reaction, until obtaining heavily fortified point
Tough slim diaphragm structure, and the fiber that microstructure is less than 2 μm；
(6) cut, pack, sterilization steps
The diaphragm obtained in step (5) is cut into required shape and specification, is packed by medical instrument usual manner, and
It is sterilized by the way of irradiation or epoxyethane fumigation, obtains the 3D printing gelatin fiber guiding tissue available for Dental implant surgery
Regeneration membrane.
Embodiment two
For the production technology of the gelatin fiber guide tissue regeneration film of Dental implant surgery, comprise the steps of：
(1) base soln step is prepared
Under 22 DEG C of temperature conditionss, water, acetic acid, ethyl acetate three are put into reaction vessel simultaneously, wherein, acetic acid
Dispensing ratio with water is 7:3, the dispensing ratio of acetic acid and ethyl acetate is 7:4, it is uniformly mixed juxtaposition magnetic stirring apparatus and continues
Stirring put magnetic stirring apparatus persistently stir 25 it is small when be made base soln, before adding in main component to next step after mixing, room temperature
Storage time is no more than 15 days, and 4-8 DEG C of storage is no more than 30 days；
(2) main component step is added in base soln
Gelatin or collagen are added in step (1) prepares the base soln formed, gelatin/collagen solution is made, it is bright
The mass concentration of glue/collagen solution be 16%, stirred and evenly mixed after addition in the range of 10-30 DEG C, room temperature need to stir 1-30 it is small when,
It can store in the range of 0-30 DEG C after mixing, be raised with temperature, storable number of days is reduced, and storage at room temperature is no more than 10 days；
(3) crosslinking agent step is added in into gelatin/collagen solution
Crosslinking agent is added in the gelatin/collagen solution prepared to step (2), and the crosslinking agent is glyoxal, additional proportion
For 1000 μ l/100ml, add in and react lasting in solution after crosslinking agent and occur, 15 DEG C of solution temperature need to be kept, and after 4h is stored
Start for 3D printing, control the completion 3D printing process operation in 16h.
(4) 3D printing step
Solution will be obtained in above-mentioned steps (3), by task equipment progress 3D printing, water when basis matches somebody with somebody liquid in print procedure
Divide content different, stringent to control print area humiture, temperature is 18 DEG C, relative humidity 50%, and persistently to printing head spray
Protective gas is penetrated, solution is avoided to cure accumulation at nozzle, controls electric field strength as cathode voltage 25kV, cathode voltage 3.5kV,
Printing distance is 14cm, with the diaphragm fibre diameter of acquisition uniformly or by the lasting variation of design；
(5) drying steps
The diaphragm obtained in step (4) is placed in baking oven and is further dried, strengthens cross-linking reaction, until obtaining heavily fortified point
Tough slim diaphragm structure, and the fiber that microstructure is less than 2 μm；
(6) cut, pack, sterilization steps
The diaphragm obtained in step (5) is cut into required shape and specification, is packed by medical instrument usual manner, and
It is sterilized by the way of irradiation or epoxyethane fumigation, obtains the 3D printing gelatin fiber guiding tissue available for Dental implant surgery
Regeneration membrane.
Embodiment three
For the production technology of the gelatin fiber guide tissue regeneration film of Dental implant surgery, comprise the steps of：
(1) base soln step is prepared
Under 35 DEG C of temperature conditionss, water, acetic acid, ethyl acetate three are put into reaction vessel simultaneously, wherein, acetic acid
Dispensing ratio with water is 5:4, the dispensing ratio of acetic acid and ethyl acetate is 5:7, it is uniformly mixed juxtaposition magnetic stirring apparatus and continues
Stir 0.5 it is small when be made base soln, before adding in main component to next step after mixing, the room temperature storage time is no more than 15 days,
4-8 DEG C of storage is no more than 30 days；
(2) main component step is added in base soln
Gelatin or collagen are added in step (1) prepares the base soln formed, gelatin/collagen solution is made, it is bright
The mass concentration of glue/collagen solution be 22%, stirred and evenly mixed after addition in the range of 10-30 DEG C, room temperature need to stir 1-30 it is small when,
It can store in the range of 0-30 DEG C after mixing, be raised with temperature, storable number of days is reduced, and storage at room temperature is no more than 10 days；
(3) crosslinking agent step is added in into gelatin/collagen solution
Crosslinking agent is added in the gelatin/collagen solution prepared to step (2), and the crosslinking agent is glyoxal, additional proportion
For 2000 μ l/100ml, add in and react lasting in solution after crosslinking agent and occur, 30 DEG C of solution temperature need to be kept, and after 8h is stored
Start for 3D printing, and 3D printing process operation is completed in 2h, the beginning and ending time of 3D printing is adjusted according to solution temperature；
(4) 3D printing step
Solution will be obtained in above-mentioned steps (3), by task equipment progress 3D printing, water when basis matches somebody with somebody liquid in print procedure
Divide content different, stringent to control print area humiture, temperature is 35 DEG C, relative humidity 85%, and persistently to printing head spray
Protective gas is penetrated, solution is avoided to cure accumulation at nozzle, controlling electric field strength, cathode voltage 7kV is beaten for cathode voltage 35kV
Print distance is 25cm, with the diaphragm fibre diameter of acquisition uniformly or by the lasting variation of design；
(5) drying steps
The diaphragm obtained in step (4) is placed in baking oven and is further dried, strengthens cross-linking reaction, until obtaining heavily fortified point
Tough slim diaphragm structure, and the fiber that microstructure is less than 2 μm；
(6) cut, pack, sterilization steps
The diaphragm obtained in step (5) is cut into required shape and specification, is packed by medical instrument usual manner, and
It is sterilized by the way of irradiation or epoxyethane fumigation, obtains the 3D printing gelatin fiber guiding tissue available for Dental implant surgery
Regeneration membrane.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvement or replacement can also be made, these improve or replace
It should be regarded as protection scope of the present invention.
Claims (4)
1. the production technology of the gelatin fiber guide tissue regeneration film for Dental implant surgery, which is characterized in that include following step
Suddenly：
(1) base soln step is prepared
Under 10-35 DEG C of temperature conditionss, the water, organic acid and small molecular ester of certain volume part are put into reaction simultaneously and held
It in device, stirs and evenly mixs, the organic acid is volatile organic acid, and esters are that the acid no more than six carbon contracts with the alcohol no more than six carbon
Close formed esters, three mix postposition magnetic stirring apparatus persistently stir 0.5-50 it is small when base soln is made, stirring can be in 4-
It is carried out within the temperature range of 35 DEG C, when stirring minimum no less than 0.5 is small, before adding in main component to next step after mixing, room temperature
Storage time is no more than 15 days, and 4-8 DEG C of storage is no more than 30 days；
(2) main component step is added in base soln
Gelatin or collagen are added in step (1) prepares the base soln formed, gelatin/collagen solution, gelatin/glue is made
The mass concentration of original solution be 10-22%, stirred and evenly mixed after addition in the range of 10-30 DEG C, room temperature need to stir 1-30 it is small when, mix
It can store in the range of 0-30 DEG C after even, be raised with temperature, storable number of days is reduced, and storage at room temperature is no more than 10 days；
(3) crosslinking agent step is added in into gelatin/collagen solution
Add in crosslinking agent in the gelatin/collagen solution prepared to step (2), the crosslinking agent be containing 2 or more can with it is bright
The organic compound that amino or carboxyl in glue/collagen react, the mass concentration of the crosslinking agent is 0.05%-5%, is added
Enter to react lasting after crosslinking agent in solution and occur, 4-30 DEG C of solution temperature need to be kept, and start after 1min-8h store to be used for 3D
Printing, and 3D printing process operation is completed in 2-30h, the beginning and ending time of 3D printing is adjusted according to solution temperature；
(4) 3D printing step
Solution will be obtained in above-mentioned steps (3), 3D printing is carried out by task equipment, is contained in print procedure according to moisture when matching somebody with somebody liquid
Amount is different, stringent to control print area humiture, and temperature is 10-35 DEG C, relative humidity 15-85%, and persistently to printing head
Injecting protective gas avoids solution from curing accumulation at nozzle, controls electric field strength as cathode voltage 15-35kV, and cathode voltage-
0.01-7kV, printing distance are 3-25cm, with the diaphragm fibre diameter of acquisition uniformly or by the lasting variation of design；
(5) drying steps
The diaphragm obtained in step (4) is placed in baking oven and is further dried, strengthens cross-linking reaction, until obtaining tough and tensile
Slim diaphragm structure, and the fiber that microstructure is less than 2 μm；
(6) cut, pack, sterilization steps
The diaphragm obtained in step (5) is cut into required shape and specification, packs, and uses by medical instrument usual manner
The mode of irradiation or epoxyethane fumigation sterilizes, and obtains the 3D printing gelatin fiber guide tissue regeneration available for Dental implant surgery
Film.
2. the production technology of the gelatin fiber guide tissue regeneration film according to claim 1 for Dental implant surgery,
It is characterized in that：Esters described in step (1) are ethyl acetate or butyl acetate.
3. the production technology of the gelatin fiber guide tissue regeneration film according to claim 1 for Dental implant surgery,
It is characterized in that：The organic acid is acetic acid, and the esters are ethyl acetate, and the adding proportion of the acetic acid and water is 9:1-5:4,
The adding proportion of acetic acid and ethyl acetate is 9:2-5:7.
4. the production technology of the gelatin fiber guide tissue regeneration film according to claim 1 for Dental implant surgery,
It is characterized in that：Organic compound is dialdehyde, polyaldehyde, polyalcohol, epoxides, flavones and flavonoid class object in step (3)
Matter.
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