CN104524640A - Porous polyurethane film used for artificial skin and having gradient porous structure and preparation method of porous polyurethane - Google Patents
Porous polyurethane film used for artificial skin and having gradient porous structure and preparation method of porous polyurethane Download PDFInfo
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Abstract
The invention discloses a preparation method of a porous polyurethane film with a gradient porous structure. The preparation method is characterized by comprising the following steps: adding polyurethane into a solvent for dissolving, adding a pore-foaming agent, and mechanically stirring for a period of time to obtain suspension; defoaming the suspension in vacuum, carrying out film casting on a mold, carrying out curing film formation in absolute ethyl alcohol coagulation bath, soaking the film in deionized water to dissolve the pore-foaming agent and completely remove the pore-foaming agent; taking out the film, drying the film in a blast oven to obtain the porous polyurethane film with the gradient porous structure, the upper and lower surfaces of the porous polyurethane film are trim and not curled, and the hand feeling is good. The film can be used as artificial skin and has the advantages of good water and air permeability, high water absorption, excellent mechanical properties, good biological affinity, etc.
Description
Technical field,
The present invention relates to a kind of graded pore structure porous polyurethane film for artificial skin and preparation method thereof, belong to biological engineering material technical field.
Background technology
Skin is the maximum organ of human body, is the natural cover for defense of protection human body.Perception, thermoregulation, secretion, excretion, absorption are played a part to human body, especially the first line of defence of human immune system.When skin is subject to serious wound or burn, may cause Water-Electrolyte unbalance, suffer a shock, infect a series of serious problems, be now badly in need of autologous skin and come wound coverage face.But autologous skin source is limited, therefore have certain mechanical strength, toughness, waterproof and breathable by one, the artificial skin close to people's real skin temporarily substitutes corium and seems particularly important, can reduce the misery of patient to a certain extent, saves the life of patient.
Medical polyurethane has excellent mechanical property, has excellent water-resistance, meanwhile, its have good biocompatibility, anticoagulant property, nontoxic, without teratogenesis.Polyurethane is easily processed on the other hand, has larger MOLECULE DESIGN degree of freedom.At present it is widely used in the preparation of artificial blood vessel, artificial cartilage, artificial heart blood pump, operation suture thread and medical dressing medical article.
Artificial skin is the focus of many countries research in recent years.First commercial artificial skin is Integra in the world, is the dermal substitute of heterologous source, is developed, have double-decker by people such as Burke and Yannas.Lower floor is cross-linked to form the support with certain hole by the Ι collagen type (tendon) and aminopolysaccharide (chondroitin sulfate) extracting cattle, aperture is between 30 ~ 120 μm, porosity can reach 98%, the generation of Various Tissues cell, macrophage, lymph corpuscle and blood tubule can be allowed, with human body without immunological rejection, do not degrade; Upper strata is nontoxic silicon rubber film, can resist the intrusion of extraneous antibacterial, controls the evaporation of wound moisture.But this artificial skin also exists some shortcomings on Clinical practice: can not life-time service, require higher to wound surface, needing secondary to make skin graft could flap coverage.In addition, its mechanical strength is poor.Upper layer of silicon rubber is fine and close, poor air permeability.And expensive, cost is higher.
Biobrane is a kind of double-layered artificial skin, and upper strata is silica gel thin film, and lower floor is nylon fiber net, fills the collagen protein of extraction from Corii Sus domestica in mesh.It has good flexibility, avirulence and aseptic.But it can not be used for deep third degree burn, can not forever use; Its mechanical strength is low simultaneously, and upper layer film is comparatively fine and close, poor air permeability.The people such as US Patent No. 2009/0232878, Woodroof describe a kind of double-layered artificial skin being similar to Biobrane.Lower floor has the knitting nylon net being uniformly distributed cavity; Upper strata is the silicon rubber film that one deck is very thin, and aperture is at 0.75 ~ 1.05mm.Protect preferably although it can give wound, it is not still suitable for deep third degree burn, and upper layer of silicon rubber aperture is excessive simultaneously, is difficult to resist extraneous bacterial invasion, does not also reach the effect of waterproof.
Summary of the invention
A kind of graded pore structure porous polyurethane film for artificial skin provided for the deficiencies in the prior art and preparation method thereof is provided.Be characterized in combining the immersion precipitation in phase separation method and porogen filter drop method, polyurethane is dissolved and adds porogen afterwards in a solvent, form suspension, casting film-forming on mould, solidifies in phase separation in dehydrated alcohol, forms aperture, elimination porogen in deionized water, form macropore, substep pore-forming, finally dries the porous polyurethane film obtaining graded pore structure.The method obtains the Polyurethane Porous Membranes of graded pore structure, and aperture has and increases gradually from top to bottom.
Object of the present invention is realized by following technical measures, and wherein said raw material number, except specified otherwise, is mass concentration.
Graded pore structure porous polyurethane film and preparation method thereof for artificial skin comprises the following steps:
1) add in the middle of solvent by polyurethane, carry out stirring and dissolving completely temperature 20 ~ 70 DEG C, obtain the polyurethane solutions that concentration is 50 ~ 200g/L, then adding particle diameter is 20 ~ 250 μm, and concentration is the porogen of 50 ~ 750g/L, obtains suspension after stirring;
2) by above-mentioned suspension deaeration 10 ~ 60min under room temperature, vacuum 0.06 ~ 0.08MPa;
3) pour in mould by the suspension after above-mentioned deaeration, curtain coating becomes thin film, and coating thickness is 0.5 ~ 4mm;
4) above-mentioned thin film is put into the dehydrated alcohol that temperature is 20 ~ 50 DEG C, carry out the exchange that is separated, make its film-forming;
5) thin film of above-mentioned solidification is put into the deionized water that temperature is 5 ~ 95 DEG C, elimination porogen;
6) above-mentioned thin film is carried out drying, obtain the porous polyurethane film of graded pore structure, polyurethane cellular membrane aperture increases from top to bottom gradually.
Described solvent is any one in DMF, dioxane or oxolane.
Described mould is any one in glass, politef, polyester, polyethylene, polypropylene, polrvinyl chloride, polyvinyl alcohol, polyacrylonitrile or polysulfones.
Described porogen is any one in sodium chloride, potassium chloride, sodium citrate, potassium citrate, sodium bicarbonate or potassium bicarbonate.
The preparation method of the porous polyurethane film of graded pore structure prepares the porous polyurethane film of graded pore structure.
The porous polyurethane film of graded pore structure is used for the treatment of the artificial skin of people and other mammiferous skin injury.
Structural characterization and performance test:
1) pore structure of the upper surface of the porous polyurethane film of sem observation graded pore structure, lower surface, section is utilized.
Formula 25g polyurethane, 200mL N is pressed by embodiment 1, the sample of dinethylformamide and 80g sodium citrate and embodiment 2 preparation is through its each several part pattern of sem observation, concrete steps are as follows: clip one section of 1cm is long, the wide sample of 0.5cm, put into liquid nitrogen and carry out brittle failure and obtain section.The sample of clip 0.5cm × 0.5cm, for the observation of upper and lower surface.Sem observation can be carried out, the results detailed in shown in Fig. 1 to Fig. 6 after carrying out metal spraying process to wanting sightingpiston.
2) pore size of Image-Pro computed in software graded pore structure porous polyurethane film upper surface, lower surface, section is adopted.
Result shows, and the graded pore structure porous polyurethane film upper surface that embodiment 1 obtains has more aperture, and mean pore size is 1.69 μm; The macropore mean pore size of lower surface is 87.5 μm; There is macropore and small structure in section, macropore average pore size is 143.5 μm simultaneously, and aperture average pore size is 21.6 μm.
3) stretching mechanical experiment is carried out to graded pore structure porous polyurethane film, measured tensile break strength and elongation at break.
With cut-off knife, sample prepared by embodiment 1 is cut into tensile bars, the long 30mm of sample tensile test part, wide 3.7mm.Test its tensile break strength and elongation at break with universal testing machine, result is as shown in table 1.
Result shows: the graded pore structure porous polyurethane film prepared by this invention has excellent mechanical property, and tensile break strength can reach 2.17MPa, and elongation at break can reach 424%.This mechanical property can meet the user demand of artificial skin.
4) the water vapo(u)r transmission energy of graded pore structure porous polyurethane film is measured.
Sample prepared by embodiment 1 and embodiment 2 is cut into 33cm
2circular film, be placed in water vapor permeation rate tester and test, often organize test 3 Duplicate Samples, probe temperature is 37.5 DEG C, and testing humidity is 90%R H, and result is as shown in table 2 and table 3.
Result shows: along with the increase of porogen consumption, and the moisture-vapor transmission of sample increases thereupon, can find out that the porous polyurethane film water vapo(u)r transmission energy schedulable of this graded pore structure is larger data; Coating times is from being once increased to three times, and water vapo(u)r transmission can strengthen greatly, and this is mainly because gradation film accelerates phase exchange velocity, and the small aperture of formation is comparatively large, the better reason of the penetrability between Kong Yukong.
5) water absorption rate and the porosity of graded pore structure porous polyurethane film is measured.
Sample prepared by embodiment 1 being cut into the length of side is that its dry weight measured by the square sample of 0.5cm, and in deionized water, 72h waits and measures its weight in wet base, and calculate water absorption and the porosity of sample thus, result is as shown in table 4 in submergence.
Result shows: graded pore structure porous polyurethane film water absorption rate prepared by this invention can reach 467%, and porosity reaches 83%, illustrates that this perforated membrane can effectively absorb skin dialysate, for wound healing ensures a moistening environment.
The present invention has the following advantages:
1) upper surface aperture is little, and aperture is only 1 ~ 2 μm, can effectively resist extraneous antibacterial;
2) section aperture distribution gradient, increased gradually to lower surface (with mould contact surface) aperture by upper surface, thickness can regulate according to specific needs.This structure can effectively absorb damaged skin dialysate, keeps good permeability simultaneously.The graded pore structure porous polyurethane film of monolayer has the dual-use function resisting extraneous antibacterial and absorption dialysate of double-layered artificial skin;
3) section pore structure can be divided into macropore and aperture, and macropore is formed by porogen elimination, and aperture is formed by mechanisms of phase separation, and this structure is conducive to ensure that good water permeability energy, can keep wound moist again simultaneously;
4) have excellent mechanical property, tensile break strength can reach more than 2MPa, and elongation at break reaches more than 400% simultaneously;
5) have smooth outward appearance, comfortable feel, lower surface is large relative to upper surface hole, and thus feel is more soft;
6) preparation technology of the present invention is very simple, and energy consumption is low, and the performance of perforated membrane is easy to control;
7) solvent in preparation process of the present invention, the equal recoverable of coagulating bath solvent, do not produce waste gas and waste liquid, environmentally friendly;
8) the finished product security performance that obtains of the present invention is excellent, does not have toxic and side effects to animal body.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope image of porous polyurethane film section under 100 times of the graded pore structure of embodiment 1
Fig. 2 is the scanning electron microscope image of porous polyurethane film under 100 times of the graded pore structure of embodiment 4
Fig. 3 is the scanning electron microscope image in Fig. 1 Upper rectangular frame under 2000 multiplying powers
Fig. 4 is the scanning electron microscope image in the middle part of Fig. 1 in rectangle frame under 2000 multiplying powers
Fig. 5 is the scanning electron microscope image of porous polyurethane film upper surface under 1000 times of the graded pore structure of embodiment 1
Fig. 6 is the scanning electron microscope image of porous polyurethane film lower surface under 1000 times of the graded pore structure of embodiment 1
Detailed description of the invention
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that the present embodiment is only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field content according to the present invention can make some nonessential improvement and adjustment.
Embodiment 1
Four parts of 25g medical grade polyurethane are dissolved at 60 DEG C the N of 200mL respectively, in dinethylformamide, then the sodium citrate that 60g, 80g, 100g, 120g particle diameter is 75 ~ 150 μm is added respectively, after mechanical agitation 1h, deaeration 20min under room temperature, vacuum are 0.06MPa.Be poured in Teflon mould by the uniform suspension after deaeration, coating thickness is 2mm, and the dehydrated alcohol then putting into 25 DEG C is separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 25 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 2
25g medical grade polyurethane is dissolved in the DMF of 200mL at 60 DEG C, then adds the sodium citrate 80g that particle diameter is 75 ~ 150 μm, after mechanical agitation 1h, deaeration 20min under room temperature, vacuum are 0.06MPa.Divided by suspension after deaeration and be evenly poured in Teflon mould for three times, each coating thickness is 1mm, and the dehydrated alcohol putting into 25 DEG C after film is separated, film-forming.The deionized water that Polyurethane Porous Membranes after third time curing of coating puts into 25 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 3
10g medical grade polyurethane is dissolved in the DMF of 200mL at 20 DEG C, then adds the sodium citrate 10g that particle diameter is 20 ~ 75 μm, after mechanical agitation 1h, deaeration 10min under room temperature, vacuum are 0.06MPa.Be poured in glass mold by the uniform suspension after deaeration, coating thickness is 1mm, and the dehydrated alcohol then putting into 20 DEG C is separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 5 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 4
15g medical grade polyurethane is dissolved in the DMF of 200mL at 20 DEG C, then adds the sodium chloride 30g that particle diameter is 20 ~ 75 μm, after mechanical agitation 1h, deaeration 20min under room temperature, vacuum are 0.06MPa.Be poured over by uniform suspension after deaeration in polyester mould, coating thickness is 1mm, and the dehydrated alcohol then putting into 30 DEG C is separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 25 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 5
20g medical grade polyurethane is dissolved in the dioxane of 200mL at 30 DEG C, then adds the potassium chloride 50g that particle diameter is 20 ~ 75 μm, after mechanical agitation 1h, deaeration 30min under room temperature, vacuum are 0.07MPa.Be poured over by uniform suspension after deaeration in polyethylene tool, coating thickness is 2mm, and the dehydrated alcohol then putting into 35 DEG C is separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 45 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 6
25g medical grade polyurethane is dissolved in the dioxane of 200mL at 40 DEG C, then adds the potassium citrate 70g that particle diameter is 75 ~ 150 μm, after mechanical agitation 1h, deaeration 40min under room temperature, vacuum are 0.07MPa.Be poured in polypropylene molds by the uniform suspension after deaeration, coating thickness is 2mm, and the dehydrated alcohol then putting into 45 DEG C is separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 65 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 7
30g medical grade polyurethane is dissolved in the dioxane of 200mL at 50 DEG C, then adds the sodium bicarbonate 90g that particle diameter is 75 ~ 150 μm, after mechanical agitation 1h, deaeration 50min under room temperature, vacuum are 0.07MPa.Be poured over by uniform suspension after deaeration in polrvinyl chloride tool, coating thickness is 3mm, and the 50 DEG C of dehydrated alcohol then put into are separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 85 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 8
40g medical grade polyurethane is dissolved in the oxolane of 200mL at 60 DEG C, then adds the potassium bicarbonate 110g that particle diameter is 150 ~ 250 μm, after mechanical agitation 1h, deaeration 60min under room temperature, vacuum are 0.08MPa.Be poured over by uniform suspension after deaeration in polyvinyl alcohol mould, coating thickness is 3mm, then puts into 25 DEG C of dehydrated alcohol and is separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 95 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 9
50g medical grade polyurethane is dissolved in the DMF of 200mL at 60 DEG C, then adds the sodium citrate 130g that particle diameter is 150 ~ 250 μm, after mechanical agitation 1h, deaeration 20min under room temperature, vacuum are 0.08MPa.Be poured over by uniform suspension after deaeration in polyacrylonitrile mould, coating thickness is 4mm, and the dehydrated alcohol then putting into 25 DEG C is separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 25 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
Embodiment 10
25g medical grade polyurethane is dissolved in respectively in the DMF of 200mL at 70 DEG C, then adds the sodium citrate 150g that particle diameter is 150 ~ 250 μm, after mechanical agitation 1h, deaeration 20min under room temperature, vacuum are 0.08MPa.Then be poured in polysulfones mould by the uniform suspension after deaeration, coating thickness is 4mm, and the dehydrated alcohol then putting into 25 DEG C is separated, film-forming.The deionized water that Polyurethane Porous Membranes after solidification puts into 25 DEG C soaks the abundant elimination porogen of 72h, changes a water every 24h.The convection oven that the Polyurethane Porous Membranes of elimination porogen puts into 40 DEG C is dried, and obtains the porous polyurethane film of graded pore structure.
The mechanical property of table 1. embodiment 1 sample
The water vapo(u)r transmission energy of table 2. embodiment 1 sample
The water vapo(u)r transmission of table 3. embodiment 1 and embodiment 2 same recipe goods can contrast
The water absorption rate of table 4. embodiment 1 sample and porosity
Note: the medical grade polyurethane elastomer used in above example is commercially available, polyurethane elastomer used in the present invention is the Pellet hane 2363-80AE of Lubrizol company of the U.S..
Claims (6)
1. a preparation method for the porous polyurethane film of graded pore structure, is characterized in that the method comprises the following steps:
1) polyurethane is added in the middle of solvent, stir temperature 20 ~ 70 DEG C, dissolve completely, obtain the polyurethane solutions that concentration is 50 ~ 200g/L, then add that particle diameter is 20 ~ 250 μm, concentration is the porogen of 50 ~ 750g/L, after stirring, obtain suspension;
2) by above-mentioned suspension deaeration 10 ~ 60min under room temperature, vacuum 0.06 ~ 0.08MPa;
3) pour in mould by the suspension after above-mentioned deaeration, curtain coating becomes thin film, and coating thickness is 0.5 ~ 4mm;
4) above-mentioned thin film is put into the dehydrated alcohol that temperature is 20 ~ 50 DEG C, be separated, make its film-forming;
5) thin film of above-mentioned solidification being put into temperature is that the deionized water of 5 ~ 95 DEG C places 72h, elimination porogen;
6) above-mentioned thin film is carried out drying, obtain the porous polyurethane film of graded pore structure, polyurethane cellular membrane aperture increases from top to bottom gradually.
2. the preparation method of the porous polyurethane film of graded pore structure according to claim 1, is characterized in that solvent is any one in DMF, dioxane or oxolane.
3. the preparation method of the porous polyurethane film of graded pore structure according to claim 1, is characterized in that porogen is any one in sodium chloride, potassium chloride, sodium citrate, potassium citrate, sodium bicarbonate or potassium bicarbonate.
4. the preparation method of the porous polyurethane film of graded pore structure according to claim 1, is characterized in that mould is any one in glass, politef, polyester, polyethylene, polypropylene, polrvinyl chloride, polyvinyl alcohol, polyacrylonitrile or polysulfones.
5., according to the preparation method of the porous polyurethane film of the described graded pore structure of one of Claims 1 to 4, it is characterized in that the method prepares the porous polyurethane film of graded pore structure.
6. the purposes of the porous polyurethane film of graded pore structure according to claim 5, is characterized in that the porous polyurethane film of graded pore structure is used for the treatment of the artificial skin of people and other mammiferous skin injury.
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| CN107007866A (en) * | 2017-03-20 | 2017-08-04 | 张家丽 | A kind of covering material preparation method for skin nursing |
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| CN111844827B (en) * | 2020-07-23 | 2022-05-27 | 天津工业大学 | Preparation method of microfiber leather facing layer film with microporous channel |
| CN112341591A (en) * | 2020-10-27 | 2021-02-09 | 上海伊纯实业有限公司 | Polyurethane material and preparation method and application thereof |
| CN113480770A (en) * | 2021-07-23 | 2021-10-08 | 上海交通大学 | Shape memory polyurethane open-cell foam material and preparation method thereof |
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