CN104947320A - Biomedical energy-storage and temperature-adjusting fibrous membrane and preparation method thereof - Google Patents
Biomedical energy-storage and temperature-adjusting fibrous membrane and preparation method thereof Download PDFInfo
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- CN104947320A CN104947320A CN201510281491.6A CN201510281491A CN104947320A CN 104947320 A CN104947320 A CN 104947320A CN 201510281491 A CN201510281491 A CN 201510281491A CN 104947320 A CN104947320 A CN 104947320A
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- polyethylene glycol
- tunica fibrosa
- regenerated silk
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Abstract
The invention relates to a biomedical energy-storage and temperature-adjusting fibrous membrane and a preparation method thereof. The fibrous membrane is composed of 50 to 80 percents of regenerated silk protein and 20 to 50 percents of polyethylene glycol. The polyethylene glycol and the regenerated silk protein are combined through a hydrogen-bond interaction. The regenerated silk protein is used as basis materials. The polyethylene glycol is used as phase energy storage materials. The preparation method of the biomedical energy-storage and temperature-adjusting fibrous membrane comprises the steps that the polyethylene glycol with weight-average molecular weight ranging from 600 to 1000 is added to aqueous solution of the regenerated silk protein to obtain spinning solution, and the fibrous membrane is obtained through electrostatic spinning. The preparation method of the biomedical energy-storage and temperature-adjusting fibrous membrane has the advantages of being simple, convenient, environmental-protection, free from pollution and low in cost and is suitable for industrial production; the fibrous membrane has excellent temperature adjusting performance and proper mechanical property, biocompatibility is good, and the fibrous membrane can be applied to the fields of wound healing, tissue regeneration and the like.
Description
Technical field
The invention belongs to boiomacromolecule nonwoven cloth material technical field, in particular to a kind of bio-medical energy-saving and temperature-regulating tunica fibrosa and preparation method thereof, this tunica fibrosa is made up of regenerated silk fibroin and polyethylene glycol, biodegradable and and bio-compatible, can use as the tunica fibrosa of carrying medicament.
Background technology
Regenerated silk fibroin (Regenerated Silk Fibroin, RSF) be a kind of native protein obtained by silk cocoon, there is good biocompatibility and degradability, the good ventilative and excellent properties such as poisture-penetrability, reduced immunogenicity, make it be widely used in the fields such as biological medicine in recent years.And the regenerated silk fibroin nanofiber obtained by electrostatic spinning technique, has that yardstick is little, a characteristic such as the large and excellent physical properties of specific area, more expand its application prospect in fields such as bioengineered tissue support, wound surface reparations.Because native protein nano fibrous membrane has the characteristics such as aperture is little, specific area is high, not only effectively can stop bacterium intrusion, hemostasis reaction can also be promoted; Its loose structure and good ventilative oxygen permeability are conducive to the breathing of cell and do not cause wound dry, and inducing skin cells is better repaired, thus contributes to wound healing and skin regeneration.In addition, regenerated silk fibroin nanofiber or the ideal material of carrying medicament, can realize the Co ntrolled release to medicine, more can simulate natural extracellular matrix, is beneficial to growth and the propagation of cell, promotes regeneration.
Energy-saving and temperature-regulating fiber is by phase-changing energy storage material and fiber composite, obtains the intelligent fiber that automatically can regulate temperature.Phase-change material contained by it utilizes the heat absorption and release that produce in phase transition process, deals with the change of environment temperature, thus reaches the balance of fiber to local microenvironment temperature and the object of adjustment.Therefore, energy-saving and temperature-regulating fiber is as a kind of new material, and not only have a wide range of applications in fields such as clothes fabric, building and Aero-Space, also gradually in medical textile field, even wound repair field occupies one seat.
The preparation method of current energy-saving and temperature-regulating fiber mainly contains co-blended spinning method (as Chinese patent 200710014607.5, 201110310334.5, 201210227516.0), microcapsules composite spinning method is (as Chinese patent 200610157441.8, 200610069976.X, 201110213102.8) and the method such as chemical graft process (as Chinese patent 201110310334.5), the energy-saving and temperature-regulating fiber prepared by above technology, health care product are widely used in, household articles, the aspects such as protective device, substantially increase temperature protective and the comfort level of textiles.
Polyethylene glycol is a kind of conventional phase-changing energy storage material, and nonflammable, nontoxic, pollution-free, phase transformation enthalpy is high, without surfusion and the problem such as to be separated, compared with inorganic hydrated salt and paraffin etc., is ideal phase-changing energy storage material.At present, the mode that polyethylene glycol is used as phase-changing energy storage material generally has three kinds: one to be utilize perlite, diatomite, the porose material such as expanded graphite carries out physical absorption, form composite phase-change material (Karaman S, Karaipekli A, Sari A, et al. Polyethyleneglycol (PEG)/diatomite composite as a novel form-stable phase change material for thermal energy storage [J]. Solar Energy Materials and Solar Cells. 2011, 95 (7): 1647-1653.), two is utilize chemical graft, make the hydroxyl of the peg molecule end of the chain with as the functional group reactions on the macromolecular chain of matrix material, form new solid-solid phase transition material (Jiang Y, Ding E, Li G. Study on the transition characteristics of PEG-CAD solid-solid phase change materials [J]. Polymer. 2002,43:117-122.).Three is adopt microcapsule coated technique, utilizes inorganic or has casing material, coated with polyethylene glycol being become microcapsules (Chinese publication 201310192189).
Polyethylene glycol is also paid close attention to as the application of phase-changing energy storage material in energy-saving and temperature-regulating fiber art.The people such as Zhang Mei, by by polyethylene glycol and polyvinyl alcohol blending, obtain energy-saving and temperature-regulating electrostatic spinning nano fiber film, but the fibre forming property of fiber are poor, and gained fiber is uneven, and (military supplies are studied for the research of phase-change material and heat-accumulation temperature-adjustment functional fibre, Zhang Mei, 2002,3:40-44).Ginger to be pushed ahead vigorously etc. and adopts wet spinning process, by polyethylene glycol and the direct co-blended spinning of polyvinyl alcohol, obtain polyethylene glycol/polyvinyl alcohol phase-change accumulation energy composite fibre, but due to being separated in use cannot be avoided, phase-change material in fiber system very easily runs off, and causes the energy storage of fiber to decline thereupon.They then carry out in-situ cross-linked to the fiber obtained, together with being fixed on by polyethylene glycol, avoid the loss (Chinese patent 201210569858) of energy storage component with polyvinyl alcohol.The people such as Hou Min utilize the reactivity of end group in peg molecule chain, adopt chemical graft process to obtain phase-change energy-storage fibre, but the percent grafting of fiber is lower, and fibre forming property are by the impact of phase-change material content, is unfavorable for the spinning technique of fiber.The people such as Zhang Hong adopt graft reaction, have directly been grafted to by polyethylene glycol on polypropylene long-chain, by melt spinning, obtain polypropylene/polyethylene glycol composite fibre (Chinese patent 201110310334).
In the preparation method of the above polyethylene glycol energy-saving and temperature-regulating fiber, still there is phase-change material to be easy to run off, the fibre forming property of fiber is poor, and the shortcoming such as the energy storage of fiber is not good, processing technology is loaded down with trivial details, therefore, inquire under the prerequisite not destroying fiber fibre forming property and energy storage, obtain the problem that high-performance poly ethylene glycol energy-saving and temperature-regulating tunica fibrosa is still researcher's concern.
Summary of the invention
The above-mentioned many defects existed for avoiding prior art, the invention provides a kind of bio-medical energy-saving and temperature-regulating tunica fibrosa, preparation method and application, this energy-saving and temperature-regulating tunica fibrosa is made up of regenerated silk fibroin and polyethylene glycol, biodegradable and and bio-compatible, can use as the tunica fibrosa of carrying medicament ideally.
Bio-medical energy-saving and temperature-regulating tunica fibrosa provided by the invention, be made up of the polyethylene glycol of mass percent to be the regenerated silk fibroin of 50%-80% and mass percent be 20%-50%, polyethylene glycol is combined by hydrogen bond action with regenerated silk fibroin, and described tunica fibrosa is smooth nano fibrous membrane.
In this tunica fibrosa, the weight average molecular weight of polyethylene glycol used is 600-10000.The weight average molecular weight of regenerated silk fibroin used is 80000-110000.
Fibre diameter in described energy-saving and temperature-regulating tunica fibrosa is 100-2000 nm, and heat accumulation enthalpy is 20-80J/g.
The preparation method of above-mentioned bio-medical energy-saving and temperature-regulating tunica fibrosa, comprise the steps: that polyethylene glycol being dissolved in concentration is in the regenerated silk fibroin water solution of 10wt%-20wt%, stir the mixed liquor obtaining transparent and homogeneous, in this mixed liquor, polyethylene glycol and regenerated silk fibroin mass ratio are 20-50: 50-80; Above-mentioned mixed liquor is condensed into the spinning solution that concentration is 25wt%-38wt%, then injects electrostatic spinning apparatus and carry out electrostatic spinning, obtain regenerated silk fibroin/polyethylene glycol nano fibrous membrane.
Wherein, the weight average molecular weight of polyethylene glycol used is 600-10000.The weight average molecular weight of regenerated silk fibroin used is 80000-110000.
Fibre diameter in described tunica fibrosa is 100-2000 nm, and heat accumulation enthalpy is 20-80J/g.The phase transition temperature of described tunica fibrosa is controlled by the polyethylene glycol of composite different molecular weight.
Described regenerated silk fibroin water solution can be adopted and obtain with the following method: in 35-45
oat C temperature, fibroin albumen is dissolved 2h in the LiBr aqueous solution of 9Mol/L, after being dialysed in deionized water 48-72 hour by gained regenerated silk fibroin water solution, being concentrated into concentration is 10wt%-20wt%.
In preferred enforcement, the concentration of described spinning solution is 30wt%-35.5wt%.
The application of bio-medical energy-saving and temperature-regulating tunica fibrosa of the present invention, described tunica fibrosa uses as the tunica fibrosa of carrying medicament, comprises the component of wound healing and promote the component of regeneration in described carrying medicament.As, hyaluronic acid skin repair component, chitosan disinfectant component or anti-inflammation and sterilization medicine etc.
Bio-medical energy-saving and temperature-regulating tunica fibrosa of the present invention is made up of regenerated silk fibroin and polyethylene glycol, regenerated silk fibroin is matrix material, polyethylene glycol is phase-changing energy storage material, polyethylene glycol is combined by hydrogen bond action with regenerated silk fibroin, biodegradable and and bio-compatible, can use as drug-loading fibre film ideally.After adding the bactericidal components such as skin repair component, shitosan such as hyaluronic acid or other anti-inflammation and sterilization medicines, can be applicable to the field such as wound healing and regeneration.
Wherein regenerated silk fibroin has good biocompatibility and degradability, good ventilative and poisture-penetrability, the performance that reduced immunogenicity etc. are excellent; Polyethylene glycol is a kind of Prof. Du Yucang degradability Green Polymer, have nontoxic, without characteristics such as antigen, good biocompatibilities, and energy storage efficiency is higher.
This method is under the prerequisite not destroying fiber fibre forming property and energy storage, polyethylene glycol is combined by hydrogen bond action with regenerated silk fibroin, and utilize the Static Spinning performance of regenerated silk fibroin water solution excellence, obtain polyethylene glycol energy-saving and temperature-regulating electrostatic spinning fiber film, the energy storage of its fiber is good.This method is simple and direct, environment friendly and pollution-free, with low cost, is suitable for suitability for industrialized production.
accompanying drawing illustrates:
Fig. 1 is the SEM figure of the energy-saving and temperature-regulating nano fibrous membrane that the embodiment of the present invention 1 obtains.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment 1
(1) accurately take the polyethylene glycol that 1g weight average molecular weight is 1000, adding concentration is in the 20g regenerated silk fibroin water solution of 20wt%, and normal temperature lower magnetic force stirs 15min and obtains transparent mixed liquor, and then is condensed into the spinning solution that concentration is 33.5wt%.
(2) spinning solution of gained is transferred in syringe, take aluminium foil as receiving system, Static Spinning is carried out in normal temperature environment, Static Spinning condition is: voltage is 23kV, syringe pump advances speed to be 0.6ml/h, receiving range is 16cm, obtains regenerated silk fibroin/polyethylene glycol energy-saving and temperature-regulating composite nano-fiber membrane.With reference to figure 1, nanofiber average diameter is 150 ± 44.12nm, and phase transition temperature is 38.5
oc, heat accumulation enthalpy is 21J/g.
Embodiment 2
(1) take the polyethylene glycol that 2g weight average molecular weight is 2000, adding concentration is in the 20g regenerated silk fibroin water solution of 20wt%, and normal temperature lower magnetic force stirs 15min and obtains transparent mixed liquor, and then is condensed into concentration 32.3wt% spinning solution.
(2) spinning solution of gained is transferred in syringe, take aluminium foil as receiving system, Static Spinning is carried out in normal temperature environment, Static Spinning condition is: voltage is 25kV, syringe pump advances speed to be 0.7ml/h, and receiving range is 12cm, obtains regenerated silk fibroin/polyethylene glycol energy-saving and temperature-regulating composite nano-fiber membrane, nanofiber average diameter is 220 ± 74.46nm, and phase transition temperature is 52.5
oc, heat accumulation enthalpy is 48J/g.
Embodiment 3
(1) accurately take the polyethylene glycol that 3g weight average molecular weight is 800, adding concentration is in the 20g regenerated silk fibroin water solution of 20wt%, and normal temperature lower magnetic force stirs 15min and obtains transparent mixed liquor, and is condensed into concentration 35.4wt% spinning solution.
(2) spinning solution of gained is transferred in syringe, take aluminium foil as receiving system, Static Spinning is carried out in normal temperature environment, Static Spinning condition is: voltage is 19kV, syringe pump advances speed to be 0.7ml/h, and receiving range is 15cm, obtains regenerated silk fibroin/polyethylene glycol energy-saving and temperature-regulating composite nano-fiber membrane, nanofiber average diameter is 101 ± 14.23nm, and phase transition temperature is 29.6
oc, heat accumulation enthalpy is 53J/g.
Embodiment 4
(1) accurately take the polyethylene glycol that 2.5g weight average molecular weight is 600, adding concentration is in the 20g regenerated silk fibroin water solution of 20wt%, and normal temperature lower magnetic force stirs 15min and obtains transparent mixed liquor, and is condensed into the spinning solution of concentration 33.5wt%.
(2) spinning solution of gained is transferred in syringe, take aluminium foil as receiving system, Static Spinning is carried out in normal temperature environment, Static Spinning condition is: voltage is 20kV, syringe pump advances speed to be 0.7ml/h, and receiving range is 15cm, obtains regenerated silk fibroin/polyethylene glycol energy-saving and temperature-regulating composite nano-fiber membrane, nanofiber average diameter is 98 ± 24.03nm, and phase transition temperature is 21.7
oc, heat accumulation enthalpy is 15J/g.
Embodiment 5
(1) accurately take the polyethylene glycol that 2g weight average molecular weight is 6000, adding concentration is in the 20g regenerated silk fibroin water solution of 10wt%, and normal temperature lower magnetic force stirs 15min and obtains transparent mixed liquor, and is condensed into the spinning solution of concentration 33.5wt%.
(2) spinning solution of gained is transferred in syringe, take aluminium foil as receiving system, Static Spinning is carried out in normal temperature environment, Static Spinning condition is: voltage is 28kV, syringe pump advances speed to be 0.7ml/h, and receiving range is 10cm, obtains regenerated silk fibroin/polyethylene glycol energy-saving and temperature-regulating composite nano-fiber membrane, nanofiber average diameter is 956 ± 274.46nm, and phase transition temperature is 58.3
oc, heat accumulation enthalpy is 76J/g.
In above-described embodiment 1-5, regenerated silk fibroin water solution method for making used is as follows:
By the 0.5wt% Na that silk cocoon is boiling
2cO
3the medium and small fire of the aqueous solution boils 2 times, each 30min, cleans and obtains fibroin albumen; By the fibroin albumen that obtains in 40
ounder C, in the LiBr aqueous solution of 9Mol/L, dissolve 2h, obtain regenerated silk fibroin water solution; After being dialysed in deionized water 3 days by gained regenerated silk fibroin water solution, being concentrated into concentration expressed in percentage by weight is 10wt%-20wt%.
Above by specific embodiment to invention has been detailed description, these specific descriptions can not think that the present invention is only only limitted to the content of these embodiments.Those skilled in the art according to the present invention's design, these describe and any improvement made in conjunction with general knowledge known in this field, equivalents, all should be included in the protection domain of the claims in the present invention.
Claims (10)
1. a bio-medical energy-saving and temperature-regulating tunica fibrosa, it is characterized in that, described tunica fibrosa is made up of the polyethylene glycol of mass percent to be the regenerated silk fibroin of 50%-80% and mass percent be 20%-50%, polyethylene glycol is combined by hydrogen bond action with regenerated silk fibroin, and described tunica fibrosa is smooth nano fibrous membrane.
2. tunica fibrosa according to claim 1, is characterized in that, the weight average molecular weight of described polyethylene glycol is 600-10000.
3. tunica fibrosa according to claim 1, is characterized in that, it is characterized in that: the weight average molecular weight of described regenerated silk fibroin is 80000-110000.
4. tunica fibrosa according to claim 1, is characterized in that, the fibre diameter in described tunica fibrosa is 100-2000 nm, and heat accumulation enthalpy is 20-80J/g.
5. a preparation method for bio-medical energy-saving and temperature-regulating tunica fibrosa, is characterized in that,
Polyethylene glycol is dissolved in the mixed liquor stirring in regenerated silk fibroin water solution and obtain transparent and homogeneous, in this mixed liquor, polyethylene glycol and regenerated silk fibroin mass ratio are 20-50: 50-80;
Above-mentioned mixed liquor is concentrated into 25wt%-38wt%, then injects electrostatic spinning apparatus and carry out electrostatic spinning, obtain tunica fibrosa.
6. preparation method according to claim 5, is characterized in that, the phase transition temperature of described tunica fibrosa is controlled by the polyethylene glycol of composite different molecular weight, and the weight average molecular weight of described polyethylene glycol is 600-10000.
7. preparation method according to claim 5, is characterized in that: the molecular weight of described regenerated silk fibroin is 80000-110000, and the concentration of described regenerated silk fibroin water solution is 10wt%-20wt%.
8. preparation method according to claim 5, is characterized in that: the fibre diameter in described tunica fibrosa is 100-2000 nm, and heat accumulation enthalpy is 20-80J/g.
9. preparation method according to claim 5, is characterized in that, described regenerated silk fibroin water solution method for making comprises the steps: in 35-45
oat C temperature, fibroin albumen is dissolved 2h in the LiBr aqueous solution of 9Mol/L, after being dialysed in deionized water 48-72 hour by gained regenerated silk fibroin water solution, being concentrated into concentration is 10wt%-20wt%.
10. the application of claim 1-4 bio-medical energy-saving and temperature-regulating tunica fibrosa described in any one, described tunica fibrosa uses as the tunica fibrosa of carrying medicament, comprises the component of wound healing and promote the component of regeneration in described carrying medicament.
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| CN105297289A (en) * | 2015-12-07 | 2016-02-03 | 清华大学深圳研究生院 | Preparation method of silk fibroin energy storage and temperature regulation fiber membrane |
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| CN114832145A (en) * | 2022-05-20 | 2022-08-02 | 武汉纺织大学 | Porous skin-core structure phase-change temperature-regulating controlled-release fiber dressing and preparation method thereof |
| CN116478495A (en) * | 2023-04-21 | 2023-07-25 | 广东丙辛新材料有限公司 | Biodegradable polyethylene and preparation method thereof |
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Address after: Shenzhen Graduate School of Guangdong Province, Shenzhen City Xili 518055 Nanshan District University City Tsinghua University Patentee after: Shenzhen International Graduate School of Tsinghua University Address before: Shenzhen Graduate School of Guangdong Province, Shenzhen City Xili 518055 Nanshan District University City Tsinghua University Patentee before: GRADUATE SCHOOL AT SHENZHEN, TSINGHUA University |
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Granted publication date: 20171114 |
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