WO2019100197A1 - Procédé de préparation d'un pansement hydrogel - Google Patents

Procédé de préparation d'un pansement hydrogel Download PDF

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Publication number
WO2019100197A1
WO2019100197A1 PCT/CN2017/112076 CN2017112076W WO2019100197A1 WO 2019100197 A1 WO2019100197 A1 WO 2019100197A1 CN 2017112076 W CN2017112076 W CN 2017112076W WO 2019100197 A1 WO2019100197 A1 WO 2019100197A1
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WO
WIPO (PCT)
Prior art keywords
solution
aqueous solution
mass
aqueous
polyvinyl alcohol
Prior art date
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Ceased
Application number
PCT/CN2017/112076
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English (en)
Chinese (zh)
Inventor
陈少军
王彩
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Shenzhen University
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Shenzhen University
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Publication date
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Priority to PCT/CN2017/112076 priority Critical patent/WO2019100197A1/fr
Publication of WO2019100197A1 publication Critical patent/WO2019100197A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/02—Adhesive bandages or dressings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F7/00—Heating or cooling appliances for medical or therapeutic treatment of the human body
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F7/00—Heating or cooling appliances for medical or therapeutic treatment of the human body
    • A61F7/02—Compresses or poultices for effecting heating or cooling

Definitions

  • the invention belongs to a preparation method of a hydrogel dressing, and relates to the technical field of polymer materials.
  • medical dressings can replace the damaged skin as a temporary barrier during wound healing, play a role in controlling the exudate of the wound, avoid or control the wound infection, and thus facilitate the healing of the wound.
  • the rapid development of science and technology has changed people's understanding and understanding of wound healing principles and wound care processes.
  • Many new materials have been used on medical dressings on a large scale. For example, films, foams, hydrogels, alginates and hydrocolloids, and pharmaceuticals.
  • Hydrogel dressings have excellent biocompatibility and are also very absorbent, and do not cause adhesion to the wound when changing the drug. Therefore, the hydrogel dressing is applied to uneven wounds with good adhesion. Sex, can ensure the cleanliness and hygiene of the wound surface, while reducing the possibility of wound infection.
  • phase change hydrogels are mainly used as medical dressings.
  • one method is to place porous nano powder, triallyl isocyanurate, polyethylene glycol diacrylate, polyethylene glycol and initiator in water, using decompression ultrasound The method of dispersion, finally obtaining the energy storage temperature-regulating material after centrifugal dehydration. After the material is dried, it is blended and granulated with a polymer chip extruder, and then melt-spun to obtain a temperature-regulating fiber.
  • Another method is to disperse the prepared phase change microcapsules into a dilute solution containing chitosan, and the phase change microcapsules are uniformly mixed in a dilute solution to obtain a spinning dope, and the phase change thermostat microcapsule fiber is transformed by a phase change.
  • the microcapsule material and the chitosan solution are prepared by a wet spinning process, and the spray spinning dope is solidified by a mixture of NaOH and ethanol to obtain a phase change thermostat microcapsule material.
  • the first method has a high temperature for melt spinning, and is easy to damage microcapsules, resulting in poor storage and temperature regulation.
  • the second method is highly polluting, there is a risk of wound exposure, and there is no guarantee that the wound will be in a humid environment.
  • the two methods are complicated in process and are not suitable for large-scale use.
  • the present invention provides a method for preparing a hydrogel dressing, which aims to solve the above-mentioned drawbacks of the preparation method.
  • the present invention provides a method for preparing a hydrogel dressing, comprising: mixing 1-8 parts by mass of an aqueous silk fibroin solution and 3-6 parts by mass of an aqueous polyurethane solution, and adding 1 to 5 parts by mass of an aqueous solution of polyvinyl alcohol.
  • the reaction is carried out at a stirring rate of 500 to 700 for 20 to 30 minutes to obtain a composite aqueous solution, wherein the mass fraction of the aqueous silk fibroin solution, the aqueous polyurethane solution and the aqueous polyvinyl alcohol solution are respectively: 1 to 10%, 20 to 40%, and 8 ⁇ 12.5%;
  • phase change energy storage microcapsules are mixed with the composite aqueous solution according to the mass ratio of 1:10 to 50, and poured into a mold to be solidified to obtain a hydrogel dressing.
  • the invention provides a preparation method of a hydrogel dressing, which avoids the use of a reagent which is not polluting and does not pollute the environment, and the method adopts a low-temperature curing method, and does not damage the capsule and its mechanical properties. Reduces the risk of wound exposure.
  • the method is simple for large-scale applications.
  • Example 1 is a physical diagram of a hydrogel dressing prepared in Example 1 of the present invention.
  • Example 2 is an infrared thermography image of a hydrogel dressing prepared in Example 1 of the present invention
  • Figure 3 is a scanning electron micrograph of a hydrogel dressing prepared in Example 1 of the present invention.
  • the invention provides a preparation method of a hydrogel dressing, which mainly comprises the following steps:
  • Step 1 Mix 1 to 8 parts by mass of the silk fibroin aqueous solution and 3 to 6 parts by mass of the aqueous polyurethane solution, add 1 to 5 parts by mass of the polyvinyl alcohol aqueous solution, and react at a stirring rate of 500 to 700 for 20 to 30 minutes. , a composite aqueous solution;
  • the mass fraction of the aqueous silk fibroin solution, the aqueous polyurethane solution and the aqueous polyvinyl alcohol solution are respectively: 1 to 10%, 20 to 40%, and 8 to 12.5%;
  • Step 2 mixing the phase change energy storage microcapsules with the composite aqueous solution according to the mass ratio of 1:10 to 50, and pouring into a mold to solidify to obtain a hydrogel dressing.
  • the invention provides a preparation method of a hydrogel dressing, which avoids the use of a reagent which is not polluting and does not pollute the environment, and the method adopts a low-temperature curing method, and does not damage the capsule and its mechanical properties. Reduces the risk of wound exposure.
  • the method is simple for large-scale applications.
  • the silk fibroin aqueous solution is prepared by dissolving the degummed silk in a lithium bromide solution and dialysis in distilled water for 24 to 72 hours to obtain a silk fibroin aqueous solution having a mass fraction of 1 to 10%.
  • the molar ratio of degummed silk to lithium bromide is 1 ⁇ 3:1 ⁇ 3, and the concentration of lithium bromide solution is 8 ⁇ 10mol/L.
  • the degummed silk is silk protein, spider silk protein or soy protein, collagen and lysine. At least one degummed silk.
  • the polyvinyl alcohol aqueous solution is prepared by adding the polyvinyl alcohol of the grade 1799 to the water of 90-95 ° C for several times, and magnetically stirring for 20-40 min to obtain a polyvinyl alcohol aqueous solution having a mass fraction of 8 to 12.5%.
  • the aqueous polyurethane solution is prepared by mixing the bio-based polyol and the isocyanate according to the molar ratio of the group NCO of the polyisocyanate to the OH of the bio-based polyol group of 1.1 to 1.2:1, and hydrating the chain to obtain a mass fraction of 20 ⁇ 40% aqueous polyurethane solution.
  • the bio-based polyol is at least one of polycaprolactone, vegetable oil, polyhydroxyalkanoate, polylactic acid, and polyethylene glycol.
  • the core material of the phase change energy storage capsule is an organic phase change material having a phase transition temperature of 18 to 38 ° C, and the phase change organic material includes a higher aliphatic alkane, an alcohol, an acid, and a lipid. At least one.
  • the core material is coated with a polymer shell composed of an organic polymer monomer, and the organic polymer monomer is any one of a melamine resin, a urea resin, a phenol resin, a polyurea resin, a polystyrene, and a polyacrylate. .
  • the hydrogel dressing can undergo a corresponding phase change at a phase transition temperature of 18 to 38 ° C to internalize it.
  • the molecular form changes between the crystallization zone and the amorphous zone, and there is a phenomenon of endothermic and exothermic during the conversion process, thereby storing or releasing heat to adjust the changes of the surrounding environment, and placing the material on the wound can be beneficial to Heal.
  • the hydrogel dressing when the hydrogel dressing is cured, it can be placed in an ultraviolet box and cured by ultraviolet light, or it can be frozen in a refrigerator at -25 ° C for 6-8 h, and then It is thawed at room temperature for 3 ⁇ 4h, and is solidified by freezing-thawing for 3 ⁇ 5 times.
  • a phase change energy storage capsule having a diameter of 30 um was mixed with the composite aqueous solution prepared in the first step according to a mass ratio of 1:50, stirred, and ultrasonically dispersed for 15 minutes to obtain a mixed solution.
  • the mixed solution obtained in the step 2 was poured into a mold of 10 mm ⁇ 10 mm ⁇ 2 mm square, and frozen in a refrigerator at -25 ° C for 8 hours, then thawed at room temperature for 4 hours, and frozen-thawed 5 times under the conditions.
  • FIGS. 1 to 3 are hydrogels prepared in Example 1 and related test charts.
  • Figure 2 is an infrared thermography image of continuous heating of the hydrogel material.
  • Figure 2 shows that the hydrogel of the composite phase change energy storage material shows good under continuous heating. Temperature regulation capability.
  • Figure 3 is a scanning electron micrograph of a hydrogel dressing. As can be seen from Figure 3, the hydrogel material is a porous structure.
  • a phase change energy storage capsule having a diameter of 25 ⁇ m was mixed with the composite aqueous solution prepared in the first step according to a mass ratio of 1:40, stirred, and ultrasonically dispersed for 15 minutes to obtain a mixed solution.
  • the mixed solution obtained in the step 2 was poured into a mold of 10 mm ⁇ 5 mm ⁇ 1 mm square, and frozen in a refrigerator at -25 ° C for 6 hours, then thawed at room temperature for 3 hours, and frozen-thawed 5 times under the conditions.
  • a phase change energy storage capsule having a diameter of 20 ⁇ m was mixed with the composite aqueous solution prepared in the first step according to a mass ratio of 1:30, stirred, and ultrasonically dispersed for 15 minutes to obtain a mixed solution.
  • the mixed solution obtained in the step 2 was poured into a mold of 10 mm ⁇ 10 mm ⁇ 1 mm square, and frozen in a refrigerator at -25 ° C for 5 hours, then thawed at room temperature for 2 hours, and frozen-thawed 5 times under the conditions.
  • a phase change energy storage capsule having a diameter of 50 um was mixed with the composite aqueous solution prepared in the first step according to a mass ratio of 1:20, stirred, and ultrasonically dispersed for 15 minutes to obtain a mixed solution.
  • step 3 pour the mixed solution obtained in step 2 into a circular mold with a diameter of 10 mm and a thickness of 1 mm, and freeze in a refrigerator at -25 ° C for 6 h, then thaw at room temperature for 3 h, and freeze-thaw under such conditions. Times.
  • a phase change energy storage capsule having a diameter of 50 um was mixed with the composite aqueous solution prepared in the first step according to a mass ratio of 1:10, stirred, and ultrasonically dispersed for 15 minutes to obtain a mixed solution.
  • the mixed solution obtained in the step 2 was poured into a circular mold having a diameter of 10 mm and a thickness of 1 mm, and placed in an ultraviolet curing box, and photocured for 2 minutes.

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  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Heart & Thoracic Surgery (AREA)
  • Vascular Medicine (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Materials For Medical Uses (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne un procédé de préparation d'un pansement hydrogel, qui se rapporte au domaine technique des matériaux polymères, comprenant : le mélange de 1 à 8 parties en masse d'une solution aqueuse de fibroïne de soie et de 3 à 6 parties en masse d'une solution aqueuse de polyuréthane; l'ajout de 1 à 5 parties en masse d'une solution aqueuse d'alcool polyvinylique; la réaction à un taux d'agitation de 500 à 700 pendant 20 à 30 minutes pour obtenir une solution aqueuse composite, les fractions de masse de la solution aqueuse de fibroïne de soie, la solution aqueuse de polyuréthane et la solution aqueuse d'alcool polyvinylique étant respectivement : 1 à 10 %, 20 à 40 %, et 8 à 12,5 %; le mélange d'une microcapsule de stockage d'énergie à changement de phase avec la solution aqueuse composite selon un rapport de masse de 1 : 10 à 50; le versement de ce mélange obtenu dans un moule pour un durcissement pour obtenir un pansement hydrogel. Le procédé est simple et est approprié pour une utilisation à grande échelle.
PCT/CN2017/112076 2017-11-21 2017-11-21 Procédé de préparation d'un pansement hydrogel Ceased WO2019100197A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2017/112076 WO2019100197A1 (fr) 2017-11-21 2017-11-21 Procédé de préparation d'un pansement hydrogel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2017/112076 WO2019100197A1 (fr) 2017-11-21 2017-11-21 Procédé de préparation d'un pansement hydrogel

Publications (1)

Publication Number Publication Date
WO2019100197A1 true WO2019100197A1 (fr) 2019-05-31

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030195448A1 (en) * 2002-04-16 2003-10-16 Jensen Jeffrey L. Heat regulating wound dressing
TW200716189A (en) * 2005-10-19 2007-05-01 Taiwan Textile Res Inst Temperature regulating geland article comprising the same
CN101455856A (zh) * 2008-12-26 2009-06-17 深圳清华大学研究院 运动损伤护理用相变蓄能材料
CN105561900A (zh) * 2015-12-29 2016-05-11 唐山师范学院 相变微胶囊及其制备方法
WO2017127768A1 (fr) * 2016-01-21 2017-07-27 Imanano, Inc. Dispositif, système et procédé de pansement stérile à régulation de température
CN107913434A (zh) * 2017-11-21 2018-04-17 深圳大学 一种水凝胶敷料的制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030195448A1 (en) * 2002-04-16 2003-10-16 Jensen Jeffrey L. Heat regulating wound dressing
TW200716189A (en) * 2005-10-19 2007-05-01 Taiwan Textile Res Inst Temperature regulating geland article comprising the same
CN101455856A (zh) * 2008-12-26 2009-06-17 深圳清华大学研究院 运动损伤护理用相变蓄能材料
CN105561900A (zh) * 2015-12-29 2016-05-11 唐山师范学院 相变微胶囊及其制备方法
WO2017127768A1 (fr) * 2016-01-21 2017-07-27 Imanano, Inc. Dispositif, système et procédé de pansement stérile à régulation de température
CN107913434A (zh) * 2017-11-21 2018-04-17 深圳大学 一种水凝胶敷料的制备方法

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