CN106519615A - 聚羟基丁酸酯抗菌薄膜的制备方法 - Google Patents

聚羟基丁酸酯抗菌薄膜的制备方法 Download PDF

Info

Publication number
CN106519615A
CN106519615A CN201611015054.0A CN201611015054A CN106519615A CN 106519615 A CN106519615 A CN 106519615A CN 201611015054 A CN201611015054 A CN 201611015054A CN 106519615 A CN106519615 A CN 106519615A
Authority
CN
China
Prior art keywords
thin film
psph
preparation
bacteria
polyhydroxybutyrate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201611015054.0A
Other languages
English (en)
Inventor
王耀斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi Shengmai Petroleum Co Ltd
Original Assignee
Shaanxi Shengmai Petroleum Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi Shengmai Petroleum Co Ltd filed Critical Shaanxi Shengmai Petroleum Co Ltd
Priority to CN201611015054.0A priority Critical patent/CN106519615A/zh
Publication of CN106519615A publication Critical patent/CN106519615A/zh
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
    • C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • C08J2483/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Laminated Bodies (AREA)
  • Wrappers (AREA)

Abstract

本发明涉及功能材料技术领域，具体涉及一种聚羟基丁酸酯抗菌薄膜的制备方法。聚羟基丁酸酯抗菌薄膜的制备方法，包括如下步骤：（1）制备海因钠盐；（2）制备SPH；（3）制备PSPH；（4）PHB/PSPH复合薄膜的制备；（5）氯化、滴定。本发明采用溶剂挥发法将卤胺抗菌剂PSPH添加至PHB中制备出高效抗菌薄膜，加入PSPH后，薄膜表面孔隙率增大且孔径变大;薄膜疏水作用增强，耐紫外稳定性较好;释放到水中氯含量较小，对环境不会产生影响。薄膜抗菌性能良好，能够在5min内将金黄色葡萄球菌和大肠杆菌全部杀死。

Description

聚羟基丁酸酯抗菌薄膜的制备方法
技术领域
本发明涉及功能材料技术领域，具体涉及一种聚羟基丁酸酯抗菌薄膜的制备方法。
背景技术
随着人们环保意识的提高，生物可降解材料逐渐受到人们的广泛关注。脂肪族聚酯作为生物可降解材料中的一种，因其分子结构中含有酯键而易被自然环境中的微生物降解。聚β-羟基丁酸酯(PHB)是由1925年法国巴斯德研究所在巨大芽孢杆菌中发现的。由于PHB 优良的生物降解性、生物相容性、光学活性、抗紫外辐射、抗凝血性和压电性等，在食品包装及手术缝合线、药物释放载体、整形外科装置、骨组织支架材料等医学、组织工程领域具有潜在的应用。
细菌、真菌等微生物在日常生活中无处不在。食品在存储包装时，若接触到细菌、霉菌等微生物，只要条件适宜，微生物就会大量繁殖，加速食品腐坏变质。目前，食品包装材料虽种类较多，但大部分化学稳定性较强，难以降解，极易造成白色污染。此外，以医药品为代表的生物医学材料，若含有一定量有害微生物，机体防御功能低下，致病微生物同样会引起患者的严重感染、导致疾病发生。
PHB 结晶度高、脆性、热稳定性较差，大大限制了其加工应用。所以目前科研工作者对PHB 的改性研究主要还是集中在改善其物理机械性能和热稳定性，而对其抗菌改性研究少有报道。但基于PHB 在食品包装、生物医学等领域的潜在应用价值，仅仅弥补上述两方面缺陷是远远不够的。想要进一步提高PHB 的使用价值，对其进行抗菌改性有着极其重要的意义。
发明内容
本发明旨在提出一种聚羟基丁酸酯抗菌薄膜的制备方法。
本发明的技术方案在于：
聚羟基丁酸酯抗菌薄膜的制备方法，包括如下步骤：
（1）制备海因钠盐
取0.1 mol 5，5-二甲基海因，加入150mL乙醇使其溶解，然后加入0.1 mol氢氧化钠，油浴环境下不断搅拌至完全溶解，90℃反应10min，旋转蒸发去除溶剂，制备得到的海因钠盐于45℃真空干燥；
（2）制备SPH
将海因钠盐溶于150mL DMF，加入0.1molγ-氯丙基三乙氧基硅烷，95~100℃回流反应8h；反应结束后，过滤除去NaCl副产物，减压除去溶剂，得到产物SPH；
（3）制备PSPH
配置质量比为2∶1∶2的SPH/乙醇/水混合溶液，用稀HCl调节pH值至3.4~5.5，85℃冷凝回流5h，加热去除水和乙醇，得到玻璃状透明固体，即为PSPH；
（4）PHB/PSPH 复合薄膜的制备
称取PHB 和PSPH并分别溶解于CHCl3和DMF 中混合后搅拌至均一溶液，将溶液缓慢倾倒入模具中，室温下挥发24h 成膜，于真空烘箱中干燥至恒重；
（5）氯化、滴定
取质量分数为10％的次氯酸钠水溶液，室温下将样品浸渍1h；结束后用去离子水洗涤，于45℃烘箱中烘1h 以去除样品中残留的自由氯，制备得到抗菌薄膜。
本发明的技术效果在于：
本发明采用溶剂挥发法将卤胺抗菌剂PSPH 添加至PHB 中制备出高效抗菌薄膜，加入PSPH 后，薄膜表面孔隙率增大且孔径变大;薄膜疏水作用增强，耐紫外稳定性较好;释放到水中氯含量较小，对环境不会产生影响。薄膜抗菌性能良好，能够在5min内将金黄色葡萄球菌和大肠杆菌全部杀死。
具体实施方式
聚羟基丁酸酯抗菌薄膜的制备方法，包括如下步骤：
（1）制备海因钠盐
取0.1 mol 5，5-二甲基海因，加入150mL乙醇使其溶解，然后加入0.1 mol氢氧化钠，油浴环境下不断搅拌至完全溶解，90℃反应10min，旋转蒸发去除溶剂，制备得到的海因钠盐于45℃真空干燥；
（2）制备SPH
将海因钠盐溶于150mL DMF，加入0.1molγ-氯丙基三乙氧基硅烷，95~100℃回流反应8h；反应结束后，过滤除去NaCl副产物，减压除去溶剂，得到产物SPH；
（3）制备PSPH
配置质量比为2∶1∶2的SPH/乙醇/水混合溶液，用稀HCl调节pH值至3.4~5.5，85℃冷凝回流5h，加热去除水和乙醇，得到玻璃状透明固体，即为PSPH；
（4）PHB/PSPH 复合薄膜的制备
称取PHB 和PSPH并分别溶解于CHCl3和DMF 中混合后搅拌至均一溶液，将溶液缓慢倾倒入模具中，室温下挥发24h 成膜，于真空烘箱中干燥至恒重；
（5）氯化、滴定
取质量分数为10％的次氯酸钠水溶液，室温下将样品浸渍1h；结束后用去离子水洗涤，于45℃烘箱中烘1h 以去除样品中残留的自由氯，制备得到抗菌薄膜。

Claims (1)

1.聚羟基丁酸酯抗菌薄膜的制备方法，其特征在于：包括如下步骤：
（1）制备海因钠盐
取0.1 mol 5，5-二甲基海因，加入150mL乙醇使其溶解，然后加入0.1 mol氢氧化钠，油浴环境下不断搅拌至完全溶解，90℃反应10min，旋转蒸发去除溶剂，制备得到的海因钠盐于45℃真空干燥；
（2）制备SPH
将海因钠盐溶于150mL DMF，加入0.1molγ-氯丙基三乙氧基硅烷，95~100℃回流反应8h；反应结束后，过滤除去NaCl副产物，减压除去溶剂，得到产物SPH；
（3）制备PSPH
配置质量比为2∶1∶2的SPH/乙醇/水混合溶液，用稀HCl调节pH值至3.4~5.5，85℃冷凝回流5h，加热去除水和乙醇，得到玻璃状透明固体，即为PSPH；
（4）PHB/PSPH 复合薄膜的制备
称取PHB 和PSPH并分别溶解于CHCl3和DMF 中混合后搅拌至均一溶液，将溶液缓慢倾倒入模具中，室温下挥发24h 成膜，于真空烘箱中干燥至恒重；
（5）氯化、滴定
取质量分数为10％的次氯酸钠水溶液，室温下将样品浸渍1h；结束后用去离子水洗涤，于45℃烘箱中烘1h 以去除样品中残留的自由氯，制备得到抗菌薄膜。
CN201611015054.0A 2016-11-18 2016-11-18 聚羟基丁酸酯抗菌薄膜的制备方法 Pending CN106519615A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611015054.0A CN106519615A (zh) 2016-11-18 2016-11-18 聚羟基丁酸酯抗菌薄膜的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611015054.0A CN106519615A (zh) 2016-11-18 2016-11-18 聚羟基丁酸酯抗菌薄膜的制备方法

Publications (1)

Publication Number Publication Date
CN106519615A true CN106519615A (zh) 2017-03-22

Family

ID=58352670

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611015054.0A Pending CN106519615A (zh) 2016-11-18 2016-11-18 聚羟基丁酸酯抗菌薄膜的制备方法

Country Status (1)

Country Link
CN (1) CN106519615A (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112679925A (zh) * 2020-12-22 2021-04-20 中国农业科学院植物保护研究所 一种复合抗菌膜及其制备方法与应用
CN116535859A (zh) * 2023-07-06 2023-08-04 汕头市永昌钦发针织实业有限公司 一种柔性亲肤硅胶及其制备方法和在硅胶内衣中的应用

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112679925A (zh) * 2020-12-22 2021-04-20 中国农业科学院植物保护研究所 一种复合抗菌膜及其制备方法与应用
CN112679925B (zh) * 2020-12-22 2021-11-23 中国农业科学院植物保护研究所 一种复合抗菌膜及其制备方法与应用
CN116535859A (zh) * 2023-07-06 2023-08-04 汕头市永昌钦发针织实业有限公司 一种柔性亲肤硅胶及其制备方法和在硅胶内衣中的应用
CN116535859B (zh) * 2023-07-06 2023-08-25 汕头市永昌钦发针织实业有限公司 一种柔性亲肤硅胶及其制备方法和在硅胶内衣中的应用

Similar Documents

Publication Publication Date Title
Gao et al. Electrospun antibacterial nanofibers: Production, activity, and in vivo applications
Lin et al. Polyphenol-driving assembly for constructing chitin-polyphenol-metal hydrogel as wound dressing
Zargar et al. A review on chitin and chitosan polymers: structure, chemistry, solubility, derivatives, and applications
Agnihotri et al. Development of nano-antimicrobial biomaterials for biomedical applications
CN106048892B (zh) 一种载有纳米银粒子的go/sa/pva复合纳米纤维膜的制备方法
Arora et al. Polymer based antimicrobial coatings as potential biomaterial: A review
Valle Mendoza et al. Electrospun biodegradable polymers loaded with bactericide agents
CN107595878A (zh) 一种壳聚糖‑植酸钠纳米颗粒及其制备方法和抑菌剂
CN108066805A (zh) 一种ε-聚赖氨酸仿生抑菌膜及其制备和应用
ES2850125T3 (es) Sistema antimicrobiano, insecticida y acaricida
CN107670506A (zh) 一种水过滤用抗菌耐污染的pvdf超滤膜的制备方法
CN109206645A (zh) 一种可食性涂膜及其制备方法
CN104098831B (zh) 一种无迁移抗菌聚烯烃膜及其制备方法
Dhiman et al. Silver-based polymeric nanocomposites as antimicrobial coatings for biomedical applications
Li et al. Biocidal poly (vinyl alcohol) films incorporated with N-halamine siloxane
CN106519615A (zh) 聚羟基丁酸酯抗菌薄膜的制备方法
Pihl et al. Osseointegration and antibacterial effect of an antimicrobial peptide releasing mesoporous titania implant
JP2017510648A (ja) 感染の処置での使用のための治療剤
CN104857556A (zh) 一种化学接枝型长效缓释抗菌真丝缝合线及其制备方法
Bazaka et al. Surface modification of biomaterials for biofilm control
CN103933617B (zh) 一种具有抗细菌粘附的气管导管的制备方法
Vineis et al. Natural polymer-based electrospun fibers for antibacterial uses
CN105254913A (zh) 一种表面兼有抗菌性和生物相容性的聚酯材料及制备与应用
CN107875865A (zh) 一种水过滤用抗菌耐污染的pvdf超滤膜
Santos et al. Production of medical grade silicone for facial prosthesis with bactericidal properties from the inclusion of poly (diallyldimethylammonium chloride): An in vitro study

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170322

WD01 Invention patent application deemed withdrawn after publication