具有温敏性的Diatomite@PNIPAm稳定Pickering乳液的制备及表征

Preparation and research of Diatomite@PNIPAm-stabilized Pickering emulsion with temperature responsiveness

  • 摘要: 针对由表面活性剂所稳定的乳液具有毒性且不环保的缺点,对硅藻土颗粒(Diatomite,DE)进行改性,并对其所制备的具有温度响应性的Pickering乳液进行了研究。由于硅藻土颗粒具有生物相容性好的优势,在化妆品和制药领域具有应用潜力。先通过硅烷偶联剂(MPS)疏水改性DE得到Diatomite@MPS,再接枝温敏型聚合物聚N-异丙基丙烯酰胺(PNIPAm),成功合成了具有温度响应性的改性硅藻土颗粒(Diatomite@PNIPAm)。由TGA结果表明制备Diatomite@PNIPAm的最佳MPS与NIPAm摩尔比为1∶1。随后,将Diatomite@PNIPAm作为乳化剂分别在不同浓度的条件下制备了水包油(O/W)型Pickering乳液,确定了3.0wt%为最佳浓度。此外,确定Diatomite@PNIPAm浓度后,分别从1∶9到9∶1的不同油水体积比制备乳液,结果表明油水体积比为7∶3时最佳。通过差示扫描量热仪(DSC)测定所制备的Pickering乳液的低临界溶解温度(LCST)为40℃,且乳液至少可以进行6次破乳-再乳化循环,具备良好的破乳-再乳化循环性能。

     

    Abstract: Aiming at the shortcomings of the emulsion stabilized by surfactant due to toxicity and non-environmental protection, modified diatomite particles (DE), the temperature-responsive Pickering emulsion was studied. Due to the advantages of superior biocompatibility, DE have application potential in the field of cosmetics and pharmaceuticals. First, the Diatomite@MPS was obtained by silane coupling agent (MPS) hydrophobic modified DE. Then, modified DE (Diatomite@PNIPAm) with temperature responsiveness was synthesized successfully by grafting the temperature-responsive polymer poly N-isopropylacrylamide (PNIPAm). According to the characterization results of FTIR testing and water contact angle testing, the diatomaceous earth was modified successfully. The TGA results showed that the optimal molar ratio of the Diatomite@PNIPAm prepared from MPS to NIPAm was 1∶1. Subsequently, oil-in-water (O/W) Pickering emulsions were prepared with Diatomite@PNIPAm as an emulsifier at different concentrations, and 3.0wt% was determined as the optimal concentration. In addition, the emulsion was prepared with different oil-water volume ratios from 1∶9 to 9∶1 after determining the Diatomite@PNIPAm concentration, and the results showed that the oil-water volume ratio was 7∶3 as the best. The characterization results of differential scanning calorimeter (DSC) testing showed that the lower critical solution temperature (LCST) of the Pickering emulsion was 40℃. The emulsion can undergo at least 6 demulsification-reemulsification cycles, and possesses excellent demulsification-reemulsification cycle performance.

     

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