CN110552253A - 一种高耐折、超平滑、高雾度的透明全纤维素复合薄膜及其制备方法 - Google Patents

一种高耐折、超平滑、高雾度的透明全纤维素复合薄膜及其制备方法 Download PDF

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CN110552253A
CN110552253A CN201810538255.1A CN201810538255A CN110552253A CN 110552253 A CN110552253 A CN 110552253A CN 201810538255 A CN201810538255 A CN 201810538255A CN 110552253 A CN110552253 A CN 110552253A
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composite film
cellulose
holocellulose
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CN110552253B (zh
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方志强
胡稳
陈港
刘宇
宁洪龙
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South China University of Technology SCUT
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Abstract

本发明公开了一种高耐折、超平滑、高雾度的透明全纤维素复合薄膜及其制备方法。该方法如下：（1）以木质纤维为原料，通过纤维疏解、纸页成型、干燥，形成纤维交织网络结构；（2）将纤维素及纤维素衍生物溶于水中形成纤维素溶液；（3）通过浸渍或涂布，将纤维素溶液填充到纤维交织网络结构中，形成全纤维素复合薄膜；（4）将全纤维素复合薄膜贴于玻璃表面，再干燥得全纤维素复合薄膜。该全纤维素复合薄膜的耐折度为2000~4000次，抗张强度为90~160MPa，表面粗糙度为0.5~1纳米，在550纳米的可见光区透光率为88~91%，在550纳米的雾度为60‑85%，在LED照明、平板显示、光伏器件领域有潜在的应用前景。

Description

一种高耐折、超平滑、高雾度的透明全纤维素复合薄膜及其制 备方法
技术领域
本发明属于透明全纤维素复合薄膜领域，尤其涉及一种高耐折、超平滑、高雾度的透明全纤维素复合薄膜及其制备方法。
背景技术
高雾度高透明纤维素基薄膜是一种适用于光电器件的新型衬底材料，具有可生物降解、可再生、价格低廉、性能可调等优点，有望推动光电器件朝着柔性、低成本、可降解的方向发展。[Zhu H, Luo W, Ciesielski P N, et al. Wood-derived materials forgreen electronics, biological devices, and energy applications[J]. Chemicalreviews, 2016, 116(16): 9305-9374.]。现有制备高雾度高透明纤维素基薄膜的方法主要有：（1）以TEMPO氧化浆为原料，通过真空过滤和干燥制备而成 [Fang Z, Zhu H, YuanY, et al. Novel nanostructured paper with ultrahigh transparency andultrahigh haze for solar cells[J]. Nano letters, 2014, 14(2): 765-773。（2）将石油基透明树脂浸渍到复印纸中制备而成[Yao Y, Tao J, Zou J, et al. Lightmanagement in plastic–paper hybrid substrate towards high-performanceoptoelectronics[J]. Energy & Environmental Science, 2016, 9(7): 2278-2285.]；（3）通过部分溶解纸张内部纤维的表面，实现溶解纤维素对多孔纤维交织网络的填充[ZhuH, Fang Z, Wang Z, et al. Extreme light management in mesoporous woodcellulose paper for optoelectronics[J]. ACS nano, 2015, 10(1): 1369-1377.]；（4） 通过对木片进行脱木素处理，然后进行加压制备而成[Zhu M, Wang Y, Zhu S, etal. Anisotropic, transparent films with aligned cellulose nanofibers[J].Advanced Materials, 2017, 29(21).
但是上述方法在实现优异光学性能的同时，却难以兼顾制备效率、高的力学性能（尤其是耐折性）和高平滑度。因此开发出既能获得优异的光学性能，又能获得优良的力学性能和表面性能的高效制造技术，不仅有利于推动高雾度高透明纤维素基薄膜的规模化、低成本的制造，同时有助于拓宽纤维素薄膜的应用领域。
发明内容
本发明的目的在于克服现有技术的不足和缺点，提供一种高耐折、超平滑、高雾度透明全纤维素复合薄膜及其制备方法。
本发明的目的通过以下技术方案实现。
一种高耐折、超平滑、高雾度透明全纤维素复合薄膜及其制备方法，所述制备方法包括以下步骤：
（1）以微米级的木质纤维为原料，通过纤维疏解、纸页成型、干燥三道工序，形成三维多孔纤维交织网络结构，并以此为骨架，赋予复合薄膜高的雾度和优异的力学性能；
（2）将分子级纤维素或其衍生物溶于水中形成纤维素溶液，经过400目的聚酯网过滤，去除大尺寸的纤维素基原料，并以此为填充物，赋予复合薄膜高的透光率和高的平滑度；
（3）通过浸渍或涂布工艺，将步骤（1）中的木质纤维素形成三维多孔纤维交织网络结构与步骤（2）中的分子级纤维素及其衍生物相结合形成高雾度透明全纤维素复合薄膜；
（4）将步骤（3）中的薄膜贴于玻璃表面，进行干燥获得高耐折、超平滑、高雾度透明全纤维素复合薄膜。
进一步优化地，步骤（1）中微米级的木质纤维为针叶木浆、阔叶木浆、非木浆、废纸浆、绒毛浆和棉浆中任一种。其打浆度介于12~40 °SR。
进一步优化地，步骤（1）中纤维交织网络结构的定量为15~60 g/m2。其作用是为复合薄膜提供优异的力学性能和高雾度。
进一步优化地，步骤（2）中纤维素衍生物为甲基纤维素、羧甲基纤维素、羟乙基纤维素、羟丙基纤维素和羟丙基甲基纤维素中任何一种。其作用是为复合薄膜提供优异的透光率和高的平滑度。
进一步优化地，步骤（2）中纤维素衍生物的分子量为9000~700000 D。
进一步优化地，步骤（2）中纤维素溶液质量浓度0.5%~2%。
进一步优化地，步骤（3）所述纤维素溶液与纤维交织网络结构的质量比介于7:3和9:1之间。
进一步优化地，步骤（4）中干燥温度为38~100 ℃。
进一步优化地，步骤（4）中干燥时间为2~8 h。
由上述的制备方法制得一种高耐折、超平滑、高雾度透明全纤维素符合薄膜，该全纤维素复合薄膜的耐折度为2000~4000次，抗张强度为90~160MPa，表面粗糙度为0.5~1纳米，在550纳米的可见光区透光率为88~91%，在550纳米的雾度为60~85%。
本发明以微米级木质纤维为原料，通过纤维疏解、纸页成型、干燥三道工序，形成均匀的三维多孔纤维交织网络结构，并以此为骨架，赋予透明全纤维素复合薄膜优异的力学性能和高的雾度；将分子级纤维素及其衍生物溶解于水中形成水溶液，并以此为填充物，赋予透明全纤维素复合薄膜优异的透光率和高的平滑度；再通过浸渍或涂布工艺，将分子级纤维素及其衍生物填充到三维多孔木质纤维交织网络中，形成全纤维素复合薄膜；最后将上述复合薄膜贴于玻璃表面，进行干燥获得高耐折、超平滑、高雾度透明全纤维素复合薄膜。
与现有技术相比，本发明的有益效果如下：
（1）本发明提出的高耐折、超平滑、高雾度的透明全纤维素复合薄膜制备方法，显著改善了薄膜的力学性能，尤其是耐折度提高到2000次以上；
（2）本发明提出的高耐折、超平滑、高雾度的透明全纤维素复合薄膜制备方法，使复合薄膜获得了超平滑的表面。
（3）本发明所采用的纸页成型和纸张后加工技术简便，大大降低了薄膜的制造成本。该高耐折、超平滑、高雾度的透明全纤维素复合薄膜在LED照明、平板显示、光伏器件领域有潜在的应用前景。
具体实施方式
以下结合具体实例来对本发明作进一步说明，但本发明说要求保护的范围并不局限于实施例所涉及之范围。
下述实施例中，纤维素薄膜的透光率和雾度根据GB/T 2410-2008国家标准测定；耐折度采用GB/T 457—2008国家标准测试；拉伸强度测试采用GB/T1040—2006国家标准测试；表面粗糙度利用原子力显微镜表征。
实施例1
纤维素衍生物溶液的制备：分别称量8 g分子量为90000 D的甲基纤维素（MC）、792 g去离子水，先将去离子水加入到烧杯中升温至85 ℃，在1000 rpm搅拌速度下加入MC，继续搅拌1 h，冷却至室温，使用滤网进行过滤得到质量浓度为1%的MC溶液。
纤维交织网络结构的制备；疏解针叶木浆（打浆度20 °SR），抄造定量为15 g/m2，风干处理得到纤维交织网络结构。
全纤维素复合薄膜的制备：通过浸渍工艺，将423.9 g质量浓度为1%的MC溶液和15g/m2的纤维交织网络结构充分结合，MC溶液与纤维交织网络结构的质量比9:1，得到全纤维素复合薄膜。
全纤维素复合薄膜的干燥：将全纤维素复合薄膜放置在温度40℃，湿度70%下干燥3 h。
通过以上步骤得到的全纤维素复合薄膜，其耐折度为2200次，抗张强度为92 MPa，表面粗糙度为0.6纳米，可见光区透光率为91%（550纳米），雾度为60%（550纳米）。
实施例2
纤维素衍生物溶液的制备：分别称量6 g分子量为700000 D的羧甲基纤维素（CMC）、794g去离子水，先将去离子水加入到烧杯中，在1000 rpm搅拌速度下加入CMC，继续搅拌升温至72 ℃，时间2 h，冷却至室温，使用滤网进行过滤得到质量浓度为0.75%的CMC溶液。
纤维交织网络结构的制备；疏解阔叶木浆（打浆度20 °SR），抄造定量为15 g/m2，风干处理得到纤维交织网络结构。
全纤维素复合薄膜的制备：通过浸渍工艺，146.5 g质量浓度为0.75%的CMC溶液和15 g/m2的纤维交织网络结构充分结合，CMC溶液与纤维交织网络结构的质量比7:3，得到全纤维素复合薄膜。
全纤维素复合薄膜的干燥：将全纤维素复合薄膜放置在温度40℃，湿度70%下干燥3 h。
通过以上步骤得到的全纤维素复合薄膜，其耐折度为4000次，抗张强度为90 MPa，表面粗糙度为0.6纳米，可见光区透光率为91%（550纳米），雾度为60%（550纳米）。
实施例3
纤维素衍生物溶液的制备：分别称量6 g分子量为700000 D的羟乙基纤维素（HEC）、794g去离子水，将去离子水加入到烧杯中，在1000 rpm搅拌速度下加入HEC，搅拌1 h，使用滤网进行过滤得到质量浓度为0.75%的HEC溶液。
纤维交织网络结构的制备；疏解阔叶木浆（打浆度20 °SR），抄造定量为60 g/m2，风干处理得到纤维交织网络结构。
全纤维素复合薄膜的制备：通过浸渍工艺，586.1 g质量浓度为0.75%的HEC溶液和60 g/m2的纤维交织网络结构充分结合，HEC溶液与纤维交织网络结构的质量比7:3，得到全纤维素复合薄膜。
全纤维素复合薄膜的干燥：将全纤维素复合薄膜放置在温度40℃，湿度70%下干燥3 h。
通过以上步骤得到的全纤维素复合薄膜，其耐折度为2000次，抗张强度为130MPa，表面粗糙度为0.8纳米，可见光区透光率为89%（550纳米），雾度为85%（550纳米）。
实施例4
纤维素衍生物溶液的制备：分别称量16 g分子量为90000 D的羟丙基纤维素（HPC）、784g去离子水，将去离子水加入到烧杯中，在1000 rpm搅拌速度下加入HPC搅拌2 h，使用滤网进行过滤得到质量浓度为2%的HPC溶液。
纤维交织网络结构的制备；疏解针叶木浆（打浆度20 °SR），抄造定量为60 g/m2，风干处理得到纤维交织网络结构。
全纤维素复合薄膜的制备：通过浸渍工艺，219.8 g质量浓度为2%的HPC溶液和60g/m2的纤维交织网络结构充分结合，HPC溶液与纤维交织网络结构的质量比7:3，得到全纤维素复合薄膜。
全纤维素复合薄膜的干燥：将全纤维素复合薄膜放置在温度40℃，湿度70%下干燥3 h。
通过以上步骤得到的全纤维素复合薄膜，其耐折度为2050次，抗张强度为150MPa，表面粗糙度为0.7纳米，可见光区透光率为88%（550纳米），雾度为85%（550纳米）。
实施例5
纤维素衍生物溶液的制备：分别称量6 g分子量为90000 D的羟丙基甲基纤维素（HPMC）、794 g去离子水，先将去离子水加入到烧杯中，在1000 rpm搅拌速度下加入HPMC，继续搅拌升温至72 ℃，时间2 h，冷却至室温，使用滤网进行过滤得到质量浓度为0.75%的HPMC溶液。
纤维交织网络结构的制备；疏解针叶木浆（打浆度30 °SR），抄造定量为30 g/m2，风干处理得到纤维交织网络结构。
全纤维素复合薄膜的制备：通过浸渍工艺，502.4 g质量浓度为0.75%的HPMC溶液和30 g/m2的纤维交织网络结构充分结合，HPMC溶液与纤维交织网络结构的质量比4:1，得到全纤维素复合薄膜。
全纤维素复合薄膜的干燥：将全纤维素复合薄膜放置在温度40℃，湿度70%下干燥3 h。
通过以上步骤得到的全纤维素复合薄膜，其耐折度为4000次，抗张强度为140MPa，表面粗糙度为0.9纳米，可见光区透光率为90%（550纳米），雾度为72.5%（550纳米）。

Claims (10)

1.一种高耐折、超平滑、高雾度的透明全纤维素复合薄膜的制备方法，其特征在于，包括以下制备步骤：
（1）以微米级的木质纤维为原料，通过纤维疏解、纸页成型、干燥三道工序，形成均匀的三维多孔纤维交织网络结构；
（2）将分子级纤维素或纤维素衍生物溶解于水中形成纤维素溶液；
（3）通过浸渍或涂布工艺，将步骤（2）中的纤维素溶液填充到步骤（1）中的三维多孔纤维交织网络结构中，形成全纤维素复合薄膜；
（4）将步骤（3）中的全纤维素复合薄膜贴于玻璃表面，通过干燥获得高耐折、超平滑、高雾度的透明全纤维素复合薄膜。
2.根据权利要求1所述的制备方法，其特征在于：步骤（1）所述微米级的木质纤维为针叶木浆、阔叶木浆、非木浆、废纸浆、绒毛浆和棉浆中任一种。
3.根据权利要求1所述的制备方法，其特征在于：步骤（1）所述微米级的木质纤维的打浆度为12~40°SR。
4.根据权利要求1所述的制备方法，其特征在于：步骤（1）所述纤维交织网络结构的定量为15~60 g/m2。
5.根据权利要求1所述的制备方法，其特征在于：步骤（2）所述纤维素衍生物为甲基纤维素、羧甲基纤维素、羟乙基纤维素、羟丙基纤维素和羟丙基甲基纤维素中任何一种。
6.根据权利要求1所述的制备方法，其特征在于：步骤（2）所述纤维素衍生物的分子量为9000~700000 D。
7.根据权利要求1所述的制备方法，其特征在于：步骤（2）所述纤维素溶液的质量浓度0.5%~2%。
8.根据权利要求1所述的制备方法，其特征在于：步骤（3）所述纤维素溶液与纤维交织网络结构的质量比为7:3-9:1。
9.根据权利要求1所述的制备方法，其特征在于：步骤（4）所述干燥的温度为38~100℃，干燥的时间为2~8 h。
10.由权利要求1-9任一项所述的制备方法制得的一种高耐折、超平滑、高雾度的透明全纤维素复合薄膜，其特征在于：该全纤维素复合薄膜的耐折度为2000~4000次，抗张强度为90~160MPa，表面粗糙度为0.5~1纳米，在550纳米的可见光区透光率为88~91%，在550纳米的雾度为60~85%。
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