Summary

缓释碱源负载碱性过氧化氢体系中苎麻纤维的提取

Published: February 06, 2018
doi:

Summary

本文介绍了一种在受控释碱源支持的碱性过氧化氢体系中提取苎麻纤维的方案。

Abstract

本协议演示了一种在受控释碱源支持的碱过氧化氢系统中, 在苎麻纤维上精练的方法。苎麻提取纤维是一种重要的纺织材料。在以前的研究中, 苎麻纤维被提取的碱过氧化氢系统只支持氢氧化钠。然而, 由于氢氧化钠的强碱性, 过氧化氢的氧化反应速度难以控制, 从而对处理后的纤维造成很大的损害。在本协议中, 一种由氢氧化钠和氢氧化镁组成的控释碱源, 用于提供碱性条件和缓冲碱氢 peroxidesystem 的 pH 值。氢氧化镁的取代率可以调节过氧化氢体系的 pH 值, 对纤维性能有很大的影响。ph 值和氧化还原电位值, 代表了碱过氧化氢系统的氧化能力, 分别采用 ph 计和检测仪进行监测。采用高锰酸钾4滴定法测定了萃取过程中碱过氧化氢体系中的剩余过氧化氢含量, 以及纤维萃取后废水的化学需氧量 (COD) 值。用精密电子天平测量纤维的收率, 用化学分析法测定纤维的残余牙龈。用乌粘度计测定了纤维的聚合度 (PD 值)。用纤维强度仪测定纤维的拉伸性能, 包括韧性、伸长率和断裂。利用傅里叶变换红外光谱和 X 射线衍射对纤维的官能团和晶体性质进行了表征。该方案证明, 控释碱源能改善碱性过氧化氢体系中提取的纤维的性能。

Introduction

苎麻, 俗称 “中国草”, 是一种多年生草本植物, 其纤维可作为纺织工业的优良材料1,2。它是中国原产的主要经济作物之一;中国苎麻产量占世界总产量的90% 以上1,2。苎麻纤维是最强和最长的植物纤维之一, 光泽与几乎柔滑的外观3,4。苎麻纤维长的长度使其适合于单纤维纺丝, 在麻纤维中很少见到。苎麻纤维织物具有冷却、抗菌、导热性能优异、透气性好等优点,3,4

纤维素是苎麻纤维的主要成分, 苎麻中的其他成分如果胶、木质素、水溶性物质等, 被定义为牙龈5,6。苎麻纤维可通过溶于含有化学试剂的溶液中的牙龈来提取, 该过程定义为脱胶5,6。主要有两种苎麻纤维提取方法: 化学脱胶和生物脱胶。传统化学脱胶工艺中脱胶废水的能耗、时间消耗和 COD 值都比较高, 在高压下用浓碱液精练法提取纤维素纤维6至 8 h7,8.另外, 生物脱胶是苎麻纤维提取的一种环保选择。然而, 苛刻的反应条件和先进的设备抑制其进一步的工业应用9,10。因此, 用碱过氧化氢进行氧化脱胶, 提出了一种有价值的、可供选择的应用重点, 因为它需要较短的脱胶时间和较低的脱胶温度11,12。然而, 由于过氧化物的强氧化能力, 在脱胶过程中可能会发生大量的纤维素降解, 这会对纤维性能造成很大的损害13,14。这是苎麻碱氧化脱胶的最大缺点。

在以前的研究中, 苎麻纤维被提取的碱过氧化氢系统只支持氢氧化钠15。然而, 由于氢氧化钠的强碱性, 过氧化氢的氧化反应速度难以控制, 从而对处理后的纤维7造成很大的损害。为了改善苎麻纤维的性能, 本研究采用氢氧化钠和氢氧化镁组成的控释碱源, 为碱性过氧化氢系统的 pH 值提供了一个碱条件和缓冲剂16,17

这项技术背后的基本原理可以描述如下。氢氧化镁在蒸馏水中略有溶解性, 它可以用 OH的消耗逐渐溶入脱胶溶液, 并使脱胶液的 pH 值和氧化能力保持在适当的范围内18。氢氧化镁的取代率 (SR) 被定义为氢氧化镁在总碱用量为10% 时所取代的氢氧化钠的摩尔比例, 并可通过以下公式计算替代率。此外, Mg2 +可以防止过度氧化导致的纤维素降解,19,20

Equation 1

在这里, M2 (g) 是重量的 Mg (OH)2, M1 (g) 是氢氧化钠的重量, 40 是氢氧化钠的分子量, 58 是分子量的 mg (oh)2, 2 是在 mg (oh)2中的 “职业” 的数量, 而 SR 是替代率。

本协议的技术可以推广到碱式过氧化氢系统中的植物材料的提取、漂白和改性。然而, 必须指出的是, 碱性过氧化氢系统的 pH 值和反应温度的选择是这项技术的关键21。碱性过氧化氢系统的 pH 值可以通过改变置换率17来调整。碱过氧化氢体系的 pH 值和氧化能力随取代率的增加而降低。当反应温度设定在85° c 时, 自由基反应在系统中起主要作用, 系统的强氧化性适合于溶解物料;当反应温度设定在125° c 时, 自由基反应被抑制, 系统中存在大量的呼出, 使系统适合漂白19

Protocol

1. 苎麻的氧化脱胶 氧化脱胶液的制备 溶解 2 g H2O2, 1 克碱 (混合镁 (OH)2和氢氧化钠), 0.4 克 Na5P3O10, 0.1 克蒽醌和0.2 克 HEDP 在100毫升蒸馏水中做脱胶解决方案。 苎麻的氧化脱胶 在脱胶液中浸泡10克生苎麻, 并在85° c 下冲刷60分钟。 将温度提高到125° c (压力为0.6 公斤), 再冲刷60?…

Representative Results

研究了在蒸馏水和脱胶溶液中 Mg (OH)2的溶解度 (图 1)。测试了镁 (OH)2取代率对脱胶溶液 pH 值和可解性值 (图 2) 的影响。用不同 Mg (OH)2替代率计算了纤维脱胶的脱胶率和残余牙龈 (图 3)。用 DP 值、结晶度、纤维拉伸性能 (图 4) 和废水 COD 值 (图 5<…

Discussion

Mg (OH)2的设置取代率和反应温度是该协议的重点。Mg (OH)2取代率可以影响脱胶溶液的 pH 值和氧化能力。最好的 Mg (OH)2替代率苎麻脱胶是 20%, 因为纤维素不能得到足够的保护下的替代率低于 20%, 和过量的剩余牙龈 (低 DP 值和结晶度) 将保留在纤维低于 20% (图 4A) 的替代率。

反应温度会影响过氧化氢的反应途径。苎麻氧化脱胶过程中?…

Disclosures

The authors have nothing to disclose.

Acknowledgements

这项工作得到了中国农业科学与技术创新研究院 (grant CARS-19)、中国农业科技学院 (ASTIP-IBFC07)、创新基金 (赠款号) 等专项基金的支持。为东华大学研究生 (格兰特号 16D310107), “小萍科技创新团队” (产业化综合研究 & 开发的麻纤维生物脱胶), 中国奖学金委员会。

Materials

Hydrogen peroxide, 30% Fisher Scientific H325-100 Chemical for degumming
Magnesium hydroxide, 99% Fisher Scientific AA1236722 Chemical for degumming
Sodium hydroxide Fisher Scientific S318-1 Chemical for degumming
Sodium bisulfite Fisher Scientific S654-500 Chemical for degumming
Sodium tripolyphosphate Fisher Scientific AC218675000 Chemical for degumming
Anthraquinone, >98% Fisher Scientific AC104930500 Chemical for degumming
1-Hydroxy Ethylidene-1,1-Diphosphonic Acid Fisher Scientific 50-901-10243 Chemical for degumming
Degumming oil Minglong auxiliaries limited liability company, Yiyang, Hunan,China —— Chemical for degumming
Ethyl alcohol Fisher Scientific A962-4 Chemical for testing
Benzene Fisher Scientific AA43817AE Chemical for testing
Copper wire,0.5mm (0.02in) dia Fisher Scientific AA10783H4 Chemical for testing
Cupriethylenediamine solution 1mol/L Fisher Scientific 24991 Chemical for testing, caution toxic
Nitric acid (65% ~68% ) Fisher Scientific A200-612GAL Chemical for testing, caution
Ethylenediamine Fisher Scientific AC118420100 Chemical for testing
Potassium permanganate Fisher Scientific P279-500 Chemical for testing
Sulphuric acid Fisher Scientific A300C-212 Chemical for testing
Silver sulfate Fisher Scientific S190-25 Chemical for testing
Raw ramie Guangyuan limited liability company, Changde, Hunan,China —— Raw materials
Electric-heated thermostatic water bath Senxin Experiment equipment limited liability company,Shanghai,China DK-S28 Equipments for degumming
High temperature lbaorator dyeing machine Shanghai Longda chemcials Crop. RY-1261 Equipments for degumming
Thermometer Sichuan Shubo (group)Co.,Ltd 100 °C Equipments for degumming
Vacuum suction machine Yukang KNET ,Shanghai,China SHB-IIIA Equipments for testing Mg(OH)2 solublity
Suction flask Sichuan Shubo (group)Co.,Ltd 1000mL Equipments for testing Mg(OH)2 solublity
Sand-core funnels Sichuan Shubo (group)Co.,Ltd 35mL Equipments for testing Mg(OH)2 solublity
Oxidation reduction potential meter Dapu instrument, Shanghai, China MODEL 421 Equipments for testing ORP value
pH meter Hanna instruments,Beijing,China HI 98129 Equipments for testing pH value
Acid burette Sichuan Shubo (group)Co.,Ltd 50mL Equipments for testing H2O2 content
Flask Sichuan Shubo (group)Co.,Ltd 250mL/500mL Equipments for testing H2O2 content;  residual gums content
Electric furnace Jiangyi Experiment instruments limited liability company,Shanghai,China 800-2000W Equipments for testing residual gums content
Reflux condensing tube Sichuan Shubo (group)Co.,Ltd 250mL Equipments for testing residual gums content; COD value
Fiber cutter (40mm) Changzhou No.2 Textile Machine Co.,Ltd Y171A Equipments for testing fiber density
Ostwald viscometer Taizhou, jiaojiang, glass instruments company 0.6mm Equipments for testing fiber PD value
Spherical fat extractor Sichuan Shubo (group)Co.,Ltd 250mL Equipments for testing fiber PD value
Soxhlet extractor Sichuan Shubo (group)Co.,Ltd 250mL Equipments for testing fiber PD value
Torsion balance Liangping instrucments Co.,Ltd,Shanghai, China JN-B Equipments for testing fiber density
Fiber strength instrument Xinxian instruments, shanghai,China XQ-2 Equipments for testing fiber tensile property
Tension clamp Depu textile technology Co.,Ltd, Changzhou, jiangsu, China 0.3cN/dtex Equipments for testing fiber tensile property
COD thermostatic heater Qiangdao Xuyu environment protection technology Lit company DL-801A Equipments for testing COD value
FTIR Thermo Fisher, America Nicolet FTIR analysis
XRD Rigaku, Japan D/max-2550 PC XRD analysis
Electronic balance Shanghai jingtian Electronic instrument Co.,Ltd FA2004A Generral equipments
Drying oven Tonglixinda  instruments, Tianjin,China 101-2AS Generral equipments
Weighing bottle Sichuan Shubo (group)Co.,Ltd 50×30 Generral equipments
Beaker Sichuan Shubo (group)Co.,Ltd 500mL Generral equipments
Sample sieve Xiaojin hardware instruments Co.,Ltd, Shangyu, Zhejiang 120 mesh Generral equipments
Glass rod Sichuan Shubo (group)Co.,Ltd —— Generral equipments
Cylinder Sichuan Shubo (group)Co.,Ltd 250mL, 50mL Generral equipments
Pipette Sichuan Shubo (group)Co.,Ltd 5mL, 10mL Generral equipments
Rubber suction bulb Sichuan Shubo (group)Co.,Ltd —— Generral equipments
Orign OriginLab 8.0 Software for figure drawing

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Cite This Article
Meng, C., Li, Z., Wang, C., Yu, C., Bi, X., Wang, S. Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source. J. Vis. Exp. (132), e56461, doi:10.3791/56461 (2018).

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