Name: extraction of ramie fiber in alkali hydrogen peroxide system supported by controlled-release alkali source
Uploaded: 2018-02-06T13:30:00
Description: Watch this Scientific Journal Video about Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source at JoVE.com

This work was supported by the earmarked fund for China Agriculture Research System for Bast and Leaf Fiber Crops (grant number CARS-19), The China Academy of Agricultural Science and Technology Innovation Project (grant number ASTIP-IBFC07), The innovation fund for graduate students in Donghua University (grant number 16D310107), The &#39;Xiaoping science and technology innovation team&#39; (industrialization integrated R &#38; D group of bast fiber biological degumming), China Scholarship Council.

1. Oxidation Degumming of Ramie
<ol>
	<li>Preparing the oxidation degumming solution
	<ol>
		<li>Dissolve 2 g H2O2, 1 g alkali (a mixture of Mg(OH)2 and NaOH), 0.4 g Na5P3O10, 0.1 g anthraquinone, and 0.2 g HEDP in 100 mL distilled water to make the degumming solution.</li>
	</ol>
	</li>
	<li>Oxidation degumming of ramie
	<ol>
		<li>Immerse 10 g raw ramie in the degumming solution and scour it under 85 &#176;C for 60 min...

<ol>
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R., Li, Z. L., Wang, C. Y., Yu, C. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Alkali+Source+Used+in+the+Oxidation+Degumming+of+Ramie.">Alkali Source Used in the Oxidation Degumming of Ramie.</a> Text Res J. 87 (10), 1155-1164 (2017).</li><li>Gorski, D., Engstrand, P., Hill, J., Axelsson, P., Johansson, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mg(OH)2-based+hydrogen+peroxide+refiner+bleaching:+influence+of+extractives+content+in+dilution+water+on+pulp+properties+and+energy+efficiency.">Mg(OH)2-based hydrogen peroxide refiner bleaching: influence of extractives content in dilution water on pulp properties and energy efficiency.</a> Appita Journal. 63 (3), 218-225 (2010).</li><li>Leduc, C., Martel, J., Danea, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Efficiency+and+effluent+characteristic+from+Mg(OH)2-based+hydrogen+peroxide+bleaching+of+high-yield+pulps+and+deinked+pulp.">Efficiency and effluent characteristic from Mg(OH)2-based hydrogen peroxide bleaching of high-yield pulps and deinked pulp.</a> Cellulose Chemistry &amp; Technology. 44 (7-8), 271-276 (2010).</li></ol>

The setting of Mg(OH)2 substitution rate and reaction temperature was the key point of this protocol. Mg(OH)2 substitution rate can influence the pH value and thus oxidation ability of degumming solution. The best Mg(OH)2 substitution rate for ramie degumming was 20%, because cellulose cannot receive enough protection under a substitution rate below 20%, and an excessive amount of residual gums (low DP value and crystallinity) would be retained in fiber under a substitution rate above 20%...

Ramie, commonly known as &#39;China grass&#39; is a perennial herb whose fiber can be used as an excellent material for the textile industry1,2. It is one of the main economic crops native to China; the production of ramie in China has accounted for more than 90% of the total yield in the world1,2. Ramie fiber is one of the strongest and longest plant fibers, lustrous with an almost silky appearance3,4. The long length of ramie fiber make it suitable for single fiber spinning, which is seldom seen in bast fiber. The textile made from ramie fiber possesses many excellent properties, such as coolness, antibacterial, excellent thermal conductivity, ventilation, etc.3,4
Cellulose is the main component of ramie fibers, and the other components in ramie, such as pectin, lignin, water soluble materials, are defined as gums5,6. Ramie fiber can be extracted by dissolving the gums in solution containing chemical reagents, in a process defined as degumming5,6. Mainly two approaches of ramie fiber extraction exist: chemical degumming and bio-degumming. The energy consumption, time consumption, and COD value of degumming wastewater in traditional chemical degumming is rather high, as cellulose fiber is extracted by scouring raw ramie in concentrated NaOH under high pressure for 6 to 8 h7,8. Alternatively, bio-degumming is an eco-friendly option for ramie fiber extraction. Nevertheless, the harsh reaction condition and sophisticated equipment inhibit its further industrial application9,10. Therefore, oxidation degumming with alkali hydrogen peroxide presents a valuable and alternative application to focus on, for it requires shorter degumming time and lower degumming temperature11,12. However, due to the strong oxidation ability of the peroxides, substantial cellulose degradation may occur during the degumming process, which can cause great damage to fiber properties13,14. This is the biggest drawback of alkali peroxide oxidation degumming of ramie.
In previous studies, ramie fiber was extracted in an alkali hydrogen peroxide system supported only by sodium hydroxide15. However, due to the strong alkalinity of sodium hydroxide, the oxidation reaction speed of hydrogen peroxide was difficult to control and thus resulted in great damage to the treated fiber7. To improve the properties of ramie fiber, a controlled-release alkali source, which is composed of sodium hydroxide and magnesium hydroxide, is used in this study to offer an alkali condition and buffer the pH value of alkali hydrogen peroxide system16,17.
The rationale behind this technology can be described as follows. Magnesium hydroxide is slightly soluble in distilled water, and it can dissolve gradually into the degumming solution with the consumption of OH- and keep the pH value and thus oxidation ability of degumming solution in an appropriate range18. The substitution rate (SR) of magnesium hydroxide is defined as the mole proportion of NaOH replaced by magnesium hydroxide under the total alkali dosage of 10%, and the substitution rate can be calculated by the following equation. Moreover, Mg2+ can prevent cellulose degradation caused by over oxidation19,20.
<img alt="Equation 1" src="/files/ftp_upload/56461/56461eq1.jpg" />
Here, M2 (g) is the weight of Mg(OH)2, M1 (g) is the weight of NaOH, 40 is the molecular weight of NaOH, 58 is the molecular weight of Mg(OH)2, 2 is the number of OHs in Mg(OH)2, and SR is the substitution rate.
The technology of this protocol can be extended to the extracting, bleaching, and modifying of plant materials in an alkali hydrogen peroxide system. However, it must be noted that the selection of pH value and reaction temperature of the alkali hydrogen peroxide system is key for this technology21. The pH value of the alkali hydrogen peroxide system can be adjusted by changing the substitution rate17. The pH value and thus oxidation ability of the alkali hydrogen peroxide system decrease with the increasing of substitution rate. When the reaction temperature is set at 85 &#176;C, the free radical reaction plays the main role in the system and the strong oxidation of the system is suitable for dissolving materials; when the reaction temperature is set at 125 &#176;C, the free radical reaction is inhibited and a large amount of HOO exists in the system, which makes the system suitable for bleaching19.

<table>
	<tbody>
		<tr>
			<td>Hydrogen peroxide, 30%</td>
			<td>Fisher Scientific</td>
			<td>H325-100</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Magnesium hydroxide, 99%</td>
			<td>Fisher Scientific</td>
			<td>AA1236722</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Sodium hydroxide</td>
			<td>Fisher Scientific</td>
			<td>S318-1</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Sodium bisulfite</td>
			<td>Fisher Scientific</td>
			<td>S654-500</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Sodium tripolyphosphate</td>
			<td>Fisher Scientific</td>
			<td>AC218675000</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Anthraquinone, &#62;98%</td>
			<td>Fisher Scientific</td>
			<td>AC104930500</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>1-Hydroxy Ethylidene-1,1-Diphosphonic Acid</td>
			<td>Fisher Scientific</td>
			<td>50-901-10243</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Degumming oil</td>
			<td>Minglong auxiliaries limited liability company, Yiyang, Hunan,China</td>
			<td>&#8212;&#8212;</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Ethyl alcohol</td>
			<td>Fisher Scientific</td>
			<td>A962-4</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Benzene</td>
			<td>Fisher Scientific</td>
			<td>AA43817AE</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Copper wire,0.5mm (0.02in) dia</td>
			<td>Fisher Scientific</td>
			<td>AA10783H4</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Cupriethylenediamine solution 1mol/L</td>
			<td>Fisher Scientific</td>
			<td>24991</td>
			<td>Chemical for testing, caution toxic</td>
		</tr>
		<tr>
			<td>Nitric acid (65% ~68% )</td>
			<td>Fisher Scientific</td>
			<td>A200-612GAL</td>
			<td>Chemical for testing, caution</td>
		</tr>
		<tr>
			<td>Ethylenediamine</td>
			<td>Fisher Scientific</td>
			<td>AC118420100</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Potassium permanganate</td>
			<td>Fisher Scientific</td>
			<td>P279-500</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Sulphuric acid</td>
			<td>Fisher Scientific</td>
			<td>A300C-212</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Silver sulfate</td>
			<td>Fisher Scientific</td>
			<td>S190-25</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Raw ramie</td>
			<td>Guangyuan limited liability company, Changde, Hunan,China</td>
			<td>&#8212;&#8212;</td>
			<td>Raw materials</td>
		</tr>
		<tr>
			<td>Electric-heated&#160;thermostatic&#160;water&#160;bath</td>
			<td>Senxin Experiment equipment limited liability company,Shanghai,China</td>
			<td>DK-S28</td>
			<td>Equipments for degumming</td>
		</tr>
		<tr>
			<td>High temperature lbaorator dyeing machine</td>
			<td>Shanghai Longda chemcials Crop.</td>
			<td>RY-1261</td>
			<td>Equipments for degumming</td>
		</tr>
		<tr>
			<td>Thermometer</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>100 &#176;C</td>
			<td>Equipments for degumming</td>
		</tr>
		<tr>
			<td>Vacuum suction machine</td>
			<td>Yukang KNET ,Shanghai,China</td>
			<td>SHB-IIIA</td>
			<td>Equipments for testing Mg(OH)2 solublity</td>
		</tr>
		<tr>
			<td>Suction flask</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>1000mL</td>
			<td>Equipments for testing Mg(OH)2 solublity</td>
		</tr>
		<tr>
			<td>Sand-core funnels</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>35mL</td>
			<td>Equipments for testing Mg(OH)2 solublity</td>
		</tr>
		<tr>
			<td>Oxidation reduction potential meter</td>
			<td>Dapu instrument, Shanghai, China</td>
			<td>MODEL 421</td>
			<td>Equipments for testing ORP value</td>
		</tr>
		<tr>
			<td>pH meter</td>
			<td>Hanna instruments,Beijing,China</td>
			<td>HI 98129</td>
			<td>Equipments for testing pH value</td>
		</tr>
		<tr>
			<td>Acid burette</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>50mL</td>
			<td>Equipments for testing H2O2 content</td>
		</tr>
		<tr>
			<td>Flask</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL/500mL</td>
			<td>Equipments for testing H2O2 content;&#160; residual gums content</td>
		</tr>
		<tr>
			<td>Electric furnace</td>
			<td>Jiangyi Experiment instruments limited liability company,Shanghai,China</td>
			<td>800-2000W</td>
			<td>Equipments for testing residual gums content</td>
		</tr>
		<tr>
			<td>Reflux condensing tube</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL</td>
			<td>Equipments for testing residual gums content; COD value</td>
		</tr>
		<tr>
			<td>Fiber cutter (40mm)</td>
			<td>Changzhou No.2 Textile Machine Co.,Ltd</td>
			<td>Y171A</td>
			<td>Equipments for testing fiber density</td>
		</tr>
		<tr>
			<td>Ostwald viscometer</td>
			<td>Taizhou, jiaojiang, glass instruments company</td>
			<td>0.6mm</td>
			<td>Equipments for testing fiber PD value</td>
		</tr>
		<tr>
			<td>Spherical fat extractor</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL</td>
			<td>Equipments for testing fiber PD value</td>
		</tr>
		<tr>
			<td>Soxhlet extractor</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL</td>
			<td>Equipments for testing fiber PD value</td>
		</tr>
		<tr>
			<td>Torsion&#160;balance</td>
			<td>Liangping instrucments Co.,Ltd,Shanghai, China</td>
			<td>JN-B</td>
			<td>Equipments for testing fiber density</td>
		</tr>
		<tr>
			<td>Fiber strength instrument</td>
			<td>Xinxian instruments, shanghai,China</td>
			<td>XQ-2</td>
			<td>Equipments for testing fiber tensile property</td>
		</tr>
		<tr>
			<td>Tension clamp</td>
			<td>Depu textile technology Co.,Ltd, Changzhou, jiangsu, China</td>
			<td>0.3cN/dtex</td>
			<td>Equipments for testing fiber tensile property</td>
		</tr>
		<tr>
			<td>COD&#160;thermostatic&#160;heater</td>
			<td>Qiangdao Xuyu environment protection technology Lit company</td>
			<td>DL-801A</td>
			<td>Equipments for testing COD value</td>
		</tr>
		<tr>
			<td>FTIR</td>
			<td>Thermo Fisher, America</td>
			<td>Nicolet</td>
			<td>FTIR analysis</td>
		</tr>
		<tr>
			<td>XRD</td>
			<td>Rigaku, Japan</td>
			<td>D/max-2550 PC</td>
			<td>XRD analysis</td>
		</tr>
		<tr>
			<td>Electronic balance</td>
			<td>Shanghai jingtian Electronic instrument Co.,Ltd</td>
			<td>FA2004A</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Drying oven</td>
			<td>Tonglixinda&#160; instruments, Tianjin,China</td>
			<td>101-2AS</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Weighing bottle</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>50x30</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Beaker</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>500mL</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Sample sieve</td>
			<td>Xiaojin hardware instruments Co.,Ltd, Shangyu, Zhejiang</td>
			<td>120 mesh</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Glass rod</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>&#8212;&#8212;</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Cylinder</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL, 50mL</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Pipette</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>5mL, 10mL</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Rubber&#160;suction&#160;bulb</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>&#8212;&#8212;</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
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extraction of ramie fiber in alkali hydrogen peroxide system supported by controlled-release alkali source

This protocol demonstrates a method for ramie fiber extraction by scouring raw ramie in an alkali hydrogen peroxide system supported by a controlled-release alkali source. The fiber extracted from ramie is a type of textile material of great importance. In previous studies, ramie fiber was extracted in an alkali hydrogen peroxide system supported only by sodium hydroxide.However, due to the strong alkalinity of sodium hydroxide, the oxidation reaction speed of hydrogen peroxide was difficult to control and thus resulted in great damage to the treated fiber. In this protocol, a controlled-release alkali source, which is composed of sodium hydroxide and magnesium hydroxide, is used to provide an alkali condition and buffer the pH value of the alkali hydrogen peroxidesystem. The substitution rate of magnesium hydroxide can adjust the pH value of the hydrogen peroxide system and has great influence on the fiber properties. The pH value and oxidation-reduction potential (ORP) value, which represents the oxidation ability of alkali hydrogen peroxide system, were monitored using a pH meter and ORP meter, respectively. The residual hydrogen peroxide content in the alkali hydrogen peroxide system during the extraction process and the chemical oxygen demand (COD) value of wastewater after fiber extraction are tested by KMnO4 titration method. The yield of fiber is measured using a precision electronic balance, and residual gums of fiber are tested by a chemical analysis method. The polymerization degree (PD value) of fiber is tested by an intrinsic viscosity method using the Ubbelohde viscometer. The tensile property of fiber, including tenacity, elongation, and rupture, is measured using a fiber strength instrument. Fourier transform infrared spectroscopy and X-ray diffraction are used to characterize the functional groups and crystal property of fiber. This protocol proves that the controlled-release alkali source can improve the properties of the fiber extracted in an alkali hydrogen peroxide system.

The solubility of Mg(OH)2 in distilled water and degumming solution was studied (Figure 1). The effect of Mg(OH)2 substitution rate on pH value and ORP value (Figure 2) of the degumming solution was tested. The degumming yield and residual gums of fiber degummed under various Mg(OH)2 substitution rate were calculated (Figure 3). DP value, crystallinity, tensile proper...

Watch this Scientific Journal Video about Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source at JoVE.com

Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source

Presented here is a protocol for extraction of ramie fiber in alkali hydrogen peroxide system supported by controlled-release alkali source.

This protocol demonstrates a method for ramie fiber extraction by scouring raw ramie in an alkali hydrogen peroxide system supported by a ...

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