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 ...

The overall goal of this procedure is to improve the tensile properties of ramie fiber, prepared in a hydrogen peroxide oxidation degumming system by using a controlled release alkali source made by partially replacing sodium hydroxide with magnesium hydroxide. This method can help answer key questions in the field of oxidative extraction of natural fibers, such as extraction of ramie and flax fiber prepared in hydrogen peroxide oxidation degumming system. The main advantage of this technique is that pH and thus oxidation ability of the degumming solution can be controlled by adjusting the substitute rate of the magnesium hydroxide.We first had the idea for this method when we found that if sodium hydroxide was used as a alkaline source, the pH value of the degumming solution dropped quickly, making it difficult to control the hydrogen peroxide reaction speed. First, dissolve hydrogen peroxide, alkali, sodium triphosphate, anthraquinone, and HEDP in 100 milliliters of distilled water to make the degumming solution. Immerse 10 grams of raw ramie in the degumming solution and scour it at 85 degrees Celsius for 60 minutes.Following this, increase the temperature to 125 degrees Celsius and scour for another 60 minutes. Now, dissolve 0.4 grams of sodium bisulfite in 100 milliliters of distilled water to prepare the reducing solution. After scouring, treat the degummed ramie fiber in the reducing solution at 90 degrees Celsius for 60 minutes.After reducing the degummed ramie fiber, wash it thoroughly with deionized water. Immerse the fiber in degumming oil at 90 degrees Celsius for 15 minutes, then dry the fiber in an oven at 125 degrees Celsius for four hours. Prepare degumming solutions with magnesium hydroxide substitution rates of zero, 20, 40, 60, 80, and 100%as previously described.Immerse the raw ramie in the degumming solutions, then scour at 85 degrees Celsius for 60 minutes. Wash the combined ORP electrode with distilled water. After air drying, immerse the combined ORP electrode in the degumming solutions to record the ORP value every 10 minutes.Immerse the pH electrode in the degumming solutions to record the pH value every 10 minutes. Next, test the hydrogen peroxide content of the degumming solutions every 10 minutes by the potassium permanganate titration method according to the Chinese standard. Degrease the ramie fiber by submerging it in a two to one mixture of benzene and ethyl alcohol.After allowing the solvent to evaporate, cut the fiber into short pieces using scissors. Place the samples in a weighing container, and keep them in a controlled humidity atmosphere until it reaches equilibrium water content before removing for test purposes. Now, immerse a copper wire in concentrated nitric acid, followed by 98%anhydrous ethylenediamine.Then, wash the copper wire thoroughly with distilled water. Place the fiber sample and copper wire in a flask. Add 10 milliliters of distilled water and 10 milliliters of one mol per liter cupriethylenediamine solution to the glass bottle.Add a magnetic stir bar to the flask and stir the mixture for one hour to prepare the ramie fiber cupriethylenediamine solution. Following this, transfer 6.5 milliliters of the ramie fiber solution to an Ubbelohde viscometer to measure its intrinsic viscosity. Finally, set the clamping distance at 20 millimeters, and the descending speed of the bottom clamp at 20 millimeters per minute.After equilibrating the fiber samples under standard atmospheric conditions, test the tenacity, breaking elongation, and work of rupture of the fiber using the fiber strength instrument under the appropriate conditions. Although the solubility of magnesium hydroxide in degumming solution was higher than distilled water, due to the slight effect of degumming auxiliaries, it was still insufficiently soluble. When a controlled release alkali source was applied, the pH was stable, and decreased with increasing substitution rate.Decrease of the ORP value was slower under higher substitution rate. Residual gum analysis revealed that the yield of degumming and residual gums of fiber increased with the substitution rate. The DP value, crystallinity, and tensile properties increased with the substitution rate, but decreased with substitution rate higher than 20%The COD value decreased by 20%under the substitution rate of magnesium hydroxide.In FTIR patterns of the fiber, signals due to the stretching vibration of CH and OH and cellulose were observed. The carbinol peak was attributed to the CO stretching of COH bending and hemicellulose, and this signal was stronger when the substitution rate was lower, which indicates that hemicellulose can be removed more effectively under a lower substitution rate. Although the residual hydrogen peroxide contents increased when using the controlled release alkali source, the substitution rate did not influence the residual hydrogen peroxide content.Once mastered, this technique can be done in about 200 minutes if it is performed appropriately. While attempting this procedure, it's important to remember to control the substitution rate of the magnesium hydroxide. After its development, this technique paved the way for researchers in the field of oxidation natural fiber extraction, or bleaching.After watching this video, you should have a good understanding of how to adjust the pH value of working solution, with a controlled release alkali source, and the method of natural fiber extraction. Don't forget that working with cupriethylenediamine can be extremely hazardous, and appropriate precautions should always be taken while performing this procedure.

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