CN102660779A - Production method of carex meyeriana fiber - Google Patents

Production method of carex meyeriana fiber Download PDF

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CN102660779A
CN102660779A CN2012101835273A CN201210183527A CN102660779A CN 102660779 A CN102660779 A CN 102660779A CN 2012101835273 A CN2012101835273 A CN 2012101835273A CN 201210183527 A CN201210183527 A CN 201210183527A CN 102660779 A CN102660779 A CN 102660779A
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fiber
degumming
carex meyeriana
alkali
water
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CN102660779B (en
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王春红
白肃跃
马海军
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Tianjin Polytechnic University
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Abstract

The invention discloses a production method of a carex meyeriana fiber. The production method adopts the following process flow: taking carex meyeriana raw grass, boiling, carrying out primary processing, carrying out pre-degumming treatment by an ultrasonic wave, carrying out primary washing, carrying out alkali oxidation and degumming bath, pickling, carrying out secondary washing, drying, feeding oil, opening and carding to obtain the carex meyeriana fiber, wherein water is used as a medium in the step of the pre-degumming treatment by the ultrasonic wave, when the frequency is 28-40HZ and the temperature is 50-70 DEG C, the pre-degumming treatment by the ultrasonic wave is carried out for 60-90 minutes, and NaOH is added when the treatment is carried out within 20-30 minutes so as to enable the alkali concentration of the solution to reach 5-15g/l; in the step of alkali oxidation and degumming bath process, carex meyeriana can be put in an alkali oxidation extracting solution to enable the temperature to rise to 90-100 DEG C, heat preservation and boiling are performed for 1-2 hours; the alkali oxidation extracting solution is prepared from the following ingredients: 6-9g/l of sodium hydroxide, 8-12g/l of hydrogen peroxide, 2-4% of sodium polyphosphate serving as an additive of carex meyeriana mass, 2-4% of magnesium sulfate and 1-3% of sodium sulfite.

Description

Production method of carex meyeriana fibers
Technical Field
The invention relates to a textile material technology, in particular to a production method of Meyer sedge fiber.
Background
Wula grass is one of three treasures in northeast, and is popular among people due to its unique cold-proof and warm-keeping properties and natural antibacterial and deodorant properties. At present, the carex meyeriana is mainly applied to the fields of carex meyeriana insoles, carex meyeriana medical pillows, carex meyeriana waist support and the like, and precious resources are not well utilized.
The production of the carex meyeriana fiber mainly comprises two parts of degumming and post-treatment, wherein the degumming is a key link for extracting the carex meyeriana fiber. The existing degumming technology has two methods: the method is characterized in that the method comprises an alkali boiling method (see 'a production process of Meyer sedge fiber silk and a product (application number 200410010645. X)'), the Meyer sedge retting degumming of the process is to extract Meyer sedge fiber by adopting an alkali boiling method or a high-temperature high-pressure alkali boiling method, and the process has the defects that the Meyer sedge retting degumming treatment time is longer than 48 hours, the treatment effect is uneven, the use high-pressure cost is high, the bleaching process is complicated, the bleaching reagent is not environment-friendly and the like. Secondly, alkali-oxygen one-bath process (see lihong et al, wula sedge fibre-a new type textile fibre material [ J)]Shandong textile and science, 2006, (1): 54-56), the degumming method of the process adopts a method combining the procedures of alkali boiling and bleaching, the process has the defects of insufficient contact between NaOH and the carex meyeriana and poor degumming effect of the carex meyeriana under the condition of not adding any chemical auxiliary agent, and simultaneously, the H temperature is high2O2The decomposition speed is not controlled, the bleaching effect is poor, and the cellulose can be oxidized, so that the damage effect on the fiber is serious. As shown by the measurement of the chemical component content of the unreummed carex meyeriana fiber by Lihong et al, the chemical component content of the carex meyeriana fiber is similar to that of the hemp fiber, and the degumming of the hemp mainly comprises a chemical degumming method, a biological enzyme degumming method, an ultrasonic degumming method and the like, wherein the ultrasonic degumming method comprises the ultrasonic degummingThe method is simple to operate, clean and environment-friendly. However, experimental studies find that the single ultrasonic degumming effect is not ideal and cannot meet the production requirements of the carex meyeriana fiber.
Disclosure of Invention
Aiming at the problems of complex operation, higher cost, environmental pollution and the like of the existing carex meyeriana production process, the invention aims to solve the technical problem of providing a carex meyeriana fiber production method, which adopts an ultrasonic-chemical combined degumming process to extract carex meyeriana fibers with excellent performance, and has the characteristics of simple operation, cost saving, cleanness, environmental protection, energy saving, high efficiency and the like.
The technical scheme for solving the technical problems is as follows: a production method of Meyer sedge fiber is designed, and the production method adopts the following processes:
the process flow is as follows: meyer sedge raw grass → water boiling → primary processing → ultrasonic wave pre-degumming → front water washing → alkali oxygen one-bath degumming → acid washing → rear water washing → drying → oil feeding → opening and carding → Meyer sedge fiber; wherein,
the water boiling process is to boil the Meyer sedge raw grass in boiling water for 1-2h, and take out after cooling to normal temperature;
the preliminary processing technology is that mechanical facilities are adopted to roll, tear and comb the taken-out carex meyeriana so as to process the carex meyeriana into filaments;
the ultrasonic pre-degumming treatment process is to carry out ultrasonic degumming treatment by using water as a medium at the ultrasonic frequency of 28-40KHZ and the temperature of 50-70 ℃ for 60-90min, and to add NaOH when the ultrasonic treatment is carried out for 20-30min so that the alkali concentration of the solution reaches 5-15g/l, and to cool the solution to normal temperature after the set treatment time is reached;
the front and back water washing processes are to wash the carex meyeriana fiber to be neutral by using water at 50-70 ℃;
the alkali-oxygen one-bath degumming process comprises the steps of putting the carex meyeriana fibers which are washed in advance into a prepared alkali-oxygen extracting solution, heating the temperature to a preset temperature of 90-100 ℃ from normal temperature at a heating speed of 1 ℃/min, and boiling for 1-2 hours in a heat preservation manner; the alkaline oxygen extracting solution is prepared as follows: 6-9g/l of sodium hydroxide and 8-12g/l of hydrogen peroxide, and adding 2-4% of auxiliary agent sodium polyphosphate, 2-4% of magnesium sulfate and 1-3% of sodium sulfite relative to the mass of the carex meyeriana;
the acid washing process is to neutralize the alkali liquor remained on the carex meyeriana fiber by using 0.5-1.5g/l of low-concentration sulfuric acid solution.
Compared with the prior art, the production method of the carex meyeriana fiber has the beneficial effects that: the ultrasonic wave is used as the pre-degumming process, the method is simple to operate, clean and environment-friendly, and high in efficiency; after the ultrasonic wave is acted for a period of time by using water as medium liquid, a certain amount of sodium hydroxide is added, so that the degumming effect on the carex meyeriana is enhanced; the alkali-oxygen one-bath degumming replaces a plurality of boiling and bleaching processes, and a chemical auxiliary agent suitable for extracting the carex meyeriana fiber is added, so that the fiber damage is prevented or reduced, the degumming effect is enhanced, the ultrasonic treatment is combined with the alkali-oxygen one-bath method, the process flow is reduced, the time and the cost are saved, the waste liquid is easy to recycle, and the environment protection is facilitated; the production method can extract the wula sedge fiber with excellent performance.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
The production method (short for method) of the wula sedge fiber designed by the invention adopts the following process: :
the process flow is as follows: meyer sedge raw grass → water boiling → primary processing → ultrasonic wave pre-degumming → front water washing → alkali oxygen one-bath degumming → acid washing → rear water washing → drying → oil feeding → opening and carding → Meyer sedge fiber; wherein,
the water boiling process comprises the following steps: boiling raw Meyer sedge in boiling water for 1-2h, cooling to normal temperature, and taking out Meyer sedge;
the primary processing technology comprises the following steps: beating and mechanically tearing the taken-out Meyer sedge by adopting a mechanical facility to flatten the Meyer sedge firstly and then tearing and carding the Meyer sedge into a plurality of filaments;
the ultrasonic pre-degumming treatment process comprises the following steps: placing mechanically torn Meyer sedge into a beaker with distilled water, placing the beaker into an ultrasonic instrument, carrying out ultrasonic pre-degumming treatment at the ultrasonic frequency of 28-40KHZ and the temperature of 50-70 ℃ for 60-90min, adding NaOH when carrying out ultrasonic treatment for 20-30min to make the alkali concentration of the solution reach 5-15g/l, taking out the beaker after reaching the set treatment time, and cooling to normal temperature;
the pre-washing process comprises the following steps: washing Meyer sedge fiber with 50-70 deg.C water to neutral;
the alkali-oxygen one-bath degumming process comprises the following steps: putting washed Meyer sedge fiber into prepared alkaline oxygen extracting solution, keeping the heating rate of 1 ℃/min, heating from normal temperature to a preset temperature of 90-100 ℃, and boiling for 1-2h in a heat preservation way; the alkaline-oxygen extracting solution is prepared at the normal temperature as follows: 6-9g/l of sodium hydroxide, 8-12g/l of hydrogen peroxide, and 2-4% of sodium polyphosphate, 2-4% of magnesium sulfate and 1-3% of sodium sulfite which are added into the auxiliary agent and are relative to the mass of the carex meyeriana; the components of sodium hydroxide and hydrogen peroxide in the alkali-oxygen extracting solution form an alkali-oxygen one-bath process.
In order to further improve the degumming effect of sodium hydroxide and improve the quality of the carex meyeriana, the method is further characterized in that in the alkali-oxygen one-bath degumming process, when the temperature is raised to 80-90 ℃, sodium hydroxide is added again, so that the total concentration of alkali (sodium hydroxide) in the bath solution is more than 9g/l and less than or equal to 12 g/l.
The acid washing or neutralizing process comprises the following steps: neutralizing the alkaline solution remained on the carex meyeriana fiber with 0.5-1.5g/l of low-concentration sulfuric acid solution;
the post-washing process comprises the following steps: washing Meyer sedge fiber with 50-70 deg.C water to neutral;
the drying process comprises the following steps: drying the washed neutral carex meyeriana fiber, and adjusting the moisture regain to be about 12%;
the oil feeding process comprises the following steps: uniformly spraying a carding agent on the carex meyeriana fibers with the adjusted moisture regain of about 12%, wherein the usage amount of the carding agent is 4-6% of the mass of the fibers, the carding agent is diluted by adding water with the mass of 6-10% of the mass of the fibers and then sprayed, and the carding agent is TFD 1212-carding agent (a commercial product) at room temperature for 8-12 h;
and finally, opening and carding: feeding the carex meyeriana fiber after oil feeding into a carding machine for opening and carding to obtain the carex meyeriana fiber.
The procedures of drying, oil feeding, opening and carding in the process flow of the invention are basically the same as or similar to the existing hemp fiber post-treatment method, but the procedures of water boiling, primary processing, ultrasonic treatment, water washing, alkali oxygen bath, acid washing and the like are different from the existing Meyer sedge fiber extraction method, and the invention is a new procedure and process which are innovatively designed aiming at the defects of the existing Meyer sedge fiber production process.
The method of the invention takes ultrasonic wave as a degumming pretreatment process, and adds a certain amount of sodium hydroxide after the ultrasonic wave is acted for a period of time by using water as a medium liquid, compared with the method which only uses water as the medium liquid, the degumming effect of the carex meyeriana can be obviously enhanced. The method aims at the degumming of the carex meyeriana, combines the ultrasonic wave with the alkali-oxygen one-bath method, and can enhance the degumming effect compared with the pure ultrasonic degumming and the pure alkali-oxygen one-bath method; the alkali-oxygen one-bath degumming method in the chemical degumming part can not only achieve the effect of scouring and degumming, but also provide an alkaline environment for hydrogen peroxide bleaching, and particularly, a chemical auxiliary agent suitable for Meyer sedge degumming is added, so that the contact degree of NaOH and Meyer sedge can be increased, the decomposition of hydrogen peroxide is stabilized, the damage to Meyer sedge fibers is prevented, and an alkali-oxygen extracting solution can be prepared for chemical degumming. The post-treatment part combines with the mature hemp fiber post-treatment process to produce the carex meyeriana fiber. Compared with the existing Meyer sedge production process, the Meyer sedge production process provided by the invention has the characteristics of simplicity in operation, cleanness, environmental protection, energy conservation, high efficiency and the like.
The main parameters of the carex meyeriana fiber obtained by the method are as follows: the diameter of the carex meyeriana fiber is 30-110 μm, the length is 40-160mm, the fineness is 2-3tex, the elongation at break is 2.0-3.5%, the breaking strength is 30-80cN, the breaking strength is 15-23cN/tex, the dynamic friction coefficient is 0.147-0.179, the static friction coefficient is 0.132-0.180, and the mass specific resistance is 6.7 multiplied by 108-7.2×108Ω·g/cm2. The Meyer sedge fiber is suitable for further textile processing and is also suitable for being made into composite materials.
Nothing in this specification is said to apply to the prior art.
Specific examples of the present invention are given below. These examples are only for illustrating the technical solutions of the present invention in detail, and do not limit the scope of the claims of the present application.
Example 1
Boiling 15g of Meyer sedge grass in boiling water for 2h, cooling to normal temperature, performing preliminary processing, putting the Meyer sedge grass after preliminary processing into a beaker filled with 750ml of distilled water, putting the beaker into an ultrasonic instrument, selecting the frequency of 40KHZ and the temperature of 60 ℃, performing ultrasonic pre-degumming treatment, after 20min, adding 7.5g of sodium hydroxide into the beaker, continuing to perform ultrasonic degumming for 40min, washing with warm water at 60 ℃ for 4 times after the ultrasonic pre-degumming is finished until the temperature is neutral, putting the cleaned Meyer sedge fiber into a prepared 750ml of alkaline oxygen extract for degumming, wherein the alkaline oxygen extract comprises 750ml of distilled water, 5.25g of sodium hydroxide, 6g of hydrogen peroxide, 0.45g of sodium polyphosphate, 0.45g of magnesium sulfate and 0.30g of sodium sulfite, starting from normal temperature, keeping the temperature rising speed at 1 ℃/min, raising the temperature to 90 ℃, adding 2.25g of sodium hydroxide into the alkaline oxygen extract, heating to 100 deg.C, timing, steaming for 60min, washing with 1g/l sulfuric acid solution for 2min, and washing with 60 deg.C warm water for 3 times until it is neutral; drying to adjust moisture regain of the carex meyeriana fiber to be 12% to obtain 8.5g of fiber, uniformly spraying 1.105g of diluted oiling agent TFD1212 (wherein TFD 1212-carding agent 0.425g and water 0.68 g), stewing for 8h at room temperature, feeding the carex meyeriana fiber into a small carding machine for opening and carding to obtain the carex meyeriana fiber.
Through detection, the Meyer sedge fiber obtained in the embodiment has the average diameter of 67.59um, the average length of 108.94mm, the fineness of 2.5tex, the average elongation at break of 2.7 percent, the average breaking strength of 55.94cN, the average breaking strength of 22.38cN/tex, the average dynamic friction coefficient of 0.153, the average static friction coefficient of 0.161 and the mass specific resistance of 7.2 multiplied by 108Ω·g/cm2
Example 2
Boiling 15g of Meyer sedge grass in boiling water for 2h, cooling to normal temperature, performing preliminary processing, putting the Meyer sedge grass after preliminary processing into a beaker filled with 750ml of distilled water, putting the beaker into an ultrasonic instrument, selecting the frequency of 28KHZ, performing ultrasonic pre-degumming at the temperature of 60 ℃, adding 3.75g of sodium hydroxide after 20min, continuing to perform ultrasonic degumming for 40min, after the ultrasonic action is finished, washing with warm water at the temperature of 60 ℃ for 4-5 times until the temperature is neutral, putting the cleaned Meyer sedge grass fiber into a prepared alkaline oxygen extract of 750ml for degumming, wherein the alkaline oxygen extract comprises 6g of sodium hydroxide, 7.5g of hydrogen peroxide, 0.45g of sodium polyphosphate, 0.45g of magnesium sulfate and 0.30g of sodium sulfite, keeping the heating rate from normal temperature at 1 ℃/min, starting timing when the temperature is raised to 100 ℃, steaming for 80min, then flushing the Meyer sedge grass fiber with a prepared sulfuric acid solution of 1g/l for 2min, continuously washing with 60 deg.C warm water for 4 times until the fiber is neutral, oven drying to adjust moisture regain of Meyer sedge fiber to 12% to obtain 9g fiber, uniformly spraying 1.35g diluted oiling agent TFD 1212-carding agent (wherein TFD 1212-carding agent is 0.45g, water is 0.9 g), stewing for 9h at room temperature, feeding Meyer sedge fiber into small carding machine for opening and carding to obtain Meyer sedge fiber.
The Meyer sedge fiber obtained in the embodiment has the average diameter of 69.76um, the average length of 92.51mm, the fineness of 2.51tex, the average elongation at break of 2.4 percent, the average breaking strength of 47.68cN, the average breaking strength of 18.99cN/tex, the average dynamic friction coefficient of 0.173, the average static friction coefficient of 0.173 and the mass specific resistance of 6.7 multiplied by 108Ω·g/cm2
Example 3
Boiling 15g of Meyer sedge grass in boiling water for 2h, cooling to normal temperature, performing preliminary processing, putting the Meyer sedge grass after preliminary processing into a beaker filled with 750ml of distilled water, putting the beaker into an ultrasonic instrument, selecting the frequency of 40KHZ, performing ultrasonic pre-degumming at the temperature of 60 ℃, adding 10.75g of sodium hydroxide after 20min, continuing to perform ultrasonic pre-degumming for 50min, after the ultrasonic action is finished, washing with warm water at the temperature of 60 ℃ for 4-5 times until the temperature is neutral, putting the cleaned Meyer sedge grass fiber into a prepared alkaline oxygen extract of 750ml for degumming, wherein the alkaline oxygen extract comprises 4.5g of sodium hydroxide, 6g of hydrogen peroxide, 0.45g of sodium polyphosphate, 0.45g of magnesium sulfate and 0.30g of sodium sulfite, keeping the heating rate from normal temperature at 1 ℃/min, starting timing when the temperature is raised to 100 ℃, steaming for 100min, and then washing the Meyer sedge grass fiber with a prepared sulfuric acid solution of 1g/l for 2min, continuously washing with 60 deg.C warm water for 4 times until the fiber is neutral, oven drying to adjust moisture regain of carex meyeriana fiber to 12% to obtain 9g fiber, uniformly spraying 0.99g diluted TFD 1212-carding agent (wherein TFD 1212-carding agent is 0.45g, and water is 0.54 g), standing at room temperature for 8 hr, feeding carex meyeriana fiber into small carding machine, and opening and carding to obtain carex meyeriana fiber.
The Meyer sedge fiber obtained in the embodiment has the average diameter of 67.9um, the average length of 101.6mm, the fineness of 2.5tex, the average elongation at break of 3.0 percent, the average breaking strength of 50cN, the average breaking strength of 20cN/tex, the average kinetic friction coefficient of 0.155, the average static friction coefficient of 0.152 and the mass specific resistance of 7 multiplied by 108Ω·g/cm2

Claims (3)

1. A production method of Meyer sedge fiber adopts the following processes:
the process flow is as follows: meyer sedge raw grass → water boiling → primary processing → ultrasonic wave pre-degumming → front water washing → alkali oxygen one-bath degumming → acid washing → rear water washing → drying → oil feeding → opening and carding → Meyer sedge fiber; wherein,
the water boiling process is to boil the Meyer sedge raw grass in boiling water for 1-2h, and take out after cooling to normal temperature;
the preliminary processing technology is that mechanical facilities are adopted to roll, tear and comb the taken-out carex meyeriana so as to process the carex meyeriana into filaments;
the ultrasonic pre-degumming treatment process is characterized in that water is used as a medium, ultrasonic pre-degumming treatment is carried out at the ultrasonic frequency of 28-40KHZ and the temperature of 50-70 ℃ for 60-90min, NaOH is added when the ultrasonic treatment is carried out for 20-30min, so that the alkali concentration of the solution reaches 5-15g/l, and the solution is cooled to the normal temperature after the set treatment time is reached;
the front and back water washing processes are to wash the carex meyeriana fiber to be neutral by using water at 50-70 ℃;
the alkali-oxygen one-bath degumming process comprises the steps of putting the carex meyeriana fibers which are washed in advance into a prepared alkali-oxygen extracting solution, heating the temperature to a preset temperature of 90-100 ℃ from normal temperature at a heating speed of 1 ℃/min, and boiling for 1-2 hours in a heat preservation manner; the alkaline oxygen extracting solution is prepared as follows: 6-9g/l of sodium hydroxide and 8-12g/l of hydrogen peroxide, and adding 2-4% of auxiliary agent sodium polyphosphate, 2-4% of magnesium sulfate and 1-3% of sodium sulfite relative to the mass of the carex meyeriana;
the acid washing process is to neutralize the alkali liquor remained on the carex meyeriana fiber by using 0.5-1.5g/l of low-concentration sulfuric acid solution.
2. The method for producing wula sedge fiber according to claim 1, wherein in the alkali-oxygen one-bath degumming process, when the temperature is increased to 80-90 ℃, sodium hydroxide is added again to make the total alkali concentration in the bath solution reach >9g/l ≤ 12 g/l.
3. A carex meyeriana fiber obtained directly by the production method of the carex meyeriana fiber of claim 1 or 2, wherein the main parameters of the carex meyeriana fiber are as follows: the diameter of the carex meyeriana fiber is 30-110 μm, the length is 40-160mm, the fineness is 2-3tex, the elongation at break is 2.0-3.5%, the breaking strength is 30-80cN, the breaking strength is 15-23cN/tex, the dynamic friction coefficient is 0.147-0.179, the static friction coefficient is 0.132-0.180, and the mass specific resistance is 6.7 multiplied by 108 -7.2×108Ω·g/cm2
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CN103498200A (en) * 2013-10-17 2014-01-08 齐齐哈尔大学 Meyer sedge fiber extraction method
CN104726939A (en) * 2015-03-19 2015-06-24 苏州陈恒织造有限公司 Marihuana degumming process based on flash explosion-ultrasonic wave combined action
CN105177729A (en) * 2014-06-16 2015-12-23 李林 Production method of Carex meyeriana fibers
CN105734682A (en) * 2016-04-14 2016-07-06 武汉纺织大学 High-frequency vibrating high-temperature high-pressure low-concentration alkaline water degumming and separation device
CN106119980A (en) * 2016-09-09 2016-11-16 天津工业大学 A kind of preparation method that becoming more meticulous of meyer sedge fiber
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CN107858827A (en) * 2017-11-21 2018-03-30 常州创索新材料科技有限公司 A kind of preparation method of antibacterial haze screen material
CN109837655A (en) * 2019-03-01 2019-06-04 天津工业大学 A kind of meyer sedge fiber Wet laid nonwoven material and its preparation method and application
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CN106245174B (en) * 2015-06-10 2020-09-29 天津工业大学 Preparation method of carex meyeriana blended fasciated yarn
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CN112841815A (en) * 2021-02-03 2021-05-28 浙江奥康鞋业股份有限公司 Preparation method of regenerated fiber Meyer sedge middle puller cloth
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CN113089163A (en) * 2021-03-16 2021-07-09 上海水星家用纺织品股份有限公司 Preparation method of wula sedge yarn and fabric and prepared fabric
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CN103498200A (en) * 2013-10-17 2014-01-08 齐齐哈尔大学 Meyer sedge fiber extraction method
CN103498200B (en) * 2013-10-17 2016-08-24 齐齐哈尔大学 A kind of method that meyer sedge fiber extracts
CN105177729A (en) * 2014-06-16 2015-12-23 李林 Production method of Carex meyeriana fibers
CN106149063A (en) * 2015-03-10 2016-11-23 天津工业大学 A kind of chemical-biological combined preparation process of meyer sedge fiber
CN104726939A (en) * 2015-03-19 2015-06-24 苏州陈恒织造有限公司 Marihuana degumming process based on flash explosion-ultrasonic wave combined action
CN106245174B (en) * 2015-06-10 2020-09-29 天津工业大学 Preparation method of carex meyeriana blended fasciated yarn
CN105734682B (en) * 2016-04-14 2018-02-09 武汉纺织大学 Dither HTHP low concentration buck degumming separation equipment
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CN109837655A (en) * 2019-03-01 2019-06-04 天津工业大学 A kind of meyer sedge fiber Wet laid nonwoven material and its preparation method and application
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CN110670146A (en) * 2019-11-08 2020-01-10 西安工程大学 Method for preparing lotus stem fibers
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