WO2011038568A1 - 溶剂法高湿模量竹纤维及其制备方法 - Google Patents
溶剂法高湿模量竹纤维及其制备方法 Download PDFInfo
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- WO2011038568A1 WO2011038568A1 PCT/CN2010/001359 CN2010001359W WO2011038568A1 WO 2011038568 A1 WO2011038568 A1 WO 2011038568A1 CN 2010001359 W CN2010001359 W CN 2010001359W WO 2011038568 A1 WO2011038568 A1 WO 2011038568A1
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- bamboo fiber
- solvent
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- spinning
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C1/00—Treatment of vegetable material
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/04—Dry spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
Definitions
- the invention relates to a bamboo fiber and a preparation method thereof, in particular to a solvent method high-humidity modulus bamboo fiber and a preparation method thereof.
- bamboo fiber fabrics can still guarantee their original characteristics after repeated washing and sun exposure. It is different from other fabrics that add antibacterial agents, anti-UV agents and other finishing agents in the post-treatment, so it does not cause any allergic adverse reactions to human skin, but has health care effects and bactericidal effects on human skin. It is a true pro. Skin care products, a wide range of applications.
- bamboo fiber fabrics have also been praised by the industry as "the most promising healthy fabric in the 21st century.”
- bamboo fiber production and preparation methods usually use the viscose method to prepare bamboo fiber.
- this method has problems such as long production process and serious environmental pollution.
- Environmental protection has become the biggest drawback of developing recycled bamboo fiber.
- the natural characteristics of the bamboo were destroyed during the processing, and the deodorizing, antibacterial and anti-ultraviolet functions of the fiber were significantly reduced.
- various fibers produced by the viscose method contain residual sulfur in the finished product, and sulfur generates hydrogen sulfide during high-temperature printing and dyeing, and is prone to odor during processing. Therefore, in order to overcome the above technical problems existing in the viscose method, the solvent method has begun to be used in the preparation process of bamboo cellulose fibers.
- Chinese Patent Application Publication No. CN1190531C discloses a method for producing a solvent-based bamboo cellulose fiber, which has the following defects: 1.
- the volume of the polymerization vessel is in the range of 5-300 liters, according to the conventional, 5-300 liters.
- the volumetric polymerizer is not in the category of industrial production; 2.
- the prior art lists the "pulp dewatering" step, which takes up to 8 hours of dehydration, which is time consuming and energy consuming.
- Chinese invention patent application publication specification CN1760412A discloses a method for producing bamboo fiber cellulose by solvent method, but has the following defects: 1.
- the production process is complicated, such as hydrolysis, acid hydrolysis, enzymatic hydrolysis, etc. in the pulp pretreatment process.
- the pretreatment process takes a long time: the hydrolysis time is 3-14 hours; the acid hydrolysis time is 3-11 hours; the hydrolysis time is 2.2-14 hours.
- the technical solution lacks a pre-dissolution process, which will result in unstable slurry quality.
- Chinese invention patent application publication specification CN1851115A discloses a method for directly manufacturing recycled bamboo fiber from paper-making bamboo pulp, the production method adopts high-energy ray irradiation method to treat pulp, high equipment investment, high energy consumption, and production environment High requirements and potential physical threats to operators. Summary of the invention
- One of the technical problems to be solved by the present invention is to provide a method for preparing a high wet modulus bamboo fiber by a solvent method.
- the method has the advantages of operating the cylinder, no industrial pollution, low energy consumption and high safety performance, and is suitable for the manufacture of solvent-based bamboo fiber for large-scale industrial continuous production.
- the second technical problem to be solved by the present invention is to provide a solvent method high humidity modulus bamboo fiber Dimensions, prepared by the above method.
- a method for preparing a high-moisture modulus bamboo fiber by a solvent method comprising the following steps:
- the above porridge is subjected to vacuum dehydration and pressing to obtain cellulose having a water content of 10-60% by mass after pressing; and the above-mentioned pressed water cellulose is added to a mass percentage of 50-88% N-mercaptomorpholine-N.
- an aqueous solution of an oxide to obtain a pre-dissolved slurry; after the pre-dissolved slurry is introduced into a dissolving machine, heated and vacuumed, dehydrated, dissolved, homogenized, and defoamed to obtain a slurry;
- the slurry is conveyed by a booster pump, enters the metering pump, and is sprayed through a spinneret, and is formed by dry-wet spinning to obtain bamboo fiber;
- the deionized water conductivity in the step (1) is ⁇ 5 s/cm 2 , the pH is 6-8, and the temperature is 50.
- the cellulase in the step (1) is a liquid cellulase.
- the outlet temperature in the step (3) is 50-80 °C.
- the predissolved pulp cellulose in the step (3) has a mass content of 8-12% and a pH of 8-12.
- the mass ratio of the aqueous cellulose in the step (3) to the aqueous solution of 50-88% N-mercaptomorpholine-N-oxide is 1:2 - 1:12.
- the degree of vacuum in the step (4) is 1.0 kpa to 15.0 kPa, and the temperature is 60 to 120 °C.
- the cellulose in the step (4) has a cellulose content of 11-15%.
- the spinning speed in the step (5) is 35-100 m/min, the spinning air gap is 5-50 mm, the spinning blowing temperature is 10-25 ° C, the spinning blowing flow rate is 100-500 L/H, and the blowing relative humidity is 50- 80%, the coagulation bath concentration is 10-30%, and the coagulation bath temperature is 5-30 °C.
- the water washing temperature in the step (6) is 25-60 °C.
- step (7) hydrogen peroxide bleaching is adopted, wherein the hydrogen peroxide cycle concentration is 0.05-1.0%, and the hydrogen peroxide cycle PH value is 8-13.
- the oil circulation concentration in the step (8) is 0.5-5%, the oil circulation PH value is 6-9, and the oil circulation temperature is 50-70 °C.
- the drying temperature in the step (9) is 80-15 (TC.
- the present invention provides a solvent-method high-humidity modulus bamboo fiber which is prepared by the above method.
- the advantages of the technical solution of the present invention are mainly embodied in the following aspects:
- the operation cylinder is single, no industrial pollution is generated, the energy consumption is low, and the safety is low.
- the bamboo fiber prepared according to the method can effectively maintain the original deodorizing, antibacterial and ultraviolet shielding functions without destroying the natural characteristics of the bamboo.
- the bamboo fiber prepared by the invention not only retains the natural physical and chemical properties of the bamboo fiber, but also has no harmful chemical residues, thereby ensuring safe wearing.
- the bamboo fiber prepared by the invention has a high wet modulus and its wet modulus>
- the bamboo fiber prepared by the invention has good dimensional stability, is not easy to be deformed during wet finishing and laundering, is convenient for continuous dyeing, and is convenient for printing and dyeing, and is advantageous for producing high-end fabric.
- a method for preparing a high-moisture modulus bamboo fiber by a solvent method comprising the following steps: (1) activation
- the activation process is simple, the chemical reagents are added less, and the whole process is only about one hour, which is short in time and convenient to operate. details as follows:
- Adjust pH Adjust with acid and alkali
- Termination activation adding alkali to adjust pH
- the hydrous content of water cellulose is 10-60%, and the size of water cellulose after pulverization is 3cm*3cm.
- the pre-dissolution step is particularly increased, which not only helps to stabilize the amount of pulp, but also facilitates dissolution.
- Pulp The amount of W is increased to produce a high quality finished yarn. The steps are as follows:
- the pressed water cellulose is added to an aqueous solution containing 50-88% by mass of N-mercaptomorpholine-N-oxide, wherein the water cellulose and 50-88% N-mercaptomorpholine-N-oxide
- the ratio of the aqueous solution shield is 1:2 - 1:12, which makes the pulp swell, which is more conducive to uniform dissolution and stable slurry;
- outlet temperature 50-80 ° C pre-dissolved pulp composition: cellulose content of 8-12%, PH value 8-12; after the pre-dissolving machine mixture into the dissolving machine, after heating vacuum, dehydration After being dissolved, homogenized, and defoamed, an amber transparent homogeneous slurry is obtained;
- the washed fiber is bleached with aerobic water and stabilizer to achieve the required whiteness.
- Parameters hydrogen peroxide cycle concentration 0.05-1.0%, hydrogen peroxide cycle pH 8-13, hydrogen peroxide cycle temperature 75 °C, stabilizer LAVATEX9188 And DELINOL 9258, Manufacturer: Dr.Th.bohme KQ Chem. Fabrik Gmbh&Co
- the bleached fiber after oiling, reaches the required oiling rate
- the oiled fiber is heated to achieve the required fiber moisture content; Parameters: Drying temperature 80-150 ° C Example 1:
- the bamboo pulp having a degree of polymerization of 500 is added to the process water having a conductivity of ⁇ 5 s/cm 2 , a pH of 6.8, a temperature of 50 ° C, a pH of 4.5, a cellulase activation for one hour, and hydrogen addition.
- Sodium oxide terminates activation, adjusts the pH to 11, and after the activated porridge is vacuum-dehydrated, the water content of the water cellulose is controlled to be 45%, and the pulverized 3cm*3cm particles are added to the mass percentage of 78% N.
- the slurry is transported by a booster pump, sprayed through a spinneret, and formed by dry-wet spinning.
- the spinning speed is 50m/min
- the spinning air gap is 15mm
- the spinning air temperature is 14°C
- the spinning air flow is 200L H.
- the relative humidity of the blower is 50%
- the concentration of the coagulation bath is 15%
- the temperature of the coagulation bath is 8 °C
- the fiber is washed with water
- the washing temperature is 60 °C
- the washed fiber is bleached with hydrogen peroxide and stabilizer
- the hydrogen peroxide cycle concentration is 0.20%.
- hydrogen peroxide cycle PH value 10.8 hydrogen peroxide cycle temperature 75 °C, bleached fiber, after oiling, oil circulation concentration 1.8%, oil cycle PH value 6.5, oil cycle temperature 50 ° C, after oiling Fiber drying, temperature 125 ° C, the finished fiber: fineness at 1.58 dtex, dry breaking strength 3.5 cN / dtex, wet breaking strength 3.0 cN / dtex, dry elongation at break 14.8%, wet elongation at break 17.2%, wet modulus 17.9cN/dtex, dry strength coefficient of variation 10%, whiteness 58%, oil content 0.23%, resurgence 11.2%.
- Example 2 Example 2:
- the bamboo pulp having a degree of polymerization of 550 is added to the process water having a conductivity of ⁇ 5 s/cm 2 , a pH of 6.0, a temperature of 50 ° C, a pH of 4.2, a cellulase activation for one hour, and hydrogen addition.
- Sodium oxide terminates the activation, adjusts the pH to 12, terminates the activated porridge, and after vacuum dehydration and pressing, controls the water cellulose to have a water content percentage of 55%, pulverizes into 3cm*3cm particles, and adds 85% by mass.
- aqueous solution of N-mercaptomorpholine-N-oxide wherein the mass ratio of aqueous cellulose to N-mercaptomorpholine-N-oxide is 1:3, the slurry is swollen, and the outlet temperature is 68 °C.
- Predissolved pulp composition cellulose 9.5%, pH 9.0, after the pre-dissolving machine mixture into the dissolving machine, the control vacuum degree 7.0kpa, the slurry composition: cellulose 11.2%.
- the slurry is transported by a booster pump, sprayed through a spinneret, and formed by dry-wet spinning.
- the spinning speed is 40m/min
- the spinning air gap is 25mm
- the spinning air temperature is 16°C
- the spinning air flow is 350L H.
- the relative humidity of the blower is 60%
- the concentration of the coagulation bath is 15%
- the temperature of the coagulation bath is 10 °C
- the fiber is washed with water
- the washing temperature is 40 °C
- the washed fiber is bleached with hydrogen peroxide and stabilizer
- the hydrogen peroxide cycle concentration is 0.35%.
- hydrogen peroxide cycle PH value 10.5 hydrogen peroxide cycle temperature 75 °C, bleached fiber, after oiling, oil circulation concentration 2.5%, oil agent cycle pH 7.0, oil cycle temperature 60 ° C, after oiling
- the fiber is dry, the temperature is 110 °C, and the finished fiber is: 2.18 dtex, dry breaking strength 3.33 cN/dtex, wet breaking strength 2.98 cN/dtex, dry elongation at break 15.2%, wet elongation at break 17.4%, wet modulus 16.8cN/dtex, dry strength coefficient of variation 10%, whiteness 55%, oil content 0.25%, regain 10.5%.
- Example 3 Example 3:
- Wool fiber The bamboo pulp having a degree of polymerization of 600 is added to the process water having a conductivity of ⁇ 5 s/cm 2 , a pH of 7.3, a temperature of 50 ° C, a pH of 5.8, a cellulase activation for one hour, and hydrogen addition.
- Sodium oxide terminates activation, adjusts the pH to 12.5, and after the activated porridge is vacuum-dehydrated, the water content of the water cellulose is controlled by 25%, and the pulverized 3cm*3cm particles are added to the mass percentage of 60% N.
- the slurry is transported by a booster pump, sprayed through a spinneret, and formed by dry-wet spinning.
- the spinning speed is 35m/min
- the spinning air gap is 40mm
- the spinning air temperature is 20°C
- the spinning air flow is 500L H.
- the relative humidity of the blower is 68%
- the concentration of the coagulation bath is 23%
- the temperature of the coagulation bath is 20 °C
- the fiber is washed with water
- the washing temperature is 50 °C
- the washed fiber is bleached by hydrogen peroxide and stabilizer
- the hydrogen peroxide cycle concentration is 0.6%.
- the fiber is dry, the temperature is 105 °C, and the finished fiber is: 3.21 dtex, dry breaking strength 3.28 cN/dtex, wet breaking strength 2.85 cN/dtex, dry elongation at break 15.4%, wet elongation at break 17.8%, wet modulus 15.2cN/dtex, dry strength coefficient of variation 10%, whiteness 50%, oil content 0.3%, resurgence 11%.
- the bamboo fiber prepared by the present invention has a high wet modulus and a wet mold of 3 ⁇ 4>15 cN/dtex.
- Example 4
- Test conditions (1) the fabric is woven; (2) under the same atmospheric conditions, 20 °C, relative humidity 58%; (3) using M988 shrink machine.
- the fabrics of the bamboo fibers prepared in Examples 1-3 were compared with the viscose bamboo fiber fabrics. The specific data is shown in Table 2.
- the fabric of the bamboo fiber prepared by the present invention has a lower shrinkage rate than the fabric of the viscose bamboo fiber, and the dimensional stability of the fabric is good.
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Description
溶剂法高湿模量竹纤维及其制备方法
技术领域
本发明涉及一种竹纤维及其制备方法, 尤其涉及一种溶剂法高湿 模量竹纤维及其制备方法。 背景技术
竹纤维产品以其高科技含量, 及其柔滑软暖、 凉爽舒适、 抑菌抗 菌、 绿色环保、 天然保健的独特品质牢握市场脉搏, 独树一帜。
竹纤维织物的天然抗菌、 抑菌、 抗紫外线作用在经多次反复洗涤、 日晒后, 仍能保证其原有的特点。 更不同于其它在后处理中加入抗菌 剂、 抗紫外线剂等整理剂的织物, 所以它不会对人体皮肤造成任何过 敏性不良反应, 反而对人体皮肤具有保健作用和杀菌效果, 是真正的 亲肤保健产品, 应用领域宽广。
竹纤维面料在床上用品的应用, 给广大消费者带来一个健康、 舒 适、 凉爽的夏季。 竹纤维面料也被业内人士誉为 "二十一世纪最具有 发展前景的健康面料"。
竹纤维的生产制备方法, 通常采用粘胶法来制备竹纤维, 但是该 方法存在着生产工艺过程过长, 对环境污染严重等问题, 环保问题更 成了发展再生竹纤维的最大弊端; 同时该方法在加工过程中竹子的天 然特性遭到破坏, 纤维的除臭、 抗菌、 防紫外线功能明显下降。 并且 采用粘胶法生产的各种纤维, 其成品中均含有残硫量, 硫在高温印染 过程中会产生硫化氢的物质, 在加工过程中易产生异味。
因此, 为克服粘胶法存在的上述技术问题, 溶剂法开始运用于竹 纤维素纤维的制备过程中。
中国发明专利申请公开说明书 CN1190531C公开了一种溶剂法竹 纤维素纤维的生产方法, 其工艺方法中存在如下缺陷: 1、 聚合釜的体 积在 5-300立升, 根据常规, 5-300立升容积的聚合釜, 并不属于工业 化生产的范畴; 2、 该现有技术列示了 "浆粕脱水" 步骤, 脱水时间长 达 8小时, 耗时费能。
中国发明专利申请公开说明书 CN1760412A公开了一种溶剂法再 生竹纤维纤维素的生产方法, 但存在如下缺陷: 1、 生产工艺复杂, 如 在浆粕预处理过程中有水解、 酸解、 酶解等三个工序。 预处理过程时 间较长: 水解时间在 3-14小时;、 酸解时间在 3-11小时; 酶解时间在 2.2-14小时。且预处理过程中会因水解、 酸解产生大量的工业废水。 2、 该技术方案缺乏预溶解工艺, 会造成浆液质量不稳定。
中国发明专利申请公开说明书 CN1851115A公开了一种由造纸级 竹浆粕直接制造再生竹纤维的方法, 其生产方法采用高能射线幅照方 法处理浆粕, 设备投资高、 能耗大, 并且对生产环境要求高, 同时会 对操作人员造成潜在的身体威胁。 发明内容
本发明所要解决的技术问题之一是提供一种溶剂法高湿模量竹纤 维的制备方法。 该方法操作筒单、 无工业污染产生、 能耗低、 安全性 能高, 适用于大规模工业化连续性生产的溶剂法竹纤维制造。
本发明所要解决的技术问题之二是提供一种溶剂法高湿模量竹纤
维, 采用上述方法制备而成。
为解决上述技术问题, 本发明通过以下技术方案来实现: 一种溶剂法高湿模量竹纤维的制备方法, 由下述步骤组成:
( 1 )活化
将聚合度 400-1000的竹浆粕, 加入到去离子水中, 调节 PH值在 4-6, 加入纤维素酶进行活化, 再加入碱, 调节 PH值在 10-13, 终止活 化, 得到浆粥;
(2)压榨
将上述浆粥经过真空脱水压榨, 得到压榨后的含水率为质量百分 比 10-60%的纤维素; 将上述压榨后的水纤维素加入含有质量百分比 50-88%N-曱基吗啉 -N-氧化物的水溶液, 得到预溶解浆; 将上述预溶解浆进入溶解机后, 经过加热抽真空, 脱水、 溶解、 匀化、 脱泡后, 得到浆液;
(5) 纺丝
将上述浆液经过增压泵输送, 进入计量泵后, 通过喷丝板喷出, 采用干湿法纺丝成型, 得到竹纤维;
(6) 水洗;
(7) 漂白;
(8) 上油;
(9) 烘干。
进一步的, 在本发明中:
所述步骤(1 )中的去离子水电导率 <5 s/cm2, PH值 6-8, 温度 50
°C。
所述步骤(1 ) 中的纤维素酶为液态纤维素酶。
所述步骤(3 ) 中的出口温度 50-80°C。
所述步骤(3 )中的预溶解浆纤维素质量含量为 8-12%、PH值 8-12。 所述步骤(3 ) 中的水纤维素与 50-88%N-曱基吗啉 -N-氧化物的水 溶液质量比为 1 :2 - 1 :12。
所述步骤(4 ) 中的真空度为 1.0kpa-15.0kpa, 温度为 60-120°C。 所述步骤(4 ) 中的浆液中纤维素质量含量为 11-15%。
所述步骤(5 )中的纺丝速度 35-100m/min, 纺丝气隙 5-50mm, 纺 丝吹风温度 10-25 °C,纺丝吹风流量 100-500L/H,吹风相对湿度 50-80%, 凝固浴浓度 10-30%, 凝固浴温度 5-30°C。
所述步骤(6 ) 中的水洗温度 25-60°C。
所述步骤( 7 )中采用双氧水漂白,其中双氧水循环浓度 0.05-1.0%, 双氧水循环 PH值 8-13。
所述步骤( 8 ) 中的油剂循环浓度 0.5-5%, 油剂循环 PH值 6-9, 油剂循环温度 50-70°C。
所述步骤(9 ) 中的烘干温度 80-15(TC。
另外, 本发明还提供了一种溶剂法高湿模量竹纤维, 采用上述方 法制备而成。
本发明技术方案的优点主要体现在以下几方面: 采用本发明制备方法, 操作筒单、 无工业污染产生、 能耗低且安
全性能高, 适用于大规模工业化连续性生产的溶剂法竹纤维制造。 采用本发明制备方法, 不会破坏竹子的天然特性, 依据本方法制 备的竹纤维, 能够有效保持其原有的除臭、 抗菌、 防紫外线功能。
采用本发明制备的竹纤维, 既保留了竹纤维天然的物理和化学性 能, 又没有有害化学残留物, 从而保证了穿着安全。
采用本发明制备的竹纤维, 具有较高的湿模量, 其湿模量>
15cN/dtex, 采用本发明制备的竹纤维所制成品尺寸稳定性好, 湿整理 及洗烫时不易变形, 利于连续染色, 便于印染, 利于生产高端织物。 具体实施方式
一种溶剂法高湿模量竹纤维的制备方法, 由下述步骤组成: ( 1 ) 活化
此活化工艺流程筒单, 化工试剂添加少, 整个流程仅 1小时左 右, 耗时短, 操作方便。 具体如下:
调配工艺水→加入浆粕→调节 PH值→加入纤维素酶→终止活化 调配工艺水: 采用去离子水;
参数: 电导率 <5 s/cm2, PH值: 6-8, 温度: 50 °C
加入浆粕: 竹浆粕
参数: 聚合度 400-1000
调节 PH值: 用酸碱调节
参数: PH值 4-6
加入纤维素酶: 液态纤维素酶
参数: 名称 CelluPract ®AL70、 产品编号 IPL 5B06610、 供应
商 BIOPRACT
终止活化: 加入碱调节 PH值
参数: PH值 10-13
( 2 ) 压榨
浆粥经过真空脱水压榨后, 得到工艺要求的含水率;
参数: 水纤维素的含水质量百分比 10-60%, 粉碎后的水纤维 素大小 3cm*3cm 在本发明中特别地增加了预溶解这一步骤, 不但有利于稳定 浆 量, 同时也有利于溶解。 浆: W量得到提高, 才能做出高质 量的成品丝。 其步骤具体如下:
经压榨后的水纤维素加入含有质量百分比 50-88%N-曱基吗啉 -N-氧化物的水溶液,其中水纤维素与 50-88%N-曱基吗啉 -N-氧化物 的水溶液盾量比为 1:2 - 1 :12, 使浆粕溶胀, 更利于溶解均匀和浆液 的稳定;
参数: 出口温度 50-80°C , 预溶解浆组成:纤维素质量含量为 8-12%、 PH值 8-12; 经预溶解机后的混合液进入溶解机后,经过加热抽真空,脱水、 溶解、 匀化、 脱泡后达到琥珀色透明均质的浆液;
参数:真空度 1.0kpa-15.0kpa,温度 60-120 °C,浆液组成:纤维素质 量含量为 11-15%;
(5) 纺丝
浆液经过增压泵输送, 进入计量泵后, 通过喷丝板喷出, 用干 湿法纺丝成型;
参数: 纺丝速度 35-100m/min, 纺丝气隙 5-50mm, 纺丝吹风温 度 10-25°C, 纺丝吹风流量 100-500L/H, 吹风相对湿度 50-80%,凝 固浴浓度 10-30%,凝固浴温度 5-3(TC
(6) 水洗
水洗将纤维经过水清洗后, 回收溶剂 N-曱基吗啉 -N-氧化物, 提高溶剂的回收率;
参数: 水洗温度 25-60 °C
(7) 漂白
水洗后的纤维,经过欢氧水和稳定剂的漂白,达到要求的白度; 参数: 双氧水循环浓度 0.05-1.0%, 双氧水循环 PH值 8-13, 双 氧水循环温度 75 °C, 稳定剂为 LAVATEX9188和 DELINOL 9258, 制造商: Dr.Th.bohme KQ Chem. Fabrik Gmbh&Co
(8) 上油
漂白后的纤维, 经过上油后, 达到要求的上油率;
参数: 油剂循环浓度 0.5-5%, 油剂循环 PH值 6-9, 油剂循环 温度 50-70 °C, 油剂油剂为 Lemin OR , Lemin WQ Lemin AN , 制造 商: CLARIANT
(9) 烘干
将上油后的纤维, 通过加热, 达到要求的纤维含水率; 参数: 烘干温度 80-150°C
实施例 1:
棉型纤维:
将聚合度 500的竹浆粕,加入到电导率 <5 s/cm2,PH值: 6.8, 温度: 50°C的工艺水中, 调节 PH值在 4.5, 加入纤维素酶活化一小时, 加入 氢氧化钠终止活化, 调节 PH值在 11, 终止活化后的浆粥经过真空脱 水压榨后, 控制水纤维素的含水质量百分比 45%, 粉碎为的 3cm*3cm 的颗粒, 加入含有质量百分比 78%N-曱基吗啉 -N-氧化物的水溶液, 其 中水纤维素与 N-曱基吗啉 -N-氧化物的水溶液质量比为 1 :4, 使浆粕溶 胀, 出口温度 70°C, 预溶解浆组成:纤维素 11.5%、 PH值 9.5, 经预溶 解机后的混合液进入溶解机后, 控制真空度 5.0kpa,浆液组成:纤维素 13.8%。
浆液经过增压泵输送, 通过喷丝板喷出, 用干湿法纺丝成型, 纺丝 速度 50m/min, 纺丝气隙 15mm, 纺丝吹风温度 14°C, 纺丝吹风流量 200L H, 吹风相对湿度 50%,凝固浴浓度 15%,凝固浴温度 8 °C, 将纤维 经过水清洗后, 水洗温度 60°C, 水洗后的纤维, 经过双氧水和稳定剂 的漂白, 双氧水循环浓度 0.20%, 双氧水循环 PH值 10.8 , 双氧水循环 温度 75 °C, 漂白后的纤维, 经过上油后, 油剂循环浓度 1.8%, 油剂循 环 PH值 6.5, 油剂循环温度 50°C , 将上油后的纤维烘干, 温度 125°C, 得出的成品纤维: 纤度在 1.58dtex, 干断裂强度 3.5cN/dtex, 湿断裂强 度 3.0 cN/dtex, 干断裂伸长率 14.8%, 湿断裂伸长率 17.2%, 湿模量 17.9cN/dtex,干强变异系数 10%, 白度 58%,含油 0.23%, 回潮 11.2%。 实施例 2:
中长型纤维:
将聚合度 550的竹浆粕,加入到电导率 <5 s/cm2,PH值: 6.0, 温度: 50°C的工艺水中, 调节 PH值在 4.2, 加入纤维素酶活化一小时, 加入 氢氧化钠终止活化, 调节 PH值在 12, 终止活化后的浆粥, 经过真空 脱水压榨后,控制水纤维素的含水质量百分比 55%,粉碎为的 3cm*3cm 的颗粒, 加入含有质量百分比 85%N-曱基吗啉 -N-氧化物的水溶液, 其 中水纤维素与 N-曱基吗啉 -N-氧化物的水溶液质量比为 1 :3, 使浆粕溶 胀, 出口温度 68 °C, 预溶解浆组成:纤维素 9.5%、 PH值 9.0, 经预溶 解机后的混合液进入溶解机后, 控制真空度 7.0kpa,浆液组成:纤维素 11.2%。
浆液经过增压泵输送, 通过喷丝板喷出, 用干湿法纺丝成型, 纺丝 速度 40m/min, 纺丝气隙 25mm, 纺丝吹风温度 16°C, 纺丝吹风流量 350L H, 吹风相对湿度 60%,凝固浴浓度 15%,凝固浴温度 10°C , 将纤 维经过水清洗后, 水洗温度 40°C, 水洗后的纤维, 经过双氧水和稳定 剂的漂白, 双氧水循环浓度 0.35%, 双氧水循环 PH值 10.5 , 双氧水循 环温度 75 °C , 漂白后的纤维, 经过上油后, 油剂循环浓度 2.5%, 油剂 循环 PH值 7.0, 油剂循环温度 60°C , 将上油后的纤维供干, 温度 110 °C, 得出的成品纤维: 纤度在 2.18dtex, 干断裂强度 3.33cN/dtex, 湿 断裂强度 2.98 cN/dtex, 干断裂伸长率 15.2%, 湿断裂伸长率 17.4%, 湿模量 16.8cN/dtex, 干强变异系数 10%, 白度 55%, 含油 0.25%, 回 潮 10.5%。 实施例 3:
毛型纤维:
将聚合度 600的竹浆粕,加入到电导率 <5 s/cm2,PH值: 7.3, 温度: 50°C的工艺水中, 调节 PH值在 5.8, 加入纤维素酶活化一小时, 加入 氢氧化钠终止活化,调节 PH值在 12.5 ,终止活化后的浆粥经过真空脱 水压榨后, 控制水纤维素的含水质量百分比 25%, 粉碎为的 3cm*3cm 的颗粒, 加入含有质量百分比 60%N-曱基吗啉 -N-氧化物的水溶液, 其 中水纤维素与 N-曱基吗啉 -N-氧化物的水溶液质量比为 1 :7, 使浆粕溶 胀, 出口温度 75 °C, 预溶解浆组成:纤维素 9.1%、 PH值 10, 经预溶 解机后的混合液进入溶解机后, 控制真空度 2.5kpa,浆液组成:纤维素 12%。
浆液经过增压泵输送, 通过喷丝板喷出, 用干湿法纺丝成型, 纺丝 速度 35m/min, 纺丝气隙 40mm, 纺丝吹风温度 20°C, 纺丝吹风流量 500L H, 吹风相对湿度 68%,凝固浴浓度 23%,凝固浴温度 20 °C , 将纤 维经过水清洗后, 水洗温度 50°C, 水洗后的纤维, 经过双氧水和稳定 剂的漂白, 双氧水循环浓度 0.6%, 双氧水循环 PH值 11.5 , 双氧水循 环温度 75 °C , 漂白后的纤维, 经过上油后, 油剂循环浓度 4.0%, 油剂 循环 PH值 7.9, 油剂循环温度 65 °C , 将上油后的纤维供干, 温度 105 °C, 得出的成品纤维: 纤度在 3.21dtex, 干断裂强度 3.28cN/dtex, 湿 断裂强度 2.85 cN/dtex, 干断裂伸长率 15.4%, 湿断裂伸长率 17.8%, 湿模量 15.2cN/dtex, 干强变异系数 10%, 白度 50%, 含油 0.3%, 回潮 11%。 将本发明实施例 1-3所制备的竹纤维各物理指标与 CN1190531C、 CN1851115A 所公开的数据及棉型竹材粘胶短纤维标准 FZ/T
52006-2006一等品指标进行比较, 具体数据详见表 1。
表 1
从实施例 1-3可以看出,釆用本发明制备的竹纤维,具有较高的湿 模量, 其湿模 ¾>15cN/dtex。 实施例 4:
缩水率测试
测试条件: ( 1 ) 织物为机织物; (2)在相同的大气条件下,
20 °C, 相对湿度 58%; ( 3 )采用 M988缩水机。 将实施例 1-3 所制备的竹纤维织所造成织物与粘胶竹纤维织物进 行比较, 具体数据详见表 2。
表 2
由上述数据可以看出, 采用本发明制备的竹纤维的织物比粘胶竹 纤维的织物缩水率低 ί艮多, 织物的尺寸稳定性 ί艮好。 实施例 5:
纱线沸水缩水率测试
测试时, 纱线为 32 So 将实施例 1-3 所制备的竹纤维织所造成纱线与粘胶竹纤维纱线进 行比较, 具体数据详见表 3。
由上述数据可以看出采用本发明制备的竹纤维的纱线缩水率仅为
0.5%左右, 大大低于粘胶竹纤维。
毫无疑问, 本发明, 还可以具有多种变换及改型, 并不限于上述 实施方式的具体实施例。 总之, 本发明的保护范围应包括那些对于本 领域普通技术人员来说显而易见的变换或替代以及改型。
Claims
1、 一种溶剂法高湿模量竹纤维的制备方法, 其特征在于, 由下 述步骤组成:
( 1 )活化
将聚合度 400- 1000的竹浆粕,加入到去离子水中,调节 PH值在 4-6, 加入纤维素酶进行活化, 再加入碱, 调节 PH值在 10-13, 终止 活化, 得到浆粥;
(2)压榨
将上述浆粥经过真空脱水压榨,得到压榨后的含水率为质量百分 比 10-60%的纤维素; 将上述压榨后的水纤维素加入含有质量百分比 50-88%N-曱基吗 啉 -N-氧化物的水溶液, 得到预溶解浆;
(4) 溶解
将上述预溶解浆进入溶解机后, 经过加热抽真空, 脱水、 溶解、 匀化、 脱泡后, 得到浆液;
(5) 纺丝
将上述浆液经过增压泵输送, 进入计量泵后, 通过喷丝板喷出, 釆用干湿法纺丝成型, 得到竹纤维;
(6) 水洗;
(7) 漂白;
(8) 上油;
(9) 烘干。
2、 如权利要求 1 所述的溶剂法高湿模量竹纤维的制备方法, 其特 征在于, 所述步骤(3 ) 中的出口温度 50-80°C。
3、 如权利要求 1 所述的溶剂法高湿模量竹纤维的制备方法, 其特 征在于, 所述步骤(3 ) 中的预溶解浆纤维素质量含量为 8-12%、 PH 值 8-12。
4、 如权利要求 1 所述的溶剂法高湿模量竹纤维的制备方法, 其特 征在于, 所述步骤(3 ) 中的水纤维素与 50-88%N-曱基吗啉 -N-氧化物 的水溶液质量比为 1:2 - 1 : 12。
5、 如权利要求 1 所述的溶剂法高湿模量竹纤维的制备方法, 其特 征在于, 所述步骤(4 ) 中的真空度为 1.0kpa-15.0kpa, 温度为 60-120 °C。
6、 如权利要求 1 所述的溶剂法高湿模量竹纤维的制备方法, 其特 征在于, 所述步骤(4 ) 中的浆液中纤维素质量含量为 11-15%。
7、 如权利要求 1 所述的溶剂法高湿模量竹纤维的制备方法, 其特 征在于,所述步骤( 5 )中的纺丝速度 35-100m/min, 纺丝气隙 5-50mm, 纺丝吹风温度 10-25 °C, 纺丝吹风流量 100-500L/H, 吹风相对湿度 50-80%,凝固浴浓度 10-30%,凝固浴温度 5-30°C。
8、 如权利要求 1 所述的溶剂法高湿模量竹纤维的制备方法, 其特 征在于, 所述步骤 (7 ) 中采用双氧水漂白, 其中双氧 循环浓度 0.05-1.0%, 双氧水循环 PH值 8-13。
9、 如权利要求 1 所述的溶剂法高湿模量竹纤维的制备方法, 其特 征在于,所述步骤(8 )中的油剂循环浓度 0.5-5%,油剂循环 PH值 6-9, 油剂循环温度 50-70 °C。
替换页(细则第 26奈)
10、 一种溶剂法高湿模量竹纤维, 其特征在于, 采用权利要求 1-9中 任一项所述的方法制备而成。
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Also Published As
| Publication number | Publication date |
|---|---|
| CN101694019A (zh) | 2010-04-14 |
| US20120241669A1 (en) | 2012-09-27 |
| EP2484820A1 (en) | 2012-08-08 |
| CN101694019B (zh) | 2011-08-10 |
| EP2484820A4 (en) | 2013-06-26 |
| JP2013506060A (ja) | 2013-02-21 |
| JP5324710B2 (ja) | 2013-10-23 |
| US8926712B2 (en) | 2015-01-06 |
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