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CN106436414A - Method for preparing wheat straw cellulose microfibrils by auxiliary enzymatic pretreatment - Google Patents

Method for preparing wheat straw cellulose microfibrils by auxiliary enzymatic pretreatment Download PDF

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Publication number
CN106436414A
CN106436414A CN201610854405.0A CN201610854405A CN106436414A CN 106436414 A CN106436414 A CN 106436414A CN 201610854405 A CN201610854405 A CN 201610854405A CN 106436414 A CN106436414 A CN 106436414A
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wheat straw
fiber
cellulose microfibrils
enzyme pretreatment
cellulose
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李新平
陈家杰
王志杰
杜敏
朱晶航
侯青青
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • D21C5/005Treatment of cellulose-containing material with microorganisms or enzymes
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21DTREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
    • D21D1/00Methods of beating or refining; Beaters of the Hollander type
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21DTREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
    • D21D5/00Purification of the pulp suspension by mechanical means; Apparatus therefor
    • D21D5/02Straining or screening the pulp
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

本发明涉及一种酶预处理辅助制备麦草纤维素微纤丝的方法,先将麦草浆进行筛分处理,收集截留在筛网上的纤维组分;将步骤纤维组分用缓冲液配制成质量浓度为1%~5%的纤维悬浮液,再向纤维悬浮液中加入纤维素酶进行水解,得到酶预处理后的纤维浆料;其中纤维素酶的加入量是纤维组分绝干质量的0.5%~25%;将纤维浆料经过机械搅拌剪切,再配制成质量浓度为0.5~1.5%的纤维悬浮液,进行循环均质处理,制备出纤维素微纤丝乳状液;将纤维素微纤丝乳状液依次进行离心分离和过滤,得到麦草纤维素微纤丝。本发明可以降低机械解离能耗,利于减少酶用量,使浆料中的纤维分散均匀,能够顺利通过高压均质机分离出微纤丝。The invention relates to a method for preparing wheat straw cellulose microfibrils assisted by enzyme pretreatment. Firstly, the wheat straw pulp is sieved, and the fiber components retained on the sieve are collected; 1% to 5% of the fiber suspension, and then add cellulase to the fiber suspension for hydrolysis to obtain the fiber slurry after enzyme pretreatment; the amount of cellulase added is 0.5% of the absolute dry mass of the fiber component % to 25%; the fiber slurry is mechanically agitated and sheared, and then formulated into a fiber suspension with a mass concentration of 0.5 to 1.5%, which is subjected to circulation and homogenization treatment to prepare a cellulose microfibril emulsion; the cellulose microfibril emulsion The fibril emulsion is sequentially subjected to centrifugation and filtration to obtain wheat straw cellulose microfibrils. The invention can reduce the energy consumption of mechanical dissociation, is beneficial to reduce the amount of enzymes, makes the fibers in the slurry uniformly dispersed, and can successfully separate microfibrils through a high-pressure homogenizer.

Description

一种酶预处理辅助制备麦草纤维素微纤丝的方法A method for preparing wheat straw cellulose microfibrils assisted by enzyme pretreatment

【技术领域】【Technical field】

本发明属于植物纤维素生物质精炼领域,尤其是涉及一种酶预处理辅助制备麦草纤维素微纤丝的方法。The invention belongs to the field of plant cellulose biomass refining, in particular to a method for assisting preparation of wheat straw cellulose microfibrils through enzyme pretreatment.

【背景技术】【Background technique】

纤维素是自然界中含量最丰富的可再生性天然高分子聚合物,广泛存在于木材、禾本科、棉麻类等天然植物中。由于纤维素在性能上存在某些缺点,如热解性能差、不耐化学腐蚀、强度有限等,这就限制了它的应用范围。研究发现,当纤维直径达到纳米水平时,将会具备许多新的性质,其结晶度、亲水性、杨氏模量、强度和透明度等性能都有很大的提高,使其具有更广阔的应用范围。从天然纤维素中制备出来的纤维素微纤丝(cellulosemicrofibril,简称CMF)现在已经广泛的应用于纳米器件、包装材料、食品添加剂、太阳能电池和纳米纸等领域。Cellulose is the most abundant renewable natural polymer in nature, widely present in natural plants such as wood, grasses, cotton and hemp. Because cellulose has some disadvantages in performance, such as poor pyrolysis performance, chemical corrosion resistance, limited strength, etc., this limits its application range. Studies have found that when the fiber diameter reaches the nanometer level, it will have many new properties, and its crystallinity, hydrophilicity, Young's modulus, strength and transparency will all be greatly improved, making it have a wider range of applications. application range. Cellulose microfibril (CMF for short) prepared from natural cellulose has been widely used in the fields of nano-devices, packaging materials, food additives, solar cells and nano-paper.

我国是农作物秸秆资源丰富的国家,每年产生的农作物秸秆产量可达7亿吨左右,其中22%是麦草秸秆。农作物秸秆中蕴含着大量的纤维素成分、工业原料成分和热值。合理利用秸秆,有利于工业、农业和农村经济的合理发展,否则直接焚烧秸秆,不仅释放的大量气体严重污染环境,而且造成能源资源的重大浪费。若能将这部分纤维素成分加以精制,获得高纯度的纳米纤维素,则是实现麦草秸秆资源高附加值利用的重点。my country is a country rich in crop straw resources, and the annual output of crop straw can reach about 700 million tons, of which 22% is wheat straw. Crop straw contains a large amount of cellulose components, industrial raw material components and calorific value. Rational use of straw is conducive to the rational development of industry, agriculture and rural economy. Otherwise, direct burning of straw will not only release a large amount of gas that will seriously pollute the environment, but also cause a major waste of energy resources. If this part of cellulose can be refined to obtain high-purity nanocellulose, it will be the focus of realizing high value-added utilization of wheat straw resources.

麦草浆中细杂组份(通过100目,其中大部分是杂细胞,如薄壁细胞、表皮细胞等)的化学组分、物理形态和表面性质与纤维细胞有很大的差异,比表面积较大且结晶程度较低,对酶的吸附作用和水解作用较强,在酶水解过程中部分细杂组分容易首先被溶解,消耗更多的酶用量,因此,研究以筛分细杂组分后的麦草浆为原料制备纤维素微纤丝对改善制备方法,提高产品性质具有重要的现实意义。The chemical composition, physical form and surface properties of fine miscellaneous components in wheat straw pulp (through 100 meshes, most of which are miscellaneous cells, such as parenchyma cells, epidermal cells, etc.) are very different from those of fiber cells, and the specific surface area is relatively large. Large and low degree of crystallization, strong adsorption and hydrolysis of enzymes, part of the fine components are easy to be dissolved first in the process of enzymatic hydrolysis, and consume more enzyme dosage, therefore, the research is to screen the fine components The preparation of cellulose microfibrils from the final wheat straw pulp has important practical significance for improving the preparation method and improving the product properties.

现有技术主要以木浆为原料制备纤维素微纤丝,单纯利用机械高压均质化处理制备纤维素微纤丝能耗较高,长时间强烈的机械作用损坏纤维的晶体结构,而且原料纤维较长,容易堵塞高压均质机而使制备过程难以实现连续化;现有预处理结合机械法制备也具有一定的缺陷和局限性,酸、碱预处理对设备的抗腐蚀性要求高,分离得到纯CMF需消耗大量的水资源及动力资源,增加了成本和环境负荷;虽然TEMPO氧化预处理反应速度迅速,制备的CMF宽度较均匀,稳定性好,但是至今为止工业上还没有办法回收TEMPO催化剂,而且该法的制备原料主要为脱除木质素后的硫酸盐木浆等。The existing technology mainly uses wood pulp as raw material to prepare cellulose microfibrils, and the simple use of mechanical high-pressure homogenization treatment to prepare cellulose microfibrils consumes a lot of energy, and the long-term strong mechanical action damages the crystal structure of the fibers, and the raw material fibers Longer, it is easy to block the high-pressure homogenizer and make the preparation process difficult to achieve continuous; the existing pretreatment combined with mechanical preparation also has certain defects and limitations, acid and alkali pretreatment require high corrosion resistance of the equipment, separation Obtaining pure CMF consumes a large amount of water and power resources, which increases the cost and environmental load; although the reaction speed of TEMPO oxidation pretreatment is fast, the width of the prepared CMF is relatively uniform, and the stability is good, but so far there is no way to recover TEMPO in industry. Catalyst, and the preparation raw material of this method is mainly kraft wood pulp after de-lignification.

【发明内容】【Content of invention】

本发明的目的在于克服现有技术中存在的问题,提供一种酶预处理辅助制备麦草纤维素微纤丝的方法,浆料中纤维分散均匀,利于低能耗、无污染的连续化加工,实现农作物麦草的高值化利用。The purpose of the present invention is to overcome the problems existing in the prior art, and to provide a method for assisting the preparation of wheat straw cellulose microfibrils by enzyme pretreatment. The fibers in the slurry are evenly dispersed, which is beneficial to continuous processing with low energy consumption and pollution-free High-value utilization of crop wheat straw.

为了达到上述目的,本发明采用如下技术方案:In order to achieve the above object, the present invention adopts following technical scheme:

包括以下步骤:Include the following steps:

(1)将麦草浆进行筛分处理,收集截留在筛网上的纤维组分;(1) Sieving the wheat straw pulp to collect the fiber components trapped on the sieve;

(2)将步骤(1)得到的纤维组分用缓冲液配制成质量浓度为1%~5%的纤维悬浮液,再向纤维悬浮液中加入纤维素酶进行水解,得到酶预处理后的纤维浆料;其中纤维素酶的加入量是纤维组分绝干质量的0.5%~25%;(2) The fiber component obtained in step (1) is prepared into a fiber suspension with a mass concentration of 1% to 5% with a buffer, and then cellulase is added to the fiber suspension for hydrolysis to obtain enzyme pretreated Fiber slurry; wherein the amount of cellulase added is 0.5% to 25% of the absolute dry mass of the fiber component;

(3)将步骤(2)中得到的酶预处理后的纤维浆料经过机械搅拌剪切;(3) the fiber slurry obtained in step (2) after the enzyme pretreatment is subjected to mechanical stirring and shearing;

(4)将步骤(3)中机械搅拌剪切后的纤维浆料配制成质量浓度为0.5~1.5%的纤维悬浮液,进行循环均质处理,制备出纤维素微纤丝乳状液;(4) preparing the fiber slurry after mechanically agitating and shearing in step (3) into a fiber suspension with a mass concentration of 0.5 to 1.5%, and performing a circulation homogenization treatment to prepare a cellulose microfibril emulsion;

(5)将纤维素微纤丝乳状液依次进行离心分离和过滤,得到麦草纤维素微纤丝。(5) Centrifuging and filtering the cellulose microfibril emulsion in sequence to obtain wheat straw cellulose microfibrils.

进一步地,步骤(1)中的筛网为100目。Further, the screen mesh in step (1) is 100 mesh.

进一步地,步骤(2)中纤维组分先用水浸泡润胀6~18h,经疏解机疏解10~30min,挤干水分再配制成纤维悬浮液。Further, in step (2), the fiber components are soaked and swollen in water for 6-18 hours, then decomposed by a decomposer for 10-30 minutes, squeezed dry, and then formulated into a fiber suspension.

进一步地,步骤(2)中缓冲液采用的是浓度为0.05mol/L的磷酸缓冲液。Further, the buffer used in step (2) is a phosphate buffer with a concentration of 0.05 mol/L.

进一步地,步骤(2)中纤维素酶采用的是活性为50000u/g的固态内切葡聚糖酶。Further, the cellulase used in the step (2) is a solid-state endoglucanase with an activity of 50000u/g.

进一步地,步骤(2)中水解是在45~65℃的恒温水浴振荡锅中进行的,振荡频率为80~120r/min,水解时间为30~180min。Further, the hydrolysis in step (2) is carried out in a constant temperature water bath oscillating pot at 45-65° C., the oscillating frequency is 80-120 r/min, and the hydrolysis time is 30-180 minutes.

进一步地,步骤(3)中搅拌转速在5000~10000r/min,搅拌时间在5~15min。Further, in step (3), the stirring speed is 5000-10000 r/min, and the stirring time is 5-15 minutes.

进一步地,步骤(4)的循环均质处理中,压力在50~100MPa,循环次数为10~30次。Further, in the cyclic homogenization treatment in step (4), the pressure is 50-100 MPa, and the number of cycles is 10-30 times.

进一步地,步骤(5)中纤维素微纤丝乳状液在转速4000~8000r/min下离心分离10~30min。Further, in step (5), the cellulose microfibril emulsion is centrifuged at a rotation speed of 4000-8000 r/min for 10-30 min.

与现有技术相比,本发明具有以下有益的技术效果:Compared with the prior art, the present invention has the following beneficial technical effects:

(1)在本发明方法中,以麦草浆为原料,实现了对农作物废弃物的高值化再利用,扩大了制备纤维素微纤丝的原料来源。(2)制备过程中没有使用酸、碱、TEMPO催化剂等化学药剂,减少环境污染,而且可以降低机械解离能耗,具有良好的经济效益和环保效益。(3)在酶预处理前对麦草浆进行筛分,有利于减少浆中杂细胞对酶的消耗,然后进行合适的酶预处理和搅拌剪切处理,使浆料中的纤维分散均匀,以顺利通过高压均质机分离出微纤丝,便于连续化加工。(4)所制备的麦草纤维素微纤丝呈现乳白色凝胶状,微纤丝间相互交织成网状结构,直径为25~100nm,长度达到微米级,长径比较大且性能稳定,达到了纤维素微纤丝的质量要求。(1) In the method of the present invention, wheat straw pulp is used as a raw material to realize high-value reuse of crop waste and expand the source of raw materials for preparing cellulose microfibrils. (2) Chemical agents such as acid, alkali, and TEMPO catalyst are not used in the preparation process, which reduces environmental pollution, and can reduce energy consumption of mechanical dissociation, and has good economic and environmental benefits. (3) Sieving the wheat straw pulp before enzyme pretreatment is beneficial to reduce the consumption of enzyme by the miscellaneous cells in the pulp, and then carry out appropriate enzyme pretreatment and stirring and shearing treatment to make the fibers in the pulp evenly dispersed, so as to The microfibrils are successfully separated by a high-pressure homogenizer, which is convenient for continuous processing. (4) The prepared wheat straw cellulose microfibrils are in the form of milky white gel, and the microfibrils are interwoven into a network structure with a diameter of 25-100nm, a length of micron level, a large long-diameter ratio and stable performance, reaching Quality requirements for cellulose microfibrils.

【附图说明】【Description of drawings】

图1是实施例1制备的麦草纤维素微纤丝的扫描电镜图(加酶量5%,均质10次);Fig. 1 is the scanning electron micrograph of the wheat straw cellulose microfibril prepared in embodiment 1 (5% of enzyme amount added, homogenized 10 times);

图2是对比例1制备的麦草纤维素微纤丝的扫描电镜图(不加内切葡聚糖酶,均质10次);Fig. 2 is the scanning electron micrograph of the wheat straw cellulose microfibril prepared in comparative example 1 (without adding endoglucanase, homogenizing 10 times);

图3是实施例2制备的麦草纤维素微纤丝的扫描电镜图(加酶量25%,均质10次);Fig. 3 is the scanning electron micrograph of the wheat straw cellulose microfibril prepared in embodiment 2 (enzyme amount 25%, homogeneous 10 times);

图4是实施例3制备后的纤维扫描电镜图(加酶量25%,均质5次);Fig. 4 is the fiber scanning electron microscope picture after the preparation of embodiment 3 (enzyme amount 25%, homogeneous 5 times);

图5是实施例3制备的麦草纤维素微纤丝的扫描电镜图(加酶量25%,均质30次);Fig. 5 is the scanning electron micrograph of the wheat straw cellulose microfibril prepared in embodiment 3 (enzyme amount 25%, homogeneous 30 times);

图6是本发明制得的纤维素微纤丝的外观形貌图。Fig. 6 is a graph showing the appearance of cellulose microfibrils prepared in the present invention.

【具体实施方式】【detailed description】

下面结合附图对本发明做进一步详细说明。The present invention will be described in further detail below in conjunction with the accompanying drawings.

本发明包括以下步骤:The present invention comprises the following steps:

(1)所用原料为麦草浆,属于禾本科纤维原料,纤维较短,宽度较小,含有较多的薄壁细胞和表皮细胞等杂细胞,在预处理前对麦草浆进行筛分处理,筛出细杂组分,收集截留在100目筛网上的纤维组分,以备后续处理。(1) The raw material used is wheat straw pulp, which belongs to grass fiber raw material. The fiber is shorter, the width is smaller, and it contains more parenchyma cells and epidermal cells and other miscellaneous cells. Before pretreatment, the wheat straw pulp is sieved. The fine miscellaneous components are removed, and the fiber components retained on the 100-mesh sieve are collected for subsequent processing.

(2)将步骤(1)得到的纤维组分用水浸泡润胀6~18h后,经疏解机疏解10~30min,使麦草浆分散均匀,使后来加入的酶能与麦草纤维充分混合;挤干水分,用浓度为0.05mol/L的缓冲液配制成质量浓度为1%~5%的纤维悬浮液,然后加入相对纤维组分绝干质量0.5%~25%的纤维素酶进行水解,在恒温水浴振荡锅中保持温度45~65℃,振荡频率为80~120r/min,反应时间为30~180min。水解结束后放在沸水浴中煮沸灭活5min,然后经过蒸馏水充分洗涤,得到酶预处理后的纤维浆料。(2) Soak the fiber component obtained in step (1) in water for 6-18 hours, and then disperse it for 10-30 minutes through a decomposer to disperse the wheat straw pulp evenly, so that the enzyme added later can be fully mixed with the wheat straw fiber; squeeze dry Moisture, use a buffer solution with a concentration of 0.05mol/L to prepare a fiber suspension with a mass concentration of 1% to 5%, and then add cellulase that is 0.5% to 25% relative to the absolute dry mass of the fiber component for hydrolysis. The temperature in the water-bath oscillating pot is kept at 45-65°C, the oscillating frequency is 80-120r/min, and the reaction time is 30-180min. After the hydrolysis is completed, put it in a boiling water bath to boil and inactivate for 5 minutes, and then thoroughly wash with distilled water to obtain the fiber slurry after enzyme pretreatment.

其中步骤(2)中的缓冲液是磷酸缓冲液,所述的纤维素酶为市售的固态内切葡聚糖酶,来源于苏柯汉(潍坊)生物工程有限公司,品牌为SUKACell,活性为50000u/g。Wherein the buffer in step (2) is a phosphate buffer, and the cellulase is a commercially available solid-state endoglucanase derived from Su Kehan (Weifang) Bioengineering Co., Ltd., the brand is SUKACell, and the activity It is 50000u/g.

(3)将步骤(2)中得到的酶预处理后的纤维浆料经过适当的机械搅拌剪切,搅拌转速控制在5000~10000r/min,搅拌时间在5~15min,使浆料中较长纤维变短,纤维分散均匀,有利于顺利通过均质机。(3) The fiber slurry obtained in step (2) after the enzyme pretreatment is subjected to appropriate mechanical stirring and shearing, the stirring speed is controlled at 5000-10000r/min, and the stirring time is 5-15min, so that the slurry is longer The fibers become shorter and the fibers are evenly dispersed, which is conducive to passing through the homogenizer smoothly.

(4)将步骤(3)中得到的纤维用蒸馏水配制成100mL、质量浓度为0.5~1.5%纤维悬浮液,经过高压均质机的循环均质处理,控制高压均质机的操作压力在50~100MPa,循环次数为10~30次,制备出纤维素微纤丝乳状液。(4) the fiber that obtains in step (3) is mixed with 100mL with distilled water, and mass concentration is 0.5~1.5% fiber suspension, through the circulation homogenization treatment of high-pressure homogenizer, control the operating pressure of high-pressure homogenizer at 50 ~100MPa, the number of cycles is 10~30 times, and the cellulose microfibril emulsion is prepared.

(5)将步骤(4)得到的纤维素微纤丝乳状液在转速4000~8000r/min下离心分离10~30min,取离心液经过纤维素超滤膜过滤,收集膜面截留的固体组分,得到麦草纤维素微纤丝。(5) Centrifuge the cellulose microfibril emulsion obtained in step (4) at a rotating speed of 4000 to 8000r/min for 10 to 30 minutes, take the centrifugate and filter it through a cellulose ultrafiltration membrane, and collect the solid components retained on the membrane surface , to obtain wheat straw cellulose microfibrils.

本发明以麦草浆为原料,扩大了制备纤维素微纤丝的原料限制,在高压均质化处理前对麦草纤维进行筛分,然后进行合适的酶预处理和搅拌剪切处理,有利于减少酶用量,使浆料顺利通过高压均质机分离出微纤丝,而且制备过程不使用化学试剂,可以降低能耗,改善产品性能,降低污染负荷,有助于纤维素微纤丝的工业化生产。The present invention uses wheat straw pulp as a raw material, expands the raw material limitation for preparing cellulose microfibrils, sieves wheat straw fibers before high-pressure homogenization treatment, and then performs appropriate enzyme pretreatment and stirring and shearing treatment, which is beneficial to reduce The amount of enzyme used makes the slurry pass through the high-pressure homogenizer to separate the microfibrils smoothly, and the preparation process does not use chemical reagents, which can reduce energy consumption, improve product performance, reduce pollution load, and contribute to the industrial production of cellulose microfibrils .

下面通过具体的实施例对本发明做进一步详细说明。The present invention will be described in further detail below through specific examples.

实施例1Example 1

将麦草浆进行筛分,收集截留在100目筛网上的纤维组分,用水浸泡润胀12h后,经疏解机疏解30min,挤干水分,用浓度为0.05mol/L的磷酸缓冲液配制成浓度为3%的纤维悬浮液;然后加入相对纤维组分绝干质量5%的国产固态内切葡聚糖酶进行水解,在恒温水浴振荡锅中保持温度45℃,振荡频率为100r/min,反应时间为120min。水解结束后放在沸水浴中煮沸灭活5min,然后经过蒸馏水充分洗涤,得到酶预处理后的纤维浆料;再将纤维浆料经过适当的机械搅拌,搅拌转速控制在8000r/min,搅拌时间10min,然后配制成质量分数为0.5%纤维悬浮液100mL,经过高压均质机的循环均质处理,控制高压均质机的操作压力在80MPa,循环次数为10次,制备出纤维素微纤丝乳状液;将得到的纤维素微纤丝乳状液在转速8000r/min下离心分离30min,取离心液经过纤维素超滤膜过滤,收集膜面截留的固体组分,得到麦草纤维素微纤丝,扫描电镜图片(×100k)如图1所示。Sieve the wheat straw pulp, collect the fiber components trapped on the 100-mesh sieve, soak and swell with water for 12 hours, decompose for 30 minutes with a decomposer, squeeze out the water, and prepare the concentration with 0.05mol/L phosphate buffer solution 3% fiber suspension; then add domestic solid-state endoglucanase of 5% relative to the absolute dry mass of the fiber component for hydrolysis, keep the temperature at 45°C in a constant temperature water bath oscillating pot, and the oscillating frequency is 100r/min, the reaction The time is 120min. After the hydrolysis is completed, put it in a boiling water bath to boil and inactivate for 5 minutes, and then wash it thoroughly with distilled water to obtain the fiber slurry after enzyme pretreatment; then the fiber slurry is stirred by appropriate machinery, and the stirring speed is controlled at 8000r/min. 10min, and then it is prepared into 100mL of fiber suspension with a mass fraction of 0.5%. After the circulation homogenization treatment of the high-pressure homogenizer, the operating pressure of the high-pressure homogenizer is controlled at 80MPa, and the number of cycles is 10 times to prepare cellulose microfibrils. Emulsion: centrifuge the obtained cellulose microfibril emulsion at a rotating speed of 8000r/min for 30min, take the centrifugate and filter it through a cellulose ultrafiltration membrane, collect the solid components retained on the membrane surface, and obtain wheat straw cellulose microfibrils , and the scanning electron microscope picture (×100k) is shown in Figure 1.

制备的麦草纤维素微纤丝宽度40~100nm,长度微米级,结晶度(CrI%)74.53,聚合度(DP)235,而且均质能耗为865.9W·h。。The prepared wheat straw cellulose microfibrils have a width of 40-100 nm, a length of micron order, a crystallinity (CrI%) of 74.53, a degree of polymerization (DP) of 235, and a homogeneous energy consumption of 865.9 W·h. .

对比例1:不用酶预处理,直接高压均质处理,其他条件同实施例1Comparative example 1: without enzyme pretreatment, direct high-pressure homogeneous treatment, other conditions are the same as embodiment 1

将麦草浆进行筛分,收集截留在100目筛网上的纤维组分,用水浸泡润胀12h后,再将纤维浆料经过适当的机械搅拌,搅拌转速控制在8000r/min,搅拌时间10min,然后配制成质量分数为0.5%纤维悬浮液100mL,经过高压均质机的循环均质处理,控制高压均质机的操作压力在80MPa,循环次数为10次,制备出纤维素微纤丝乳状液;将得到的纤维素微纤丝乳状液在转速8000r/min下离心分离30min,取离心液经过纤维素超滤膜过滤,收集膜面截留的固体组分,得到麦草纤维素微纤丝,扫描电镜图片(×100k)如附图2所示。Sieve the wheat straw pulp, collect the fiber components trapped on the 100-mesh sieve, soak and swell with water for 12 hours, then put the fiber slurry through proper mechanical stirring, the stirring speed is controlled at 8000r/min, and the stirring time is 10min, and then Prepare 100mL of a fiber suspension with a mass fraction of 0.5%, undergo cyclic homogenization treatment with a high-pressure homogenizer, control the operating pressure of the high-pressure homogenizer at 80MPa, and cycle 10 times to prepare a cellulose microfibril emulsion; The obtained cellulose microfibril emulsion was centrifuged at a rotating speed of 8000r/min for 30min, the centrifuged liquid was filtered through a cellulose ultrafiltration membrane, and the solid components retained on the membrane surface were collected to obtain wheat straw cellulose microfibrils. The picture (×100k) is shown in Figure 2.

制备的纤维素微纤丝:结晶度(CrI%)63.28,聚合度(DP)318,纤维宽度50~140nm,分布不均匀,长度微米级,能耗1.03kW·h。The prepared cellulose microfibrils: crystallinity (CrI%) 63.28, degree of polymerization (DP) 318, fiber width 50-140nm, uneven distribution, length micron order, energy consumption 1.03kW·h.

在实施例1中,添加了相对纤维组分绝干质量5%的内切葡聚糖酶预处理,制备麦草纤维素微纤丝;对比例1与实施例1对比结果可知,从能耗测定上看,1.03kW·h大于865.9W·h,表明酶预处理后解离纤维能耗会降低,而且酶预处理后产品纤维素微纤丝的宽度范围变窄,尺寸更均匀,结晶度有所提高,性能得到改善。In Example 1, an endoglucanase pretreatment of 5% relative to the absolute dry mass of the fiber component was added to prepare wheat straw cellulose microfibrils; the comparative results of Comparative Example 1 and Example 1 show that, from the energy consumption measurement From the above, 1.03kW·h is greater than 865.9W·h, indicating that the energy consumption of dissociated fibers will be reduced after enzyme pretreatment, and the width range of the product cellulose microfibrils after enzyme pretreatment is narrowed, the size is more uniform, and the crystallinity is improved. performance is improved.

实施例2Example 2

其它条件同实施例1,仅内切葡聚糖酶的添加量相对纤维组分绝干质量为0.5%、2%、...25%和45%,制备麦草纤维素微纤丝,其性能测试结果如下表1所示;其中加酶量25%、均质10次得到的麦草纤维素微纤丝的扫描电镜图片(×100k)如附图3所示。Other conditions are the same as in Example 1, only the addition amount of endoglucanase is 0.5%, 2%, ... 25% and 45% relative to the absolute dry mass of the fiber component, to prepare wheat straw cellulose microfibrils, and its performance The test results are shown in Table 1 below; the scanning electron microscope pictures (×100k) of wheat straw cellulose microfibrils obtained by adding 25% enzyme and homogenizing 10 times are shown in Figure 3.

表1不同酶添加量制备的麦草纤维素微纤丝性能测试结果Table 1 Performance test results of wheat straw cellulose microfibrils prepared with different enzyme additions

酶添加量Enzyme addition 0.5%0.5% 2%2% 15%15% 25%25% 30%30% 45%45% 得率(%)Yield (%) 9393 8787 6868 5252 4848 4242 宽度(nm)Width (nm) 40~12040~120 40~11040~110 35~8535~85 30~8030~80 30~6530~65 25~6025~60 结晶度Crystallinity 71.6871.68 73.5373.53 75.7675.76 76.8676.86 76.3276.32 75.1375.13 聚合度Polymerization 287287 245245 221221 210210 189189 177177 能耗值(W·h)Energy consumption value (W h) 955.0955.0 794.3794.3 813.5813.5 672.9672.9 634.3634.3 624.6624.6

分析数据可知,其他条件不变,随着酶用量的增加,虽然产品麦草纤维素微纤丝的性能得到改善,宽度变得更加均匀,结晶度有所提高,聚合度下降,解离能耗有所降低,但是当酶用量增加到一定程度后,酶的成本提高,纤维素微纤丝的得率降低,过量的酶在有限的水解时间From the analysis data, it can be seen that, with other conditions unchanged, with the increase of the enzyme dosage, although the performance of the product wheat straw cellulose microfibrils is improved, the width becomes more uniform, the crystallinity increases, the degree of polymerization decreases, and the dissociation energy consumption decreases. However, when the amount of enzymes increases to a certain extent, the cost of enzymes increases, the yield of cellulose microfibrils decreases, and excess enzymes can be used in a limited hydrolysis time

内并没有发挥出最佳效果,因此综合考虑,选择内切葡聚糖的添加量在0.5%~25%间。Endo-glucan did not exert the best effect, so considering comprehensively, the addition amount of endo-glucan is selected to be between 0.5% and 25%.

实施例3Example 3

其它条件同实施例1,仅加酶量改为加入相对纤维组分绝干质量的25%,循环均质次数依次采用5、10、20、30和40次,制备麦草纤维素微纤丝,其中加酶量25%、均质5次得到的麦草纤维素的扫描电镜图片(×10k)如附图4所示,加酶量25%、均质30次得到的麦草纤维素微纤丝的扫描电镜图片(×100k)如附图5所示。Other conditions are the same as in Example 1, only the amount of enzyme added is changed to 25% of the absolute dry mass of the relative fiber component, and the number of cycles of homogenization is successively 5, 10, 20, 30 and 40 times to prepare wheat straw cellulose microfibrils. Wherein the scanning electron microscope picture (×10k) of the wheat straw cellulose that adds enzyme amount 25%, homogeneous 5 times obtains is as shown in accompanying drawing 4, adds enzyme amount 25%, the wheat straw cellulose microfibril that homogenizes 30 times obtains The scanning electron microscope picture (×100k) is shown in Figure 5.

结果表明:当均质次数为5次时,麦草纤维表面明显分丝起毛,纤维变短,暴露出微纤丝结构,但是微纤丝并没有完全被解离开;随着均质次数的增加,当均质次数为10次时,麦草纤维素微纤丝的宽度为30~80nm,结晶度(CrI%)76.86,聚合度(DP)210,能耗672.9W·h,当均质均质次数为30次时,制备的麦草纤维素微纤丝的宽度为25~40nm,分布均匀,结晶度(CrI%)69.87,聚合度(DP)165,能耗1.449kW·h。分析数据可知,其他条件不变,随着均质次数的增加,麦草纤维逐渐被解离成麦草纤维素微纤丝,而且纤维素微纤丝的宽度逐渐变得更窄,分布更加均匀,产品性能得到提高,但是解离能耗会逐渐增加,造成生产成本提高。综合考虑,选择均质次数在10~30次。The results showed that: when the number of homogenization was 5 times, the surface of the wheat straw fiber was obviously divided and fluffed, the fiber became shorter, and the microfibril structure was exposed, but the microfibrils were not completely dissociated; with the increase of the number of homogenization, When the number of homogenization is 10 times, the width of wheat straw cellulose microfibrils is 30-80nm, the degree of crystallinity (CrI%) is 76.86, the degree of polymerization (DP) is 210, and the energy consumption is 672.9W·h. When the number of times is 30, the width of the prepared wheat straw cellulose microfibrils is 25-40nm, the distribution is uniform, the crystallinity (CrI%) is 69.87, the degree of polymerization (DP) is 165, and the energy consumption is 1.449kW·h. The analysis of the data shows that, with other conditions unchanged, with the increase of homogenization times, the wheat straw fibers are gradually dissociated into wheat straw cellulose microfibrils, and the width of the cellulose microfibrils gradually becomes narrower and the distribution is more uniform. The performance is improved, but the dissociation energy consumption will gradually increase, resulting in an increase in production costs. Comprehensive consideration, choose the number of homogenization in 10 to 30 times.

由实施例1至3制备得到的实验结果可知,本发明所述的制备方法能够降低能耗,提高产品性能,获得的麦草纤维素微纤丝呈现乳白色凝胶状,如图6所示;微纤丝间相互交织成网状结构,直径为25~100nm,长度达到微米级,长径比较大且性能稳定,达到了纤维素微纤丝的质量要求。From the experimental results prepared in Examples 1 to 3, it can be seen that the preparation method of the present invention can reduce energy consumption and improve product performance, and the obtained wheat straw cellulose microfibrils present milky white gel, as shown in Figure 6; Fibrils interweave to form a network structure with a diameter of 25-100nm, a length of micron level, a relatively large length and diameter, and stable performance, which meets the quality requirements of cellulose microfibrils.

实施例4Example 4

将麦草浆进行筛分,收集截留在100目筛网上的纤维组分,用水浸泡润胀6h后,经疏解机疏解25min,挤干水分,用浓度为0.05mol/L的磷酸缓冲液配制成浓度为2%的纤维悬浮液;然后加入相对纤维组分绝干质量10%的国产固态内切葡聚糖酶进行水解,在恒温水浴振荡锅中保持温度50℃,振荡频率为120r/min,反应时间为60min。水解结束后放在沸水浴中煮沸灭活5min,然后经过蒸馏水充分洗涤,得到酶预处理后的纤维浆料;再将纤维浆料经过适当的机械搅拌,搅拌转速控制在6000r/min,搅拌时间5min,然后配制成质量分数为1%纤维悬浮液100mL,经过高压均质机的循环均质处理,控制高压均质机的操作压力在50MPa,循环次数为15次,制备出纤维素微纤丝乳状液;将得到的纤维素微纤丝乳状液在转速7000r/min下离心分离20min,取离心液经过纤维素超滤膜过滤,收集膜面截留的固体组分,得到麦草纤维素微纤丝。Sieve the wheat straw pulp, collect the fiber components trapped on the 100-mesh sieve, soak and swell with water for 6 hours, decompose for 25 minutes with a decomposer, squeeze out the water, and prepare the concentration with 0.05mol/L phosphate buffer solution 2% fiber suspension; then add domestic solid-state endoglucanase of 10% relative to the dry weight of the fiber component for hydrolysis, keep the temperature at 50°C in a constant temperature water bath oscillating pot, and the oscillating frequency is 120r/min, the reaction The time is 60 minutes. After the hydrolysis is completed, put it in a boiling water bath to boil and inactivate for 5 minutes, and then wash it thoroughly with distilled water to obtain the fiber slurry after enzyme pretreatment; then, the fiber slurry is stirred by appropriate machinery, and the stirring speed is controlled at 6000r/min. 5min, then be prepared into 100mL of fiber suspension with a mass fraction of 1%, through the circulation homogenization treatment of the high-pressure homogenizer, the operating pressure of the high-pressure homogenizer is controlled at 50MPa, and the number of cycles is 15 times to prepare cellulose microfibrils Emulsion: centrifuge the obtained cellulose microfibril emulsion at a speed of 7000r/min for 20min, take the centrifugate and filter it through a cellulose ultrafiltration membrane, collect the solid components retained on the membrane surface, and obtain wheat straw cellulose microfibrils .

实施例5Example 5

将麦草浆进行筛分,收集截留在100目筛网上的纤维组分,用水浸泡润胀18h后,经疏解机疏解10min,挤干水分,用浓度为0.05mol/L的磷酸缓冲液配制成浓度为4%的纤维悬浮液;然后加入相对纤维组分绝干质量15%的国产固态内切葡聚糖酶进行水解,在恒温水浴振荡锅中保持温度55℃,振荡频率为110r/min,反应时间为90min。水解结束后放在沸水浴中煮沸灭活5min,然后经过蒸馏水充分洗涤,得到酶预处理后的纤维浆料;再将纤维浆料经过适当的机械搅拌,搅拌转速控制在5000r/min,搅拌时间8min,然后配制成质量分数为1.5%纤维悬浮液100mL,经过高压均质机的循环均质处理,控制高压均质机的操作压力在100MPa,循环次数为25次,制备出纤维素微纤丝乳状液;将得到的纤维素微纤丝乳状液在转速6000r/min下离心分离25min,取离心液经过纤维素超滤膜过滤,收集膜面截留的固体组分,得到麦草纤维素微纤丝。Sieve the wheat straw pulp, collect the fiber components trapped on the 100-mesh sieve, soak and swell with water for 18 hours, then disperse it with a decomposer for 10 minutes, squeeze out the water, and prepare the concentration with 0.05mol/L phosphate buffer solution. 4% fiber suspension; then add domestic solid-state endoglucanase of 15% relative to the absolute dry mass of the fiber component for hydrolysis, keep the temperature at 55°C in a constant temperature water bath oscillating pot, and the oscillation frequency is 110r/min, and the reaction The time is 90 minutes. After the hydrolysis is completed, put it in a boiling water bath to boil and inactivate for 5 minutes, and then wash it thoroughly with distilled water to obtain the fiber slurry after enzyme pretreatment; then, the fiber slurry is stirred by appropriate machinery, and the stirring speed is controlled at 5000r/min. 8min, and then it is prepared into 100mL of fiber suspension with a mass fraction of 1.5%. After the circulation homogenization treatment of the high-pressure homogenizer, the operating pressure of the high-pressure homogenizer is controlled at 100MPa, and the number of cycles is 25 times to prepare cellulose microfibrils. Emulsion: centrifuge the obtained cellulose microfibril emulsion at a speed of 6000r/min for 25min, take the centrifugate and filter it through a cellulose ultrafiltration membrane, collect the solid components retained on the membrane surface, and obtain wheat straw cellulose microfibrils .

实施例6Example 6

将麦草浆进行筛分,收集截留在100目筛网上的纤维组分,用水浸泡润胀10h后,经疏解机疏解15min,挤干水分,用浓度为0.05mol/L的磷酸缓冲液配制成浓度为5%的纤维悬浮液;然后加入相对纤维组分绝干质量20%的国产固态内切葡聚糖酶进行水解,在恒温水浴振荡锅中保持温度60℃,振荡频率为90r/min,反应时间为30min。水解结束后放在沸水浴中煮沸灭活5min,然后经过蒸馏水充分洗涤,得到酶预处理后的纤维浆料;再将纤维浆料经过适当的机械搅拌,搅拌转速控制在10000r/min,搅拌时间12min,然后配制成质量分数为1.2%纤维悬浮液100mL,经过高压均质机的循环均质处理,控制高压均质机的操作压力在90MPa,循环次数为18次,制备出纤维素微纤丝乳状液;将得到的纤维素微纤丝乳状液在转速5000r/min下离心分离15min,取离心液经过纤维素超滤膜过滤,收集膜面截留的固体组分,得到麦草纤维素微纤丝。Sieve the wheat straw pulp, collect the fiber components trapped on the 100-mesh sieve, soak and swell with water for 10 hours, decompose for 15 minutes with a decomposer, squeeze out the water, and prepare the concentration with 0.05mol/L phosphate buffer solution. 5% fiber suspension; then add domestic solid-state endoglucanase of 20% relative to the dry weight of the fiber component for hydrolysis, keep the temperature at 60°C in a constant temperature water bath oscillating pot, and the oscillation frequency is 90r/min, and the reaction The time is 30 minutes. After the hydrolysis is completed, put it in a boiling water bath to boil and inactivate for 5 minutes, and then fully wash with distilled water to obtain the fiber slurry after enzyme pretreatment; then the fiber slurry is properly mechanically stirred, and the stirring speed is controlled at 10000r/min. 12min, then it is prepared into 100mL of fiber suspension with a mass fraction of 1.2%. After the circulation homogenization treatment of the high-pressure homogenizer, the operating pressure of the high-pressure homogenizer is controlled at 90MPa, and the number of cycles is 18 times to prepare cellulose microfibrils. Emulsion: centrifuge the obtained cellulose microfibril emulsion at a rotating speed of 5000r/min for 15min, take the centrifugate and filter it through a cellulose ultrafiltration membrane, collect the solid components intercepted on the membrane surface, and obtain wheat straw cellulose microfibrils .

实施例7Example 7

将麦草浆进行筛分,收集截留在100目筛网上的纤维组分,用水浸泡润胀15h后,经疏解机疏解20min,挤干水分,用浓度为0.05mol/L的磷酸缓冲液配制成浓度为1%的纤维悬浮液;然后加入相对纤维组分绝干质量8%的国产固态内切葡聚糖酶进行水解,在恒温水浴振荡锅中保持温度65℃,振荡频率为80r/min,反应时间为180min。水解结束后放在沸水浴中煮沸灭活5min,然后经过蒸馏水充分洗涤,得到酶预处理后的纤维浆料;再将纤维浆料经过适当的机械搅拌,搅拌转速控制在9000r/min,搅拌时间15min,然后配制成质量分数为0.8%纤维悬浮液100mL,经过高压均质机的循环均质处理,控制高压均质机的操作压力在60MPa,循环次数为20次,制备出纤维素微纤丝乳状液;将得到的纤维素微纤丝乳状液在转速4000r/min下离心分离10min,取离心液经过纤维素超滤膜过滤,收集膜面截留的固体组分,得到麦草纤维素微纤丝。Sieve the wheat straw pulp, collect the fiber components trapped on the 100-mesh sieve, soak and swell with water for 15 hours, then disperse it with a decomposer for 20 minutes, squeeze out the water, and prepare a concentration of 0.05mol/L with phosphate buffer solution 1% fiber suspension; then add domestic solid-state endoglucanase of 8% relative to the absolute dry mass of the fiber component for hydrolysis, keep the temperature at 65°C in a constant temperature water bath oscillating pot, and the oscillating frequency is 80r/min, the reaction The time is 180min. After the hydrolysis is completed, put it in a boiling water bath to boil and inactivate for 5 minutes, and then wash it thoroughly with distilled water to obtain the fiber slurry after enzyme pretreatment; then, the fiber slurry is stirred by appropriate machinery, and the stirring speed is controlled at 9000r/min. 15min, then it is prepared into 100mL of fiber suspension with a mass fraction of 0.8%. After the circulation homogenization treatment of the high-pressure homogenizer, the operating pressure of the high-pressure homogenizer is controlled at 60MPa, and the number of cycles is 20 times to prepare cellulose microfibrils. Emulsion: centrifuge the obtained cellulose microfibril emulsion at a rotating speed of 4000r/min for 10min, take the centrifugate and filter it through a cellulose ultrafiltration membrane, collect the solid components intercepted on the membrane surface, and obtain wheat straw cellulose microfibrils .

本发明公开了一种酶预处理辅助制备麦草纤维素微纤丝的方法,是选取麦草浆为原料,筛出细杂组分后将得到的纤维组分经过水浸泡,然后加入相对纤维组分绝干质量0.5%~25%的纤维素酶进行水解,在45~65℃水浴振荡水浴锅中处理30~180min,得到酶预处理后的纤维浆料;适当搅拌剪切后经过高压均质机的机械解离作用,均质循环次数为10~30次,得到麦草纤维素微纤丝乳状液,经由纤维素超滤膜过滤收集得到乳白色凝胶状的麦草纤维素微纤丝产品。麦草纤维经过本发明方法后制备出了纤维素微纤丝,有利于扩大纤维原料来源,缓解直接焚烧麦草秸秆带来的资源浪费和环境污染,实现了对农作物废弃物的高值化再利用,而且可以降低机械解离能耗,减少环境污染,提高产品性能,具有良好的经济效益和环保效益。同时,本发明在高压均质化处理前对麦草纤维进行合适的预处理,克服现有技术存在的部分缺陷,有利于纤维素微纤丝制备技术的进一步优化和节能环保。The invention discloses a method for preparing wheat straw cellulose microfibrils assisted by enzyme pretreatment. The method is to select wheat straw pulp as raw material, sieve out fine and impurity components, soak the obtained fiber components in water, and then add relative fiber components. Cellulase with 0.5% to 25% of absolute dry mass is hydrolyzed, and treated in a oscillating water bath at 45 to 65°C for 30 to 180 minutes to obtain fiber slurry after enzyme pretreatment; after proper stirring and shearing, it passes through a high pressure homogenizer The mechanical dissociation effect of the homogenization cycle is 10 to 30 times to obtain the wheat straw cellulose microfibril emulsion, which is collected by filtration through a cellulose ultrafiltration membrane to obtain a milky white gelatinous wheat straw cellulose microfibril product. The cellulose microfibrils are prepared from wheat straw fiber through the method of the present invention, which is conducive to expanding the source of fiber raw materials, alleviating resource waste and environmental pollution caused by direct burning of wheat straw straw, and realizing high-value reuse of crop waste. Moreover, it can reduce the energy consumption of mechanical dissociation, reduce environmental pollution, improve product performance, and have good economic and environmental benefits. At the same time, the invention properly pretreats the wheat straw fiber before the high-pressure homogenization treatment, overcomes some defects in the prior art, and is beneficial to the further optimization of the cellulose microfibril preparation technology and energy saving and environmental protection.

Claims (9)

1.一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:包括以下步骤:1. a kind of enzyme pretreatment assists the method for preparing wheat straw cellulose microfibril, it is characterized in that: comprise the following steps: (1)将麦草浆进行筛分处理,收集截留在筛网上的纤维组分;(1) Sieving the wheat straw pulp to collect the fiber components trapped on the sieve; (2)将步骤(1)得到的纤维组分用缓冲液配制成质量浓度为1%~5%的纤维悬浮液,再向纤维悬浮液中加入纤维素酶进行水解,得到酶预处理后的纤维浆料;其中纤维素酶的加入量是纤维组分绝干质量的0.5%~25%;(2) The fiber component obtained in step (1) is prepared into a fiber suspension with a mass concentration of 1% to 5% with a buffer, and then cellulase is added to the fiber suspension for hydrolysis to obtain enzyme pretreated Fiber slurry; wherein the amount of cellulase added is 0.5% to 25% of the absolute dry mass of the fiber component; (3)将步骤(2)中得到的酶预处理后的纤维浆料经过机械搅拌剪切;(3) the fiber slurry obtained in step (2) after the enzyme pretreatment is subjected to mechanical stirring and shearing; (4)将步骤(3)中机械搅拌剪切后的纤维浆料配制成质量浓度为0.5~1.5%的纤维悬浮液,进行循环均质处理,制备出纤维素微纤丝乳状液;(4) preparing the fiber slurry after mechanically agitating and shearing in step (3) into a fiber suspension with a mass concentration of 0.5 to 1.5%, and performing a circulation homogenization treatment to prepare a cellulose microfibril emulsion; (5)将纤维素微纤丝乳状液依次进行离心分离和过滤,得到麦草纤维素微纤丝。(5) Centrifuging and filtering the cellulose microfibril emulsion in sequence to obtain wheat straw cellulose microfibrils. 2.根据权利要求1所述的一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:步骤(1)中的筛网为100目。2. A kind of enzyme pretreatment-assisted method for preparing wheat straw cellulose microfibrils according to claim 1, characterized in that: the sieve in step (1) is 100 mesh. 3.根据权利要求1所述的一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:步骤(2)中纤维组分先用水浸泡润胀6~18h,经疏解机疏解10~30min,挤干水分再配制成纤维悬浮液。3. A method for preparing wheat straw cellulose microfibrils assisted by enzyme pretreatment according to claim 1, characterized in that: in step (2), the fiber components are first soaked and swelled in water for 6-18 hours, and then decomposed by a decomposer After 10-30 minutes, squeeze out the water and make a fiber suspension. 4.根据权利要求1所述的一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:步骤(2)中缓冲液采用的是浓度为0.05mol/L的磷酸缓冲液。4. A method for preparing wheat straw cellulose microfibrils assisted by enzyme pretreatment according to claim 1, characterized in that: the buffer used in step (2) is a phosphate buffer with a concentration of 0.05mol/L. 5.根据权利要求1所述的一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:步骤(2)中纤维素酶采用的是活性为50000u/g的固态内切葡聚糖酶。5. a kind of enzyme pretreatment according to claim 1 assists the method for preparing wheat straw cellulose microfibril, it is characterized in that: what cellulase adopts in step (2) is that activity is the solid-state endoglucose of 50000u/g Glycanase. 6.根据权利要求1所述的一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:步骤(2)中水解是在45~65℃的恒温水浴振荡锅中进行的,振荡频率为80~120r/min,水解时间为30~180min。6. A method for assisting preparation of wheat straw cellulose microfibrils by enzyme pretreatment according to claim 1, characterized in that: the hydrolysis in step (2) is carried out in a constant temperature water bath oscillating pot at 45-65°C, The oscillation frequency is 80-120r/min, and the hydrolysis time is 30-180min. 7.根据权利要求1所述的一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:步骤(3)中搅拌转速在5000~10000r/min,搅拌时间在5~15min。7. A method for preparing wheat straw cellulose microfibrils assisted by enzyme pretreatment according to claim 1, characterized in that: in step (3), the stirring speed is 5000-10000r/min, and the stirring time is 5-15min. 8.根据权利要求1所述的一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:步骤(4)的循环均质处理中,压力在50~100MPa,循环次数为10~30次。8. A method for preparing wheat straw cellulose microfibrils assisted by enzyme pretreatment according to claim 1, characterized in that: in the circulation homogenization treatment of step (4), the pressure is 50-100 MPa, and the number of cycles is 10 ~30 times. 9.根据权利要求1所述的一种酶预处理辅助制备麦草纤维素微纤丝的方法,其特征在于:步骤(5)中纤维素微纤丝乳状液在转速4000~8000r/min下离心分离10~30min。9. A method for preparing wheat straw cellulose microfibrils assisted by enzyme pretreatment according to claim 1, characterized in that: in step (5), the cellulose microfibril emulsion is centrifuged at a rotating speed of 4000 to 8000r/min Separation for 10-30 minutes.
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