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CN109183495B - Preparation method of high-transparency transparent paper using bismuth-containing material - Google Patents

Preparation method of high-transparency transparent paper using bismuth-containing material Download PDF

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CN109183495B
CN109183495B CN201811119560.3A CN201811119560A CN109183495B CN 109183495 B CN109183495 B CN 109183495B CN 201811119560 A CN201811119560 A CN 201811119560A CN 109183495 B CN109183495 B CN 109183495B
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bismuth
parts
suspension
transparent paper
containing material
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CN109183495A (en
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王晓芳
余长春
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Hubei Yi Meng packing material Co.,Ltd.
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Hubei Yi Meng Packing Material Co ltd
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    • 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
    • D21H15/00Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
    • D21H15/02Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
    • D21H15/10Composite fibres
    • 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
    • D21C9/00After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001Modification of pulp properties
    • D21C9/002Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21FPAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
    • D21F13/00Making discontinuous sheets of paper, pulpboard or cardboard, or of wet web, for fibreboard production
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21FPAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
    • D21F13/00Making discontinuous sheets of paper, pulpboard or cardboard, or of wet web, for fibreboard production
    • D21F13/10Making discontinuous sheets of paper, pulpboard or cardboard, or of wet web, for fibreboard production using board presses
    • 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
    • D21H11/08Mechanical or thermomechanical 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
    • D21H11/16Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
    • D21H11/20Chemically or biochemically modified fibres

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Biochemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Paper (AREA)

Abstract

本发明涉及造纸新材料制备领域,具体关于一种使用含铋材料的高透明度透明纸的制备方法;本发明方法公开的一种使用含铋材料的高透明度透明纸的制备方法,本发明制备成了一种含铋纳米纤维素悬浮液,用该种含铋纳米纤维素悬浮液填充木材纤维网络的多孔结构,提高了的光线透过率,经过热压,制备除了一种使用含铋材料的高透明度透明纸。这种透明纸不仅具有优异的光学性能和表面粗糙度,同时还保留了传统纸张的可书写性能,可用与手绘导电电路器件的制备;具有优异的形态稳定性,满足后续水性涂布的要求。The invention relates to the field of preparation of new materials for papermaking, in particular to a method for preparing high-transparency transparent paper using bismuth-containing materials; the method of the invention discloses a method for preparing high-transparency transparent paper using bismuth-containing materials. A bismuth-containing nanocellulose suspension is used to fill the porous structure of the wood fiber network with the bismuth-containing nanocellulose suspension, and the light transmittance is improved. High transparency transparent paper. This transparent paper not only has excellent optical properties and surface roughness, but also retains the writable properties of traditional paper, which can be used for the preparation of hand-painted conductive circuit devices; it has excellent morphological stability and meets the requirements of subsequent water-based coating.

Description

一种使用含铋材料的高透明度透明纸的制备方法A kind of preparation method of high transparency transparent paper using bismuth-containing material

技术领域technical field

本发明涉及材料制备领域,具体关于一种使用含铋材料的高透明度透明纸的制备方法。The invention relates to the field of material preparation, in particular to a preparation method of high-transparency transparent paper using a bismuth-containing material.

背景技术Background technique

透明纸属于一种特种纸,因具有优良的光学性能和美观的视觉效果,广泛应用于标签、装饰、食品包装、绝缘等领域,更有望取代塑料薄膜来制备下一代“绿色”电子器件;因其轻质、低成本的优点,也是应用于透光建筑物和太阳能电池的绝佳材料。Transparent paper is a kind of special paper. Because of its excellent optical properties and beautiful visual effects, it is widely used in labels, decoration, food packaging, insulation and other fields. It is more expected to replace plastic films to prepare the next generation of "green" electronic devices; Its light weight and low cost make it an excellent material for light-transmitting buildings and solar cells.

CN106917311A公开了一种透明纸的制备方法,属于纳米/微米微结构材料及其制备技术。该发明所指的透明纸是指由纳米级和微米级木质纤维材料组成的、透明度大于70%的纤维材料。其制备方法为:将木质材料加工成木屑或木粉;然后将这些木屑或木粉与次氯酸钠溶液在一定温度下混合反应一定时间,去除木质材料中的木质素;用水多次清洗去除反应结束残留的次氯酸钠,再将清洗后的浆料去除大部分水;将经上述步骤得到的产物置于压机中,在一定压力下保压一段时间,去除剩余的水分,获得透明纸。该发明的方法具有可适用木质材料种类多、成本低、资源丰富、易于操作、环境友好、高产出,不需要复杂的设备与器件,可大批量快速生产的特点。CN106917311A discloses a preparation method of transparent paper, which belongs to nano/micron microstructure materials and preparation technology thereof. The transparent paper referred to in the invention refers to the fiber material composed of nano-scale and micro-scale wood fiber material and whose transparency is greater than 70%. The preparation method is as follows: processing the wood material into wood chips or wood powder; then mixing the wood chips or wood powder with a sodium hypochlorite solution at a certain temperature for a certain period of time to remove the lignin in the wood material; washing with water for multiple times to remove the residue after the reaction Then, most of the water is removed from the cleaned slurry; the product obtained through the above steps is placed in a press, and kept under a certain pressure for a period of time to remove the remaining water to obtain transparent paper. The method of the invention has the characteristics of many types of applicable wood materials, low cost, abundant resources, easy operation, environmental friendliness, high output, no need for complicated equipment and devices, and can be quickly produced in large quantities.

CN106012667A公开一种全纤维素透明纸及其制备方法,以传统造纸工艺得到的纸张或植物纤维为网络骨架,以一定溶解度的纤维素均相溶液为填充剂和溶解介质,均匀涂布到纸张或植物纤维表面,以高效率、低成本的方式填充内部孔隙和溶解纤维素侧链或部分纤维素,降低孔隙率;通过后期整饰工艺提高平整度,形成一体化的纤维素复合结构,进而制备一种全新的低成本全纤维素透明纸,有望实现大规模的卷对卷工业化生产。CN106012667A discloses an all-cellulose transparent paper and a preparation method thereof. The paper or plant fiber obtained by the traditional papermaking process is used as the network skeleton, and the homogeneous cellulose solution with a certain solubility is used as the filler and dissolving medium, and the paper is evenly coated on the paper or the dissolving medium. The surface of plant fiber fills the internal pores and dissolves cellulose side chains or part of cellulose in a high-efficiency and low-cost manner to reduce the porosity; improve the flatness through the post-finishing process to form an integrated cellulose composite structure, and then prepare A new low-cost all-cellulose transparent paper is expected to achieve large-scale roll-to-roll industrial production.

CN106915121A公开了一种具有表面微结构透明纸的制备方法,属于纳米/微米微结构材料及其制备技术。该发明的制备方法为:先将木材切成单板,然后将单板置于次氯酸钠溶液中反应一段时间,以去除木素;待木素去除之后,将处理过的单板放于具有微结构的模板上,同时在单板上方垫以滤膜,并通过机械加压的方式将模板的图案转移到透明纸表面,从而得到表面具有微结构的透明纸。该发明的方法与其它现有方法相比,具有成本低、制备步骤简单、制备时间短等特点。CN106915121A discloses a preparation method of transparent paper with surface microstructure, belonging to nano/micron microstructure material and preparation technology thereof. The preparation method of the invention is as follows: firstly, the wood is cut into veneers, and then the veneer is placed in a sodium hypochlorite solution to react for a period of time to remove the lignin; after the lignin is removed, the treated veneer is placed in a microstructure At the same time, a filter membrane is placed above the veneer, and the pattern of the template is transferred to the surface of the transparent paper by means of mechanical pressure, so as to obtain the transparent paper with microstructures on the surface. Compared with other existing methods, the method of the invention has the characteristics of low cost, simple preparation steps, short preparation time and the like.

以上专利以及现有技术制备的透明纸的生产方法主要有三种:过滤、挤出成型和浸渍,其生产的纸品的透明度一般都小于80%,而且纸张的表面粗糙度较高,不能满足例如电子器件等领域的要求,限制了透明纸的应用范围。There are mainly three production methods for the transparent paper prepared by the above patents and the prior art: filtration, extrusion molding and dipping. The transparency of the paper products produced by them is generally less than 80%, and the surface roughness of the paper is relatively high, which cannot meet the requirements of, for example, Requirements in fields such as electronic devices limit the application range of transparent paper.

发明内容SUMMARY OF THE INVENTION

为了解决上述问题,本发明提供了一种使用含铋材料的高透明度透明纸的制备方法。In order to solve the above problems, the present invention provides a preparation method of high-transparency transparent paper using bismuth-containing material.

一种使用含铋材料的高透明度透明纸的制备方法,制备技术方案如下:A kind of preparation method of the high-transparency transparent paper using bismuth-containing material, the preparation technical scheme is as follows:

按照质量份数,将0.5-2份的木浆纤维分散于80-150份的去离子水中,然后加入50-80份的含铋纳米纤维素悬浮液,搅拌均匀后超声分散20-30min,形成混悬液备用;然后另取20-40份的含铋纳米纤维素悬浮液,使用微孔滤膜过滤,形成一层纳米纤维素层;然后将混悬液继续在该微孔滤膜上过滤,形成纤维素层;将纤维素层从微孔滤膜上剥离下来,使用清洁平整的模具放入到50-70℃的热压机上进行热压30-60min,然后关掉热压机的加热系统,保压条件下冷却,即可得到所述的一种使用含铋材料的高透明度透明纸。According to the parts by mass, 0.5-2 parts of wood pulp fibers are dispersed in 80-150 parts of deionized water, then 50-80 parts of bismuth-containing nanocellulose suspension are added, and after stirring evenly, ultrasonically disperse for 20-30 minutes to form The suspension is for subsequent use; then another 20-40 parts of the bismuth-containing nanocellulose suspension is taken, and filtered with a microporous membrane to form a layer of nanocellulose; then the suspension is continued to be filtered on the microporous membrane , to form a cellulose layer; peel off the cellulose layer from the microporous filter membrane, use a clean and flat mold to put it into a hot press at 50-70 ° C for 30-60min, and then turn off the heating of the hot press system, and cooling under pressure-holding conditions, the high-transparency transparent paper using the bismuth-containing material can be obtained.

所述的含铋纳米纤维素悬浮液按照以下方法制备:The described bismuth-containing nanocellulose suspension is prepared according to the following method:

按照质量份数,将2-10份的木浆纤维分散于100-200份的二甲基亚砜中,然后加入0.8-1.8份的氢氧化钠、0.2-1份的2-(三甲基硅烷基)乙氧甲基氯、0.01-0.05份的4-氧-2,2,6,6-四甲基哌啶-1-氧自由基和0.1-0.5份的铋六氟-2,4-戊二酮酸,控温50-60℃,搅拌反应40-60min;完成反应后将5-15份的次氯酸钠加入到反应釜中,升温到70-80℃,反应5-10h;完成反应后过滤,用大量的去离子水洗涤三次;然后将纤维配制成0.5%-5%的悬浮液,采用高压匀质机,匀质,离心后取上清液即可得到所述的含铋纳米纤维素悬浮液。According to the parts by mass, 2-10 parts of wood pulp fibers are dispersed in 100-200 parts of dimethyl sulfoxide, and then 0.8-1.8 parts of sodium hydroxide, 0.2-1 parts of 2-(trimethyl sulfoxide) are added. Silyl)ethoxymethyl chloride, 0.01-0.05 parts of 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical and 0.1-0.5 parts of bismuth hexafluoro-2,4 - pentanedione acid, the temperature is controlled at 50-60°C, and the reaction is stirred for 40-60min; after the reaction is completed, 5-15 parts of sodium hypochlorite is added to the reaction kettle, the temperature is raised to 70-80°C, and the reaction is performed for 5-10h; after the reaction is completed Filter, wash three times with a large amount of deionized water; then prepare the fiber into a 0.5%-5% suspension, use a high-pressure homogenizer, homogenize, and take the supernatant after centrifugation to obtain the bismuth-containing nanofibers Suspension.

所述的木浆纤维为漂白针叶木浆或阔叶木浆。The wood pulp fiber is bleached softwood pulp or hardwood pulp.

所述的微孔滤膜为孔径为0.3-0.8μm的聚四氟乙烯滤膜。The microporous filter membrane is a polytetrafluoroethylene filter membrane with a pore size of 0.3-0.8 μm.

所述的热压机热压压力为3-7MPa。The hot pressing pressure of the hot press is 3-7MPa.

本发明方法公开的一种使用含铋材料的高透明度透明纸的制备方法,本发明将木浆纤维分散于二甲基亚砜中,然后在氢氧化钠、2-(三甲基硅烷基)乙氧甲基氯、4-氧-2,2,6,6-四甲基哌啶-1-氧自由基和铋六氟-2,4-戊二酮酸的环境中处理一段时间;然后用次氯酸钠与纤维素反应,制备成了一种含铋络合物的纳米纤维素悬浮液,用该种含铋纳米纤维素悬浮液填充木材纤维网络的多孔结构,提高了的光线透过率,经过热压,制备除了一种使用含铋材料的高透明度透明纸。这种透明纸不仅具有优异的光学性能和表面粗糙度,同时还保留了传统纸张的可书写性能,可用与手绘导电电路器件的制备;具有优异的形态稳定性,满足后续水性涂布的要求。The method of the invention discloses a preparation method of high-transparency transparent paper using bismuth-containing materials. In the invention, wood pulp fibers are dispersed in dimethyl sulfoxide, and then mixed with sodium hydroxide, 2-(trimethylsilyl) Ethoxymethyl chloride, 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical and bismuth hexafluoro-2,4-pentanedione acid for a period of time; then A kind of nanocellulose suspension containing bismuth complex is prepared by reacting sodium hypochlorite with cellulose, and the porous structure of wood fiber network is filled with this kind of nanocellulose suspension containing bismuth, which improves the light transmittance, After hot pressing, a high-transparency transparent paper using bismuth-containing material was prepared. This transparent paper not only has excellent optical properties and surface roughness, but also retains the writable properties of traditional paper, which can be used for the preparation of hand-painted conductive circuit devices; it has excellent morphological stability and meets the requirements of subsequent water-based coating.

具体实施方式Detailed ways

下面通过具体实施例对该发明作进一步说明:This invention is further described below by specific embodiment:

实施例1Example 1

一种使用含铋材料的高透明度透明纸的制备方法,制备技术方案如下:A kind of preparation method of the high-transparency transparent paper using bismuth-containing material, the preparation technical scheme is as follows:

按照质量份数,将1.3份的木浆纤维分散于120份的去离子水中,然后加入60份的含铋纳米纤维素悬浮液,搅拌均匀后超声分散25min,形成混悬液备用;然后另取30份的含铋纳米纤维素悬浮液,使用微孔滤膜过滤,形成一层纳米纤维素层;然后将混悬液继续在该微孔滤膜上过滤,形成纤维素层;将纤维素层从微孔滤膜上剥离下来,使用清洁平整的模具放入到60℃的热压机上进行热压40min,然后关掉热压机的加热系统,保压条件下冷却,即可得到所述的一种使用含铋材料的高透明度透明纸。According to the parts by mass, 1.3 parts of wood pulp fibers were dispersed in 120 parts of deionized water, then 60 parts of bismuth-containing nanocellulose suspension were added, and after stirring, ultrasonically dispersed for 25 minutes to form a suspension for later use; 30 parts of the bismuth-containing nanocellulose suspension was filtered using a microporous membrane to form a layer of nanocellulose; then the suspension was continuously filtered on the microporous membrane to form a cellulose layer; the cellulose layer was Peel off from the microporous filter membrane, put a clean and flat mold into a hot press at 60°C for 40 minutes, then turn off the heating system of the hot press, and cool under pressure-holding conditions to obtain the described A high-transparency transparent paper using bismuth-containing materials.

所述的含铋纳米纤维素悬浮液按照以下方法制备:The described bismuth-containing nanocellulose suspension is prepared according to the following method:

按照质量份数,将5份的木浆纤维分散于150份的二甲基亚砜中,然后加入1.2份的氢氧化钠、0.6份的2-(三甲基硅烷基)乙氧甲基氯、0.03份的4-氧-2,2,6,6-四甲基哌啶-1-氧自由基和0.3份的铋六氟-2,4-戊二酮酸,控温55℃,搅拌反应50min;完成反应后将10份的次氯酸钠加入到反应釜中,升温到75℃,反应8h;完成反应后过滤,用大量的去离子水洗涤三次;然后将纤维配制成2.5%的悬浮液,采用高压匀质机,匀质,离心后取上清液即可得到所述的含铋纳米纤维素悬浮液。According to the parts by mass, 5 parts of wood pulp fibers are dispersed in 150 parts of dimethyl sulfoxide, and then 1.2 parts of sodium hydroxide and 0.6 parts of 2-(trimethylsilyl)ethoxymethyl chloride are added. , 0.03 part of 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical and 0.3 part of bismuth hexafluoro-2,4-pentanedione acid, temperature controlled at 55°C, stirring The reaction was carried out for 50 minutes; after the reaction was completed, 10 parts of sodium hypochlorite were added to the reaction kettle, the temperature was raised to 75 ° C, and the reaction was carried out for 8 hours; after the reaction was completed, the reaction was filtered and washed three times with a large amount of deionized water; then the fibers were prepared into a 2.5% suspension, The bismuth-containing nanocellulose suspension can be obtained by using a high-pressure homogenizer to homogenize and centrifuge the supernatant.

所述的木浆纤维为漂白针叶木浆。The wood pulp fiber is bleached softwood pulp.

所述的微孔滤膜为孔径为0.5μm的聚四氟乙烯滤膜。The microporous filter membrane is a polytetrafluoroethylene filter membrane with a pore size of 0.5 μm.

所述的热压机热压压力为5MPa。The hot pressing pressure of the hot press is 5MPa.

本实验制备的透明纸的透明度为91.6%,其抗张强度为102.7MPa。The transparency of the transparent paper prepared in this experiment is 91.6%, and its tensile strength is 102.7MPa.

实施例2Example 2

一种使用含铋材料的高透明度透明纸的制备方法,制备技术方案如下:A kind of preparation method of the high-transparency transparent paper using bismuth-containing material, the preparation technical scheme is as follows:

按照质量份数,将0.5份的木浆纤维分散于80份的去离子水中,然后加入50份的含铋纳米纤维素悬浮液,搅拌均匀后超声分散20min,形成混悬液备用;然后另取20份的含铋纳米纤维素悬浮液,使用微孔滤膜过滤,形成一层纳米纤维素层;然后将混悬液继续在该微孔滤膜上过滤,形成纤维素层;将纤维素层从微孔滤膜上剥离下来,使用清洁平整的模具放入到50℃的热压机上进行热压30min,然后关掉热压机的加热系统,保压条件下冷却,即可得到所述的一种使用含铋材料的高透明度透明纸。According to the parts by mass, 0.5 parts of wood pulp fibers were dispersed in 80 parts of deionized water, then 50 parts of bismuth-containing nanocellulose suspension were added, and after stirring evenly, ultrasonically dispersed for 20 minutes to form a suspension for later use; 20 parts of the bismuth-containing nanocellulose suspension was filtered using a microporous membrane to form a layer of nanocellulose; then the suspension was continuously filtered on the microporous membrane to form a cellulose layer; the cellulose layer was Peel off the microporous filter membrane, put a clean and flat mold into a hot press at 50°C for 30 minutes, then turn off the heating system of the hot press, and cool under pressure-holding conditions to obtain the A high-transparency transparent paper using bismuth-containing materials.

所述的含铋纳米纤维素悬浮液按照以下方法制备:The described bismuth-containing nanocellulose suspension is prepared according to the following method:

按照质量份数,将2份的木浆纤维分散于100份的二甲基亚砜中,然后加入0.8份的氢氧化钠、0.2份的2-(三甲基硅烷基)乙氧甲基氯、0.01份的4-氧-2,2,6,6-四甲基哌啶-1-氧自由基和0.1份的铋六氟-2,4-戊二酮酸,控温50℃,搅拌反应40min;完成反应后将5份的次氯酸钠加入到反应釜中,升温到70℃,反应5h;完成反应后过滤,用大量的去离子水洗涤三次;然后将纤维配制成0.5%的悬浮液,采用高压匀质机,匀质,离心后取上清液即可得到所述的含铋纳米纤维素悬浮液。According to the parts by mass, 2 parts of wood pulp fibers are dispersed in 100 parts of dimethyl sulfoxide, and then 0.8 parts of sodium hydroxide and 0.2 parts of 2-(trimethylsilyl)ethoxymethyl chloride are added. , 0.01 part of 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical and 0.1 part of bismuth hexafluoro-2,4-pentanedione acid, temperature controlled at 50°C, stirring The reaction was carried out for 40 minutes; after the reaction was completed, 5 parts of sodium hypochlorite was added to the reaction kettle, the temperature was raised to 70 ° C, and the reaction was carried out for 5 hours; after the reaction was completed, filtration was performed and washed three times with a large amount of deionized water; then the fibers were prepared into a 0.5% suspension, The bismuth-containing nanocellulose suspension can be obtained by using a high-pressure homogenizer to homogenize and centrifuge the supernatant.

所述的木浆纤维为阔叶木浆。The wood pulp fiber is hardwood pulp.

所述的微孔滤膜为孔径为0.3μm的聚四氟乙烯滤膜。The microporous filter membrane is a polytetrafluoroethylene filter membrane with a pore size of 0.3 μm.

所述的热压机热压压力为3MPa。The hot pressing pressure of the hot press is 3MPa.

本实验制备的透明纸的透明度为89.7%,其抗张强度为98.3MPa。The transparency of the transparent paper prepared in this experiment is 89.7%, and its tensile strength is 98.3MPa.

实施例3Example 3

一种使用含铋材料的高透明度透明纸的制备方法,制备技术方案如下:A kind of preparation method of the high-transparency transparent paper using bismuth-containing material, the preparation technical scheme is as follows:

按照质量份数,将2份的木浆纤维分散于150份的去离子水中,然后加入80份的含铋纳米纤维素悬浮液,搅拌均匀后超声分散30min,形成混悬液备用;然后另取40份的含铋纳米纤维素悬浮液,使用微孔滤膜过滤,形成一层纳米纤维素层;然后将混悬液继续在该微孔滤膜上过滤,形成纤维素层;将纤维素层从微孔滤膜上剥离下来,使用清洁平整的模具放入到70℃的热压机上进行热压60min,然后关掉热压机的加热系统,保压条件下冷却,即可得到所述的一种使用含铋材料的高透明度透明纸。According to the parts by mass, 2 parts of wood pulp fibers were dispersed in 150 parts of deionized water, then 80 parts of bismuth-containing nanocellulose suspension were added, and after stirring evenly, ultrasonically dispersed for 30 min to form a suspension for later use; 40 parts of the bismuth-containing nanocellulose suspension was filtered using a microporous membrane to form a layer of nanocellulose; then the suspension was continuously filtered on the microporous membrane to form a cellulose layer; the cellulose layer was Peel off the microporous filter membrane, use a clean and flat mold to put it into a hot press at 70°C for 60 minutes, then turn off the heating system of the hot press, and cool it under pressure-holding conditions to obtain the described A high-transparency transparent paper using bismuth-containing materials.

所述的含铋纳米纤维素悬浮液按照以下方法制备:The described bismuth-containing nanocellulose suspension is prepared according to the following method:

按照质量份数,将10份的木浆纤维分散于200份的二甲基亚砜中,然后加入1.8份的氢氧化钠、1份的2-(三甲基硅烷基)乙氧甲基氯、0.05份的4-氧-2,2,6,6-四甲基哌啶-1-氧自由基和0.5份的铋六氟-2,4-戊二酮酸,控温60℃,搅拌反应60min;完成反应后将15份的次氯酸钠加入到反应釜中,升温到80℃,反应10h;完成反应后过滤,用大量的去离子水洗涤三次;然后将纤维配制成5%的悬浮液,采用高压匀质机,匀质,离心后取上清液即可得到所述的含铋纳米纤维素悬浮液。According to the parts by mass, 10 parts of wood pulp fibers are dispersed in 200 parts of dimethyl sulfoxide, and then 1.8 parts of sodium hydroxide and 1 part of 2-(trimethylsilyl)ethoxymethyl chloride are added. , 0.05 part of 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical and 0.5 part of bismuth hexafluoro-2,4-pentanedione acid, temperature controlled at 60°C, stirring The reaction was carried out for 60 minutes; after the reaction was completed, 15 parts of sodium hypochlorite were added to the reaction kettle, the temperature was raised to 80 ° C, and the reaction was carried out for 10 h; after the reaction was completed, filtration was performed, and washed three times with a large amount of deionized water; then the fibers were prepared into a 5% suspension, The bismuth-containing nanocellulose suspension can be obtained by using a high-pressure homogenizer to homogenize and centrifuge the supernatant.

所述的木浆纤维为棉浆。The wood pulp fiber is cotton pulp.

所述的微孔滤膜为孔径为0.8μm的聚四氟乙烯滤膜。The microporous filter membrane is a polytetrafluoroethylene filter membrane with a pore size of 0.8 μm.

所述的热压机热压压力为7MPa。The hot pressing pressure of the hot press is 7MPa.

本实验制备的透明纸的透明度为92.3%,其抗张强度为112.3MPa。The transparency of the transparent paper prepared in this experiment is 92.3%, and its tensile strength is 112.3MPa.

实施例4Example 4

一种使用含铋材料的高透明度透明纸的制备方法,制备技术方案如下:A kind of preparation method of the high-transparency transparent paper using bismuth-containing material, the preparation technical scheme is as follows:

按照质量份数,将0.5份的木浆纤维分散于80份的去离子水中,然后加入50份的含铋纳米纤维素悬浮液,搅拌均匀后超声分散20min,形成混悬液备用;然后另取20份的含铋纳米纤维素悬浮液,使用微孔滤膜过滤,形成一层纳米纤维素层;然后将混悬液继续在该微孔滤膜上过滤,形成纤维素层;将纤维素层从微孔滤膜上剥离下来,使用清洁平整的模具放入到50℃的热压机上进行热压30min,然后关掉热压机的加热系统,保压条件下冷却,即可得到所述的一种使用含铋材料的高透明度透明纸。According to the parts by mass, 0.5 parts of wood pulp fibers were dispersed in 80 parts of deionized water, then 50 parts of bismuth-containing nanocellulose suspension were added, and after stirring evenly, ultrasonically dispersed for 20 minutes to form a suspension for later use; 20 parts of the bismuth-containing nanocellulose suspension was filtered using a microporous membrane to form a layer of nanocellulose; then the suspension was continuously filtered on the microporous membrane to form a cellulose layer; the cellulose layer was Peel off the microporous filter membrane, put a clean and flat mold into a hot press at 50°C for 30 minutes, then turn off the heating system of the hot press, and cool under pressure-holding conditions to obtain the A high-transparency transparent paper using bismuth-containing materials.

所述的含铋纳米纤维素悬浮液按照以下方法制备:The described bismuth-containing nanocellulose suspension is prepared according to the following method:

按照质量份数,将10份的木浆纤维分散于200份的二甲基亚砜中,然后加入1.8份的氢氧化钠、1份的2-(三甲基硅烷基)乙氧甲基氯、0.05份的4-氧-2,2,6,6-四甲基哌啶-1-氧自由基和0.5份的铋六氟-2,4-戊二酮酸,控温60℃,搅拌反应60min;完成反应后将15份的次氯酸钠加入到反应釜中,升温到80℃,反应10h;完成反应后过滤,用大量的去离子水洗涤三次;然后将纤维配制成5%的悬浮液,采用高压匀质机,匀质,离心后取上清液即可得到所述的含铋纳米纤维素悬浮液。According to the parts by mass, 10 parts of wood pulp fibers are dispersed in 200 parts of dimethyl sulfoxide, and then 1.8 parts of sodium hydroxide and 1 part of 2-(trimethylsilyl)ethoxymethyl chloride are added. , 0.05 part of 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical and 0.5 part of bismuth hexafluoro-2,4-pentanedione acid, temperature controlled at 60°C, stirring The reaction was carried out for 60 minutes; after the reaction was completed, 15 parts of sodium hypochlorite were added to the reaction kettle, the temperature was raised to 80 ° C, and the reaction was carried out for 10 h; after the reaction was completed, filtration was performed, and washed three times with a large amount of deionized water; then the fibers were prepared into a 5% suspension, The bismuth-containing nanocellulose suspension can be obtained by using a high-pressure homogenizer to homogenize and centrifuge the supernatant.

所述的木浆纤维为漂白针叶木浆。The wood pulp fiber is bleached softwood pulp.

所述的微孔滤膜为孔径为0.3μm的聚四氟乙烯滤膜。The microporous filter membrane is a polytetrafluoroethylene filter membrane with a pore size of 0.3 μm.

所述的热压机热压压力为7MPa。The hot pressing pressure of the hot press is 7MPa.

本实验制备的透明纸的透明度为91.5%,其抗张强度为107.2MPa。The transparency of the transparent paper prepared in this experiment is 91.5%, and its tensile strength is 107.2 MPa.

实施例5Example 5

一种使用含铋材料的高透明度透明纸的制备方法,制备技术方案如下:A kind of preparation method of the high-transparency transparent paper using bismuth-containing material, the preparation technical scheme is as follows:

按照质量份数,将2份的木浆纤维分散于150份的去离子水中,然后加入80份的含铋纳米纤维素悬浮液,搅拌均匀后超声分散30min,形成混悬液备用;然后另取40份的含铋纳米纤维素悬浮液,使用微孔滤膜过滤,形成一层纳米纤维素层;然后将混悬液继续在该微孔滤膜上过滤,形成纤维素层;将纤维素层从微孔滤膜上剥离下来,使用清洁平整的模具放入到70℃的热压机上进行热压60min,然后关掉热压机的加热系统,保压条件下冷却,即可得到所述的一种使用含铋材料的高透明度透明纸。According to the parts by mass, 2 parts of wood pulp fibers were dispersed in 150 parts of deionized water, then 80 parts of bismuth-containing nanocellulose suspension were added, and after stirring evenly, ultrasonically dispersed for 30 min to form a suspension for later use; 40 parts of the bismuth-containing nanocellulose suspension was filtered using a microporous membrane to form a layer of nanocellulose; then the suspension was continuously filtered on the microporous membrane to form a cellulose layer; the cellulose layer was Peel off the microporous filter membrane, use a clean and flat mold to put it into a hot press at 70°C for 60 minutes, then turn off the heating system of the hot press, and cool it under pressure-holding conditions to obtain the described A high-transparency transparent paper using bismuth-containing materials.

所述的含铋纳米纤维素悬浮液按照以下方法制备:The described bismuth-containing nanocellulose suspension is prepared according to the following method:

按照质量份数,将2份的木浆纤维分散于100份的二甲基亚砜中,然后加入0.8份的氢氧化钠、0.2份的2-(三甲基硅烷基)乙氧甲基氯、0.01份的4-氧-2,2,6,6-四甲基哌啶-1-氧自由基和0.1份的铋六氟-2,4-戊二酮酸,控温50℃,搅拌反应40min;完成反应后将5份的次氯酸钠加入到反应釜中,升温到70℃,反应5h;完成反应后过滤,用大量的去离子水洗涤三次;然后将纤维配制成0.5%的悬浮液,采用高压匀质机,匀质,离心后取上清液即可得到所述的含铋纳米纤维素悬浮液。According to the parts by mass, 2 parts of wood pulp fibers are dispersed in 100 parts of dimethyl sulfoxide, and then 0.8 parts of sodium hydroxide and 0.2 parts of 2-(trimethylsilyl)ethoxymethyl chloride are added. , 0.01 part of 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical and 0.1 part of bismuth hexafluoro-2,4-pentanedione acid, temperature controlled at 50°C, stirring The reaction was carried out for 40 minutes; after the reaction was completed, 5 parts of sodium hypochlorite was added to the reaction kettle, the temperature was raised to 70 ° C, and the reaction was carried out for 5 hours; after the reaction was completed, filtration was performed and washed three times with a large amount of deionized water; then the fibers were prepared into a 0.5% suspension, The bismuth-containing nanocellulose suspension can be obtained by using a high-pressure homogenizer to homogenize and centrifuge the supernatant.

所述的木浆纤维为棉浆。The wood pulp fiber is cotton pulp.

所述的微孔滤膜为孔径为0.3μm的聚四氟乙烯滤膜。The microporous filter membrane is a polytetrafluoroethylene filter membrane with a pore size of 0.3 μm.

所述的热压机热压压力为6MPa。The hot pressing pressure of the hot press is 6MPa.

本实验制备的透明纸的透明度为91.9%,其抗张强度为105.7MPa。The transparency of the transparent paper prepared in this experiment is 91.9%, and its tensile strength is 105.7MPa.

对比例1Comparative Example 1

不加含铋纳米纤维素悬浮液,其它同实施例1。No bismuth-containing nanocellulose suspension was added, and others were the same as in Example 1.

本实验制备的透明纸的透明度为35.8%,其抗张强度为32.8MPa。The transparency of the transparent paper prepared in this experiment is 35.8%, and its tensile strength is 32.8MPa.

对比例2Comparative Example 2

不加铋六氟-2,4-戊二酮酸,其它同实施例1。Without adding bismuth hexafluoro-2,4-pentanedione acid, the others are the same as in Example 1.

本实验制备的透明纸的透明度为81.5%,其抗张强度为76.3MPa。The transparency of the transparent paper prepared in this experiment is 81.5%, and its tensile strength is 76.3MPa.

对比例3Comparative Example 3

不加2-(三甲基硅烷基)乙氧甲基氯,其它同实施例1。Without adding 2-(trimethylsilyl)ethoxymethyl chloride, the others are the same as in Example 1.

本实验制备的透明纸的透明度为83.9%,其抗张强度为76.7MPa。The transparency of the transparent paper prepared in this experiment is 83.9%, and its tensile strength is 76.7MPa.

对比例4Comparative Example 4

不加4-氧-2,2,6,6-四甲基哌啶-1-氧自由基,其它同实施例1。Without adding 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical, the others are the same as in Example 1.

本实验制备的透明纸的透明度为80.1%,其抗张强度为72.9MPa。The transparency of the transparent paper prepared in this experiment is 80.1%, and its tensile strength is 72.9MPa.

Claims (5)

1. A preparation method of high-transparency transparent paper using a bismuth-containing material adopts the following preparation technical scheme:
dispersing 0.5-2 parts of wood pulp fiber in 80-150 parts of deionized water according to the mass parts, then adding 50-80 parts of bismuth-containing nano cellulose suspension, stirring uniformly, and performing ultrasonic dispersion for 20-30min to form suspension for later use; then, filtering another 20-40 parts of bismuth-containing nano-cellulose suspension by using a microporous filter membrane to form a nano-cellulose layer; then continuing to filter the suspension on the microporous filter membrane to form a cellulose layer; and (3) stripping the cellulose layer from the microporous filter membrane, putting the cellulose layer on a hot press with the temperature of 50-70 ℃ by using a clean and flat die for hot pressing for 30-60min, then closing a heating system of the hot press, and cooling under the pressure maintaining condition to obtain the high-transparency transparent paper using the bismuth-containing material.
2. The method for preparing a high transparency clear paper using bismuth-containing material according to claim 1, wherein: the bismuth-containing nano-cellulose suspension is prepared according to the following method:
dispersing 2-10 parts of wood pulp fiber in 200 parts of dimethyl sulfoxide (100), then adding 0.8-1.8 parts of sodium hydroxide, 0.2-1 part of 2- (trimethylsilyl) ethoxymethyl chloride, 0.01-0.05 part of 4-oxo-2, 2,6, 6-tetramethylpiperidine-1-oxygen radical and 0.1-0.5 part of bismuth hexafluoro-2, 4-pentanedionic acid, controlling the temperature to be 50-60 ℃, and stirring for reaction for 40-60 min; after the reaction is finished, adding 5-15 parts of sodium hypochlorite into the reaction kettle, heating to 70-80 ℃, and reacting for 5-10 hours; filtering after the reaction is finished, and washing with a large amount of deionized water for three times; then preparing the fiber into 0.5-5% suspension, homogenizing by a high-pressure homogenizer, centrifuging and taking supernatant fluid to obtain the bismuth-containing nano cellulose suspension.
3. The method for preparing a high transparency clear paper using bismuth-containing material according to claim 1, wherein: the wood pulp fiber is bleached softwood pulp or hardwood pulp.
4. The method for preparing a high transparency clear paper using bismuth-containing material according to claim 1, wherein: the microporous filter membrane is a polytetrafluoroethylene filter membrane with the aperture of 0.3-0.8 mu m.
5. The method for preparing a high transparency clear paper using bismuth-containing material according to claim 1, wherein: the hot pressing pressure of the hot press is 3-7 MPa.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2588495B2 (en) * 1991-04-17 1997-03-05 エルフ アトケム ソシエテ アノニム Method for producing high yield and high bleaching pulp for papermaking
CN105568747A (en) * 2015-12-17 2016-05-11 梅庆波 Method for manufacturing nanofiber transparent paper from straw
CN106024771A (en) * 2016-07-30 2016-10-12 杨超坤 Novel light-emitting diode for field of electronic devices
CN106498795A (en) * 2016-11-18 2017-03-15 陕西盛迈石油有限公司 The preparation method of high-strength transparence nano-cellulose paper
CN107056954A (en) * 2017-03-22 2017-08-18 青岛科技大学 A kind of efficient Cellulose nanocrystal preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2588495B2 (en) * 1991-04-17 1997-03-05 エルフ アトケム ソシエテ アノニム Method for producing high yield and high bleaching pulp for papermaking
CN105568747A (en) * 2015-12-17 2016-05-11 梅庆波 Method for manufacturing nanofiber transparent paper from straw
CN106024771A (en) * 2016-07-30 2016-10-12 杨超坤 Novel light-emitting diode for field of electronic devices
CN106498795A (en) * 2016-11-18 2017-03-15 陕西盛迈石油有限公司 The preparation method of high-strength transparence nano-cellulose paper
CN107056954A (en) * 2017-03-22 2017-08-18 青岛科技大学 A kind of efficient Cellulose nanocrystal preparation method

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