CN103343486B - Preparation method of paper with magnetic characteristic and luminescent characteristic - Google Patents

Preparation method of paper with magnetic characteristic and luminescent characteristic Download PDF

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CN103343486B
CN103343486B CN201310251081.8A CN201310251081A CN103343486B CN 103343486 B CN103343486 B CN 103343486B CN 201310251081 A CN201310251081 A CN 201310251081A CN 103343486 B CN103343486 B CN 103343486B
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paper
magnetic
stirred
stirring
characteristics
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CN103343486A (en
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高档妮
李志健
郭宏伟
莫祖学
刘盼
闫松明
张文亮
段国杰
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陕西科技大学
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Abstract

本发明公开了一种具有磁特性和发光特性纸的制备方法,通过将可发光的无机强磁特性材料与普通纸浆的复合,制备出了同时具有磁特性和发光特性的特种纸张。 The present invention discloses a method for preparing magnetic properties and having the light emitting properties of the paper, can emit light by the magnetic properties of the inorganic composite material ordinary pulp, prepared a special paper having both magnetic characteristics and light emitting characteristics. 所制备的纸张不仅具有无机材料不导电,耐温高,化学性能优良,抗老化等一系列优点,而且所制备的纸张力学性能优良,不易燃烧;在相同的力学性能下,厚度比普通的纸张厚度减少20~30%;所制备的纸张还表现出强的顺磁性和发红光的特殊性能;本发明得到的纸张因具有磁响应、磁记录等磁特性,可用于票据纸、包装纸、书法纸等需要有特殊身份证明高防伪的特种纸制品。 The prepared sheet having not only an inorganic material is not conductive, high temperature, excellent chemical resistance, aging series of advantages, but also excellent mechanical properties of the paper produced, nonflammable; at the same mechanical properties than normal paper thickness 20 to 30% reduction in thickness; the paper produced also exhibits strong paramagnetic and red special properties; sheet obtained by the present invention having the magnetic characteristics of the magnetic response of the magnetic recording and the like, can be used for ticket paper, wrapping paper, calligraphy paper requires a special high-security identification of specialty paper products. 本发明在纸张制备过程中不需要特殊的设备,操作简单,易于工业化生产;且磁性为永久性,不易消磁,隐蔽性强,不易被仿造。 In the paper manufacturing process according to the present invention does not require special equipment, easy to operate, easy industrial production; and a permanent magnetic, easily demagnetized concealed and difficult to counterfeit.

Description

一种具有磁特性和发光特性纸的制备方法 A magnetic properties and methods of preparation having the light emitting characteristics of the paper

技术领域 FIELD

[0001] 本发明涉及一种纸张的制造方法,特别涉及一种具有磁特性和发光特性纸的制备方法。 [0001] The present invention relates to a method for producing paper, more particularly to a method of preparing the magnetic properties and having the light emitting characteristics of the paper.

背景技术 Background technique

[0002] 随着科学技术的发展,各种各样的假冒伪略产品层出不穷。 [0002] With the development of science and technology, a variety of fake pseudo little product after another. 票据、产品包装、书法、绘画等特殊纸制品可为伪造者带来巨大的利润,因此不惜利用各种尖端的新技术(例如计算机图形处理软件、彩印、高精度扫描、数字化印刷等)来仿造,使原有的防伪很容易失去其特有的隐秘性。 Notes, packaging, calligraphy, painting and other special paper products can be enormous profits for counterfeiters, thus at the tip using a variety of new technologies (e.g., computer graphics software, color printing, high-precision scanning, digital printing, etc.) is simulated , so that the original security easily lose its unique secrecy. 因此,亟需开发研宄各种新型特种高效的防伪技术。 Therefore, the need for the development of special study based on a variety of new efficient anti-counterfeiting technology. CN1609919公开了一种防伪膜内标贴纸及其制备方法和应用,包括表面印有防伪标识层(I)的标纸层(2)、涂覆于防伪标识层(I)上的胶膜层(3),该胶膜层(3)上具有压纹(4)。 CN1609919 discloses a security sticker labeled membrane preparation method and applications, including security logo printed on the surface layer (I) of the standard paper layer (2), the coating film layer on the anti-counterfeit labels in layer (I) ( 3), the embossed film layer has a (4) (3). 克服了现有标贴纸的缺点,并具有完全的防伪功能,无需成型后贴标签。 Overcomes the disadvantages of the prior tattoo, and with full security features, without post-molding labeling. 但是所制备的贴纸不耐高温,强度差。 However, no sticker prepared high temperature strength is poor. CN101381975提供了一种在纸张中表现出可透光性的透明纤维,还提供了该透明纤维的制备方法以及含有这种透明纤维的纸制品。 CN101381975 is provided a paper sheet can exhibit a light-transmissive transparent fibers, it is also provided a method for preparing the transparent fibers and paper products containing such transparent fibers. 所述透明纤维是对包含以下组成的原料经干法纺丝或湿法纺丝而得到的合成纤维:聚乙烯醇:75 - 97%,壳聚糖:1 - 15%,羧甲基纤维素:0.5 - 10%。 The following is a transparent fiber material by dry spinning or wet spinning the composition obtained synthetic fibers: polyvinyl alcohol: 75 - 97%, the chitosan: 1 - 15%, carboxymethylcellulose : 0.5 --10%. 同样,所制备的纸张不耐高温,防伪耐久效果差。 Similarly, the sheet produced is not high temperature, durable security poor.

[0003] 磁性纸与其他记录形式相比,最大优点是:在视觉不见的磁层里,贮存有大量有用的记录,具有高度的隐蔽性,而且携带、使用尤为方便、反馈迅速(向机内一插,短短几秒钟内便会有显示或动作)。 [0003] Compared with other magnetic paper recording format, the maximum advantage is: the visual missing magnetic layer, the reservoir has a number of useful recording, having a high degree of concealment and carry, especially convenient, rapid feedback (to the machine a plug, or a display operation will be just a few seconds). 从保密角度来看,其应用领域将会有更多地拓展,比如生产管理、通讯联络、经营销售、防盗防爆等。 From the point of view of confidentiality, their applications will have more to expand, such as production management, communications liaison, sales management, theft-proof and so on. 目前,制备磁性纸所用的磁性材料大多为铁氧体包括Fe3O4(杨欣.细胞腔填充法制备磁性纸研宄[D].江南大学,2008.;李海蜂.原位复合法磁性纸张的制备及磁性能研宄[D].江南大学,2008.)、γ -Fe2O3(唐爱民,张宏伟,陈港等.磁性纳米复合纤维及磁性纸的制备与性能[J].华南理工大学学报(自然科学版),2009,37 (3):75 - 80.), Mn1^xZnxFe2O4 (于刚,段明珠,吕键.细胞内填充法制备磁性纸用纤维[J].上海造纸,2008,39(1):32 -35.)等。 Currently, the preparation of the magnetic sheet material in use comprises a ferrite mostly of Fe3O4 (Yang Xin. Preparation of cell lumen filled magnetic paper study based on [D]. Jiangnan University, the magnetic sheet prepared Lee bee situ compounding method 2008 .; and magnetic study based on [D]. Jiangnan University, 2008.), γ -Fe2O3 (Tang Aimin, Zhang Hongwei, Chen Hong Kong and so on. preparation and magnetic properties of magnetic nano-composite fiber and paper [J]. south China University of Technology (Natural Science), (3) 2009,37:. 75 - 80.), Mn1 ^ xZnxFe2O4 (just in, pearl section, prepare key intracellular LV filling SYSTEM magnetic paper fiber [J] Shanghai paper, 2008,39 (. 1): 32-35) and the like. 而铁氧体材料电阻较小,不耐酸碱,不能透光,而且制备的纸张白度相对较低,在印刷等方面有一定的限制。 And ferrite material of the resistance is small, no acid is not light-transmissive, and relatively low whiteness prepared, has certain limitations in terms of printing and the like. CN102587215A公开了一种带有磁特性纸张的制备方法,具体地说是在纸浆纤维的细胞腔中填充具有磁性的无机材料而制得带有磁特性的纸张。 CN102587215A discloses a method for preparing a sheet having magnetic properties, particularly an inorganic filler material of the magnetic sheet prepared with the magnetic characteristics in the cell chamber the pulp fibers. 该方法所制备的纸张仅具有磁防伪特性,防伪功能单一。 The method of preparing paper having the magnetic security features only a single anti-counterfeiting features. CN102587194A公开了一种高强度磁性纸的制备方法,通过在纸张中加入无机非金属耐高温非晶体材料,制备了具有磁特性的纸张。 CN102587194A discloses a method for preparing a high-strength magnetic paper by addition of a non-metallic refractory inorganic amorphous material in the sheet, a sheet having magnetic properties prepared. 所制备的无机非金属耐高温非晶体材料制备工艺简单,具有光学各项同性,化学稳定性优良,不导电,力学性能优良,磁性强。 Preparation of high-temperature inorganic non-metallic amorphous material prepared simply, having optical isotropy, excellent chemical stability, non-conductive, good mechanical properties, strong magnetic. 采用人工拉丝,避免了拉丝过程中无机纤维结晶失透现象的产生。 Artificial drawing, drawing process to avoid the generation of the inorganic fibers of crystalline devitrification. 该发明专利尽管所制备的纸张强度高,但依然存在防伪性单一的缺点。 The patent despite the high strength of the paper produced, but still the presence of a single security disadvantages.

[0004]目前,对于一些特殊用途的纸张,如人民币用纸,该纸张在特定波长的光激发下,即可发出特定的光,如紫外光激发后发出红色、黄绿色光等,大大增加了人民币的防伪力度。 [0004] Currently, for some special purpose paper, such as RMB sheet, the sheet at a particular wavelength of light excitation, to emit a specific light, such as to emit red, yellow and green light excitation like ultraviolet light, greatly increased anti-counterfeiting efforts of the yuan. 但目前所用的防伪发光材料多数为有机发光材料,使用时仅通过印刷的方法印制于纸币的表面,其制备工艺复杂,成本高昂。 But luminescent security materials currently used for the majority of the organic light emitting material, when only the banknotes printed on the surface by a printing method, the preparation process is complicated and costly. 而有关即具有磁特性又具有发光特性的纸张,且力学性能优良,不导电,耐高温,耐老化,防伪力度大的纸张的报道较少。 For fine paper are fewer i.e. having magnetic properties and having the light emitting characteristics and mechanical properties, non-conductive, high temperature resistant, anti-aging, anti-counterfeiting efforts large paper reported. CN2695469公开了一种蓄光发光纸,在具有背胶的进口高级纯白纸的表面喷涂上具有超长余辉发光性能的发光层,所述发光层由水晶清漆、稀释剂、固化剂、蓄光发光粉构成,该四种原料按一定比例混合均匀后分四次喷涂在纯白纸的表面上。 CN2695469 discloses a paper-storing luminous, a light emitting layer having a super-long afterglow luminescence having a surface coating of adhesive on importing advanced pure white, and the light emitting layer is composed of crystal varnish, diluent, curing agent, light-storing luminous powder configuration, a certain proportion of the four feedstocks mixed uniformly sprayed four times on a surface of a pure white. 该方法所制备的纸张存在耐磨性差,蓄光材料与纸张结合强度低等缺点。 Paper prepared by this method the presence of poor wear resistance, light-storage material and the sheet bonding strength and low defects. CN2856114公开了一种具有蓄光发光功能的防伪纸,其横截面呈层状结构,该层状结构依次是由纸底层、蓄光材料层、意向标志层、粘贴层和透明保护层组成。 CN2856114 discloses a security paper having a light-storing luminous function, its cross-section the layered structure, the layered structure is made of paper underlying turn, luminescent material layers, the intention flag layer, adhesive layer and a transparent protective layer. 该方法所制备的纸张存在耐磨性差,蓄光材料与纸张结合强度低,防伪性单一等缺点。 Paper prepared by this method the presence of poor wear resistance, light-storage material with a low binding strength of paper, a single anti-counterfeiting and other shortcomings. CN201546123U公开了一种可以快速激发的发光纸,在基质层(I)和发光材料涂层(3)间增设有玻璃微珠层(2),且发光材料涂层(3)的厚度小于玻璃微珠层的厚度,采用这种结构的发光纸,通过改善了发光纸的出光效能,在自发光材料的激发性能没有变化的条件下,实现快速激发的效果。 CN201546123U discloses a fast excitation light sheet, an additional layer between the substrate (I) and the phosphor coating (3) with a layer of glass beads (2), and the phosphor coating (3) has a thickness less than the glass microspheres the thickness of the layer of beads, light sheet using such a structure, the luminous efficacy is improved by the light sheet, in the absence of changes in the performance of self-excitation light-emitting material, to achieve the effect of the rapid excitation. 该方法所制备的纸张存在耐磨性差、防伪性单一、制备工艺复杂。 Paper prepared by this method the presence of poor wear resistance, anti-counterfeiting single, complicated preparation process. CN102174784A公开了一种蓄光发光防伪纸及其制造方法和应用。 Storing luminous CN102174784A discloses a method of manufacturing the security paper and application. 它是在普通纸上以印刷方式均匀涂覆蓄光发光油墨其中,所述的蓄光颜料是磷光性硫化锌ZnS:Cu。 It is printing on plain paper in a uniform coating of light-storing luminous ink wherein said phosphorescent pigment is a zinc sulfide phosphor of ZnS: Cu. 该方法所制备的纸张存在耐磨性差、蓄光材料与纸张结合强度低、发光材料寿命短、防伪特性单一等缺点。 Paper prepared by this method the presence of poor wear resistance, a low bonding strength with the paper-storage material, the short lifetime of the light emitting material, a single security features and other shortcomings.

发明内容 SUMMARY

[0005] 本发明的目的在于克服上述现有技术的缺点,提供了一种不导电,耐酸碱,透光性好,耐高温,抗老化,同时具有良好的磁特性和发光特性纸张的制备方法。 [0005] The object of the present invention is to overcome the above disadvantages of the prior art, there is provided a non-conductive, acid, good transparency, high temperature resistance, aging resistance, while having good magnetic characteristics and emission properties of the paper prepared method.

[0006] 为达到以上目的,本发明的技术方案为: [0006] To achieve the above object, the technical solution of the present invention is:

[0007] 包括以下步骤: [0007] comprising the steps of:

[0008] 第一步:可发光的无机强磁特性材料的制备与处理 [0008] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0009] I)首先,按照质量分数计,将12〜20%的Ge02,18〜25%的A1203,8〜12%的B203,35 〜40% 的Tb407,3 〜5% 的Eu203,0.1 〜2% 的Dy203,2 〜3% 的ZnO,3 〜5% 的Na2SiF6,0.2〜0.5%的Ce02,0.3〜0.5%的Zr02称量后放入玛瑙乳体研钵中研磨混合,形成配合料; [0009] I) First, a mass fraction, to 12~20% of Ge02,18~25% of A1203,8~12% of B203,35 ~40% of Tb407,3 ~5% of Eu203,0.1 ~ 2% Dy203,2 ~3% of ZnO, 3 ~5% of Na2SiF6,0.2~0.5% of Zr02 Ce02,0.3~0.5% of the body weighed into an agate mortar for mixing to form a batch;

[0010] 2)其次,在1380〜1410°C熔制温度下保温I〜2小时后,放入搅拌桨继续搅拌熔制,搅拌过程中温度始终保持在1380〜1410°C,得到熔液; [0010] 2) Next, after holding at 1380~1410 ° C melting temperature I~2 hours, into a stirring blade stirring continued melting, the mixing process is always maintained at a temperature of 1380~1410 ° C, to obtain a melt;

[0011] 3)然后,待步骤2)搅拌结束后,取出搅拌桨,将熔液冷却至1350°C,得到熔体; [0011] 3) Then, once step 2) After the stirring, remove the stirring blade, the melt was cooled to 1350 ° C, to give a melt;

[0012] 4)然后,将熔体倒入的铜模具中,待熔体固化后制成试样棒,开模后将试样棒放入650°C的退火炉中冷却至室温; [0012] 4) Then, the melt was poured into a copper mold, the melt is made to be a test bar after curing, into a test bar mold after 650 ° C in an annealing furnace cooled to room temperature;

[0013] 5)然后,将得到的试样棒放入拉丝机中,加热并拉制成直径为20〜30 μ m的纤维,并在纤维表面涂覆柔化浸润剂; [0013] 5) Then, the sample rods into a drawing machine to give a discharge, heated and drawn into 20~30 μ m diameter fibers, and the fiber surface to soften the coating wetting agent;

[0014] 6)最后,将涂覆有柔化浸润剂的纤维烘干水分后,剪切成长度为2〜5_纤维,即制备出可发光的无机强磁特性材料; [0014] 6) Finally, the coated fibers are dried after sizing soften water, as 2~5_ be cut into fiber, i.e., magnetic properties were prepared inorganic luminescent material;

[0015] 第二步:具有磁特性和发光特性纸的制备 [0015] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0016] I)首先,按照质量分数计,取1%〜3%的阔叶木绝干浆、5%〜10%可发光的无机强磁特性材料、0.6%〜1.5%助留助滤剂,余量为蒸馏水; [0016] I) First, a mass fraction, take 1% ~ 3% hardwood dry pulp, 5% ~ 10%, magnetic properties may be an inorganic luminescent material, 0.6% ~ 1.5%, retention and drainage aids, the balance of distilled water;

[0017] 将阔叶木绝干浆加入蒸馏水中,均匀搅拌,得到搅拌液A ; [0017] The hardwood dry pulp added to distilled water and uniformly stirred to give a solution A with stirring;

[0018] 2)其次,向搅拌液A中加入可发光的无机强磁特性材料,进行均匀搅拌,得到搅拌液B ; [0018] 2) Next, the magnetic properties of the inorganic luminescent material is added to the stirring solution A, and uniformly stirred to give a stirring solution B;

[0019] 3)然后,再向搅拌液B中加入助留助滤剂,进行均匀搅拌,得到搅拌液C ; [0019] 3) Then, solution B was added again stirred for retention and drainage aids, uniformly stirred to obtain a stirred solution C;

[0020] 4)然后,将搅拌液B移至抄片机上抄片,制成0.1〜0.3mm的纸片; [0020] 4) Then, the solution was stirred on a copy machine B move copy sheet, made of sheet 0.1~0.3mm;

[0021] 5)最后,将纸片进行烘后,自然冷却即得具有磁特性和发光特性纸。 After the [0021] 5) Finally, the sheet for drying, natural cooling to obtain magnetic characteristics having the light emitting properties of the paper.

[0022] 所述第一步中步骤3)取出搅拌桨后,以10°C /min的冷却速率将熔液冷却至1350 O。 [0022] The first step in Step 3) After removing the stirring blade, at 10 ° C / min cooling rate of the molten liquid is cooled to 1350 O.

[0023] 所述圆形的试样棒的直径为5mm。 [0023] The diameter of the circle of the test bar was 5mm.

[0024] 所述第二步中步骤I)均匀搅拌为在500〜1000转/min的搅拌机中搅拌。 [0024] The second step of step I) is stirred in a mixer homogeneously stirred 500~1000 rpm / min in.

[0025] 第二步中步骤2)均匀搅拌为在400〜600转/min搅拌机中搅拌。 [0025] The second step in Step 2) was uniformly stirred stirred at 400~600 rpm / min mixer.

[0026] 第二步中步骤3)均匀搅拌为在以800〜1500转/min搅拌机中搅拌。 [0026] The second step in Step 3) was stirred in homogeneously stirred at 800~1500 rpm / min mixer.

[0027] 所述纸片米用4〜6MPa的压力压榨3〜15min后形成。 The [0027] paper sheet m the press forming after the 4~6MPa 3~15min pressure.

[0028] 将纸片进行烘干、干燥为将纸片放入105〜110°C的烘箱中干燥。 [0028] drying the sheet, the sheet is placed in an oven dried 105~110 ° C dried.

[0029] 所述助留助滤剂为CPAM、PE1、PEO中的一种或几种。 [0029] The retention and drainage of CPAM, PE1, PEO of one or more.

[0030] 所述柔化浸润剂是将石蜡:凡士林:硬脂酸:水=1:1:1:30的质量比称量后,先将石蜡、凡士林和硬脂酸熔化后,再加入水,混合均匀后配置而成。 [0030] The wetting agent is a softening paraffin: petrolatum: Stearic acid: water = 1: 1: 1: 30 mass ratio after weighing, first paraffin, vaseline and stearic acid is melted, and then water was added mixed uniformly arranged together.

[0031] 本发明的有益效果为: [0031] Advantageous effects of the present invention are:

[0032] 本发明通过将可发光的无机强磁特性材料与普通纸浆的复合,制备出了同时具有磁特性和发光特性的特种纸张。 [0032] The present invention can emit light by the magnetic properties of the inorganic composite material ordinary pulp, prepared a special paper having both magnetic characteristics and light emitting characteristics. 所制备的纸张不仅具有无机材料不导电,耐温高,化学性能优良,抗老化等一系列优点,而且所制备的纸张力学性能优良,无机纤维材料与纸纤维结合牢固,不易燃烧;在相同的力学性能下,厚度比普通的纸张厚度减少20〜30%。 The prepared sheet having not only an inorganic material is not conductive, high temperature, excellent chemical resistance, aging series of advantages, but also excellent mechanical properties of the paper produced, inorganic fibrous material and paper fiber with a solid, non-flammable; at the same the mechanical properties, reduction in thickness of 20 to 30% than the average thickness of the sheet. 同时,所制备的纸张还表现出强的顺磁性和发红光的特殊性能。 Meanwhile, the paper produced also exhibits strong paramagnetic and special properties of red. 按照本发明制备方法制得的纸张因具有磁响应、磁记录等磁特性,可用于票据纸、包装纸、书法纸等需要有特殊身份证明的特种纸制品。 Prepared according to the method of the present invention due to paper made with magnetic characteristics of the magnetic response of the magnetic recording and the like, can be used for ticket paper, wrapping paper, specialty paper products calligraphy paper requires a special identification. 本发明在纸张制备过程中不需要特殊的设备,操作简单,易于工业化生产;且磁性为永久性,不易消磁,隐蔽性强,不易被仿造。 In the paper manufacturing process according to the present invention does not require special equipment, easy to operate, easy industrial production; and a permanent magnetic, easily demagnetized concealed and difficult to counterfeit.

附图说明 BRIEF DESCRIPTION

[0033]图1是实施例1制备的具有磁特性和发光特性纸的发光光谱图,其中横坐标为发射光波长,纵坐标为发射光强度; [0033] FIG. 1 is a light emission spectrum having emission characteristics and magnetic characteristics of the paper prepared according to Example 1, where the abscissa is the wavelength of the emitted light, the ordinate is the emission intensity;

[0034] 图2是实施例1制备的具有磁特性和发光特性纸的磁滞回线,其中横坐标为磁场强度,纵坐标为磁化强度; [0034] FIG. 2 is a magnetic hysteresis loop characteristic and the light emission properties of the paper prepared according to Example 1, in which the abscissa is the magnetic field strength, the ordinate magnetization;

[0035]图3是实施例1制备的具有磁特性和发光特性纸在扫描电子显微镜下的照片。 [0035] Figure 3 is a light-emitting characteristics and magnetic properties of paper under a scanning electron microscope photograph of Example 1 was prepared embodiment.

具体实施方式 Detailed ways

[0036] 下面结合附图对本发明做详细描述。 [0036] The following detailed description of the drawings in conjunction with the present invention.

[0037] 实施例1: [0037] Example 1:

[0038] 第一步:可发光的无机强磁特性材料的制备与处理 [0038] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0039] I)首先,按照质量分数计,将19% 的GeO2, 20% 的Al2O3,10% 的B2O3, 38% 的Tb4O7,4%的Eu2O3,1% 的Dy2O3, 3% 的ZnO, 4% 的Na2SiF6,0.5% 的CeO2,0.5% 的ZrO2称量后放入玛瑙乳体研钵中研磨混合至均匀度大于98%后,形成配合料; [0039] I) First, a mass fraction, a 19% GeO2, 20% of Al2O3,10% of B2O3, 38% of Tb4O7,4% of Eu2O3,1% of Dy2O3, 3% of ZnO, 4% Na2SiF6,0.5% of the CeO2,0.5% of ZrO2 were weighed into an agate mortar for mixing body uniformly greater than 98% to form a batch;

[0040] 2)其次,在1410°C下将配合料加入铂金坩祸中,并在1410°C熔制温度下保温I小时后,放入搅拌桨继续搅拌熔制3小时,搅拌过程中温度始终保持在1410°C ; [0040] 2) Next, at 1410 ° C the batch was added platinum crucible disaster in, and after incubation I hour, into a stirring blade stirring was continued melt at 1410 ° C melting temperature system 3 hours, the temperature during stirring kept at 1410 ° C;

[0041] 3)然后,待搅拌结束后,取出搅拌桨,以10°C /min的冷却速率,将熔液冷却至1350°C,并在1350°C保温30min,得到熔体; After the [0041] 3) Then, stirring until removed stirring blade, a cooling rate of 10 ° C / min, and the melt was cooled to 1350 ° C, and maintained at 1350 ° C 30min, to obtain a melt;

[0042] 4)然后,将熔制的熔体倒入600°C的铜模具中,待熔体固化后制成直径为5mm的试样棒,开模后将试样棒放入650°C的退火炉中,保温2h后随炉冷却至室温; [0042] 4) Then, the melting melt 600 ° C was poured into a copper mold, after the melt has solidified to be a sample rod having a diameter of 5mm, the test bar into the mold after 650 ° C annealing furnace, cooling to room temperature after the 2h incubation with the furnace;

[0043] 5)然后,将得到的试样棒放入拉丝机中,加热至1350°C,并将试样棒拉制成直径为20〜30 μ m的纤维,并在纤维表面涂覆柔化浸润剂; [0043] 5) The sample was then put into a drawing machine rod obtained, heated to 1350 ° C, and the sample drawn into rod 20~30 μ m diameter fibers, and the fiber surface is coated soft of wetting agent;

[0044] 6)最后,将涂覆有柔化浸润剂的纤维放入110°C的烘箱中,保温2h,烘干水分后,剪切成长度为2〜5mm纤维,即制备出可发光的无机强磁特性材料; [0044] 6) Finally, the coated fibers soften wetting agent put in an oven of 110 ° C and incubated for 2h, after drying the water, to be cut into 2~5mm fibers, i.e., light emission can be prepared magnetic properties of the inorganic material;

[0045] 第二步:具有磁特性和发光特性纸的制备 [0045] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0046] I)首先,取5g绝干阔叶木浆,加入500ml蒸馏水中,在1000转/min的搅拌机中进行搅拌50min,得到搅拌液A ; [0046] I) First, 5g of oven dry hardwood pulp, was added 500ml of distilled water, stirred 50min 1000 rpm in a mixer / min, the resulting solution was stirred for A;

[0047] 2)其次,向得到搅拌液A中加入1g已制取的可发光的无机强磁特性材料,再以600转/min搅拌50min,得到搅拌液B ; [0047] 2) Next, to the resulting solution stirred B A stirred solution was added 1g of inorganic material has magnetic properties of the preparation can emit light, and then to 600 rpm / min was stirred for 50min, to obtain;

[0048] 3)然后,再向得到搅拌液B中加入1.5g助留助滤剂CPAM(cat1nicpolyacryIamides,阳离子聚丙稀酰胺),以1500转/min继续搅拌80min,得到搅拌液C ; [0048] 3) Then, again solution B was added with stirring to give 1.5g retention and drainage aids CPAM (cat1nicpolyacryIamides, cationic polyacrylamide), and stirring was continued at 1500 rpm / min 80min, to give stirred solution C;

[0049] 4)然后,将得到的搅拌液C移至抄片机上抄片,采用6MPa的压力压榨15min后,形成0.1mm的纸片; After [0049] 4) Then, the resulting solution stirred on a copy machine C Move copy sheets, using a press pressure of 6MPa 15min, it forms a sheet of 0.1mm;

[0050] 5)最后,将纸片放入105°C的烘箱中,干燥30min后,自然冷却即得具有磁特性和发光特性纸。 [0050] 5) Finally, the paper sheet placed in an oven at 105 ° C, after drying 30min, allowed to cool to obtain magnetic characteristics having the light emitting properties of the paper.

[0051] 参见附图1,是所制备具有磁特性和发光特性纸张在激发波长为378nm下的光致发光光谱,其中横坐标为发射光波长,纵坐标为发射光强度。 [0051] Referring to Figure 1, is produced having magnetic properties and light emitting properties of the paper at an excitation wavelength of 378nm at the photoluminescence spectrum wherein the abscissa is the wavelength of the emitted light, the ordinate is the emission intensity. 由图1可以看出,所制备的纸张,最强发射光波长为617.4nm,强度接近1200单位,而在580.2nm,593.2nm,656.2nm,705.4nm处发射光强度很弱。 As can be seen from Figure 1, the sheet prepared, the strongest emission wavelength of 617.4nm, the strength close unit 1200, and the light emission intensity is very weak at 580.2nm, 593.2nm, 656.2nm, 705.4nm at.

[0052] 参见附图2,是所制备具有磁特性和发光特性纸张在-2000〜30000e范围内的磁滞回线,从图中可以看出,所制备的纸张具有一定的顺磁性。 [0052] Referring to Figure 2, having a magnetic hysteresis loop characteristic and a light emitting properties of the paper within the range -2000~30000e prepared, it can be seen from the figure, the paper prepared with certain paramagnetic.

[0053] 参见附图3,是所制备的具有磁特性和发光特性纸张在IK倍下的SEM照片,从图中可以看出所制备的纸张中无机纤维与纸张纤维结合紧密,且呈现均匀分布。 [0053] Referring to Figure 3, having magnetic properties and the light emission properties of the paper in the SEM photographs of the prepared IK-fold, the paper can be seen from FIG prepared inorganic fibers closely with the paper fibers, and exhibit a uniform distribution.

[0054] 实施例2: [0054] Example 2:

[0055] 第一步:可发光的无机强磁特性材料的制备与处理 [0055] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0056] I)首先,按照质量分数计,将14.5% 的GeO2, 25% 的Al2O3,11% 的B2O3, 37% 的Tb4O7,3% 的Eu2O3, 2% 的Dy2O3, 2% 的ZnO, 5% 的Na2SiF6,0.2% 的CeO2,0.3% 的ZrOj#量后放入玛瑙乳体中研磨混合至均匀度大于98%后,形成配合料; [0056] I) First, a mass fraction, and 14.5% of GeO2, 25% of Al2O3,11% of B2O3, 37% of Tb4O7,3% of Eu2O3, 2% of Dy2O3, 2% of ZnO, 5% Na2SiF6,0.2% of the ZrOj # CeO2,0.3% of the amount placed in an agate grinding uniformly mixed body of more than 98% to form a batch;

[0057] 2)其次,在1410°C下将配合料加入铂金坩祸中,并在1410°C熔制温度下保温2小时后,放入搅拌桨继续搅拌熔制2小时,搅拌过程中温度始终保持在1410°C ; [0057] 2) Next, at 1410 ° C the batch was added platinum crucible disaster in, and after a 2 hour incubation, into a stirring blade stirring was continued melt at 1410 ° C melting temperature of the system 2 hours, the temperature during stirring kept at 1410 ° C;

[0058] 3)然后,待搅拌结束后,取出搅拌桨,以10°C /min的冷却速率,将熔液冷却至1350°C,并在1350°C保温30min,得到熔体; After the [0058] 3) Then, stirring until removed stirring blade, a cooling rate of 10 ° C / min, and the melt was cooled to 1350 ° C, and maintained at 1350 ° C 30min, to obtain a melt;

[0059] 4)然后,将熔制的熔体倒入600°C的铜模具中,制成直径为1mm的试样棒,待熔体固化后开模将试样棒放入650°C的退火炉中,保温2h后随炉冷却至室温; [0059] 4) Then, the melt was poured into a melting copper mold of 600 ° C, a sample rod having a diameter of 1mm, until the melt has solidified into a test bar mold to 650 ° C in an annealing furnace, cooling to room temperature after the 2h incubation with the furnace;

[0060] 5)然后,将得到的试样棒放入拉丝机中,加热至1350°C,并将试样棒拉制成直径为30 μ m的纤维,并及时在纤维表面涂覆柔化浸润剂; [0060] 5) The sample was then put into a drawing machine rod obtained, heated to 1350 ° C, and the sample pull rod having a diameter of 30 μ m fiber, and the fiber surface is coated soften promptly wetting agents;

[0061] 6)最后,将涂覆有柔化浸润剂的纤维放入110°C的烘箱中,保温2h,烘干水分后,剪切成长度为2〜5mm,即制备出可发光的无机强磁特性材料; [0061] 6) Finally, the coated fibers soften wetting agent put in an oven of 110 ° C and incubated for 2h, after drying the water, to be cut into 2~5mm, i.e., an inorganic light emission can be prepared magnetic properties of the material;

[0062] 第二步:具有磁特性和发光特性纸的制备 [0062] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0063] I)首先,取4g绝干阔叶木浆,加入400ml蒸馏水中,在700转/分的搅拌机中进行搅拌40min,得到搅拌液A; [0063] I) First of all, taking the absolute dry hardwood 4g, 400ml of distilled water was added, the mixture was stirred 40min at mixer 700 rev / min, the resulting solution was stirred for A;

[0064] 2)其次,向得到搅拌液A中加入Sg已制取的可发光的无机强磁特性纤维,再以500转/min搅拌40min,得到搅拌液B ; [0064] 2) Next, to the resulting stirred solution was added Sg A preparation can have an inorganic luminescent magnetic properties of the fiber, and then to 500 rotations / min was stirred for 40min, stirring to obtain solution B;

[0065] 3)然后,再向搅拌液B中加入1.2g助留助滤剂PEI (Polyetherimide,聚醚酰亚胺),以1000转/min继续搅拌60min,得到搅拌液C ; [0065] 3) Then, again solution B was added with stirring 1.2g retention and drainage aids PEI (Polyetherimide, polyetherimide), stirring was continued at 1000 revolutions / min 60min, to give stirred solution C;

[0066] 4)然后,将搅拌后的搅拌液C移至抄片机上抄片,采用5MPa的压力压榨Ilmin后,形成0.2mm的纸片; [0066] 4) Then, the solution was stirred for C after stirring machine to move the copy the copy sheet, after pressure using a press Ilmin 5MPa, form a sheet of 0.2mm;

[0067] 5)最后,将纸片放入110°C的烘箱中,干燥20min后,自然冷却即得具有磁特性和发光特性纸。 [0067] 5) Finally, the paper sheet placed in an oven at 110 ° C, after drying 20min, allowed to cool to obtain magnetic characteristics having the light emitting properties of the paper.

[0068] 实施例3: [0068] Example 3:

[0069] 第一步:可发光的无机强磁特性材料的制备与处理 [0069] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0070] I)首先,按照质量分数计,将16% 的GeO2, 24% 的Al2O3,9.5% 的B2O3, 36% 的Tb4O7,5% 的Eu2O3, 2% 的Dy2O3, 2% 的ZnO, 5% 的Na2SiF6,0.3% 的CeO2,0.2% 的ZrOj#量后放入玛瑙乳体中研磨混合至均匀度大于98%后,形成配合料; [0070] I) First, a mass fraction, a 16% GeO2, 24% of Al2O3,9.5% of B2O3, 36% of Tb4O7,5% of Eu2O3, 2% of Dy2O3, 2% of ZnO, 5% Na2SiF6,0.3% of the ZrOj # CeO2,0.2% of the amount placed in an agate grinding uniformly mixed body of more than 98% to form a batch;

[0071] 2)其次,在1400°C下将配合料加入铂金坩祸中,并在1400°C熔制温度下保温2小时后,放入搅拌桨继续搅拌熔制2小时,搅拌过程中温度始终保持在1400°C ; [0071] 2) Next, at 1400 ° C the batch was added platinum crucible disaster in, and after a 2 hour incubation, placed stirred at 1400 ° C melting temperature paddle stirring was continued melting of two hours, the temperature during stirring kept at 1400 ° C;

[0072] 3)然后,待搅拌结束后,取出搅拌桨,以10°C /min的冷却速率,将熔液冷却至1350°C,并在1350°C保温30min,得到熔体; After the [0072] 3) Then, stirring until removed stirring blade, a cooling rate of 10 ° C / min, and the melt was cooled to 1350 ° C, and maintained at 1350 ° C 30min, to obtain a melt;

[0073] 4)然后,将熔制的熔体倒入600°C的铜模具中,制成直径为5mm的试样棒,待熔体固化后开模将试样棒放入650°C的退火炉中,保温2h后随炉冷却至室温; [0073] 4) Then, the melt was poured into a melting copper mold of 600 ° C, a sample rod having a diameter of 5mm, until the melt has solidified into a test bar mold to 650 ° C in an annealing furnace, cooling to room temperature after the 2h incubation with the furnace;

[0074] 5)然后,将得到的试样棒放入拉丝机中,加热至1350°C,并将试样棒拉制成直径为20〜30 μ m的纤维,并及时在纤维表面涂覆柔化浸润剂; [0074] 5) The sample was then put into a drawing machine rod obtained, heated to 1350 ° C, and the sample pull rod having a diameter of 20~30 μ m fiber, coating the fiber surface and promptly wetting agents soften;

[0075] 6)最后,将涂覆有柔化浸润剂的纤维放入110°C的烘箱中,保温2h,烘干水分后,剪切成长度为2〜5mm纤维,即制备出可发光的无机强磁特性材料; [0075] 6) Finally, the coated fibers soften wetting agent put in an oven of 110 ° C and incubated for 2h, after drying the water, to be cut into 2~5mm fibers, i.e., light emission can be prepared magnetic properties of the inorganic material;

[0076] 第二步:具有磁特性和发光特性纸的制备 [0076] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0077] I)首先,取3g绝干阔叶木浆,加入300ml蒸馏水中,在600转/min的搅拌机中进行搅拌50min,得到搅拌液A ; [0077] I) First, 3g taking absolute dry hardwood pulp, 300ml of distilled water was added, the mixture was stirred 50min at 600 stirrer revolutions / min, the resulting solution was stirred for A;

[0078] 2)其次,向搅拌液A中加入6g已制取的可发光的无机强磁特性纤维,再以600转/min搅拌20min,得到搅拌液B ; [0078] 2) Next, the preparation was added 6g may be inorganic light emitting properties of the fiber to the magnetic liquid A was stirred, and then to 600 rpm / min was stirred for 20min, stirring to obtain solution B;

[0079] 3)然后,再向搅拌液B中加入0.9g助留助滤剂PEO (聚氧化乙烯),以900转/min继续搅拌80min,得到搅拌液C ; [0079] 3) Then, again solution B was added with stirring 0.9g retention and drainage aids PEO (polyethylene oxide), and stirring was continued at 900 rpm / min 80min, to give stirred solution C;

[0080] 4)然后,将搅拌后的搅拌液C移至抄片机上抄片,采用4MPa的压力压榨15min后,形成0.1mm的纸片; [0080] 4) Then, the solution was stirred for C after stirring machine to move the copy the copy sheet, using pressure 4MPa 15min after pressing, the paper sheet is formed of 0.1mm;

[0081] 5)最后,将纸片放入105°C的烘箱中,干燥30min后,自然冷却即得具有磁特性和发光特性纸。 [0081] 5) Finally, the paper sheet placed in an oven at 105 ° C, after drying 30min, allowed to cool to obtain magnetic characteristics having the light emitting properties of the paper.

[0082] 实施例4: [0082] Example 4:

[0083] 第一步:可发光的无机强磁特性材料的制备与处理 [0083] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0084] I)首先,按照质量分数计,将17.4% 的GeO2,19% 的Al2O3,12% 的B2O3,40% 的Tb4O7,3% 的Eu2O3,1% 的Dy2O3, 3% 的ZnO, 4% 的Na2SiF6,0.3% 的CeO2,0.3% 的ZrOj#量后放入玛瑙乳体中研磨混合至均匀度大于98%后,形成配合料; [0084] I) First, a mass fraction, 17.4% of the GeO2,19% of Al2O3,12% of B2O3,40% of Tb4O7,3% of Eu2O3,1% of Dy2O3, 3% of ZnO, 4% Na2SiF6,0.3% of the ZrOj # CeO2,0.3% of the amount placed in an agate grinding uniformly mixed body of more than 98% to form a batch;

[0085] 2)其次,在1380°C下将配合料加入铂金坩祸中,并在1380°C熔制温度下保温2小时后,放入搅拌桨继续搅拌熔制3小时,搅拌过程中温度始终保持在1380°C ; [0085] 2) Next, at 1380 ° C the batch was added platinum crucible disaster in, and after a 2 hour incubation, into a stirring blade stirring was continued melt at 1380 ° C melting temperature system 3 hours, the temperature during stirring kept at 1380 ° C;

[0086] 3)然后,待搅拌结束后,取出搅拌桨,以10°C /min的冷却速率,将熔液冷却至1350°C,并在1350°C保温30min,得到熔体; After the [0086] 3) Then, stirring until removed stirring blade, a cooling rate of 10 ° C / min, and the melt was cooled to 1350 ° C, and maintained at 1350 ° C 30min, to obtain a melt;

[0087] 4)然后,将熔制的熔体倒入600°C的铜模具中,制成直径为5mm的试样棒,待熔体固化后开模将试样棒放入650°C的退火炉中,保温2h后随炉冷却至室温; [0087] 4) Then, the melt was poured into a melting copper mold of 600 ° C, a sample rod having a diameter of 5mm, until the melt has solidified into a test bar mold to 650 ° C in an annealing furnace, cooling to room temperature after the 2h incubation with the furnace;

[0088] 5)然后,将得到的试样棒放入拉丝机中,加热至1350°C,并将试样棒拉制成直径为20〜30 μ m的纤维,并及时在试样纤维表面涂覆柔化浸润剂; [0088] 5) The sample was then put into a drawing machine rod obtained, heated to 1350 ° C, and the sample pull rod having a diameter of 20~30 μ m fiber, and the fiber surface of the sample promptly wetting agents soften coating;

[0089] 6)最后,将涂覆有柔化浸润剂的纤维放入110°C的烘箱中,保温2h,烘干水分后,剪切成长度为2〜5mm纤维,即制备出可发光的无机强磁特性材料; [0089] 6) Finally, the coated fibers soften wetting agent put in an oven of 110 ° C and incubated for 2h, after drying the water, to be cut into 2~5mm fibers, i.e., light emission can be prepared magnetic properties of the inorganic material;

[0090] 第二步:具有磁特性和发光特性纸的制备 [0090] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0091] I)首先,取5g绝干阔叶木浆,加入500ml蒸馏水中,在1000转/min的搅拌机中进行搅拌50min,得到搅拌液A ; [0091] I) First, 5g of oven dry hardwood pulp, was added 500ml of distilled water, stirred 50min 1000 rpm in a mixer / min, the resulting solution was stirred for A;

[0092] 2)其次,向搅拌液中加入1g已制取的可发光的无机强磁特性材料,再以600转/min搅拌20min,得到搅拌液B ; [0092] 2) Next, the magnetic properties of the inorganic material has 1g preparing illuminable added to the stirred solution, and then to 600 rpm / min was stirred for 20min, stirring to obtain solution B;

[0093] 3)然后,再向搅拌液B中加入0.6g助留助滤剂CPAM和PEI,以8000转/min继续搅拌80min,得到搅拌液C; [0093] 3) Then, again solution B was added with stirring 0.6g CPAM retention and drainage aids and PEI, stirring is continued at 8000 rpm / min 80min, to give stirred solution C;

[0094] 4)然后,将搅拌后的搅拌液C移至抄片机上抄片,采用6MPa的压力压榨3min后,形成0.1mm的纸片; [0094] 4) Then, the solution was stirred for C after stirring machine to move the copy the copy sheet, after the pressing pressure of 6MPa employed 3min, form a sheet of 0.1mm;

[0095] 5)最后,将纸片放入110°C的烘箱中,干燥1min后,自然冷却即得具有磁特性和发光特性纸。 [0095] 5) Finally, the paper sheet placed in an oven at 110 ° C, after drying 1min, cooled naturally to obtain magnetic characteristics having the light emitting properties of the paper.

[0096] 实施例5: [0096] Example 5:

[0097] 第一步:可发光的无机强磁特性材料的制备与处理 [0097] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0098] I)首先,按照质量分数计,将18.5% 的GeO2, 20% 的Al2O3,11% 的B2O3, 39% 的Tb4O7,4% 的Eu2O3, 2% 的Dy2O3, 2% 的ZnO, 3% 的Na2SiF6,0.2% 的CeO2,0.3% 的ZrOj#量后放入玛瑙乳体中研磨混合至均匀度大于98%后,形成配合料; [0098] I) First, a mass fraction, and 18.5% of GeO2, 20% of Al2O3,11% of B2O3, 39% of Tb4O7,4% of Eu2O3, 2% of Dy2O3, 2% of ZnO, 3% Na2SiF6,0.2% of the ZrOj # CeO2,0.3% of the amount placed in an agate grinding uniformly mixed body of more than 98% to form a batch;

[0099] 2)其次,在1390°C下将配合料加入铂金坩祸中,并在1390°C熔制温度下保温2小时后,放入搅拌桨继续搅拌熔制3小时,搅拌过程中温度始终保持在1390°C ; [0099] 2) Next, at 1390 ° C the batch was added platinum crucible disaster in, and after a 2 hour incubation, into a stirring blade stirring was continued melt at 1390 ° C melting temperature system 3 hours, the temperature during stirring kept at 1390 ° C;

[0100] 3)然后,待搅拌结束后,取出搅拌桨,以10°C /min的冷却速率,将熔液冷却至1350°C,并在1350°C保温30min,得到熔体; After the [0100] 3) Then, stirring until removed stirring blade, a cooling rate of 10 ° C / min, and the melt was cooled to 1350 ° C, and maintained at 1350 ° C 30min, to obtain a melt;

[0101] 4)然后,将熔制的熔体倒入600°C的铜模具中,制成直径为5mm的试样棒,待熔体固化后开模将试样棒放入650°C的退火炉中,保温2h后随炉冷却至室温; [0101] 4) Then, the melt was poured into a melting copper mold of 600 ° C, a sample rod having a diameter of 5mm, until the melt has solidified into a test bar mold to 650 ° C in an annealing furnace, cooling to room temperature after the 2h incubation with the furnace;

[0102] 5)然后,将得到的试样棒放入拉丝机中,加热至1350°C,并将试样拉制成直径为20〜30 μ m的纤维,并及时在纤维表面涂覆柔化浸润剂; [0102] 5) The sample was then put into a drawing machine rod obtained, heated to 1350 ° C, and the sample drawn into 20~30 μ m diameter fibers, and the fiber surface soft coating promptly of wetting agent;

[0103] 6)最后,将涂覆有柔化浸润剂的纤维放入110°C的烘箱中,保温2h,烘干水分后,剪切成长度为2〜5mm纤维,即制备出可发光的无机强磁特性材料; [0103] 6) Finally, the coated fibers soften wetting agent put in an oven of 110 ° C and incubated for 2h, after drying the water, to be cut into 2~5mm fibers, i.e., light emission can be prepared magnetic properties of the inorganic material;

[0104] 第二步:具有磁特性和发光特性纸的制备 [0104] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0105] I)首先,取4g绝干阔叶木浆,加入400ml蒸馏水中,在700转/分的搅拌机中进行搅拌40min,得到搅拌液A; [0105] I) First of all, taking the absolute dry hardwood 4g, 400ml of distilled water was added, the mixture was stirred 40min at mixer 700 rev / min, the resulting solution was stirred for A;

[0106] 2)其次,向搅拌液A中加入7g已制取的可发光的无机强磁特性纤维,再以500转/分搅拌30min,得到搅拌液B ; [0106] 2) Next, 7g added may have been prepared to take the light emitting properties of the fiber to an inorganic magnetic liquid A was stirred, and then at 500 rev / min stirring for 30min, to give stirred solution B;

[0107] 3)然后,再向搅拌液B中加入1.0g助留助滤剂CPAM、PEI以及PEO,以1100转/min继续搅拌50min,得到搅拌液C ; [0107] 3) Then, again solution B was added with stirring 1.0g retention and drainage aids CPAM, PEI and PEO, stirring is continued at 1100 rpm / min 50min, to give stirred solution C;

[0108] 4)然后,将搅拌后的搅拌液C移至抄片机上抄片,采用5MPa的压力压榨1min后,形成0.2mm的纸片; After [0108] 4) Then, the solution was stirred for C after stirring machine to move the copy the copy sheet, using a press pressure of 5MPa 1min, form a sheet of 0.2mm;

[0109] 5)最后,将纸片放入105°C的烘箱中,干燥20min后,自然冷却即得具有磁特性和发光特性纸。 [0109] 5) Finally, the paper sheet placed in an oven at 105 ° C, after drying 20min, allowed to cool to obtain magnetic characteristics having the light emitting properties of the paper.

[0110] 实施例6: [0110] Example 6:

[0111] 第一步:可发光的无机强磁特性材料的制备与处理 [0111] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0112] I)首先,按照质量分数计,将15% 的GeO2,19.3% 的Al2O3,11% 的B2O3,40% 的Tb4O7,5% 的Eu2O3, 2% 的Dy2O3, 3% 的ZnO, 4% 的Na2SiF6,0.3% 的CeO2,0.4% 的ZrOj#量后放入玛瑙乳体中研磨混合至均匀度大于98%后,形成配合料; [0112] I) First, a mass fraction, GeO2,19.3% to 15% of Al2O3,11% of B2O3,40% of Tb4O7,5% of Eu2O3, 2% of Dy2O3, 3% of ZnO, 4% Na2SiF6,0.3% of the ZrOj # CeO2,0.4% of the amount placed in an agate grinding uniformly mixed body of more than 98% to form a batch;

[0113] 2)其次,在1400°C下将配合料加入铂金坩祸中,并在1400°C熔制温度下保温I小时后,放入搅拌桨继续搅拌熔制3小时,搅拌过程中温度始终保持在1400°C ; [0113] 2) Next, at 1400 ° C the batch was added platinum crucible disaster in, and after incubation I hour, into a stirring blade stirring was continued melt at 1400 ° C melting temperature system 3 hours, the temperature during stirring kept at 1400 ° C;

[0114] 3)然后,待搅拌结束后,取出搅拌桨,以10°C /min的冷却速率,将熔液冷却至1350°C,并在1350°C保温30min,得到熔体; After the [0114] 3) Then, stirring until removed stirring blade, a cooling rate of 10 ° C / min, and the melt was cooled to 1350 ° C, and maintained at 1350 ° C 30min, to obtain a melt;

[0115] 4)然后,将熔制的熔体倒入600°C的铜模具中,制成直径为5mm的试样棒,待熔体固化后开模将试样棒放入650°C的退火炉中,保温2h后随炉冷却至室温; [0115] 4) Then, the melt was poured into a melting copper mold of 600 ° C, a sample rod having a diameter of 5mm, until the melt has solidified into a test bar mold to 650 ° C in an annealing furnace, cooling to room temperature after the 2h incubation with the furnace;

[0116] 5)然后,将得到的试样棒放入拉丝机中,加热至1350°C,并将试样棒拉制成直径为20〜30 μ m的纤维,并及时在纤维表面涂覆柔化浸润剂; [0116] 5) The sample was then put into a drawing machine rod obtained, heated to 1350 ° C, and the sample pull rod having a diameter of 20~30 μ m fiber, coating the fiber surface and promptly wetting agents soften;

[0117] 6)最后,将涂覆有柔化浸润剂的纤维放入110°C的烘箱中,保温lh,烘干水分后,剪切成长度为2〜5mm纤维,即制备出可发光的无机强磁特性材料; [0117] 6) Finally, the coated fibers soften wetting agent put in an oven of 110 ° C, and incubated LH, after drying the water, to be cut into 2~5mm fibers, i.e., light emission can be prepared magnetic properties of the inorganic material;

[0118] 第二步:具有磁特性和发光特性纸的制备 [0118] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0119] I)首先,取5g绝干阔叶木浆,加入500ml蒸馏水中,在1000转/min的搅拌机中进行搅拌50min,得到搅拌液A ; [0119] I) First, 5g of oven dry hardwood pulp, was added 500ml of distilled water, stirred 50min 1000 rpm in a mixer / min, the resulting solution was stirred for A;

[0120] 2)其次,向搅拌液A中加入Sg已制取的可发光的无机强磁特性材料,再以500转/min搅拌40min,得到搅拌液B ; [0120] 2) Next, the magnetic properties of the inorganic material has Sg preparing illuminable added to the stirring solution A, then to 500 rotations / min was stirred for 40min, stirring to obtain solution B;

[0121] 3)然后,再向搅拌液B加入1.4g助留助滤剂PEI和ΡΕ0,以1200转/分继续搅拌70min,得到搅拌液C ; [0121] 3) Then, again solution B was added with stirring 1.4g PEI retention and drainage aids and ΡΕ0, minutes and stirring was continued at 1200 rpm / 70min, to give stirred solution C;

[0122] 4)然后,将搅拌后的搅拌液C移至抄片机上抄片,采用6MPa的压力压榨7min后,形成0.15mm的纸片; [0122] 4) Then, the solution was stirred for C after stirring machine to move the copy the copy sheet, after the pressing pressure of 6MPa 7min use, form a sheet of 0.15mm;

[0123] 5)最后,将纸片放入105°C的烘箱中,干燥30min后,自然冷却即得具有磁特性和发光特性纸。 [0123] 5) Finally, the paper sheet placed in an oven at 105 ° C, after drying 30min, allowed to cool to obtain magnetic characteristics having the light emitting properties of the paper.

[0124] 实施例7: [0124] Example 7:

[0125] 第一步:可发光的无机强磁特性材料的制备与处理 [0125] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0126] I)首先,按照质量分数计,将12% 的GeO2,18% 的Al2O3,8% 的B2O3, 35% 的Tb4O7,4%的Eu2O3,0.1% 的Dy2O3, 2.5% 的ZnO, 4% 的Na2SiF6,0.4% 的CeO2,0.3% 的ZrO2称量后放入玛瑙乳体中研磨混合至均匀度大于98%后,形成配合料; [0126] I) First, a mass fraction, GeO2,18% to 12% of Al2O3,8% of B2O3, 35% of Tb4O7,4% of Eu2O3,0.1% of Dy2O3, 2.5% of ZnO, 4% Na2SiF6,0.4% of the CeO2,0.3% of ZrO2 were weighed into an agate grinding bodies of more than 98% even after the mixing to form a batch;

[0127] 2)其次,在1380°C下将配合料加入铂金坩祸中,并在1380°C熔制温度下保温2小时后,放入搅拌桨继续搅拌熔制3小时,搅拌过程中温度始终保持在1380°C ; [0127] 2) Next, at 1380 ° C the batch was added platinum crucible disaster in, and after a 2 hour incubation, into a stirring blade stirring was continued melt at 1380 ° C melting temperature system 3 hours, the temperature during stirring kept at 1380 ° C;

[0128] 3)然后,待搅拌结束后,取出搅拌桨,以10°C /min的冷却速率,将熔液冷却至1350°C,并在1350°C保温30min,得到熔体; After the [0128] 3) Then, stirring until removed stirring blade, a cooling rate of 10 ° C / min, and the melt was cooled to 1350 ° C, and maintained at 1350 ° C 30min, to obtain a melt;

[0129] 4)然后,将熔制的熔体倒入600°C的铜模具中,制成直径为5mm的试样棒,待熔体固化后开模将试样棒放入650°C的退火炉中,保温Ih后随炉冷却至室温; [0129] 4) Then, the melt was poured into a melting copper mold of 600 ° C, a sample rod having a diameter of 5mm, until the melt has solidified into a test bar mold to 650 ° C in an annealing furnace, cooling to room temperature after Ih incubation with the furnace;

[0130] 5)然后,将得到的试样棒放入拉丝机中,加热至1350°C,并将试样棒拉制成直径为20〜30 μ m的纤维,并及时在试样纤维表面涂覆柔化浸润剂; [0130] 5) The sample was then put into a drawing machine rod obtained, heated to 1350 ° C, and the sample pull rod having a diameter of 20~30 μ m fiber, and the fiber surface of the sample promptly wetting agents soften coating;

[0131] 6)最后,将涂覆有柔化浸润剂的纤维放入110°C的烘箱中,保温lh,烘干水分后,剪切成长度为2〜5mm纤维,即制备出可发光的无机强磁特性材料; [0131] 6) Finally, the coated fibers soften wetting agent put in an oven of 110 ° C, and incubated LH, after drying the water, to be cut into 2~5mm fibers, i.e., light emission can be prepared magnetic properties of the inorganic material;

[0132] 第二步:具有磁特性和发光特性纸的制备 [0132] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0133] I)首先,取5g绝干阔叶木浆,加入500ml蒸馏水中,在1000转/min的搅拌机中进行搅拌50min,得到搅拌液A ; [0133] I) First, 5g of oven dry hardwood pulp, was added 500ml of distilled water, stirred 50min 1000 rpm in a mixer / min, the resulting solution was stirred for A;

[0134] 2)其次,向搅拌液A中加入Sg已制取的可发光的无机强磁特性材料,再以500转/min搅拌40min,得到搅拌液B ; [0134] 2) Next, the magnetic properties of the inorganic material has Sg preparing illuminable added to the stirring solution A, then to 500 rotations / min was stirred for 40min, stirring to obtain solution B;

[0135] 3)然后,再向搅拌液B中加入1.4g助留助滤剂CPAM和PEI,以1200转/分继续搅拌70min,得到搅拌液C; [0135] 3) Then, again solution B was added with stirring 1.4g CPAM retention and drainage aids and PEI, minutes and stirring was continued at 1200 rpm / 70min, to give stirred solution C;

[0136] 4)然后,将搅拌后的搅拌液C移至抄片机上抄片,采用6MPa的压力压榨7min后,形成0.15mm的纸片; [0136] 4) Then, the solution was stirred for C after stirring machine to move the copy the copy sheet, after the pressing pressure of 6MPa 7min use, form a sheet of 0.15mm;

[0137] 5)最后,将纸片放入105°C的烘箱中,干燥30min后,自然冷却即得具有磁特性和发光特性纸。 [0137] 5) Finally, the paper sheet placed in an oven at 105 ° C, after drying 30min, allowed to cool to obtain magnetic characteristics having the light emitting properties of the paper.

[0138] 实施例8: [0138] Example 8:

[0139] 第一步:可发光的无机强磁特性材料的制备与处理 [0139] First Step: Preparation of treated inorganic magnetic characteristics of the material capable of emitting light

[0140] I)首先,按照质量分数计,将20% 的GeO2, 22% 的Al2O3,12% 的B2O3, 35% 的Tb4O7, 3%的Eu2O3,0.5% 的Dy2O3, 2.5% 的ZnO, 5% 的Na2SiF6,0.5% 的CeO2,0.5% 的ZrO2称量后放入玛瑙乳体中研磨混合至均匀度大于98%后,形成配合料; [0140] I) First, a mass fraction, 20% of GeO2, 22% of Al2O3,12% of B2O3, 35% of Tb4O7, 3% of Eu2O3,0.5% of Dy2O3, 2.5% of ZnO, 5% Na2SiF6,0.5% of the CeO2,0.5% of ZrO2 were weighed into an agate grinding bodies of more than 98% even after the mixing to form a batch;

[0141] 2)其次,在1410°C下将配合料加入铂金坩祸中,并在1410°C熔制温度下保温I小时后,放入搅拌桨继续搅拌熔制2小时,搅拌过程中温度始终保持在1410°C ; [0141] 2) Next, at 1410 ° C the batch was added platinum crucible disaster in, and after incubation I hour, into a stirring blade stirring was continued melt at 1410 ° C melting temperature of the system 2 hours, the temperature during stirring kept at 1410 ° C;

[0142] 3)然后,待搅拌结束后,取出搅拌桨,以10°C /min的冷却速率,将熔液冷却至1350°C,并在1350°C保温30min,得到熔体; After the [0142] 3) Then, stirring until removed stirring blade, a cooling rate of 10 ° C / min, and the melt was cooled to 1350 ° C, and maintained at 1350 ° C 30min, to obtain a melt;

[0143] 4)然后,将熔制的熔体倒入600°C的铜模具中,制成直径为5mm的试样棒,待熔体固化后开模将试样棒放入650°C的退火炉中,保温2h后随炉冷却至室温; [0143] 4) Then, the melt was poured into a melting copper mold of 600 ° C, a sample rod having a diameter of 5mm, until the melt has solidified into a test bar mold to 650 ° C in an annealing furnace, cooling to room temperature after the 2h incubation with the furnace;

[0144] 5)然后,将得到的试样棒放入拉丝机中,加热至1350°C,并将试样棒拉制成直径为20〜30 μ m的纤维,并及时在试样纤维表面涂覆柔化浸润剂; [0144] 5) The sample was then put into a drawing machine rod obtained, heated to 1350 ° C, and the sample pull rod having a diameter of 20~30 μ m fiber, and the fiber surface of the sample promptly wetting agents soften coating;

[0145] 6)最后,将涂覆有柔化浸润剂的纤维放入110°C的烘箱中,保温lh,烘干水分后,剪切成长度为2〜5mm纤维,即制备出可发光的无机强磁特性材料; [0145] 6) Finally, the coated fibers soften wetting agent put in an oven of 110 ° C, and incubated LH, after drying the water, to be cut into 2~5mm fibers, i.e., light emission can be prepared magnetic properties of the inorganic material;

[0146] 第二步:具有磁特性和发光特性纸的制备 [0146] Second Step: Preparation having light-emitting characteristics and magnetic properties of paper

[0147] I)首先,取5g绝干阔叶木浆,加入500ml蒸馏水中,在1000转/min的搅拌机中进行搅拌50min,得到搅拌液A ; [0147] I) First, 5g of oven dry hardwood pulp, was added 500ml of distilled water, stirred 50min 1000 rpm in a mixer / min, the resulting solution was stirred for A;

[0148] 2)其次,向搅拌液A中加入Sg已制取的可发光的无机强磁特性材料,再以500转/min搅拌40min,得到搅拌液B ; [0148] 2) Next, the magnetic properties of the inorganic material has Sg preparing illuminable added to the stirring solution A, then to 500 rotations / min was stirred for 40min, stirring to obtain solution B;

[0149] 3)然后,再向搅拌液B中加入1.4g助留助滤剂CPAM,以1200转/分继续搅拌70min,得到搅拌液C ; [0149] 3) Then, again solution B was added with stirring 1.4g of CPAM retention and drainage aids, minutes and stirring was continued at 1200 rpm / 70min, to give stirred solution C;

[0150] 4)然后,将搅拌后的搅拌液C移至抄片机上抄片,采用6MPa的压力压榨7min后,形成0.15mm的纸片; [0150] 4) Then, the solution was stirred for C after stirring machine to move the copy the copy sheet, after the pressing pressure of 6MPa 7min use, form a sheet of 0.15mm;

[0151] 5)最后,将纸片放入105°C的烘箱中,干燥30min后,自然冷却即得具有磁特性和发光特性纸。 [0151] 5) Finally, the paper sheet placed in an oven at 105 ° C, after drying 30min, allowed to cool to obtain magnetic characteristics having the light emitting properties of the paper.

[0152]需要说明的是,本发明中所说的 GeO2, Al2O3, B2O3, Tb4O7, Eu2O3, Dy2O3, ZnO, Na2SiF6,CeO2, ZrO2*别由分析纯的氧化锗,氢氧化铝,硼酸,氧化铽,氧化铕,氧化镝,氧化锌,氟硅酸钠,氧化钟,氧化错引入。 [0152] Incidentally, the present invention refers to GeO2, Al2O3, B2O3, Tb4O7, Eu2O3, Dy2O3, ZnO, Na2SiF6, CeO2, ZrO2 * do the analytically pure germanium oxide, aluminum hydroxide, boric oxide, terbium , europium oxide, dysprosium oxide, zinc oxide, sodium fluoride, oxide clock, introducing error oxide.

[0153] 本发明通过将可发光的无机强磁特性材料与普通纸浆的复合,制备出了同时具有磁特性和发光特性的特种纸张。 [0153] The present invention can emit light by the magnetic properties of the inorganic composite material ordinary pulp, prepared a special paper having both magnetic characteristics and light emitting characteristics. 所制备的纸张不仅具有无机材料不导电,耐温高,化学性能优良,抗老化等一系列优点,而且所制备的纸张力学性能优良,不易燃烧;在相同的力学性能下,厚度比普通的纸张厚度减少20〜30%。 The prepared sheet having not only an inorganic material is not conductive, high temperature, excellent chemical resistance, aging series of advantages, but also excellent mechanical properties of the paper produced, nonflammable; at the same mechanical properties than normal paper thickness 20 to 30% reduction in thickness. 同时,所制备的纸张还表现出强的顺磁性和发红光的特殊性能。 Meanwhile, the paper produced also exhibits strong paramagnetic and special properties of red. 按照本发明制备方法制得的纸张因具有磁响应、磁记录等磁特性,可用于票据纸、包装纸、书法纸等需要有特殊身份证明高防伪的特种纸制品。 Prepared according to the method of the present invention due to paper made with magnetic characteristics of the magnetic response of the magnetic recording and the like, can be used for ticket paper, wrapping paper, calligraphy paper which require special high-security identification of specialty paper products. 本发明在纸张制备过程中不需要特殊的设备,操作简单,易于工业化生产;且磁性为永久性,不易消磁,隐蔽性强,不易被仿造。 In the paper manufacturing process according to the present invention does not require special equipment, easy to operate, easy industrial production; and a permanent magnetic, easily demagnetized concealed and difficult to counterfeit.

Claims (10)

1.一种具有磁特性和发光特性纸的制备方法,其特征在于,包括以下步骤: 第一步:可发光的无机强磁特性材料的制备与处理1)首先,按照质量分数计,将12〜20%的GeO2,18〜25%的Al2O3,8〜12 %的B2O3,35 〜40 % 的Tb4O7, 3 〜5 % 的Eu2O3,0.1 〜2 % 的Dy2O3, 2 〜3 % 的ZnO,3 〜5 % 的Na2SiF6,0.2〜0.5%的CeO2,0.3〜0.5%的ZrO2称量后放入玛瑙乳体研钵中研磨混合,形成配合料; 2)其次,在1380〜1410°C熔制温度下保温I〜2小时后,放入搅拌桨继续搅拌熔制,搅拌过程中温度始终保持在1380〜1410°C,得到熔液; 3)然后,待步骤2)搅拌结束后,取出搅拌桨,将熔液冷却至1350°C,得到熔体; 4)然后,将熔体倒入的铜模具中,待熔体固化后制成试样棒,开模后将试样棒放入650°C的退火炉中冷却至室温; 5)然后,将得到的试样棒放入拉丝机中,加热并拉制成直径为20〜30 μ m的纤维,并在纤维表面涂覆 A magnetic properties and methods of preparation of paper having a light emission characteristic, characterized by comprising: a first step: Preparation and magnetic properties of the material treated inorganic illuminable 1) First, a mass fraction, 12 GeO2,18~25% ~ 20% of the Al2O3,8~12% of B2O3,35 ~40% of Tb4O7, 3 ~5% of Eu2O3,0.1 ~2% of Dy2O3, 2 ~3% of ZnO, 3 ~ 5% Na2SiF6,0.2~0.5% of CeO2,0.3~0.5% of ZrO2 were weighed into an agate mortar for mixing thereof to form a batch; 2) next, under 1380~1410 ° C at the melting temperature after incubation I~2 hours, into a stirring blade stirring continued melting, the mixing process is always maintained at a temperature of 1380~1410 ° C, to obtain a melt; 3) then, once step 2) after the stirring, remove the stirring blade, the melt was cooled to 1350 ° C, to give a melt; 4) then, the melt was poured into a copper mold, the melt is made to be a test bar after curing, into a test bar mold after the 650 ° C annealing furnace cooling to room temperature; 5) the sample was then put into a drawing machine obtained rod was heated and drawn to a diameter of the fibers 20~30 μ m, and the coated surface of the fiber 化浸润剂; 6)最后,将涂覆有柔化浸润剂的纤维烘干水分后,剪切成长度为2〜5mm纤维,即制备出可发光的无机强磁特性材料; 第二步:具有磁特性和发光特性纸的制备1)首先,按照质量分数计,取1%〜3%的阔叶木绝干浆、5%〜10%可发光的无机强磁特性材料、0.6%〜1.5%助留助滤剂,余量为蒸馏水; 将阔叶木绝干浆加入蒸馏水中,均匀搅拌,得到搅拌液A ; 2)其次,向搅拌液A中加入所述可发光的无机强磁特性材料,进行均匀搅拌,得到搅拌液B ; 3)然后,再向搅拌液B中加入助留助滤剂,进行均匀搅拌,得到搅拌液C ; 4)然后,将搅拌液B移至抄片机上抄片,制成0.1〜0.3mm的纸片; 5)最后,将纸片进行烘后,自然冷却即得具有磁特性和发光特性纸。 Of wetting agent; 6) Finally, the coated fibers are dried after sizing soften water, as 2~5mm be cut into fiber, i.e., magnetic properties were prepared inorganic luminescent material; Step: a magnetic properties of the inorganic material produced magnetic characteristics and light emission characteristics of the paper 1) first, a mass fraction, taken 1% ~ 3% hardwood dry pulp, 5% ~ 10% may be luminescent, 0.6% ~ 1.5% co retention and drainage aids, the balance is distilled water; the hardwood dry pulp added to distilled water and uniformly stirred to give a solution a with stirring; 2) Next, magnetic properties of the inorganic light emitting material may be added to the stirring solution a, and uniformly stirred to give a solution B with stirring;. 3) then, solution B was added again stirred for retention and drainage aids, uniformly stirred to obtain a stirred solution C; 4) then, the solution was stirred on a copy machine B move copy sheet, made of sheet 0.1~0.3mm; after 5) Finally, the sheet for drying, natural cooling to obtain magnetic characteristics having the light emitting properties of the paper.
2.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,所述第一步中步骤3)取出搅拌桨后,以10°C /min的冷却速率将熔液冷却至1350°C。 According to one of the claim 1 having the magnetic characteristics and light emission characteristics of the paper production method, wherein, after said first step, step 3) Remove the stirring blade, a cooling rate of 10 ° C / min will be melt was cooled to 1350 ° C.
3.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,所述试样棒的直径为5_。 3. A method according to claim 1 having the magnetic characteristics and light emission characteristics of the paper production method, wherein the diameter of the test bar was 5_.
4.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,所述第二步中步骤I)均匀搅拌为在500〜1000转/min的搅拌机中搅拌。 According to one of the claim 1 having the magnetic characteristics and light emission characteristics of the paper production method, wherein said second step step I) is stirred in a mixer homogeneously stirred 500~1000 rpm / min in.
5.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,第二步中步骤2)均匀搅拌为在400〜600转/min搅拌机中搅拌。 5. A method according to claim 1 having the magnetic characteristics and light emission characteristics of the paper production method, wherein, in the second step in step 2) is stirred homogeneously stirred at 400~600 rpm / min mixer.
6.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,第二步中步骤3)均匀搅拌为在以800〜1500转/min搅拌机中搅拌。 6. A method according to claim 1 having the magnetic characteristics and light emission characteristics of the paper production method, wherein, in the second step in step 3) is stirred in homogeneously stirred at 800~1500 rpm / min mixer.
7.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,所述纸片采用4〜6MPa的压力压榨3〜15min后形成。 According to one of the claim 1 having the magnetic characteristics and light emission characteristics of the paper production method, wherein, after the sheet is formed using a pressure press 4~6MPa 3~15min.
8.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,将纸片进行烘干、干燥为将纸片放入105〜110°C的烘箱中干燥。 According to claim 1 having one of the magnetic characteristics and light emission characteristics of the paper production method, wherein, for drying the paper sheet, the sheet is placed in an oven dried 105~110 ° C dried.
9.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,所述助留助滤剂为CPAM、PE1、PEO中的一种或几种。 According to claim 1 having one of the magnetic properties and methods of preparation of the luminescent properties of the paper, wherein the retention aid is one or more of CPAM, PE1, PEO in.
10.根据权利要求1所述的一种具有磁特性和发光特性纸的制备方法,其特征在于,所述柔化浸润剂是将石蜡:凡士林:硬脂酸:水=1:1:1:30的质量比称量后,先将石蜡、凡士林和硬脂酸熔化后,再加入水,混合均匀后配置而成。 10. A method according to claim 1 having the magnetic characteristics and light emission characteristics of the paper production method, wherein the wetting agent is a softening paraffin: petrolatum: Stearic acid: water = 1: 1: 1: after weighing 30 mass ratio, first paraffin wax, petrolatum, and the stearic acid melted and then water was added, mixed uniformly arranged together.
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