CN104846698A - Ultraviolet double-wave excitation fluorescent transparent invisible anti-fake nano-paper preparation method - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000005284 excitation Effects 0.000 title abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052747 lanthanoid Inorganic materials 0.000 claims abstract description 12
- 150000002602 lanthanoids Chemical class 0.000 claims abstract description 11
- 230000009977 dual effect Effects 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- 229920001046 Nanocellulose Polymers 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000007639 printing Methods 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000005357 flat glass Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 230000035515 penetration Effects 0.000 claims description 4
- 238000007650 screen-printing Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 2
- 238000007641 inkjet printing Methods 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 4
- 229910052799 carbon Inorganic materials 0.000 claims 4
- 229910052772 Samarium Inorganic materials 0.000 claims 1
- 229910052771 Terbium Inorganic materials 0.000 claims 1
- -1 compound lanthanide Chemical class 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 229920003043 Cellulose fiber Polymers 0.000 abstract 1
- 239000000047 product Substances 0.000 description 3
- 239000003086 colorant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Abstract
本发明公开了一种紫外双波激发的荧光透明隐形防伪纳米纸的制备方法。本发明首先将镧系配合物与氧化纳米纤维素纤维（ONFC）进行复合，形成荧光透明纳米纸；然后将荧光碳点定点印刷在纳米纸上，得到含有隐形防伪标签的双重荧光透明纳米纸。含有隐形标签的新型荧光透明防伪纳米纸在双波段紫外光激发下具有双重荧光效应。本发明制备的防伪纳米纸高度透明，可见光下目视防伪标签不可辨识，特定紫外波长下具有双色荧光效果，大大增加了仿制难度，提高了防伪性能。
The invention discloses a preparation method of fluorescent transparent invisible anti-counterfeiting nano paper excited by ultraviolet double waves. In the invention, firstly, the lanthanide complex is compounded with oxidized nano-cellulose fiber (ONFC) to form fluorescent transparent nano-paper; then fluorescent carbon dots are fixed-point printed on the nano-paper to obtain double fluorescent transparent nano-paper with invisible anti-counterfeiting labels. A new type of fluorescent transparent anti-counterfeiting nanopaper with invisible labels has dual fluorescence effects under the excitation of dual-band ultraviolet light. The anti-counterfeiting nano-paper prepared by the invention is highly transparent, the anti-counterfeiting label cannot be recognized visually under visible light, and has a two-color fluorescent effect under a specific ultraviolet wavelength, which greatly increases the difficulty of imitation and improves the anti-counterfeiting performance.
Description
技术领域 technical field
本发明涉及一种防伪纳米纸及其制备方法，尤其涉及紫外双波段激发的荧光透明隐形防伪纳米纸的制备方法，属于防伪纳米纸制备技术领域。 The invention relates to an anti-counterfeit nano paper and a preparation method thereof, in particular to a preparation method of fluorescent transparent invisible anti-counterfeit nano paper excited by ultraviolet dual-band, and belongs to the technical field of anti-counterfeit nano paper preparation.
背景技术 Background technique
随着人们对产权保护和品牌意识的增强，防伪在证件、货币、标签、重要文档以及国家安全等各个行业的作用越来越重要，通常用于杜绝假冒伪劣、维护企业形象和保护消费者权益等商业领域。荧光效果是防伪领域常见的技术手段之一，具有制备简单、易于识别等优势。目前的荧光防伪纸制造过程中，荧光材料大多数经过涂布或印刷负载在已经成型的纸张表面，使纸张的特定区域具有荧光性能，从而达到防伪的效果。这种经过二次加工的防伪纸，其荧光材料容易从纸张表面脱落，荧光分子不够稳定，荧光效果容易被仿制。 As people's awareness of property rights protection and brand awareness increases, anti-counterfeiting plays an increasingly important role in various industries such as certificates, currency, labels, important documents, and national security. It is usually used to eliminate counterfeiting, maintain corporate image, and protect consumer rights. and other commercial fields. Fluorescent effect is one of the common technical means in the field of anti-counterfeiting, which has the advantages of simple preparation and easy identification. In the current manufacturing process of fluorescent anti-counterfeiting paper, most of the fluorescent materials are coated or printed on the surface of the formed paper, so that specific areas of the paper have fluorescent properties, thereby achieving the anti-counterfeiting effect. The fluorescent material of this secondary processed anti-counterfeiting paper is easy to fall off from the surface of the paper, the fluorescent molecules are not stable enough, and the fluorescent effect is easy to be imitated.
不同的荧光染料分子所需的激发波长不同。目前市场上常见的多为单色单波的荧光防伪纸，仿制简单，防伪能力差；而多色荧光防伪纸由于发射光谱容易重叠，会造成荧光标记难以识别。所以，开发一种稳定、多色、难仿制的新型荧光防伪纸，具有重要意义。 Different fluorescent dye molecules require different excitation wavelengths. At present, most of the fluorescent anti-counterfeiting papers in the market are single-color and single-wave fluorescent, which are easy to imitate and have poor anti-counterfeiting capabilities; and multi-color fluorescent anti-counterfeiting papers are easy to overlap due to the emission spectrum, which will make it difficult to identify fluorescent marks. Therefore, it is of great significance to develop a novel fluorescent anti-counterfeiting paper that is stable, multi-colored and difficult to imitate.
发明内容 Contents of the invention
本发明的目的在于提供一种新型的荧光透明隐形防伪纳米纸，分别通过两种荧光材料，一种添加在纸张基体内使纸张发光，另外一种印刷在纸张表面形成特定图案发光。利用两种激发波长，可以稳定的发射两种不同颜色的荧光，从而增强荧光防伪效果。其中一种荧光材料为镧系配合物，利用稀土元素的配位机制，原位嫁接镧系配合物于改性的纳米纤维素上，通过高压压滤法一步合成荧光透明纳米纸。另一种荧光材料为具有荧光性能的碳量子点溶液，将其作为墨水，通过物理渗透的方式，将防伪标签定点印刷在纳米纸上，形成具有双重防伪功能的荧光透明纳米纸。 The purpose of the present invention is to provide a new type of fluorescent transparent invisible anti-counterfeiting nano-paper. Two kinds of fluorescent materials are used respectively, one is added in the paper matrix to make the paper emit light, and the other is printed on the surface of the paper to form a specific pattern to emit light. Using two excitation wavelengths, two different colors of fluorescence can be stably emitted, thereby enhancing the anti-counterfeiting effect of fluorescence. One of the fluorescent materials is a lanthanide complex. Using the coordination mechanism of rare earth elements, the lanthanide complex is grafted on the modified nanocellulose in situ, and the fluorescent transparent nanopaper is synthesized in one step by a high-pressure filtration method. Another fluorescent material is a carbon quantum dot solution with fluorescent properties, which is used as an ink to print anti-counterfeiting labels on the nano-paper at fixed points through physical penetration, forming a fluorescent transparent nano-paper with double anti-counterfeiting functions.
本发明的目的可以通过以下技术方案得以实现： The purpose of the present invention can be achieved through the following technical solutions:
a. 荧光透明纳米纸的制备：镧系配合物与氧化纳米纤维素纤维（ONFC）进行复合成纸，将镧系配合物和ONFC均匀分散在50-100 mL乙醇溶液中，超声分散得到荧光ONFC悬浮液，其中ONFC的合适比例为0.1~1w/v%，镧系配合物的种类为Eu(dbm)3(H2O)2、Sm(dbm)3(H2O)2或Tb(Tfacac)3(H2O)2，合适比例为1~10 mg，其中镧系配合物和ONFC的质量比为1：5～1：20。将所得的悬浮液倒入高压压滤机中，调节压强为0.5~2MPa，压滤至不再有滤液流出，压滤结束，得到透明纳米纸。在特定波长的紫外光照射下，纳米纸发出均匀的荧光。 a. Preparation of fluorescent transparent nanopaper: lanthanide complexes and oxidized nanocellulose fibers (ONFC) were composited into paper, lanthanide complexes and ONFC were uniformly dispersed in 50-100 mL ethanol solution, and ultrasonically dispersed to obtain fluorescent ONFC Suspension, in which the appropriate proportion of ONFC is 0.1~1w/v%, and the type of lanthanide complex is Eu(dbm) 3 (H 2 O) 2 , Sm(dbm) 3 (H 2 O) 2 or Tb(Tfacac ) 3 (H 2 O) 2 , the proper ratio is 1~10 mg, and the mass ratio of lanthanide complex to ONFC is 1:5~1:20. Pour the obtained suspension into a high-pressure filter press, adjust the pressure to 0.5-2 MPa, press filter until no more filtrate flows out, and the filter press ends to obtain transparent nanopaper. Under the irradiation of ultraviolet light of a specific wavelength, the nanopaper emits uniform fluorescence.
b. 隐形防伪纳米纸的印刷：将粒度范围为2~10 nm的荧光碳点以0.01 mg/mL ~10 mg/mL比例分散在溶剂中，根据碳点溶解性的不同，此处溶剂性质可以为水，也可以为乙醇、异丙醇、氯仿等有机溶剂。将所述的含有荧光碳点的溶剂作为墨水，定点印刷在荧光透明纳米纸表面预定位置，然后放置在平整的玻璃片上自然晾干，得到含有特定标签的双荧光透明纳米纸。在特定紫外光照射下，纳米纸预定位置处会发出荧光，呈现出防伪标志。 b. Printing of invisible anti-counterfeiting nanopaper: Disperse fluorescent carbon dots with a particle size range of 2-10 nm in a solvent at a ratio of 0.01 mg/mL to 10 mg/mL. According to the different solubility of carbon dots, the solvent properties here can be Water may be used, and organic solvents such as ethanol, isopropanol, and chloroform may be used. The solvent containing fluorescent carbon dots is used as ink, fixed-point printed on a predetermined position on the surface of fluorescent transparent nano paper, and then placed on a flat glass sheet to dry naturally to obtain double fluorescent transparent nano paper containing specific labels. Under the irradiation of specific ultraviolet light, the predetermined position of the nano paper will emit fluorescence, presenting an anti-counterfeiting mark.
所述的防伪纸的印刷方式为喷墨打印、丝网印刷或纳米压印。所述的防伪纸中的添加的两种荧光材料分别是通过化学反应和物理渗透两种方式实现的。 The printing method of the anti-counterfeiting paper is inkjet printing, screen printing or nano-imprinting. The two kinds of fluorescent materials added in the anti-counterfeiting paper are respectively realized through chemical reaction and physical penetration.
本发明具有以下优点： The present invention has the following advantages:
（1） 本发明首次在纳米纤维素纸中添加了两种不同的荧光材料，通过化学反应和物理渗透两种方法得以实现，具有稳定的、互不干扰的荧光性能； (1) The present invention adds two different fluorescent materials to the nanocellulose paper for the first time, which is realized through two methods of chemical reaction and physical penetration, and has stable and non-interfering fluorescent properties;
（2） 本发明所提供的防伪纳米纸由氧化纳米纤维素、镧系配合物分子及碳量子点组成，所有组成材料为纳米及分子尺度，极大的降低了光散射作用，形成高度透明的防伪纳米纸，可见光下目视防伪标志不可辨识（图1），难以仿制，具有隐形防伪作用； (2) The anti-counterfeiting nanopaper provided by the present invention is composed of oxidized nanocellulose, lanthanide complex molecules and carbon quantum dots. All the constituent materials are nanometer and molecular scale, which greatly reduces the light scattering effect and forms a highly transparent Anti-counterfeiting nano-paper, the visual anti-counterfeiting mark cannot be recognized under visible light (Figure 1), it is difficult to imitate, and has invisible anti-counterfeiting effect;
（3） 本发明所提供的荧光纳米纸能够被两种不同波长的紫外光进行激发，能够清晰的呈现两种可分辨的荧光颜色（图2和图3），其激发和发射周期长，比传统常规的防伪纸具有更强的双重防伪效果； (3) The fluorescent nanopaper provided by the present invention can be excited by ultraviolet light of two different wavelengths, and can clearly present two distinguishable fluorescent colors (Figure 2 and Figure 3), and its excitation and emission cycle is longer than Traditional anti-counterfeiting paper has a stronger double anti-counterfeiting effect;
（4） 本发明提供的荧光纳米纸，其荧光颜色可以在普通紫外灯照射下目视可辨，达到不影响产品包装、简便、直观的防伪效果，具有广泛的应用前景。 (4) The fluorescent nano-paper provided by the present invention, whose fluorescent color can be recognized visually under the irradiation of ordinary ultraviolet lamps, achieves a simple and intuitive anti-counterfeiting effect that does not affect product packaging, and has a wide application prospect.
附图说明 Description of drawings
图1 可见光下荧光透明防伪纳米纸照片，虚线框显示了防伪纳米纸上隐形二维码位置。 Figure 1 Photo of fluorescent transparent anti-counterfeiting nanopaper under visible light, the dotted line box shows the invisible QR code on the anti-counterfeiting nanopaper.
图2波长254 nm紫外光激发下印有二维码的透明防伪纳米纸照片。 Figure 2 Photo of transparent anti-counterfeiting nanopaper printed with two-dimensional codes under the excitation of ultraviolet light with a wavelength of 254 nm.
图3波长365 nm紫外光激发下印有二维码的透明防伪纳米纸照片。 Figure 3 Photo of transparent anti-counterfeiting nanopaper printed with two-dimensional codes under the excitation of ultraviolet light with a wavelength of 365 nm.
具体实施方式 Detailed ways
实施例一Embodiment one
S1. 将ONFC均匀分散在100 mL乙醇溶液中，形成0.5w/v%的稳定悬浮液，再向溶液中加入5 mg Tb(Tfacac)3(H2O)2，超声分散均匀，然后将得到悬浮液倒入高压压滤机中，调节合适的压强，压滤至不再有滤液流出，得到透明纳米纸。 S1. Uniformly disperse ONFC in 100 mL ethanol solution to form a stable suspension of 0.5w/v%, then add 5 mg Tb(Tfacac) 3 (H 2 O) 2 to the solution, ultrasonically disperse evenly, and then obtain Pour the suspension into a high-pressure filter press, adjust the appropriate pressure, and filter until no more filtrate flows out to obtain transparent nanopaper.
S2. 将粒度大小约为4 nm的荧光碳点以0.05 mg/mL的比例分散在去离子水中作为荧光墨水，采用丝网印刷技术，将产品的二维码印刷在荧光透明纳米纸表面，其放置在平整的玻璃片上自然晾干，得到隐形的带有二维码的双荧光透明的纳米纸。 S2. Disperse fluorescent carbon dots with a particle size of about 4 nm in deionized water at a ratio of 0.05 mg/mL as fluorescent ink, and use screen printing technology to print the two-dimensional code of the product on the surface of fluorescent transparent nano-paper. Place it on a flat glass sheet to dry naturally to obtain an invisible double-fluorescence transparent nano-paper with a two-dimensional code.
S3. 荧光性能测试：在波长365 nm的紫外光激发下，碳量子点会发射蓝色荧光，透明纳米纸预定位置处会呈现出清晰的蓝光二维码标记（图2），而在波长为254 nm的紫外光激发下，碳量子点仍发射蓝色荧光，同时Tb(Tfacac)3(H2O)2发射绿色荧光，绿色透明的纳米纸上蓝色二维码清晰可见（图3）。 S3. Fluorescence performance test: Under the excitation of ultraviolet light with a wavelength of 365 nm, the carbon quantum dots will emit blue fluorescence, and a clear blue two-dimensional code mark will appear at the predetermined position of the transparent nanopaper (Figure 2), while at a wavelength of 365 nm Under the excitation of 254 nm ultraviolet light, the carbon quantum dots still emit blue fluorescence, while Tb(Tfacac) 3 (H 2 O) 2 emits green fluorescence, and the blue QR code is clearly visible on the green transparent nanopaper (Figure 3) .
实施例二 Embodiment two
S1. 将ONFC均匀分散在100 mL乙醇溶液中，形成0.5w/v%的稳定悬浮液，再向溶液中加入5 mg Eu(dbm)3(H2O)2，超声分散均匀，然后将得到悬浮液倒入高压压滤机中，调节合适的压强，压滤至不再有滤液流出，得到透明纳米纸。 S1. Uniformly disperse ONFC in 100 mL ethanol solution to form a stable suspension of 0.5w/v%, then add 5 mg Eu(dbm) 3 (H 2 O) 2 to the solution, ultrasonically disperse evenly, and then obtain Pour the suspension into a high-pressure filter press, adjust the appropriate pressure, and filter until no more filtrate flows out to obtain transparent nanopaper.
S2. 将粒度大小约为4 nm的荧光碳点以0.1 mg/mL的比例分散在无水乙醇中作为荧光墨水，采用丝网印刷技术，将产品的二维码印刷在荧光透明纳米纸表面，其放置在平整的玻璃片上自然晾干，得到隐形的带有二维码的双荧光透明的纳米纸。 S2. Disperse fluorescent carbon dots with a particle size of about 4 nm in anhydrous ethanol at a ratio of 0.1 mg/mL as fluorescent ink, and use screen printing technology to print the two-dimensional code of the product on the surface of fluorescent transparent nano-paper. It is placed on a flat glass sheet to dry naturally, and an invisible double fluorescent transparent nano-paper with a two-dimensional code is obtained.
S3. 荧光性能测试：在波长254 nm的紫外光激发下，碳量子点会发射蓝色荧光，透明纳米纸预定位置处会呈现出清晰的蓝光二维码标记，而在波长为365 nm的紫外光激发下，碳量子点仍发射蓝色荧光，同时Eu(dbm)3(H2O)2发射红色荧光，红色透明的纳米纸上蓝色二维码清晰可见。 S3. Fluorescence performance test: Under the excitation of ultraviolet light with a wavelength of 254 nm, the carbon quantum dots will emit blue fluorescence, and a clear blue two-dimensional code mark will appear at the predetermined position of the transparent nanopaper, while the ultraviolet light with a wavelength of 365 nm Under light excitation, the carbon quantum dots still emit blue fluorescence, while Eu(dbm) 3 (H 2 O) 2 emits red fluorescence, and the blue QR code is clearly visible on the red transparent nanopaper.
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| CN105417519A (en) * | 2015-11-20 | 2016-03-23 | 江南大学 | Method for preparing quantum dot invisible ink based on laser-induced technology |
| CN106009931A (en) * | 2016-05-05 | 2016-10-12 | 中国科学院长春光学精密机械与物理研究所 | Information encryption method and system and encrypted information reading method and system |
| CN106189521A (en) * | 2016-09-14 | 2016-12-07 | 天津大学 | A kind of fluorescence invisible ink based on Fluorin doped carbon quantum dot and preparation method thereof |
| CN106674557A (en) * | 2016-10-28 | 2017-05-17 | 陕西科技大学 | Rare earth-based nano-crystalline cellulose fiber film having ultraviolet ray filtering performance and preparation method thereof |
| CN106701065A (en) * | 2017-01-04 | 2017-05-24 | 华南理工大学 | Plant micro-nano cellulose fluorescence labeling method |
| CN106752380A (en) * | 2016-12-19 | 2017-05-31 | 武汉大学 | A kind of aqueous Fluorescent Falsification-resistant Ink based on graphene quantum dot |
| CN107043576A (en) * | 2017-05-12 | 2017-08-15 | 武汉大学 | The preparation of dual mode luminous ink and its method for printing screen and Application in Anti-counterfeiting |
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