CN110484016A - A kind of Yellow fluorochrome and preparation method thereof and application - Google Patents
A kind of Yellow fluorochrome and preparation method thereof and application Download PDFInfo
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- CN110484016A CN110484016A CN201910703414.3A CN201910703414A CN110484016A CN 110484016 A CN110484016 A CN 110484016A CN 201910703414 A CN201910703414 A CN 201910703414A CN 110484016 A CN110484016 A CN 110484016A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- BFMYDTVEBKDAKJ-UHFFFAOYSA-L disodium;(2',7'-dibromo-3',6'-dioxido-3-oxospiro[2-benzofuran-1,9'-xanthene]-4'-yl)mercury;hydrate Chemical compound O.[Na+].[Na+].O1C(=O)C2=CC=CC=C2C21C1=CC(Br)=C([O-])C([Hg])=C1OC1=C2C=C(Br)C([O-])=C1 BFMYDTVEBKDAKJ-UHFFFAOYSA-L 0.000 title claims 6
- 239000007850 fluorescent dye Substances 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000975 dye Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 13
- 239000004753 textile Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 6
- 238000004043 dyeing Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 239000002086 nanomaterial Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- PJKVFARRVXDXAD-UHFFFAOYSA-N 2-naphthaldehyde Chemical compound C1=CC=CC2=CC(C=O)=CC=C21 PJKVFARRVXDXAD-UHFFFAOYSA-N 0.000 claims 1
- FRTNIYVUDIHXPG-UHFFFAOYSA-N acetic acid;ethane-1,2-diamine Chemical class CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCN FRTNIYVUDIHXPG-UHFFFAOYSA-N 0.000 claims 1
- 150000002171 ethylene diamines Chemical class 0.000 claims 1
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 239000002689 soil Substances 0.000 claims 1
- 238000009941 weaving Methods 0.000 claims 1
- 230000005923 long-lasting effect Effects 0.000 abstract description 7
- 238000000502 dialysis Methods 0.000 abstract description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 abstract description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract description 3
- 229950011260 betanaphthol Drugs 0.000 abstract description 3
- 239000012141 concentrate Substances 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 21
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 239000004927 clay Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 125000000623 heterocyclic group Chemical group 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- -1 anhydride dipotassium salt Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B27/00—Preparations in which the azo group is formed in any way other than by diazotising and coupling, e.g. oxidation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0079—Azoic dyestuff preparations
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/004—Dyeing with phototropic dyes; Obtaining camouflage effects
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/02—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using azo dyes
- D06P1/04—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using azo dyes not containing metal
- D06P1/06—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using azo dyes not containing metal containing acid groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1003—Carbocyclic compounds
- C09K2211/1011—Condensed systems
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1029—Heterocyclic compounds characterised by ligands containing one nitrogen atom as the heteroatom
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Coloring (AREA)
Abstract
本发明涉及荧光染料,尤其涉及一种黄色荧光染料及其制备方法以及应用。以重量计,包括以下原料:2~10份乙二胺四乙酸、10~30份乙二胺、1~5g份1,2‑吡啶偶氮2‑萘酚。制备方法具体包括如下步骤:(1)将上述原料加水,超声混合均匀;(2)将原料液放入不锈钢反应釜,加热至180~220℃,反应4h;(3)将反应后的液混合体放入透析袋进行透析,透析2~4h;(4)使用旋转蒸发仪对混合液体进行浓缩,旋蒸温度为55~65℃;5)将上述混合液体放入超低温冰箱,冷冻24~48h。所合成的碳量子点溶液呈鲜艳的黄色,并且在紫外灯下呈现强烈的黄光,所合成的荧光几乎不衰减,形成了长效的荧光。制备方法简单方便。
The invention relates to fluorescent dyes, in particular to a yellow fluorescent dye and its preparation method and application. Calculated by weight, the following raw materials are included: 2-10 parts of ethylenediaminetetraacetic acid, 10-30 parts of ethylenediamine, and 1-5 g parts of 1,2-pyridylazo-2-naphthol. The preparation method specifically includes the following steps: (1) adding water to the above-mentioned raw materials, and ultrasonically mixing them uniformly; (2) putting the raw material liquid into a stainless steel reactor, heating to 180-220°C, and reacting for 4 hours; (3) mixing the reacted liquid Put the body into a dialysis bag for dialysis, and dialyze for 2-4 hours; (4) Use a rotary evaporator to concentrate the mixed liquid at a temperature of 55-65°C; 5) Put the above-mentioned mixed liquid in an ultra-low temperature refrigerator and freeze it for 24-48 hours . The synthesized carbon quantum dot solution is bright yellow, and shows strong yellow light under an ultraviolet lamp, and the synthesized fluorescence hardly decays, forming long-lasting fluorescence. The preparation method is simple and convenient.
Description
技术领域technical field
本发明涉及荧光染料,尤其涉及一种黄色荧光染料及其制备方法以及应用。The invention relates to fluorescent dyes, in particular to a yellow fluorescent dye and its preparation method and application.
背景技术Background technique
荧光染料本身是一种染料,可以应用于纺织、印染等行业。由于其具有荧光特性,因 此可以应用于防伪、装饰、模型构建等领域。纳米级别的荧光染料,染料颗粒很小,容易进入到所染对象组织中,同时具有分散性好、色彩均匀等优点,因此具有广阔的应用前景。Fluorescent dye itself is a kind of dye, which can be used in textile, printing and dyeing industries. Due to its fluorescent properties, it can be used in anti-counterfeiting, decoration, model building and other fields. Nanoscale fluorescent dyes have very small dye particles, which are easy to enter into the tissue of the dyed object. At the same time, they have the advantages of good dispersion and uniform color, so they have broad application prospects.
现有的荧光染料不稳定,容易分解,不具有长效性;其合成方法、纯化方法还是保存 方法,都非常地繁琐与不便。Existing fluorescent dyes are unstable, easy to decompose, and have no long-term effect; their synthesis methods, purification methods, and preservation methods are all very cumbersome and inconvenient.
201810276697.3公开了“一种荧光染料”,其采用4-氨基-3,6-二磺基-1,8-萘醛酸酐二 钾盐,0.6mol对苯二胺,因在合成原料中含有硫元素,因此具备不良的气味。201810694947.5 公开了“一种荧光染料”,其原料使用荧光剂来产生荧光,颗粒较大。首先,上述荧光染 料不属于纳米级别,不具备纳米材料诸多的性质;其次,原料中含有硫元素,会产生废气; 再次,合成的荧光染料荧光强度弱并且不持久。201810276697.3 discloses "a fluorescent dye", which uses 4-amino-3,6-disulfo-1,8-naphtalic anhydride dipotassium salt, 0.6mol p-phenylenediamine, because the synthetic raw materials contain sulfur element , so it has a bad smell. 201810694947.5 discloses "a fluorescent dye", the raw material of which uses a fluorescent agent to generate fluorescence, and the particles are relatively large. Firstly, the above-mentioned fluorescent dyes are not at the nanometer level, and do not have many properties of nanomaterials; secondly, the raw materials contain sulfur elements, which will generate waste gas; thirdly, the fluorescent dyes synthesized have weak fluorescence intensity and are not durable.
发明内容Contents of the invention
为了克服现有技术的不足,本发明提供一种黄色荧光染料及其制备方法以及应用。所 合成的碳量子点溶液呈鲜艳的黄色,并且在紫外灯下呈现强烈的黄光,所合成的荧光几乎 不衰减,形成了长效的荧光。In order to overcome the deficiencies of the prior art, the present invention provides a yellow fluorescent dye and its preparation method and application. The synthesized carbon quantum dot solution is bright yellow, and shows strong yellow light under an ultraviolet lamp, and the synthesized fluorescence hardly decays, forming long-lasting fluorescence.
为了达到上述目的,本发明采用以下技术方案实现:In order to achieve the above object, the present invention adopts the following technical solutions to realize:
一种黄色荧光染料,以重量计,包括以下原料:2~10份乙二胺四乙酸、10~30份乙二胺、1~5份1,2-吡啶偶氮2-萘酚。A yellow fluorescent dye comprises the following raw materials by weight: 2-10 parts of ethylenediaminetetraacetic acid, 10-30 parts of ethylenediamine, and 1-5 parts of 1,2-pyridylazo-2-naphthol.
一种黄色荧光染料的制备方法,该方法具体包括如下步骤:A preparation method of yellow fluorescent dye, the method specifically comprises the steps of:
(1)将上述原料加水,超声混合均匀;(1) Add water to the above-mentioned raw materials, and ultrasonically mix them evenly;
(2)将原料液放入不锈钢反应釜,加热至180~220℃,反应4h;(2) Put the raw material solution into a stainless steel reactor, heat to 180-220°C, and react for 4 hours;
(3)将反应后的液混合体放入透析袋进行透析,透析2~4h;(3) Put the reacted liquid mixture into a dialysis bag for dialysis for 2 to 4 hours;
(4)使用旋转蒸发仪对混合液体进行浓缩,旋蒸温度为55~65℃;(4) Use a rotary evaporator to concentrate the mixed liquid, and the rotary evaporation temperature is 55-65°C;
(5)将上述混合液体放入超低温冰箱,冷冻24~48h;(5) Put the above mixed liquid into an ultra-low temperature refrigerator and freeze for 24-48 hours;
(6)将冷冻后的混合物料放入冷冻干燥机,冷冻干燥即得黄色荧光纳米材料固体。(6) Put the frozen mixed material into a freeze dryer and freeze dry to obtain a solid yellow fluorescent nanomaterial.
一种黄色荧光染料具有如下应用:A yellow fluorescent dye has the following applications:
a、荧光防伪墨水a. Fluorescent anti-counterfeiting ink
将制得的黄色荧光纳米荧光染料配制成0.1~5%染料浓度的溶液,使用钢笔笔芯吸取 染料液,可在白纸上或者钱币上进行书写。The prepared yellow fluorescent nanometer fluorescent dye is formulated into a solution with a dye concentration of 0.1-5%, and the dye solution is absorbed by a pen core, and can be written on white paper or coins.
b.、黄色荧光染料在纺织上的应用b. Application of yellow fluorescent dye in textile
将制得的黄色纳米荧光染料配制成0.1~5%染料浓度的染料液,将纺织物进入其中浸 泡12~24h,即得染色后的荧光纺织物。The prepared yellow nanometer fluorescent dye is formulated into a dye solution with a dye concentration of 0.1-5%, and textiles are soaked in it for 12-24 hours to obtain dyed fluorescent textiles.
c、纳米荧光粉的应用c. Application of nano phosphor
将粉状的纳米荧光粉与活性白土混合,混合配比1:1~1:5,制成带有荧光的泥土模型。Mix powdery nano-fluorescent powder with activated clay at a mixing ratio of 1:1 to 1:5 to make a fluorescent clay model.
与现有方法相比,本发明的有益效果是:Compared with existing methods, the beneficial effects of the present invention are:
(1)本发明具备杂环(吡啶),同时又兼具苯环(萘酚)这样复杂结构的原料,同 时使用强碱性试剂去破坏吡啶环和萘酚环,在高温下,形成了非常稳定的结 构,这样有助于长效荧光的形成。以上提到的荧光,是在紫外灯下照射才会 观察到的荧光。(1) The present invention possesses heterocyclic (pyridine) and raw materials with complex structures such as benzene ring (naphthol) concurrently. At the same time, a strong alkaline reagent is used to destroy the pyridine ring and naphthol ring. At high temperature, a very Stable structure, which is conducive to the formation of long-lasting fluorescence. The fluorescence mentioned above is the fluorescence that can only be observed under ultraviolet light.
(2)无论是合成方法、纯化方法还是保存方法,都非常地简单方便。(2) Whether it is a synthesis method, a purification method or a preservation method, it is very simple and convenient.
(3)根据荧光染料的特点,打破常规,进行了一系列应用,为黄色荧光染料的突 破性实际应用提供了模板。(3) According to the characteristics of fluorescent dyes, a series of applications were carried out, which provided a template for the breakthrough practical application of yellow fluorescent dyes.
本发明长所合成的碳量子点溶液呈鲜艳的黄色,并且在紫外灯下呈现强烈的黄光,所 合成的荧光几乎不衰减,形成了长效的荧光。The carbon quantum dot solution synthesized by the present invention is bright yellow, and shows strong yellow light under an ultraviolet lamp, and the synthesized fluorescence hardly decays, forming long-lasting fluorescence.
附图说明Description of drawings
图1是本发明黄色荧光染料日光灯下的状态图;Fig. 1 is the state diagram under the yellow fluorescent dye fluorescent lamp of the present invention;
图2是本发明黄色荧光染料在紫外灯下的状态图;Fig. 2 is the state figure of yellow fluorescent dye of the present invention under ultraviolet lamp;
图3是本发明黄色荧光染料紫外、激发和发射光谱图;Fig. 3 is a yellow fluorescent dye ultraviolet, excitation and emission spectrogram of the present invention;
图4是本发明在纸上绘制的小鸟在日光灯下的状态图;Fig. 4 is the state diagram of the bird drawn on paper by the present invention under the fluorescent lamp;
图5是本发明在纸上绘制的小鸟在紫外灯下的状态图;Fig. 5 is the state diagram of the bird drawn on paper by the present invention under an ultraviolet lamp;
图6是本发明纸上绘制的校徽在日光灯下的状态图;Fig. 6 is the state diagram of the school emblem drawn on the paper of the present invention under the fluorescent lamp;
图7是本发明纸上绘制的校徽在紫外灯下的状态图;Fig. 7 is the state diagram of the school emblem drawn on the paper of the present invention under an ultraviolet lamp;
图8是本发明在钱币上书写的数字在日光灯下的状态图;Fig. 8 is a state diagram of the numbers written on the coins in the present invention under fluorescent lamps;
图9是本发明在钱币上书写的数字在紫外灯下的状态图;Fig. 9 is a state diagram of the numbers written on the coins in the present invention under an ultraviolet lamp;
图10是使用本发明在布料上染色与未使用本发明未染色在日光灯下的对比图;Fig. 10 is the contrast figure of using the present invention to dye on the cloth and not using the present invention to be undyed under the fluorescent lamp;
图11是使用本发明在布料上染色与未使用本发明未染色在紫外灯下的对比图;Fig. 11 is the contrast figure of using the present invention to dye on the cloth and not using the present invention and not dyeing under the ultraviolet lamp;
图12是使用本发明制成的工艺品在日光灯下的状态图;Fig. 12 is a state diagram using the handicraft made by the present invention under the fluorescent lamp;
图13是使用本发明制成的工艺品在紫外灯下的状态图。Fig. 13 is a state diagram of the handicraft made by the present invention under an ultraviolet lamp.
具体实施方式Detailed ways
下面对本发明的具体实施方式作进一步说明,但不用来限制本发明的范围:The specific embodiment of the present invention will be further described below, but it is not used to limit the scope of the present invention:
一种黄色荧光染料,以重量计,包括以下原料:0.2~1g乙二胺四乙酸、1~3ml乙二胺、0.01~0.05g 1,2-吡啶偶氮2-萘酚。A yellow fluorescent dye comprises the following raw materials by weight: 0.2-1g ethylenediaminetetraacetic acid, 1-3ml ethylenediamine, 0.01-0.05g 1,2-pyridylazo-2-naphthol.
一种黄色荧光染料的制备方法,该方法具体包括如下步骤:A preparation method of yellow fluorescent dye, the method specifically comprises the steps of:
(1)将上述原料加水定容至20ml后,超声混合均匀;(1) After adding water to the above raw materials to 20ml, ultrasonically mix them evenly;
(2)将原料液放入不锈钢反应釜,加热至180~220℃,反应4h;(2) Put the raw material solution into a stainless steel reactor, heat to 180-220°C, and react for 4 hours;
(3)将反应后的液混合体放入透析袋进行透析,透析2~4h;(3) Put the reacted liquid mixture into a dialysis bag for dialysis for 2 to 4 hours;
(4)使用旋转蒸发仪对混合液体进行浓缩,旋蒸温度为55~65℃;(4) Use a rotary evaporator to concentrate the mixed liquid, and the rotary evaporation temperature is 55-65°C;
(5)将上述混合液体放入超低温冰箱,冷冻24~48h;(5) Put the above mixed liquid into an ultra-low temperature refrigerator and freeze for 24-48 hours;
(6)将冷冻后的混合物料放入冷冻干燥机,冷冻干燥即得黄色荧光纳米材料固体。(6) Put the frozen mixed material into a freeze dryer and freeze dry to obtain a solid yellow fluorescent nanomaterial.
图1为黄色荧光染料在日光灯下的状态图,图2为黄色荧光染料在紫外灯下的状态图, 图3为黄色荧光染料的光谱图。由此可见,本发明长所合成的碳量子点溶液呈鲜艳的黄色, 并且在紫外灯下呈现强烈的黄光。Fig. 1 is a state diagram of the yellow fluorescent dye under a fluorescent lamp, Fig. 2 is a state diagram of the yellow fluorescent dye under an ultraviolet lamp, and Fig. 3 is a spectrum diagram of the yellow fluorescent dye. It can be seen that the carbon quantum dot solution synthesized by the present invention is bright yellow, and shows strong yellow light under an ultraviolet lamp.
实施例1:Example 1:
一种黄色荧光染料具有如下应用:A yellow fluorescent dye has the following applications:
荧光防伪墨水Fluorescent security ink
将制得的黄色荧光纳米荧光染料配制成0.1~5%染料浓度的溶液,使用钢笔笔芯吸取 染料液,可在白纸上或者钱币上进行书写。The prepared yellow fluorescent nanometer fluorescent dye is formulated into a solution with a dye concentration of 0.1-5%, and the dye solution is absorbed by a pen core, and can be written on white paper or coins.
如图4-图9所示,图4是本发明在纸上绘制的小鸟在日光灯下的状态图;图5是本发明在纸上绘制的小鸟在紫外灯下的状态图;图6是本发明纸上绘制的校徽在日光灯下的状态图;图7是本发明纸上绘制的校徽在紫外灯下的状态图;图8是本发明在钱币上书写的 数字在日光灯下的状态图;图9是本发明在钱币上书写的数字在紫外灯下的状态图。As shown in Figures 4-9, Fig. 4 is a state diagram of a bird drawn on paper by the present invention under a fluorescent lamp; Fig. 5 is a state diagram of a bird drawn on paper by the present invention under an ultraviolet lamp; Fig. 6 It is the state diagram of the school emblem drawn on the paper of the present invention under the fluorescent lamp; Fig. 7 is the state diagram of the school emblem drawn on the paper of the present invention under the ultraviolet lamp; Fig. 8 is the state diagram of the numbers written on the coins of the present invention under the fluorescent lamp ; Fig. 9 is a state diagram of the numbers written on coins of the present invention under an ultraviolet lamp.
将制得的黄色荧光纳米荧光染料配制成溶液,使用钢笔笔芯吸取染料液,可在白纸上 或者钱币上进行书写与绘画。其印记在日光下不清晰,辨别比较困难,在紫外灯下清晰可 见,呈现强烈的黄光,所合成的荧光几乎不衰减,形成了长效的荧光。The prepared yellow fluorescent nanometer fluorescent dye is prepared into a solution, and the pen core is used to absorb the dye solution, which can be used for writing and drawing on white paper or coins. Its imprint is not clear in daylight, and it is difficult to distinguish, but it is clearly visible under ultraviolet light, showing a strong yellow light, and the synthesized fluorescence hardly attenuates, forming a long-lasting fluorescence.
实施例2:Example 2:
一种黄色荧光染料具有如下应用:A yellow fluorescent dye has the following applications:
黄色荧光染料在纺织上的应用Application of Yellow Fluorescent Dye in Textile
将制得的黄色纳米荧光染料配制成0.1~5%染料浓度的染料液,将纺织物进入其中浸 泡12~24h,即得染色后的荧光纺织物。The prepared yellow nanometer fluorescent dye is formulated into a dye solution with a dye concentration of 0.1-5%, and textiles are soaked in it for 12-24 hours to obtain dyed fluorescent textiles.
如图10、图11所示,图10是使用本发明在布料上染色与未使用本发明未染色在日光 灯下的对比图;图11是使用本发明在布料上染色与未使用本发明未染色在紫外灯下的对 比图。染色后的荧光纺织物在紫外灯下发出荧光。As shown in Fig. 10 and Fig. 11, Fig. 10 is a comparison diagram of using the present invention to dye on cloth and not using the present invention without dyeing under the fluorescent lamp; Fig. 11 is using the present invention to dye on cloth and not using the present invention without dyeing Comparison chart under UV light. Dyed fluorescent textiles fluoresce under UV light.
实施例3:Example 3:
一种黄色荧光染料具有如下应用:A yellow fluorescent dye has the following applications:
纳米荧光粉的应用Application of Nano Phosphor Powder
将粉状的纳米荧光粉与活性白土混合,制成带有荧光的泥土模型。Mix powdery nano-fluorescent powder with activated clay to make a fluorescent clay model.
如图12、图13所示,图12是使用本发明制成的工艺品在日光灯下的状态图;图13是使用本发明制成的工艺品在紫外灯下的状态图。使用本发明制成的工艺品在紫外灯下发出荧光。As shown in Fig. 12 and Fig. 13, Fig. 12 is a state diagram of a handicraft made by using the present invention under a fluorescent lamp; Fig. 13 is a state diagram of a handicraft made by using the present invention under an ultraviolet lamp. The handicraft made by using the invention emits fluorescence under ultraviolet light.
本发明具备杂环(吡啶),同时又兼具苯环(萘酚)这样复杂结构的原料,同时使用强碱性试剂去破坏吡啶环和萘酚环,在高温下,形成了非常稳定的结构,这样有助于长效荧光的形成。以上提到的荧光,是在紫外灯下照射才会观察到的荧光。The present invention has heterocyclic (pyridine) and raw materials with complex structures such as benzene ring (naphthol) at the same time. At the same time, a strong basic reagent is used to destroy the pyridine ring and naphthol ring, and a very stable structure is formed at high temperature. , which contributes to the formation of long-lasting fluorescence. The fluorescence mentioned above is the fluorescence that can only be observed under ultraviolet light.
无论是合成方法、纯化方法还是保存方法,都非常地简单方便。Whether it is a synthesis method, a purification method or a preservation method, it is very simple and convenient.
根据荧光染料的特点,打破常规,进行了一系列应用,为黄色荧光染料的突破性实际 应用提供了模板。According to the characteristics of fluorescent dyes, a series of applications were broken, which provided a template for the breakthrough practical application of yellow fluorescent dyes.
本发明长所合成的碳量子点溶液呈鲜艳的黄色,并且在紫外灯下呈现强烈的黄光,所 合成的荧光几乎不衰减,形成了长效的荧光。而且无论是合成方法、纯化方法还是保存方 法,都非常地简单方便。The carbon quantum dot solution synthesized by the present invention is bright yellow, and shows strong yellow light under an ultraviolet lamp, and the synthesized fluorescence hardly decays, forming long-lasting fluorescence. And no matter it is a synthesis method, a purification method or a preservation method, it is very simple and convenient.
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任 何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发 明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。The above is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto, any person familiar with the technical field within the technical scope disclosed in the present invention, according to the technical solution of the present invention Any equivalent replacement or change of the inventive concepts thereof shall fall within the protection scope of the present invention.
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