Self-luminous cloth and preparation method thereof
阅读说明：本技术 一种自发光布及其制备方法 (Self-luminous cloth and preparation method thereof ) 是由 周梓良 王�锋 崔旭东 于 2020-06-29 设计创作，主要内容包括：本发明提供一种自发光布及其制备方法,涉及自发光技术领域。该自发光布的制备方法包括：S1,获得自发光材料：以碳酸锶59～81重量份、氧化铝38～62重量份、氧化铕0.5～4重量份、氧化镝0.5～4.5重量份和硼酸1.5～4.5重量份为原料,对所述原料进行搅拌后,烧结得到自发光材料；S2,对所述自发光材料进行粉碎,得到发光粉；S3,将所述发光粉分散在处理液中,得到处理剂,用所述处理剂对基布进行处理得到自发光布。该自发光布表面附着有自发光粉体,产品质量稳定,发光效果好。(The invention provides self-luminous cloth and a preparation method thereof, and relates to the technical field of self-luminous. The preparation method of the self-luminous cloth comprises the following steps: s1, obtaining the self-luminous material: taking 59-81 parts by weight of strontium carbonate, 38-62 parts by weight of aluminum oxide, 0.5-4 parts by weight of europium oxide, 0.5-4.5 parts by weight of dysprosium oxide and 1.5-4.5 parts by weight of boric acid as raw materials, stirring the raw materials, and sintering to obtain the self-luminous material; s2, crushing the self-luminous material to obtain luminous powder; and S3, dispersing the luminescent powder in the treatment liquid to obtain a treatment agent, and treating the base cloth with the treatment agent to obtain the self-luminescent cloth. The self-luminous cloth has self-luminous powder adhered to its surface, stable product quality and high light-emitting effect.)
1. The preparation method of the self-luminous cloth is characterized by comprising the following steps of:
s1, obtaining the self-luminous material: taking 59-81 parts by weight of strontium carbonate, 38-62 parts by weight of aluminum oxide, 0.5-4 parts by weight of europium oxide, 0.5-4.5 parts by weight of dysprosium oxide and 1.5-4.5 parts by weight of boric acid as raw materials, stirring the raw materials, and sintering to obtain the self-luminous material;
s2, crushing and screening the self-luminous material to obtain luminous powder with the particle size not larger than 400 meshes;
s3, dispersing the luminescent powder in a treatment solution to obtain a treatment agent;
and S4, processing the base cloth by using the processing agent to obtain the self-luminous cloth.
2. The method for producing a self-luminous fabric according to claim 1, wherein the self-luminous material Sr is0.97Al2O4:Eu0.01,Dy0.01。
3. The method for preparing a self-luminous fabric according to claim 1, wherein in the step S1, the sintering temperature is 1350-1500 ℃ and the sintering time is 2-4 h.
4. The method for preparing a self-luminous fabric according to claim 1, wherein 90% N is introduced during the sintering process2-10％H2And (4) mixing the gases.
5. The method for manufacturing a self-luminous fabric according to claim 1, wherein the pulverization process in the step S2 includes:
s21, crushing the self-luminous material in a crusher to obtain particles with the particle size of less than 3 cm;
s22, grinding the particles and the first grinding balls according to a volume ratio of 1: 1-2, grinding for 1-2.5 hours to obtain a first ground product, grinding the first ground product and the second grinding balls for 4-6 hours to obtain a second ground product, and screening the second ground product to obtain the luminescent powder.
6. The method for manufacturing a self-luminous cloth according to claim 5, wherein the first grinding balls are agate balls with a diameter of 20mm, the second grinding balls comprise agate balls with diameters of 15mm, 10mm and 5mm, respectively, and the mass ratio of the agate balls with diameters of 15mm, 10mm and 5mm is 2:5: 3.
7. The method for preparing a self-luminous fabric according to claim 1, wherein the treatment liquid comprises, in parts by weight: 100 parts of water, 25-35 parts of waterborne polyurethane resin, 1-3 parts of alkyl glycoside and 4-8 parts of fatty alcohol-polyoxyethylene ether.
8. The method for producing a self-luminous fabric according to claim 7, wherein the treating agent treats the base fabric in step S4 in accordance with the following steps:
dipping the base fabric in the treating agent for 10-25 min under the normal pressure condition, and pressurizing the system pressure to 1-2 MPa for dipping for 5-10 m; and repeating the normal pressure and pressurization dipping process for 2-3 times, and then drying, steaming and washing to obtain the self-luminous cloth.
9. The method for producing a self-luminous fabric according to claim 8, wherein in step S3, the light-emitting powder is subjected to surface modification treatment before being added to the treatment liquid, and the surface is treatedThe modification step comprises: mixing MgCl2And NH4And F, respectively dissolving the F in water, mixing and stirring, adding the luminescent powder, stirring and coating, drying and cleaning to obtain coated luminescent powder, placing the coated luminescent powder in a dopamine hydrochloride solution with the pH value of 8-9, stirring and reacting for 2-5 h, and centrifugally washing to obtain the surface-modified luminescent powder.
10. Self-luminous cloth characterized by being prepared by the preparation method according to any one of claims 1 to 9.
Technical Field
The invention relates to the technical field of self-luminescence, and particularly relates to self-luminescence cloth and a preparation method thereof.
Background
At present, the application fields of self-luminous cloth are more and more extensive, such as advertisement banner, sanitation work clothes, traffic police duty clothes, stage scene cloth or performance clothes and the like. At present, the luminescent materials applied to the self-luminous cloth are mainly reflective luminescent materials and energy storage luminescent materials. The application scenarios of the reflective luminescent materials are limited, and when the visibility is low, the luminescent effect is poor. The energy storage luminescent material such as a long afterglow luminescent material can store external light radiation energy and slowly release the stored energy in the form of visible light under dark conditions.
After research, the inventor finds that the long-afterglow luminescent material is applied to self-luminous cloth, and has high luminous efficiency, long luminous time and stable property. However, the existing long afterglow luminescent materials are granular, and have poor dispersibility and easy falling off when the self-luminous cloth is prepared by coating or adhering. Therefore, in the prior art, the self-luminous cloth is obtained by blending the self-luminous particles with the base materials such as polyurethane and the like and then spinning, but the preparation process of the method is complex and is difficult to be suitable for various base materials.
Disclosure of Invention
The invention aims to provide a preparation method of self-luminous cloth, which can be suitable for various base cloth materials and is simple.
Another object of the present invention is to provide a self-luminous cloth, which has a long light-emitting time and a good light-emitting effect.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of self-luminous cloth, which comprises the following steps:
s1, obtaining the self-luminous material: taking 59-81 parts by weight of strontium carbonate, 38-62 parts by weight of aluminum oxide, 0.5-4 parts by weight of europium oxide, 0.5-4.5 parts by weight of dysprosium oxide and 1.5-4.5 parts by weight of boric acid as raw materials, stirring the raw materials, and sintering to obtain the self-luminous material;
s2, crushing and screening the self-luminous material to obtain luminous powder with the particle size not greater than 400 meshes;
s3, dispersing the luminescent powder in a treatment solution to obtain a treatment agent;
and S4, processing the base cloth by using the processing agent to obtain the self-luminous cloth.
Further, in the preferred embodiment of the present invention, the self-luminous material Sr0.97Al2O4:Eu0.01,Dy0.01。
Further, in the preferred embodiment of the present invention, in step S1, the sintering temperature is 1350-1500 ℃ and the sintering time is 2-4 h.
Further, in the preferred embodiment of the present invention, 90% N is introduced during the sintering process2-10％H2And (4) mixing the gases.
Further, in the preferred embodiment of the present invention, in step S2, the crushing process includes:
s21, crushing the self-luminous material in a crusher to obtain particles with the particle size of less than 3 cm;
s22, grinding the particles and the first grinding balls according to a volume ratio of 1: 1-2, grinding for 1-2.5 hours to obtain a first ground product, grinding the first ground product and the second grinding balls for 4-6 hours to obtain a second ground product, and screening the second ground product to obtain the luminescent powder.
Further, in a preferred embodiment of the present invention, the first milling balls are agate balls with a diameter of 20mm, the second milling balls comprise agate balls with diameters of 15mm, 10mm and 5mm, respectively, and the mass ratio of the agate balls with diameters of 15mm, 10mm and 5mm is 2:5: 3.
Further, in a preferred embodiment of the present invention, the treatment liquid comprises, in parts by weight: 100 parts of water, 25-35 parts of waterborne polyurethane resin, 1-3 parts of alkyl glycoside and 4-8 parts of fatty alcohol-polyoxyethylene ether.
Further, in the preferred embodiment of the present invention, in step S4, the treating agent treats the base fabric according to the following steps:
dipping the base fabric in the treating agent for 10-25 min under the normal pressure condition, and pressurizing the system pressure to 1-2 MPa for dipping for 5-10 m; and repeating the normal pressure and pressurization dipping process for 2-3 times, and then drying, steaming and washing to obtain the self-luminous cloth.
Further, in a preferred embodiment of the present invention, in step S3, the luminescent powder is subjected to a surface modification treatment before being added into the treatment solution, and the surface modification step includes: mixing MgCl2And NH4And F, respectively dissolving the F in water, mixing and stirring, adding the luminescent powder, stirring and coating, drying and cleaning to obtain coated luminescent powder, placing the coated luminescent powder in a dopamine hydrochloride solution with the pH value of 8-9, stirring and reacting for 2-5 h, and centrifugally washing to obtain the surface-modified luminescent powder.
The invention also provides self-luminous cloth prepared by the preparation method.
The self-luminous cloth and the preparation method thereof have the advantages that:
the boric acid raw material in the self-luminous material is controlled within 4.5 parts by mass, so that the hardness of the self-luminous material is reduced, and the self-luminous material is favorably crushed. The luminescent powder is obtained by crushing and screening the self-luminescent material, the particle size of the luminescent powder is not more than 400 meshes, the good adhesion of the luminescent powder and the base cloth is ensured, and the stability of the product is high.
Furthermore, the water-based polyurethane solution is adopted as the treatment solution, and the alkyl glycoside and the fatty alcohol-polyoxyethylene ether are added, so that a good compounding effect can be formed, the luminescent powder can be quickly wetted, and the luminescent powder can be effectively dispersed in the treatment.
Further, MgCl is passed on the surface of the luminescent powder2And NH4F forms MgF2Coating filmAnd further forming a functional layer of polydopamine with high adhesiveness on the surface of the coating film. The coating film effectively protects the luminescent powder, improves the water resistance and the wear resistance, and ensures the long-acting self-luminescent effect. The polydopamine functional surface layer enables the luminescent powder to be loaded on the base cloth more uniformly and stably.
Furthermore, a light-emitting film layer is formed on the surface of the base cloth in an alternate mode of normal pressure and negative pressure impregnation, the load rate is high, compared with the mode of adding light-emitting powder into the raw material of the base cloth for blending spinning, the impregnation mode is simpler and more efficient, and the method can be applied to various cloth materials.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a graph showing the decay of afterglow of a self-luminous cloth according to example 1 of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The self-luminous fabric and the preparation method thereof according to the embodiment of the present invention will be specifically described below.
The preparation method of the self-luminous cloth provided by the embodiment of the invention comprises the following steps:
s1, obtaining the self-luminous material: 59-81 parts of strontium carbonate, 38-62 parts of aluminum oxide, 0.5-4 parts of europium oxide, 0.5-4.5 parts of dysprosium oxide and 1.5-4.5 parts of boric acid are used as raw materials, and the raw materials are stirred and sintered to obtain the self-luminous material.
Preferably, in this step, the self-luminous material Sr is obtained0.97Al2O4:Eu0.01,Dy0.01。
Preferably, in the step, the sintering temperature is 1350-1500 ℃, and the sintering time is 2-4 h.
Preferably, in this step, 90% N is introduced during sintering2-10％H2Mixing the gases to create a weakly reducing protective atmosphere.
Preferably, in this step, the temperature rise rate is 10 ℃/min.
S2, crushing and screening the self-luminous material obtained in the step S1 to obtain luminous powder with the grain size not larger than 400 meshes;
preferably, in this step, the pulverization process includes:
s21, crushing the self-luminous material in a crusher to obtain particles with the particle size of less than 3 cm;
s22, grinding the particles and the first grinding balls according to a volume ratio of 1: 1-2, grinding for 1-2.5 hours to obtain a first ground product, grinding the first ground product and the second grinding balls for 4-6 hours to obtain a second ground product, and screening the second ground product to obtain the luminescent powder with the particle size not larger than 400 meshes. For particles larger than 400 mesh, the milling and sieving is continued.
Preferably, the first grinding balls are agate balls with the diameter of 20mm, the second grinding balls comprise agate balls with the diameters of 15mm, 10mm and 5mm respectively, and the mass ratio of the agate balls with the diameters of 15mm, 10mm and 5mm is 2:5: 3. By controlling the crushing and grinding processes, the self-luminous material is gradually crushed into the luminous powder with the particle size less than 400 through three crushing processes of crushing, large particle grinding and small particle grinding. Particularly, in the final grinding stage, the agate balls with three particle sizes are adopted for grinding, so that the self-luminous material is prevented from being excessively ground to influence the luminous effect of the self-luminous material, and the self-luminous material is guaranteed to be ground to a proper particle size.
S3, dispersing the luminescent powder obtained in step S2 in the processing liquid to obtain the processing agent.
Preferably, in this step, the treatment liquid includes, in parts by weight: 100 parts of water, 25-35 parts of waterborne polyurethane resin, 1-3 parts of alkyl glycoside and 4-8 parts of fatty alcohol-polyoxyethylene ether.
Furthermore, the solid content of the waterborne polyurethane is 20-30%, and polyether type, polyester type or polyether polyester mixed polyurethane can be selected.
Further, in the step, the mass fraction of the luminescent powder in the treatment liquid is 42-64%.
Further, in step S3, the luminescent powder is subjected to a surface modification treatment in advance before being added into the treatment liquid, and the surface modification treatment step includes: mixing MgCl2And NH4And F, respectively dissolving the F in water, then mixing and stirring to obtain a mixed solution, adding the luminescent powder into the mixed solution, stirring and coating, and drying and cleaning to obtain the coated luminescent powder. And (3) placing the coated luminescent powder in a dopamine hydrochloride solution with the pH value of 8-9, stirring for reacting for 2-5 h, and centrifugally washing to obtain the surface-modified luminescent powder.
Further, the mass fraction of the luminescent powder in the mixed liquid is 12-18%. MgF is formed by coating the surface of the luminescent powder2The cladding material has no influence on the emission and excitation spectrum of the luminescent powder after cladding, the phase of the luminescent powder is not changed, and the water resistance, the wear resistance and the like of the clad luminescent powder are obviously improved.
Further, 0.02-0.04 g of coated luminescent powder is dispersed in 100ml of water, 0.01-0.03 g of dopamine hydrochloride and 0.1-0.14 g of Tris are added, and stirring reaction is carried out for 2-5 hours to obtain the surface modified luminescent powder. By dopamine, further at MgF2The surface of the coating is introduced with a polydopamine functional surface layer, so that excellent dispersibility and adhesiveness are obtained.
And S4, processing the base cloth by using the processing agent obtained in the step S3 to obtain the self-luminous cloth.
Preferably, in this step, the treating agent treats the base fabric according to the following steps:
dipping the base fabric in the treating agent for 10-25 min under the normal pressure condition, and pressurizing the system pressure to 1-2 MPa for dipping for 5-10 m; and repeating the normal pressure and pressurization dipping process for 2-3 times, and then drying and washing to obtain the self-luminous cloth.
Preferably, in this step, the drying process is: drying at 50-80 ℃. And drying after washing to obtain the self-luminous cloth.
Preferably, in this step, the base cloth may be polyester cloth, polypropylene fiber cloth, or the like.
The embodiment of the invention also provides self-luminous cloth which is prepared according to the preparation method.
The features and properties of the present invention are described in further detail below with reference to examples.
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