Multicolor fluorescent carbon fibers, and methods and applications thereof

By preparing multicolor fluorescent carbon fibers as a light conversion agent, the problems of short service life, low light conversion rate and poor compatibility of existing light conversion agents are solved, achieving the effects of long-term warming and extending film life, and possessing environmental protection and pest prevention functions.

CN119433761BActive Publication Date: 2026-01-27SOUTHWEAT UNIV OF SCI & TECH
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Patent Information

Application Number
CN202411792176.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-06
Publication Date
2026-01-27
Estimated Expiration
2044-12-06

AI Technical Summary

Technical Problem

Existing light conversion agents suffer from short service life, low light conversion efficiency, low light transmittance, poor compatibility with film resins, complex and costly preparation processes, and limited absorption of ultraviolet light by rare earth complex light conversion agents, making it difficult to achieve long-lasting heating and rapid film aging after heating.

Method used

Using multicolor fluorescent carbon fiber as a light-converting agent, fibrous amorphous carbon nanomaterials were prepared by sintering modified halloysite and waste polyester raw materials in an oxygen-free environment. The resulting multicolor fluorescent carbon fiber has stable light-converting properties and can emit blue, green and red light, which can be applied to biodegradable membranes.

Benefits of technology

It achieves long-lasting warming effect, controls pests, extends the service life of the membrane, has good biocompatibility and environmental friendliness, stable degradation performance, and low price.

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Abstract

The application relates to a multi-color fluorescent carbon fiber and a preparation method and application thereof. The preparation method of the multi-color fluorescent carbon fiber comprises the following steps: S1. modifying and treating calcined halloysite by using an amino silane to obtain modified halloysite; and S2. mixing waste polyester raw materials with the modified halloysite, and performing sintering treatment in an oxygen-free environment to obtain the multi-color fluorescent carbon fiber. The multi-color fluorescent carbon fiber prepared by using a specific method has light absorption, light conversion and temperature increasing characteristics, simultaneously emits blue light, red light and green light, and can be applied to the fields of biomedical imaging and diagnosis, sensors, light conversion films and the like as a luminescent material.
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Description

Technical Field

[0001] This application relates to the field of materials technology, specifically to a multicolor fluorescent carbon fiber, its preparation method, and its application. Background Technology

[0002] The core technology of light-converting films lies in the development of light-converting agents. The key to preparing light-converting films is to generate two peaks, blue and red, after sunlight transmission to achieve a boost in photosynthesis. Whether this is ultimately achieved depends on the light-converting agent, its compatibility with the matrix, and its light energy conversion. Traditional light-converting agents commonly employ organic fluorescent molecules, inorganic salts, and rare earth complexes. However, organic fluorescent molecules are prone to decomposition under prolonged light exposure, have short lifespans, and low light conversion rates. Inorganic salts can improve light conversion intensity and lifespan, but suffer from low transmittance, rapid light decay, and poor compatibility with film resins. Horticultural greenhouse films made from rare earth complexes have advantages such as long lifespan and high stability, making them popular among researchers. However, the relatively fixed structures of most rare earth elements and ligands limit their absorption of certain specific wavelengths of ultraviolet light, making it difficult for the light-converting film to further enhance ultraviolet absorption. Furthermore, the preparation process of rare earth complex light-converting agents is relatively complex and expensive. More importantly, existing light-converting agents present biocompatibility and environmental safety issues, making the development of safe, non-toxic, efficient, stable, and low-cost light-converting agents an urgent need. The challenges of long-term warming are: 1) Current degradable films have a service life of 60-70 days; extending this service life to more than 100 days is a significant challenge; 2) For films with warming effects, the aging rate accelerates with increasing temperature. Therefore, simultaneously achieving both warming and long service life presents a substantial technical challenge.

[0003] In summary, there is an urgent need for a light-converting agent capable of providing long-lasting temperature enhancement for light-converting films. In view of the shortcomings of the existing technology described above, this invention provides a multicolor fluorescent carbon fiber, its preparation method, and its application to meet the requirement of long-lasting temperature enhancement for light-converting films. Summary of the Invention

[0004] In view of the shortcomings of the prior art described above, the present invention provides a multicolor fluorescent carbon fiber, its preparation method and application, to meet the long-term heating requirements of light conversion films.

[0005] To achieve the above objectives, the solution proposed in this application is as follows:

[0006] In a first aspect, the present invention provides a multicolor fluorescent carbon fiber, wherein the multicolor fluorescent carbon fiber is an amorphous carbon nanomaterial in the form of fibers.

[0007] Optionally, the multicolor fluorescent carbon fiber has a diameter of 25-52 nm and a length of 176-365 nm.

[0008] Secondly, this application also provides a method for preparing multicolor fluorescent carbon fibers as described above, comprising the following steps:

[0009] S1. Modified halloysite was obtained by modifying calcined halloysite with aminosilane;

[0010] S2. The waste polyester raw material is mixed with the modified halloysite and sintered in an oxygen-free environment to obtain the multicolor fluorescent carbon fiber.

[0011] Optionally, in step S1, the aminosilane is selected from (3-aminopropyl)triethoxysilane.

[0012] Optionally, in step S1, the modification treatment of calcined halloysite with aminosilane includes: adding the calcined halloysite to an alcoholic solution of aminosilane, stirring at 70-90°C for 12-24 hours, separating, and drying.

[0013] Optionally, in step S1, the ratio of calcined halloysite to aminosilane is 10g:5-10mL.

[0014] Optionally, in step S2, the mass ratio of the waste polyester raw material to the modified halloysite is 100:0.5-10.

[0015] Thirdly, this application also provides the application of the multicolor fluorescent carbon fiber as described above or the multicolor fluorescent carbon fiber prepared according to the method described above in the preparation of biodegradable membranes.

[0016] The beneficial effects of this invention are:

[0017] The multicolor fluorescent carbon fiber prepared by this application has light-converting properties, and the membrane can emit blue, green and red light at the same time, achieving long-term warming while effectively controlling pests. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the present application;

[0019] Figure 2 Electron micrograph of the multicolor fluorescent carbon fiber prepared in Example 1;

[0020] Figure 3 The image shows the multicolor effect of the multicolor fluorescent carbon fiber prepared in Example 1.

[0021] Figure 4 The graph shows the results of the heating characteristic test. The infrared heating film is a light-converting film made of multicolor fluorescent carbon fiber from Example 1.

[0022] Figure 5The left image shows the lifetime test results of the light-conversion film made of multicolor fluorescent carbon fiber in Example 1, and the right image shows the lifetime test results of the light-conversion film made of multicolor fluorescent carbon fiber in Example 2. Detailed Implementation

[0023] The embodiments of the present invention will be described below with reference to the accompanying drawings and preferred embodiments. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention. It should be understood that the preferred embodiments are only for illustrating the present invention and not for limiting the scope of protection of the present invention.

[0024] It should be noted that the illustrations provided in the following embodiments are only schematic representations of the basic concept of the present invention. Therefore, the drawings only show the components related to the present invention and are not drawn according to the actual number, shape and size of the components in the actual implementation. In the actual implementation, the form, quantity and proportion of each component can be arbitrarily changed, and the layout of the components may also be more complex.

[0025] like Figure 1 As shown, the principle of this application is as follows:

[0026] The membrane is made of multicolor fluorescent carbon fiber, which gives it light conversion properties. The membrane can emit both blue and red light at the same time. Traditional light conversion membranes are monochromatic light conversion membranes.

[0027] Unlike existing light-converting agents, multicolor fluorescent carbon fiber exhibits stable light-converting performance, long lifespan, and low price. Furthermore, compared to the three existing light-converting agents, multicolor fluorescent carbon fiber demonstrates excellent biocompatibility and is environmentally friendly, making it safe for soil and crop environments when used as mulch film. Secondly, current technologies commonly use light-converting greenhouse films with polyethylene as the matrix. This type of material is very stable, and the film can be recycled after disposal. This application pertains to a fully degradable agricultural light-converting mulch film, using a fully biodegradable matrix. This type of material undergoes aging and degradation under light. The light-converting degradable mulch film itself emits light, requiring simultaneous solutions to the problems of luminescence and degradation rate regulation, which is significantly more challenging than traditional light-converting film technology. In this application, the light-converting agent...

[0028] It is stable, environmentally friendly, safe and non-toxic, and inexpensive; it has effects such as light conversion and warming, insect prevention, and yield increase; and its light conversion performance is stable and long-lasting, emitting light stably throughout the entire service life.

[0029] Numerous details are explored in the following description to provide a more thorough explanation of embodiments of the invention; however, it will be apparent to those skilled in the art that embodiments of the invention may be practiced without these specific details. Example 1

[0030] A method for preparing multicolor fluorescent carbon fibers, the specific steps of which are as follows:

[0031] S1. Add 10g of calcined halloysite (commercially available) to an ethanol solution of APTES (prepared by mixing 8mL of APTES and 200mL of anhydrous ethanol), stir at 80℃ for 18h, filter, and dry the filtered solid to dryness to obtain modified halloysite.

[0032] S2. Waste polyester raw materials (specifically biodegradable agricultural film containing PBAT and PLA) are mixed with modified halloysite at a mass ratio of 100:5, and then placed in a tube furnace and sintered at 800℃ for 2 hours in a nitrogen atmosphere (flow rate of 20 mL / min) to obtain multicolor fluorescent carbon fibers.

[0033] The prepared multicolor fluorescent carbon fibers were scanned by electron microscopy, and the results are as follows: Figure 2 As shown.

[0034] The multicolor fluorescent carbon fibers were verified for their multicolor effect. The specific steps were as follows: the luminescence properties were characterized using a laser confocal microscope, and the results are as follows: Figure 3 As shown.

[0035] Depend on Figure 2 It can be seen that the multicolor fluorescent carbon fiber prepared in this embodiment is fibrous, specifically a fibrous (needle-like) amorphous carbon nanomaterial.

[0036] Statistical analysis of the electron micrographs showed that the multicolor fluorescent carbon fibers prepared in this embodiment had a diameter of 25-52 nm, an average diameter of 38 nm, a maximum length of 365.6 nm, a minimum length of 176.5 nm, and an average length of 247.4 nm.

[0037] Depend on Figure 3 It can be seen that the multicolor fluorescent carbon fiber prepared in this embodiment can absorb light with a wavelength of 400-700nm and emit blue, red and green light at the same time. Example 2

[0038] A method for preparing multicolor fluorescent carbon fibers, the specific steps of which are as follows:

[0039] S1. Add 10g of calcined halloysite (commercially available) to an ethanol solution of APTES (prepared by mixing 10mL of APTES and 200mL of anhydrous ethanol), stir at 90℃ for 12h, filter, and dry the filtered solid to dryness to obtain modified halloysite.

[0040] S2. Waste polyester raw materials (a mixture of PET bottle flakes and PBAT film in a mass ratio of 1:1) are mixed with modified halloysite in a mass ratio of 100:0.5, and then placed in a tube furnace and sintered at 600°C for 3 hours in a nitrogen atmosphere (flow rate of 50 mL / min) to obtain multicolor fluorescent carbon fibers. Example 3

[0041] A method for preparing multicolor fluorescent carbon fibers, the specific steps of which are as follows:

[0042] S1. Add 10g of calcined halloysite (commercially available) to an ethanol solution of APTES (prepared by mixing 5mL APTES and 200mL anhydrous ethanol), stir at 70℃ for 24h, filter, and dry the filtered solid to dryness to obtain modified halloysite.

[0043] S2. Waste polyester raw materials (a mixture of PET, PBT and PBAT in a mass ratio of 1:1:1) are mixed with modified halloysite in a mass ratio of 100:10, and then placed in a tube furnace and sintered at 1000℃ for 1 hour in a nitrogen atmosphere (flow rate of 5 mL / min) to obtain multicolor fluorescent carbon fibers. Example 4

[0044] A method for preparing multicolor fluorescent carbon fibers, the specific steps of which are as follows:

[0045] S1. Add 10g of calcined halloysite (commercially available) to an ethanol solution of APTES (prepared by mixing 6mL of APTES and 200mL of anhydrous ethanol), stir at 75℃ for 20h, filter, and dry the filtered solid to dryness to obtain modified halloysite.

[0046] S2. Waste polyester raw materials and modified halloysite are mixed at a mass ratio of 100:8, and then placed in a tube furnace and sintered at 750°C for 1.5 h in a nitrogen atmosphere (flow rate of 2 mL / min) to obtain multicolor fluorescent carbon fibers.

[0047] Performance testing

[0048] The multicolor fluorescent carbon fibers from Examples 1-2 were used to make light-converting films;

[0049] The heating characteristics of the light-converting film prepared from the multicolor fluorescent carbon fiber in Example 1 were tested using an infrared thermal imager, and compared with those of a conventional film. The results are as follows: Figure 4 As shown;

[0050] The lifetime of the multicolor fluorescent carbon fibers prepared in Examples 1-2 was tested. The method for testing the lifetime was to conduct actual application experiments in the field and observe their service time. The results are as follows: Figure 5 As shown.

[0051] Depend on Figure 4 It can be seen that, compared with ordinary films, the temperature-increasing effect of the light-converting film made of multicolor fluorescent carbon fibers in Example 1 is significantly improved. This result shows that the multicolor fluorescent carbon fibers of the present invention can improve the temperature-increasing effect of the prepared light-converting film.

[0052] Depend on Figure 5 It is evident that the fully biodegradable light-converting films made from multicolor fluorescent carbon fibers in Examples 1-2 have a longer lifespan. This result demonstrates that this application improves the lifespan of films made from multicolor fluorescent carbon fibers.

[0053] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.

Claims

1. The application of multicolor fluorescent carbon fibers in the preparation of biodegradable membranes, characterized in that, The multicolor fluorescent carbon fiber is an amorphous carbon nanomaterial in the form of fibers; The preparation method of the multicolor fluorescent carbon fiber includes the following steps: S1. Modification of calcined halloysite using aminosilane: The calcined halloysite is added to an alcoholic solution of aminosilane, stirred at 70-90℃ for 12-24h, separated, and dried to obtain modified halloysite, wherein the aminosilane is selected from (3-aminopropyl)triethoxysilane; S2. The waste polyester raw material is mixed with the modified halloysite and sintered in an oxygen-free environment to obtain the multicolor fluorescent carbon fiber.

2. The application of the multicolor fluorescent carbon fiber as described in claim 1 in the preparation of biodegradable membranes, characterized in that, The multicolor fluorescent carbon fiber has a diameter of 25-52 nm and a length of 176-365 nm.

3. The application of the multicolor fluorescent carbon fiber as described in claim 1 in the preparation of biodegradable membranes, characterized in that, In step S1, the ratio of calcined halloysite to aminosilane is 10g:5-10mL.

4. The application of the multicolor fluorescent carbon fiber as described in claim 1 in the preparation of biodegradable membranes, characterized in that, In step S2, the mass ratio of the waste polyester raw material to the modified halloysite is 100:0.5-10.

Citation Information

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