CN113913110A - Method for preparing micron-sized photodiffusion core-shell hybrid microspheres through hydrothermal synthesis - Google Patents
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Abstract
The invention relates to a method for preparing micron-sized photodiffusion core-shell hybrid microspheres by hydrothermal synthesis. The microsphere has a polysiloxane microsphere inner core with the thickness of 4-6 mu m, an outer layer is composed of a nano inorganic compound, and the thickness of a shell layer is 50-150 nm. The optical property test after film forming shows that the light diffusion resin has excellent light diffusion effect and higher light transmittance, can be widely used for preparing various light diffusion materials, and can improve the thermal stability of the film forming resin. The microsphere is simple in preparation method, has a large potential application value, is low in cost, and is green and environment-friendly in preparation process.
Description
Technical Field
The invention relates to a method for preparing micron-sized photodiffusion core-shell hybrid microspheres by hydrothermal synthesis, belongs to the technical field of functional materials, and can be widely used for preparing multifunctional photodiffusion films.
Background
Liquid Crystal Displays (LCDs) are widely used in various display devices such as liquid crystal televisions, monitors, mobile phones, computers, and the like. With the development of people's life needs, the requirements for LCDs are also more and more targeted. At present, the research and development of domestic and foreign LCDs are developing towards light and thin, large display interface, stable display picture and the like. In the LCD structure, the functional design of the light diffusion film in the backlight module is very important. The light source provided by the liquid crystal display is an LED point light source, and the displayed soft surface light source can make people feel a picture pleasantly, wherein the conversion is mainly realized by a light diffusion film. In addition, along with the improvement of the quality of life level, people pay more and more attention to health, and the direction of scientific research in the future is also the direction for reducing the radiation of computers to people. The realization of the multi-functionalization of the light diffusion film is a direction that many companies have been working on at present.
The multifunctionalization of the light diffusion film is mainly realized by the function of the added light diffusing agent, so that the function of the light diffusion microspheres plays a direct role in determining the properties of the light diffusion film. At present, there are many methods for preparing the light diffusion microspheres, mainly including traditional emulsion polymerization, miniemulsion polymerization, suspension polymerization, dispersion polymerization, soap-free emulsion polymerization, sol-gel and hydrothermal synthesis, etc. Each method has its own advantages and disadvantages, and requires rational utilization and incorporation. Patent CN103193915 adopts a dispersion copolymerization method to prepare random copolymer microspheres of styrene (St) and methacryloxypropyl isobutyl cage type oligomeric silsesquioxane (MAiBuPOSS), which have excellent light transmittance and light scattering property and high optical efficiency as a light diffuser. The core-shell hybrid microsphere has a unique structure and composition, shows a series of novel properties, and can be used as a novel light diffusant to better scatter point light sources due to the difference of refractive indexes caused by different components of an inner layer and an outer layer. Patent CN102634067 discloses a high-permeability light-diffusing microsphere, which is prepared by coating a layer of 30-70nm porous nano titanium dioxide hollow microspheres on a silica microsphere through a sol-gel process, and the light-diffusing film prepared from the microsphere has good light-diffusing effect, high light transmittance and high flame retardancy. At present, the method for synthesizing the core-shell hybrid microspheres is carried out in a reaction device. Although a large number of compounds can be synthesized by a simple hydrothermal method, no research on synthesis of the photodiffusion core-shell hybrid microspheres in a hydrothermal reaction kettle has been reported. The invention takes siloxane polymeric microspheres prepared by a sol-gel method as a template, synthesizes a series of core-shell hybrid microspheres through a simple hydrothermal process, and has better light diffusion effect shown by optical performance test after film formation. The microsphere is simple in preparation method, has a large potential application value, is low in cost, and is green, environment-friendly and simple in preparation process.
Disclosure of Invention
The invention aims to provide a method for preparing micron-sized photodiffusion core-shell hybrid microspheres by hydrothermal synthesis. The outer layer is formed by inorganic compound hydrothermal self-assembly, and the composition and the nano structure of the outer layer play a decisive role in the functions of the prepared microspheres.
The polysiloxane microspheres are prepared by a simple sol-gel method and then are synthesized by a hydrothermal process by taking the polysiloxane microspheres as a template. The preparation process comprises the following steps:
a) mixing and stirring siloxane monomers and distilled water according to the molar ratio of 1: 35-1: 70, adjusting the pH of the mixture to 5.0-6.0 by using 0.01M dilute hydrochloric acid, reacting for 4-6 h at room temperature, adjusting the pH of the reaction solution to 8.5-9.5 by using 0.01M ammonia water, continuing reacting for 4-6 h at room temperature, standing, filtering, and washing with distilled water to be neutral to obtain the polysiloxane microspheres.
b) The method comprises the steps of adding the soluble inorganic salt and aluminum potassium sulfate into a hydrothermal high-pressure kettle according to the molar ratio of 6: 1-12: 1 and the molar ratio of urea to aluminum potassium sulfate of 6: 1-12: 1, adding distilled water into the high-pressure kettle according to the mass ratio of 40: 1-100: 1, and stirring to obtain a transparent solution. And then adding the polysiloxane microspheres into the solution according to the mass ratio of the polysiloxane microspheres to the soluble inorganic salt of 1: 4-1: 1, and uniformly stirring. And (3) filling the hydrothermal autoclave, placing the hydrothermal autoclave in a 120 ℃ oven for 6-9 h, cooling to room temperature, filtering, washing with distilled water and absolute ethyl alcohol for several times respectively, and drying in a 60 ℃ oven for 5-7 h to obtain the hybrid microspheres.
c) And b) taking the mass of the hybrid microspheres obtained in the step b) as a reference, mixing and uniformly stirring the hybrid microspheres, the UV light curing resin, the diluent and the photoinitiator 184 according to the mass ratio of 1: 10-50: 5-15: 0.1-0.4, coating a coating with the thickness of 10 micrometers on an optical PET film with the thickness of 50 micrometers, curing for 5-10 min under a 100W UV lamp (365nm) to form a film, taking out, coating the same layer on the other side of the PET, and curing to obtain the light diffusion film material.
In the method for preparing the micron-sized photodiffusion core-shell hybrid microspheres by hydrothermal synthesis, the siloxane compound in the step a) is one or more of vinyl trimethoxy silane, gamma-methacryloxypropyl trimethoxy silane and vinyl tri (beta-methoxyethoxy) silane; the soluble inorganic salt in the step b) is one of aluminum chloride, aluminum nitrate, aluminum sulfate, zinc chloride, zinc nitrate and zinc sulfate; the light-cured resin in the step c) is one of urethane acrylate, epoxy acrylic resin, phenolic resin and polyester acrylate.
Has the advantages that: the core-shell structure microsphere has multifunctional property, and has better light diffusion effect on multi-layer refraction performance in the aspect of optics. The large-size micron-sized light diffusion microspheres are very popular in the current market of raw materials for preparing light diffusion films and are easy to apply due to the fact that the large-size micron-sized light diffusion microspheres have very good light diffusion effects. The invention is prepared by a simple sol-gel method, and is synthesized by taking the sol-gel method as a template through a hydrothermal process. The outer layer is formed by inorganic compound hydrothermal self-assembly, the composition and the nano structure of the outer layer play a decisive role in the function of the prepared microsphere, and the inner layer is polysiloxane microsphere. The prepared microsphere has a good light diffusion effect, the components of the shell can be flexibly changed, and the self-assembled inorganic nano structure has a unique function. For example, the paint has a strong electromagnetic radiation resistance function, can shield serious harm to people caused by short wave, has a good ultraviolet radiation shielding effect, and enhances the thermal stability and the aging resistance. The material has great potential application value in the fields of multifunctional materials, optics and the like.
The invention has the characteristics that:
(1) the core-shell hybrid microsphere has strong ultraviolet absorption performance and obvious shielding effect on short-wave radiation.
(2) The prepared hybrid microspheres have good dispersion performance, and can not generate agglomeration when being used for thermosetting molding or UV curing molding of a light diffusion film.
(3) The hybrid microsphere has better thermal aging resistance.
(4) The preparation method of the hybrid microsphere is simple and flexible, chemical components are adjustable, and the hybrid microsphere is easy to prepare various light diffusion membranes with specific functions and multiple functions.
Detailed Description
Example 1:
adding 0.04mol of vinyl trimethoxy silane and 1.5mol of distilled water into a reaction kettle, stirring, adjusting the pH value to 5.5 by using 0.01M dilute hydrochloric acid, reacting for 4 hours at room temperature, adjusting the pH value of the reaction solution to 8.0 by using 0.01M ammonia water, continuing reacting for 4 hours at room temperature, standing, filtering, and washing with distilled water to be neutral to obtain the polysiloxane microspheres.
0.008mol of aluminum nitrate, 0.001mol of aluminum potassium sulfate, 0.008mol of urea and 150g of distilled water are added into a hydrothermal autoclave and stirred to form a transparent solution, and then 1.2g of the prepared polysiloxane microspheres are added and stirred uniformly. And (3) filling the hydrothermal autoclave, placing the hydrothermal autoclave in a 120 ℃ oven for 7h, cooling to room temperature, filtering, washing with distilled water and absolute ethyl alcohol for several times respectively, and drying in an oven at 60 ℃ for 7h to obtain the hybrid microspheres.
5g of prepared hybrid microspheres, 45g of polyurethane acrylate, 25g of diluent and 1840.3 g of photoinitiator are mixed and stirred uniformly, a coating with the thickness of 10 mu m is coated on an optical PET film with the thickness of 50 mu m, the mixture is cured for 8min under a 100W UV lamp (365nm) to form a film, the film is taken out and coated on the other side of the PET, and the light diffusion film is obtained after curing. The film has a visible transmittance of 91% and a haze of 87% as measured by a haze meter, and an ultraviolet transmittance of 13% as measured by an ultraviolet spectrometer, and can be used as a novel light diffusion film.
Example 2:
adding 0.04mol of gamma-methacryloxypropyltrimethoxysilane and 1.5mol of distilled water into another reaction kettle, stirring, adjusting the pH value to 5.5 by using 0.01M dilute hydrochloric acid, reacting for 4 hours at room temperature, adjusting the pH value of the reaction solution to 8.5 by using 0.01M ammonia water, continuing reacting for 4 hours at room temperature, standing, filtering, and washing with distilled water to be neutral to obtain the polysiloxane microspheres.
0.008mol of aluminum chloride, 0.001mol of aluminum potassium sulfate, 0.008mol of urea and 150g of distilled water are added into a hydrothermal high-pressure kettle and stirred to form a transparent solution, and then 1.2g of the prepared polysiloxane microspheres are added and stirred uniformly. And (3) filling the hydrothermal autoclave, placing the hydrothermal autoclave in a 120 ℃ oven for 7h, cooling to room temperature, filtering, washing with distilled water and absolute ethyl alcohol for several times respectively, and drying in an oven at 60 ℃ for 7h to obtain the hybrid microspheres.
5g of prepared hybrid microspheres, 45g of polyurethane acrylate, 25g of diluent and 1840.3 g of photoinitiator are mixed and stirred uniformly, a coating with the thickness of 10 mu m is coated on an optical PET film with the thickness of 50 mu m, the mixture is cured for 8min under a 100W UV lamp (365nm) to form a film, the film is taken out and coated on the other side of the PET, and the light diffusion film is obtained after curing. The film has a visible transmittance of 92% and a haze of 85% as measured by a haze meter, and an ultraviolet transmittance of 11% as measured by an ultraviolet spectrometer, and can be used as a novel luminescent light diffusion film.
Example 3:
adding 0.03mol of vinyl tri (beta-methoxyethoxy) silane and 1.5mol of distilled water into another reaction kettle, stirring, adjusting the pH value to 5.5 by using 0.01M dilute hydrochloric acid, reacting for 4 hours at room temperature, adjusting the pH value of the reaction solution to 8.0 by using 0.01M ammonia water, continuing reacting for 4 hours at room temperature, standing, filtering, and washing with distilled water to be neutral to obtain the polysiloxane microspheres.
0.008mol of zinc nitrate, 0.001mol of aluminum potassium sulfate, 0.008mol of urea and 150g of distilled water are added into a hydrothermal high-pressure kettle and stirred to form a transparent solution, and then 1.2g of the prepared polysiloxane microspheres are added and stirred uniformly. And (3) filling the hydrothermal autoclave, placing the hydrothermal autoclave in a 120 ℃ oven for 9h, cooling to room temperature, filtering, washing with distilled water and absolute ethyl alcohol for several times respectively, and drying in the 60 ℃ oven for 5h to obtain the hybrid microspheres.
5g of prepared hybrid microspheres, 45g of phenolic resin, 25g of diluent and 1840.3 g of photoinitiator are mixed and stirred uniformly, a coating with the thickness of 10 mu m is coated on an optical PET film with the thickness of 50 mu m, the mixture is cured for 8min under a 100W UV lamp (365nm) to form a film, the film is taken out and coated on the other side of the PET, and the light diffusion film is obtained after curing. The film has a visible transmittance of 91% and a haze of 84% as measured by a haze meter, and an ultraviolet transmittance of 11% as measured by an ultraviolet spectrometer, and can be used as a novel luminescent light diffusion film.
Claims (4)
1. A method for preparing micron-sized photodiffusion core-shell hybrid microspheres by hydrothermal synthesis is characterized in that the microspheres take polysiloxane microspheres prepared by a sol-gel method as an inner core, and shells of the microspheres consist of inorganic nanoparticles formed by an inorganic compound through a hydrothermal process.
2. The method for preparing micron-sized photodiffusion core-shell hybrid microspheres according to claim 1, which is characterized in that the preparation method comprises the following steps:
a) mixing and stirring siloxane monomers and distilled water according to the molar ratio of 1: 35-1: 70, adjusting the pH of the mixture to 5.0-6.0 by using 0.01M dilute hydrochloric acid, reacting for 4-6 h at room temperature, adjusting the pH of the reaction solution to 8.5-9.5 by using 0.01M ammonia water, continuing reacting for 4-6 h at room temperature, standing, filtering, and washing with distilled water to be neutral to obtain polysiloxane microspheres;
b) adding the mixture into a hydrothermal high-pressure autoclave according to the molar ratio of the soluble inorganic salt to the aluminum potassium sulfate of 6: 1-12: 1 and the molar ratio of the urea to the aluminum potassium sulfate of 6: 1-12: 1 respectively, and adding distilled water into the high-pressure autoclave according to the mass ratio of the distilled water to the soluble inorganic salt of 40: 1-100: 1 to stir the mixture into a transparent solution;
then adding the polysiloxane microspheres into the solution according to the mass ratio of the polysiloxane microspheres to the soluble inorganic salt of 1: 4-1: 1, and uniformly stirring;
filling a hydrothermal autoclave, placing the hydrothermal autoclave in a 120 ℃ oven for 6-9 h, cooling to room temperature, filtering, washing with distilled water and absolute ethyl alcohol for several times respectively, and drying in a 60 ℃ oven for 5-7 h to obtain hybrid microspheres;
c) and b) taking the mass of the hybrid microspheres obtained in the step b) as a reference, mixing and uniformly stirring the hybrid microspheres, the UV light curing resin, the diluent and the photoinitiator 184 according to the mass ratio of 1: 10-50: 5-15: 0.1-0.4, coating a coating with the thickness of 10 micrometers on an optical PET film with the thickness of 50 micrometers, curing for 5-10 min under a 100W UV lamp (365nm) to form a film, taking out, coating the same layer on the other side of the PET, and curing to obtain the light diffusion film material.
3. The method for preparing micron-sized photodiffusion core-shell hybrid microspheres according to claim 2, wherein the siloxane compound in step a) is one or more of vinyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane and vinyltris (beta-methoxyethoxy) silane.
4. The method for preparing micron-sized photodiffusion core-shell hybrid microspheres according to claim 2, wherein the soluble inorganic salt in step b) is one of aluminum chloride, aluminum nitrate, aluminum sulfate, zinc chloride, zinc nitrate and zinc sulfate; the light-cured resin is one of polyurethane acrylate, epoxy acrylic resin, phenolic resin and polyester acrylate.
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| CN113956784A (en) * | 2021-10-18 | 2022-01-21 | 丽水学院 | Water-based visible light driven film-forming finishing agent for ecological synthetic leather |
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| 胡金刚: "LCD背光模组用新型抗老化光扩散膜的设计、制备及性能研究", 《中国优秀博硕士学位论文全文数据库(博士)工程科技Ⅰ辑》 * |
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| CN113956784A (en) * | 2021-10-18 | 2022-01-21 | 丽水学院 | Water-based visible light driven film-forming finishing agent for ecological synthetic leather |
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