CN111040097A - Porous silicon dioxide light diffusant with polymethyl methacrylate connected on surface and preparation method thereof - Google Patents
Porous silicon dioxide light diffusant with polymethyl methacrylate connected on surface and preparation method thereof Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C01B33/113—Silicon oxides; Hydrates thereof
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Abstract
The invention discloses a porous silicon dioxide light diffusant with a surface bonded with polymethyl methacrylate, which is characterized by comprising silicon dioxide spheres with rough and porous surfaces and polymethyl methacrylate with the surface bonded mass of 9.0-13.0% of that of the silicon dioxide; the particle size distribution of the silicon dioxide pellets is 300-500 nm, and small holes with the aperture of 10-20nm are distributed on the surface of the silicon dioxide pellets. The light diffusion agent provided by the invention has the advantages that the light diffusion effect is greatly improved, the thickness of a plate is reduced, the material cost is reduced, the problem that the high light transmittance is high but the haze is not high in the matrix resin of the raw material is solved, the energy is saved, the efficiency is high, and the phenomenon of glare is not easy to generate.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a porous silicon dioxide light diffusant with polymethyl methacrylate connected to the surface and a preparation method thereof.
Background
With the development of science and technology and times, the traditional white weaving lamp is gradually developed. The LED light is more excellent in environmental protection and service life, and can emit richer colors to be deeply worn by people. However, the LED is a semiconductor light source, and the LED solid semiconductor is combined by a P-type semiconductor and an N-type semiconductor 2. Wherein the P-type semiconductor is dominated by holes and the N-type semiconductor is mainly filled with electrons. Once the positive direction current is switched on, the redundant energy is discharged through the photon form. Resulting in an LED light source with a point source characteristic. When the light source is unevenly distributed and the directivity is strong, glare is easily caused to people, so that the LED lamp causes certain trouble in practical use. The light diffusant is a material with special optical characteristics, has excellent light diffusion effect and light transmittance, can uniformly convert a point light source of an LED into a surface light source, enables light to form diffuse reflection, achieves the effect of light uniformization, and effectively solves the problems of glare and low light extraction efficiency of the LED light source.
Polycarbonate (PC) is a transparent thermoplastic engineering plastic with excellent overall properties, has excellent toughness, heat resistance, dimensional stability, etc., and is often used as a substrate for light diffusion materials. The mechanical properties are good before the thermoplastic material. The glass transition temperature of PC is 149 ℃, and the PC can be continuously used at about 130 ℃. Is a good choice as a substrate of the light diffusion material.
The most significant factor affecting light diffusing materials is the light diffusing agent. Light diffusers are generally classified into 3 types. Inorganic particles, organic particles and inorganic-organic hybrid particles. The hybrid inorganic-organic particles developed today have more excellent properties. Nowadays, people pay more attention to the application of organic silicon spheres as light diffusant in a matrix. The particle size of the organic silicon spheres is well controlled, so that the light absorption is low and the thermal stability is high. A great deal of research has been conducted therein.
A light diffusing agent is used for the light diffusing material. Silica is often used as a light diffusing agent due to its excellent optical properties and characteristic of easily changeable morphology, but since silica is an inorganic substance, it causes phenomena such as unstable optical properties and brittleness after being combined with a PC substrate. Therefore, the surface modification of the silica microspheres to be more complete with the PC is a research direction.
Disclosure of Invention
The invention aims to solve the problems and provides a porous silica light diffusant with polymethyl methacrylate bonded on the surface and a preparation method thereof.
The purpose of the invention is realized as follows:
the invention relates to a porous silicon dioxide light diffusant with a surface connected with polymethyl methacrylate, wherein the surface of a silicon dioxide pellet is in a rough porous shape, the surface of the silicon dioxide pellet is connected with the polymethyl methacrylate, the particle size distribution of the silicon dioxide pellet is 300-500 nm, and pores with the pore diameter of 10-20nm are distributed on the surface of the silicon dioxide pellet.
The preparation method of the porous silicon dioxide light diffusant with the surface bonded with the polymethyl methacrylate comprises the following steps:
(1) under the condition of stirring at 35 ℃, adding ammonia water and tetraethoxysilane into a mixed solution of water and ethanol, continuously reacting for 3 hours, washing and drying to prepare a silicon dioxide pellet, wherein the volume ratio of tetraethoxysilane to water is 1:4-1:8, the volume ratio of tetraethoxysilane to ethanol is 1:8-1:20, and the volume ratio of tetraethoxysilane to ammonia water is 1:2-1: 6;
(2) taking the silicon dioxide pellets prepared in the step (1) to prepare a mixed solution with the mass fraction of 3-50 wt% in deionized water, and performing ultrasonic dispersion for 30 minutes; adding a surfactant with the mass ratio of 1/10-1/20 to the silicon dioxide pellets under the stirring condition, wherein the surfactant is alkyl ammonium bromide with 16-20 carbon atoms; reacting for 2 hours; under the condition of stirring, continuously adding an alkaline substance into the mixed solution, wherein the alkaline substance is sodium hydroxide or other strong alkaline substances; controlling the concentration of the alkaline substance in the solution to be 2-10 wt%; continuously reacting for 3-5 hours, washing and drying the sample, and roasting the sample at 450 ℃ for 3 hours to prepare porous silicon dioxide spheres on the surface;
(3) dissolving the surface porous silicon dioxide pellets prepared in the step (2) in toluene to prepare a solution with the mass volume fraction controlled between 0.01 and 0.1 g/ml; adding silane coupling agent with the volume of 1-2% of that of the toluene, wherein the silane coupling agent can be 3-methacryloxypropyltrimethoxysilane; refluxing in 120-degree oil bath for 2-8 hours, washing with acetone, and drying to obtain alkylated porous silica spheres;
(4) placing the alkylated porous silicon dioxide pellets prepared in the step (3) in deionized water to form 1-5 wt%, and performing ultrasonic dispersion for 1 minute; under the condition of stirring, adding sodium dodecyl sulfate, nonylphenol polyoxyethylene ether and isopropanol, wherein the mass ratio of the sodium dodecyl sulfate to the nonylphenol polyoxyethylene ether is 2:1, the mass ratio of the sodium dodecyl sulfate to the silicon dioxide is 1:50-1:25, the mass ratio of the nonylphenol polyoxyethylene ether to the silicon dioxide is 1:100-1:50, and the volume ratio of the isopropanol to deionized water is 1:35-1: 45; after stirring for 30 minutes, slowly dropwise adding a methyl methacrylate monomer and a certain amount of 0.2 wt% potassium persulfate solution under the condition of water bath at the temperature of 60-80 ℃, wherein the volume ratio of the potassium persulfate solution to deionized water is 3:100-6:100, and the adding mass of the methyl methacrylate monomer is 1-9 times that of the alkylated porous silica spheres; and (3) continuing to react for 1 hour at 80 ℃, and washing and drying to obtain the porous silica spheres with the surface linked with the polymethyl methacrylate.
The surface of the silicon dioxide pellet light diffusant with the surface connected with the polymethyl methacrylate is subjected to light refraction for countless times to achieve the light diffusion effect, and compared with pure silicon dioxide microspheres, the silicon dioxide pellet light diffusant has the advantages that the brightness and the light transmittance are improved; the light diffusion agent has the characteristics of scraping resistance, corrosion resistance, weather resistance, good insulativity, good optical performance and heat resistance of silicon dioxide and the like of PMMA, and the light diffusion effect greatly improved by the silicon dioxide spheres with the surface connected with the polymethyl methacrylate; therefore, the thickness of the plate is reduced, the material cost is reduced, the problems of high light transmittance and low haze of the raw material matrix resin are solved, and the effects of energy conservation, high efficiency and difficulty in generating the glare phenomenon are achieved.
Drawings
FIG. 1 is a scanning electron micrograph of a superficially porous silica pellet;
FIG. 2 is a scanning electron microscope image of the porous silica bead light diffuser of the present invention with polymethyl methacrylate bonded on the surface.
Detailed Description
The invention will be further explained with reference to the drawings.
The invention discloses a porous silicon dioxide light diffusant with a surface bonded with polymethyl methacrylate, wherein the surface of a silicon dioxide pellet is in a rough porous shape, the surface bonded with polymethyl methacrylate with the mass of 9.0-13.0% of that of silicon dioxide, the particle size distribution of the silicon dioxide pellet is 300-500 nm, and pores with the pore diameter of 10-20nm are distributed on the surface.
The preparation method of the porous silicon dioxide light diffusant with the surface bonded with the polymethyl methacrylate comprises the following steps:
(1) under the condition of stirring at 25-45 ℃, adding ammonia water and tetraethoxysilane into a mixed solution of water and ethanol, continuously reacting for 2-4 hours, washing and drying to prepare a silicon dioxide pellet, wherein the volume ratio of the tetraethoxysilane to the water is 1:4-1:8, the volume ratio of the tetraethoxysilane to the ethanol is 1:8-1:20, and the volume ratio of the tetraethoxysilane to the ammonia water is 1:2-1: 6;
(2) taking the silicon dioxide pellets prepared in the step (1) to prepare a mixed solution with the mass fraction of 3-50 wt% in deionized water, and performing ultrasonic dispersion for 30 minutes; under the condition of stirring, adding a certain amount of surfactant, and reacting for 1-3 hours; under the condition of stirring, continuously adding alkaline substances into the mixed solution, and controlling the concentration of the alkaline substances in the solution to be 2-10 wt%; continuously reacting for 3-5 hours, washing and drying the sample, and roasting the sample at 450 ℃ for 2-4 hours to prepare porous silicon dioxide spheres on the surface;
(3) dissolving the surface porous silicon dioxide pellets prepared in the step (2) in toluene to prepare a solution with the mass volume fraction controlled between 0.01 and 0.1 g/ml; adding a silane coupling agent with the volume of 1-2% of that of toluene, refluxing for 2-8 hours in an oil bath with the temperature of 110-;
(4) placing the alkylated porous silicon dioxide pellets prepared in the step (3) in deionized water to form 1-5 wt%, and performing ultrasonic dispersion for 1-5 minutes; under the condition of stirring, adding sodium dodecyl sulfate, nonylphenol polyoxyethylene ether and isopropanol according to the proportion; stirring for 20-40 minutes, slowly dropwise adding a certain amount of methyl methacrylate monomer and 0.2 wt% of potassium persulfate solution under the condition of water bath at the temperature of 60-80 ℃, continuously reacting for 1 hour at the temperature of 70-90 ℃, and washing and drying to obtain the porous silica spheres with the surface linked with the polymethyl methacrylate.
Example 1:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 2:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 30 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 3:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 40 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 4:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of octadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 5:
under the condition of stirring at 35 ℃, adding 4 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 16 ml of water and 16 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; under the condition of stirring, adding 20 mg of eicosyl trimethyl ammonium bromide, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 6:
under the condition of stirring at 35 ℃, adding 12 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 30 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; under stirring, 0.8 g of other strongly basic substances (potassium hydroxide, strontium hydroxide, barium hydroxide, etc.) were added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 7:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 12 ml of water and 20 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 6 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 8:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of other silane coupling agents (vinyl triethoxysilane, vinyl trimethoxysilane and the like), refluxing for 8 hours in a 120-degree oil bath, washing a sample by acetone, and drying to obtain alkylated porous silica spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 9:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 10 ml of water and 30 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.02 g of sodium dodecyl sulfate, 0.010 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 10:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 4 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 11:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.04 g of sodium dodecyl sulfate, 0.02 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 12:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.2 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 13:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.8 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 14:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 3 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 15:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 6 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 16:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 9 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 17:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; taking the 0.4 g of silicon dioxide pellets into 10 ml of deionized water, and carrying out ultrasonic dispersion for 30 minutes; adding 20 mg of hexadecyl trimethyl ammonium bromide under the condition of stirring, and reacting for 2 hours; while stirring, 0.8 g of sodium hydroxide was further added to the mixture. Continuously reacting for 5 hours, washing and drying the sample, and roasting the sample for 3 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface; 4 g of superficially porous silica spheres were dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane serving as a silane coupling agent, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain alkylated porous silicon dioxide spheres; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.03 g of sodium dodecyl sulfate, 0.015 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 3 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the porous silica spheres with the surface bonded with the polymethyl methacrylate.
Example 18:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; 4 g of silica beads are dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 0.04 g of sodium dodecyl sulfate, 0.02 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, slowly dropwise adding 1 g of methyl methacrylate monomer and 5 ml of 0.2 wt% potassium persulfate solution under the condition of 60-degree water bath, continuing to react for 1 hour at 80 ℃, and washing and drying a sample to obtain the silica spheres with the surface bonded with the polymethyl methacrylate.
Example 19:
under the condition of stirring at 35 ℃, adding 8 ml of ammonia water and 2 ml of tetraethoxysilane into a mixed solution of 8 ml of water and 40 ml of ethanol, continuously reacting for 3 hours, and washing and drying to obtain silicon dioxide pellets; 4 g of silica beads are dissolved in 200 ml of toluene. Adding 2 ml of 3-methacryloxypropyltrimethoxysilane, refluxing for 8 hours in a 120-DEG oil bath, washing a sample by acetone, and drying to obtain an alkylated porous silicon dioxide pellet; then taking 1 g of the prepared alkylated porous silica spheres in 100 ml of deionized water, and carrying out ultrasonic dispersion for 1 minute; under the condition of stirring, 1.16 g of PMMA, 0.02 g of nonylphenol polyoxyethylene ether and 2.5 ml of isopropanol are added; after stirring for 30 minutes, the reaction was continued at 80 ℃ for 1 hour, and the sample was washed and dried to obtain silica pellets mixed with PMMA (the content of PMMA was the same as that of PMMA in the light diffuser of example 11).
Preparing a PC light diffusion plate sample 1-17:
respectively mixing 50 g of PC and 0.16 g of antioxidant with 0%, 0.10%, 0.30%, 0.70%, 1% and 1.50% of the light diffusion agent prepared in the embodiment 13 by mass percent, uniformly mixing, transferring the mixture into an internal mixer for stirring, controlling the temperature of the mixture to be between 240 ℃ and 250 ℃, stirring for 8 minutes, uniformly stirring, shearing particles, tabletting by a flat vulcanizing machine, and finally preparing PC light diffusion plate samples 1-6, wherein the molding temperature is 250 ℃;
respectively stirring and uniformly mixing 50 g of PC and 0.16 g of antioxidant with 1% of the sample light diffusion agent obtained in the embodiment 1, the embodiment 2, the embodiment 5, the embodiment 11, the embodiment 13 and the embodiment 16, then transferring the mixture into an internal mixer for stirring, controlling the temperature of the material between 240 ℃ and 250 ℃, stirring for 8 minutes, shearing the particles after uniformly stirring, flaking the particles by a flat vulcanizing machine, and finally preparing a PC light diffusion plate sample 7-12, wherein the molding temperature is 250 ℃;
respectively stirring and uniformly mixing 50 g of PC, 0.16 g of antioxidant with 1 percent of the porous silica spheres in the embodiment 11, the rough porous silica spheres with polymethyl methacrylate connected on the surface in the embodiment 11, the solid silica spheres in the embodiment 18, the silica spheres with polymethyl methacrylate connected on the surface in the embodiment 18 and the silica spheres mixed in the embodiment 19, transferring the mixture into an internal mixer for stirring, controlling the temperature of the materials to be between 240 ℃ and 250 ℃, stirring for 8 minutes, shearing the particles after uniform stirring, flaking by using a flat vulcanizing machine, controlling the molding temperature to be 250 ℃, and finally preparing PC light diffusion plate samples 13-17;
and (3) performance testing:
light transmittance and haze test: the light transmittance and haze of the prepared PC light diffusion plate samples 1-17 were measured by a light transmittance and haze tester, and the test results are shown in Table 1:
| sample (I) | Light transmittance (100%) | Haze (100%) |
| 1 | 90.57 | 10.33 |
| 2 | 90.77 | 23.1 |
| 3 | 88.3 | 46.76 |
| 4 | 86.93 | 50 |
| 5 | 85.83 | 81.6 |
| 6 | 78.73 | 83.47 |
| 7 | 72.07 | 71.85 |
| 8 | 70 | 72.98 |
| 9 | 85.83 | 81.6 |
| 10 | 90.6 | 78.55 |
| 11 | 73.6 | 76.35 |
| 12 | 72.58 | 70.85 |
| 13 | 85.2 | 27.4 |
| 14 | 85.83 | 81.6 |
| 15 | 70.2 | 38.07 |
| 16 | 64.5 | 60.2 |
| 17 | 74.6 | 50.1 |
Transmittance to sample 15: 70.2 percent; haze: 38.07, coarse porous SiO2Sample 13 of the protocol had a light transmission of 85.2% and a haze of 27.4%; compared to sample 16, sample 14 had a transmittance of 85.83%, a haze of 81.6%: both the transmittance and haze were improved for sample 14 compared to sample 17.
The test result shows that the light diffusion effect of the light diffusion agent is greatly improved, the light diffusion effect of the light diffusion agent can reduce the thickness of the plate, the material cost is reduced, the problem that the high light transmittance and the low haze of the raw material matrix resin are high is solved, the energy is saved, the efficiency is high, and the glare phenomenon is not easy to generate.
The above embodiments are provided only for illustrating the present invention and not for limiting the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, and therefore all equivalent technical solutions should also fall within the scope of the present invention, and should be defined by the claims.
Claims (5)
1. A porous silicon dioxide light diffusant with polymethyl methacrylate connected on the surface is characterized by comprising silicon dioxide pellets with rough and porous appearance on the surface and polymethyl methacrylate with the surface connection mass of 9.0-13.0% of the mass of the silicon dioxide;
the particle size distribution of the silicon dioxide pellets is 300-500 nm, and small holes with the aperture of 10-20nm are distributed on the surface of the silicon dioxide pellets.
2. The method for preparing a surface-bonded polymethylmethacrylate porous silica light diffuser according to claim 1, comprising the steps of:
(1) under the condition of stirring at 25-45 ℃, adding ammonia water and tetraethoxysilane into a mixed solution of water and ethanol, continuously reacting for 2-4 hours, washing and drying to prepare a silicon dioxide pellet, wherein the volume ratio of tetraethoxysilane to water is 1:4-1:8, the volume ratio of tetraethoxysilane to ethanol is 1:8-1:20, and the volume ratio of tetraethoxysilane to ammonia water is 1:2-1: 6;
(2) taking the silicon dioxide pellets prepared in the step (1) to prepare a mixed solution with the mass fraction of 3-50 wt% in deionized water, and performing ultrasonic dispersion for 20-40 minutes; adding a surfactant with the mass ratio of 1/10-1/20 to the silicon dioxide pellets under the stirring condition; reacting for 1-3 hours; under the condition of stirring, continuously adding an alkaline substance into the mixed solution; controlling the concentration of the alkaline substance in the solution to be 2-10 wt%; continuously reacting for 3-5 hours, washing and drying, and roasting for 2-4 hours at 450 ℃ to prepare porous silicon dioxide spheres on the surface;
(3) dissolving the surface porous silicon dioxide pellets prepared in the step (2) in toluene to prepare a solution with the mass volume fraction controlled between 0.01 and 0.1 g/ml; adding a silane coupling agent accounting for 1-2% of the volume of the toluene; refluxing in 110-130 deg.C oil bath for 2-8 hr, washing with acetone, and drying to obtain alkylated porous silica spheres;
(4) placing the alkylated porous silica spheres prepared in the step (3) into deionized water to form 1-5 wt%, and performing ultrasonic dispersion for 1-5 minutes; adding sodium dodecyl sulfate, nonylphenol polyoxyethylene ether and isopropanol under the condition of stirring, wherein the mass ratio of the sodium dodecyl sulfate to the nonylphenol polyoxyethylene ether is 2:1, the mass ratio of the sodium dodecyl sulfate to the silicon dioxide is 1:50-1:25, the mass ratio of the nonylphenol polyoxyethylene ether to the silicon dioxide is 1:100-1:50, and the volume ratio of the isopropanol to the deionized water is 1:35-1: 45; after stirring for 20-40 minutes, slowly dropwise adding a methyl methacrylate monomer and 0.2 wt% of potassium persulfate solution under the condition of water bath at 60-80 ℃, wherein the volume ratio of the potassium persulfate solution to deionized water is 3:100-6:100, and the adding mass of the methyl methacrylate monomer is 1-9 times that of the alkylated porous silica spheres; and continuously reacting for 0.5-1.5 hours at 70-90 ℃, and washing and drying to obtain the porous silica spheres with the surface linked with the polymethyl methacrylate.
3. The method for preparing a porous silica light diffuser having a surface bonded with polymethylmethacrylate according to claim 2, wherein the surfactant is alkylammonium bromide having 16 to 20 carbon atoms.
4. The method of claim 2, wherein the alkali is selected from one of sodium hydroxide, potassium hydroxide and barium hydroxide.
5. The method of claim 2, wherein the silane coupling agent is 3-methacryloxypropyltrimethoxysilane.
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| CN112480584A (en) * | 2020-12-03 | 2021-03-12 | 安徽新涛光电科技有限公司 | Acrylic light diffusion plate, preparation method thereof and light diffusion agent |
| CN114031988A (en) * | 2021-11-19 | 2022-02-11 | 吉林省铭嘉建筑材料有限公司 | Super-strong-binding-force environment-friendly waterproof material and using method thereof |
| CN114907602A (en) * | 2022-06-07 | 2022-08-16 | 江苏弘德光电材料科技有限公司 | Uniform light composite film and preparation method thereof |
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