CN113980279A - Hollow organic silicon microsphere, preparation method and application thereof - Google Patents

Hollow organic silicon microsphere, preparation method and application thereof Download PDF

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Publication number
CN113980279A
CN113980279A CN202111471524.5A CN202111471524A CN113980279A CN 113980279 A CN113980279 A CN 113980279A CN 202111471524 A CN202111471524 A CN 202111471524A CN 113980279 A CN113980279 A CN 113980279A
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hollow
coupling agent
preparation
organic silicon
silane coupling
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王启瑶
孙佳男
陈杰
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Eversun Polycarbon Sci & Tech Corp
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes
    • C08J2383/05—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/10—Transparent films; Clear coatings; Transparent materials

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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Abstract

The invention relates to the technical field of polymer synthesis, in particular to a preparation method of hollow organic silicon microspheres, which comprises the following steps: (S1) mixing an organic functional silane coupling agent and a hydrogen-containing silane coupling agent at a certain temperature, adding an acidic regulator to regulate the pH value to be acidic, and hydrolyzing for a certain time under an acidic condition to obtain an active reactant; (S2), adding silica sol and an alkaline catalyst into water at a certain temperature, uniformly mixing, adding the active reaction body, mixing for 1-30min, standing, carrying out heat preservation and aging for a certain time, filtering and separating a product, and drying to obtain the hollow organic silicon microspheres, so that the microspheres with protrusions generated by a silicon dioxide coating on the surface and a plurality of cavities in the interior are obtained, the special structure of the microspheres leads to higher light diffusion efficiency, and the hollow organic silicon microspheres with lower adding amount can realize higher light diffusion efficiency.

Description

Hollow organic silicon microsphere, preparation method and application thereof
Technical Field
The invention relates to the technical field of polymer synthesis, in particular to a hollow organic silicon microsphere, a preparation method and application thereof.
Background
In terms of performance, the LED light source is favored due to its low energy consumption, low heat, environmental protection, and long life, and has potential application values in many other aspects including signal indication, green display, special illumination, etc. due to its excellent performance.
Compared with the conventional light source, the LED is a point light source, and the light emission is concentrated and strong, so that the brightness is not uniform, and glare is generated. Therefore, in LED applications, one of the first bottleneck problems to be solved is glare. It is therefore the direction of current research to soften LED light without creating or minimizing light loss.
The current methods for solving the bottleneck mainly comprise: the color powder (such as barium sulfate and the like) is added on the basis of the original lampshade, the frosting effect is improved, and the prism is added; however, the above methods have a limited light diffusion effect and reduce the light transmittance.
The best solution now recognized is to use light diffusing resin material as the LED lamp cover, i.e. to introduce light diffusing agent in the resin matrix for light scattering purpose. The light diffusing agent is transparent nanometer or submicron spherical particle, and is added into PC, PMMA and other matrix and dispersed homogeneously. The incident light passes through the glass sphere, is refracted for countless times and then penetrates through the glass sphere, and is uniformly dispersed, so that the point light source is changed into a surface light source, the light emitting surface is enlarged, and the light is soft; meanwhile, light can penetrate through the sphere, light loss is small, the propagation direction of the light is changed for many times, the light is refracted for many times, the softness of the light of the LED lamp is achieved, the defect that the dazzling degree of the light is adjusted simply by using toner in the past can be overcome, the luminance is darkened due to the fact that the toner can shield a lot of light in the base material, and the effect of light evening and light transmission can not be achieved due to the fact that the toner cannot block a lot of light to pass through like the organic light diffusant. The material of the light diffusing agent may be inorganic or organic. Examples of commonly used light diffusers include silica, zinc oxide, titanium dioxide, zirconium oxide, zinc sulfide, barium sulfate, styrene polymers, acrylic polymers, and siloxane polymers.
The main technical parameters characterizing the properties of light-diffusing materials are light transmittance and haze. The light transmittance represents the total utilization rate of the light diffusion material to incident light, and the haze represents the degree of deviation of the incident light from the original incident direction, so that the light transmittance can be used for representing the degree of diffusion of the light diffusion material to the incident light. The light transmittance of the lampshade used in daily life is not very high, namely, a part of light energy is lost. Therefore, the development of a light diffusion material having high light transmittance and high haze is important for effectively utilizing light energy of a light source. In the light diffusion material produced on the market at present, the light transmittance and the haze of the light diffusion material are not well balanced.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, one of the purposes of the present invention is to provide a preparation method of hollow organic silicon microspheres, wherein the microspheres are provided with protrusions generated by a silica coating on the surface and a plurality of cavities inside, and the special structure of the microspheres leads to higher light diffusion efficiency and low addition amount. The preparation method has the advantages of simple operation, convenient control, high production efficiency and low production cost, and can be used for large-scale production.
The second purpose of the invention is to provide a hollow organic silicon microsphere, when light irradiates the rough porous organic silicon resin microsphere, the times that the light enters and exits interfaces with different refractive indexes on the surface of the microsphere and in the cavity are increased, so that the higher light diffusion efficiency is obtained with smaller addition amount.
It is a further object of the present invention to provide a use of hollow silicone microspheres as a light diffuser for thermoplastic resin articles, and a light diffuser plate obtained therefrom has excellent transmittance, haze, brightness, light resistance, and the like.
The purpose of the invention is realized by the following technical scheme: a preparation method of hollow organic silicon microspheres comprises the following steps:
(S1) mixing an organic functional silane coupling agent and a hydrogen-containing silane coupling agent at a certain temperature, adding an acidic regulator to regulate the pH value to be acidic, and hydrolyzing for a certain time under an acidic condition to obtain an active reactant;
(S2), adding silica sol and an alkaline catalyst into water at a certain temperature, uniformly mixing, adding the active reactant, mixing for 1-30min, standing, preserving heat, aging for a certain time, filtering and separating a product, and drying to obtain the hollow organic silicon microspheres.
According to the preparation method of the hollow organic silicon microsphere, the microsphere with the surface provided with the protrusions generated by the silicon dioxide coating and the inner part provided with the plurality of cavities is obtained, the special structure of the microsphere leads the microsphere to have higher light diffusion efficiency, and the hollow organic silicon microsphere with lower addition amount can realize better light diffusion efficiency. Wherein, in the step (S1), under acidic condition, the organic functional silane coupling agent and the hydrogen-containing silane coupling agent react with water to hydrolyze, so that micromolecular alcohol, organic functional silane coupling agent containing hydroxyl and hydrogen-containing silane coupling agent are removed, and dehydration condensation reaction between the organic functional silane coupling agent and the hydrogen-containing silane coupling agent can be avoided. In the invention, in order to more fully and uniformly mix the organic functional silane coupling agent and the hydrogen-containing silane coupling agent, the organic functional silane coupling agent and the hydrogen-containing silane coupling agent are selected to be firstly cohydrolyzed under an acidic condition and then condensed under an alkaline catalysis condition in the step (S2), so that the phenomenon that the product is difficult to generate due to the fact that the two coupling agents are directly condensed under the alkaline catalysis condition and the reaction activity and affinity are different is avoided. In the step (S2), the organic functional silane coupling agent and the hydrogen-containing silane coupling agent are catalyzed and polycondensed by the alkaline catalyst under the condition of better reaction activity, the polycondensation process is gradually carried out, at the beginning, because the hydroxyl in the coupling agent is lost, the molecular weight is increased, and the coupling agent is gradually incompatible with water, the condensed coupling agent forms droplets because the silica sol mainly acts as a release agent, takes on a spherical shape due to surface tension, and then continues to be crosslinked, in the process, the hydrogen-containing silane coupling agent in the liquid drop releases hydrogen to form a cavity, and finally the cavity is solidified into spherical resin particles, in this process, because the droplets are large (2-10 μm), and the silica sol particles are of the nanometer scale, and the surface electrical property and the liquid drop of the silica sol are different, the large particle area and the electrical property are complementary, so that the silica microspheres in the silica sol can be adsorbed on the surface of the spherical resin particles. Meanwhile, because the silica microspheres of the silica sol contain a great number of silicon hydroxyl groups, the hydroxyl groups can also be subjected to condensation polymerization with a system to form Si-O-Si bonds, so that the silica microspheres are not easy to separate from the spherical resin particles, namely, the silica microspheres are fused into a whole, and the surfaces of the spherical resin particles have a protruding structure, namely, the rough hollow organic silicon microspheres with surface protruding structures are provided.
Preferably, the organofunctional silane coupling agent, the hydrogen-containing silane coupling agent, the acidity regulator, the water, the silica sol and the basic catalyst are used in amounts of 1 to 50 parts, 20 to 99 parts, 20 to 100 parts, 20 to 80 parts, 1 to 20 parts and 0.2 to 10 parts, respectively, by weight.
By adopting the technical scheme, the raw materials are controlled to fully play the roles; more preferably, the organofunctional silane coupling agent, the hydrogen-containing silane coupling agent, the acidity regulator, water, the silica sol and the basic catalyst are used in amounts of 10 to 50 parts, 30 to 70 parts, 30 to 90 parts, 30 to 60 parts, 3 to 15 parts and 0.5 to 6 parts, respectively, by weight.
Preferably, in the step (S1), the temperature condition is 20 to 70 ℃; in the step (S2), the temperature condition is 20 to 70 ℃.
By adopting the technical scheme, the reaction process is ensured and even accelerated. More preferably, in the step (S1), the temperature condition is 40 to 70 ℃; in the step (S2), the temperature condition is 40 to 70 ℃.
Preferably, in the step (S1), the hydrolysis time is 1-8 h; in the step (S2), the heat preservation and aging time is 24-48 h.
By adopting the technical scheme, the hydrolysis time is 1-8h, and an active reactant can be obtained; the heat preservation and aging time is 24-48h, so that the active reactant can crosslink the solidified layer microspheres under the alkaline catalysis, and the silica sol is adsorbed on the surfaces of the microspheres.
Preferably, the acidity regulator is an inorganic acid-water solution or a carboxylic acid-water solution, and the concentration of the carboxylic acid-water solution is 0.1-2 wt%.
By adopting the technical scheme, further, the inorganic acid is hydrochloric acid or sulfuric acid, the carboxylic acid is selected from monocarboxylic acid, dicarboxylic acid or polycarboxylic acid, and the polycarboxylic acid is tartaric acid, oxalic acid, malic acid, citric acid or ascorbic acid. The carboxylic acid is preferably oxalic acid in order to facilitate both controlled hydrolysis of the organosilanols produced.
Preferably, the organofunctional silane coupling agent has the general chemical formula (R)xSi(OR)yWherein x is an integer of 0 to 3, y is an integer of 1 to 4, and x + y is 4, R is an alkyl group having 1 to 6 carbon atoms, a vinyl group having 1 to 6 carbon atoms, an aryl group having 6 to 20 carbon atoms, or an alkyl-substituted aryl group having 6 to 20 carbon atoms.
With the above technical solution, more preferably, the organofunctional silane coupling agent includes, but is not limited to, at least one of methyltrimethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltris (β -methoxyethoxy) silane, γ -methacryloxypropyltrimethoxysilane, γ -aminopropyltriethoxysilane, or γ -glycidoxypropyltrimethoxysilane.
Preferably, the hydrogen-containing silane coupling agent has a chemical formula of H (R)nSi(OR)mWherein n is an integer of 0 to 2, m is an integer of 1 to 3, and n + m is 3, R is an alkyl group having 1 to 6 carbon atoms, a vinyl group having 1 to 6 carbon atoms, an aryl group having 6 to 20 carbon atoms, or an alkyl-substituted aryl group having 6 to 20 carbon atoms.
With the above technical solution, more preferably, the hydrogen-containing silane coupling agent includes, but is not limited to, at least one of trimethoxysilane, methyldimethoxysilane, methyldiethoxysilane, or triethoxysilane.
Preferably, the silica sol is acidic silica sol or alkaline silica sol; the alkaline catalyst is inorganic alkali.
By adopting the technical scheme, more preferably, the silica sol is alkaline silica sol and can be selected from AM3005, AM3010, AM4010 or AM4020 of a Baite new material. The inorganic base is selected from ammonia, sodium hydroxide or potassium hydroxide.
The second purpose of the invention is realized by the following technical scheme: the hollow organic silicon microsphere is prepared by the preparation method of the hollow organic silicon microsphere.
The third purpose of the invention is realized by the following technical scheme: the hollow organic silicon microspheres are applied to a thermoplastic resin product as a light diffusion agent, and the thermoplastic resin comprises at least one of polyvinyl chloride resin, styrene resin, SAN resin, acrylic-styrene resin, polyester resin, ABS resin or polycarbonate resin.
The invention has the beneficial effects that: according to the preparation method of the hollow organic silicon microsphere, the microsphere with the surface provided with the protrusions generated by the silicon dioxide coating and the inner part provided with a plurality of cavities is obtained, and the special structure of the microsphere leads the microsphere to have higher light diffusion efficiency and low addition amount; the preparation method has the advantages of simple operation, convenient control, high production efficiency and low production cost, and can be used for large-scale production.
When the rough porous organic silicon resin microsphere is irradiated by light rays, the times that the light rays enter and exit interfaces with different refractive indexes on the surface of the sphere and in the cavity are increased, so that the hollow organic silicon microsphere can obtain higher light diffusion efficiency with smaller addition amount.
The hollow organosilicon microspheres are applied to thermoplastic resin products and used as light diffusant, and the light diffusion plate obtained by the hollow organosilicon microspheres has excellent transmissivity, haze, brightness, light resistance and the like.
Drawings
FIG. 1 is an SEM scan of hollow silicone microspheres of example 1 of the present invention;
fig. 2 is an optical microscope test chart of the hollow silicone microspheres of example 1 of the present invention, wherein the test conditions are eyepiece 5 x objective 10 x.
Detailed Description
For the understanding of those skilled in the art, the present invention will be further described with reference to the following examples and drawings, which are not intended to limit the present invention.
Example 1
A preparation method of hollow organic silicon microspheres comprises the following steps:
(S1) mixing 30 parts of organic functional silane coupling agent and 70 parts of hydrogen-containing silane coupling agent at the temperature of 50 ℃, adding 50 parts of acid regulator to regulate the pH value to be acidic, and hydrolyzing for 3 hours under the acidic condition to obtain an active reactant;
(S2), adding 10 parts of silica sol and 0.5 part of alkaline catalyst into 70 parts of water at the temperature of 30 ℃, uniformly mixing, adding the active reactant, mixing for 5min, standing, preserving heat, aging for 25h, filtering and separating a product, and drying to obtain the white hollow organic silicon microspheres.
The acidity regulator is acetic acid-water solution with the concentration of 0.5 wt%.
The organofunctional silane coupling agent is methyltrimethoxysilane.
The hydrogen-containing silane coupling agent is trimethoxy silane.
The silica sol is ammonium silica sol AM 3010; the alkaline catalyst is sodium hydroxide.
The hollow organic silicon microspheres are applied to thermoplastic resin products and used as light diffusant.
Example 2
A preparation method of hollow organic silicon microspheres comprises the following steps:
(S1) mixing 1 part of organofunctional silane coupling agent and 20 parts of hydrosilane coupling agent at the temperature of 20 ℃, adding 20 parts of acidic regulator to regulate the pH value to be acidic, and hydrolyzing for 1h under the acidic condition to obtain an active reactant;
(S2), at the temperature of 20 ℃, adding 1 part of silica sol and 0.2 part of alkaline catalyst into 20 parts of water, uniformly mixing, adding the active reactant, mixing for 1min, standing, preserving heat, aging for 24h, filtering and separating a product, and drying to obtain the white hollow organic silicon microspheres.
The acidity regulator is a carboxylic acid-water solution with the concentration of 0.1 wt%, and the carboxylic acid is oxalic acid.
The organic functional silane coupling agent is formed by mixing methyltrimethoxysilane and vinyl trimethoxy silane according to the weight ratio of 1: 1.
The hydrogen-containing silane coupling agent is methyldimethoxysilane.
The silica sol is ammonium type silica sol AM 4010; the alkaline catalyst is sodium hydroxide.
The hollow organic silicon microspheres are applied to thermoplastic resin products and used as light diffusant.
Example 3
A preparation method of hollow organic silicon microspheres comprises the following steps:
(S1) mixing 50 parts of organic functional silane coupling agent and 99 parts of hydrogen-containing silane coupling agent at the temperature of 70 ℃, adding 100 parts of acid regulator to regulate the pH value to be acidic, and hydrolyzing for 8 hours under the acidic condition to obtain an active reactant;
(S2), at the temperature of 70 ℃, adding 20 parts of silica sol and 10 parts of alkaline catalyst into 80 parts of water, uniformly mixing, adding the active reactant, mixing for 30min, standing, preserving heat, aging for 48h, filtering and separating a product, and drying to obtain the white hollow organic silicon microspheres.
The acidity regulator is a carboxylic acid-water solution with the concentration of 2 wt%, and the carboxylic acid is oxalic acid.
The organofunctional silane coupling agent is methyltrimethoxysilane.
The hydrogen-containing silane coupling agent is methyl diethoxy silane.
The silica sol is ammonium silica sol AM 3010; the alkaline catalyst is ammonia water with the concentration of 25 wt%.
The hollow organic silicon microspheres are applied to thermoplastic resin products and used as light diffusant.
Example 4
A preparation method of hollow organic silicon microspheres comprises the following steps:
(S1) mixing 50 parts of organic functional silane coupling agent and 50 parts of hydrogen-containing silane coupling agent at the temperature of 50 ℃, adding 50 parts of acid regulator to regulate the pH value to be acidic, and hydrolyzing for 3 hours under the acidic condition to obtain an active reactant;
(S2), at the temperature of 30 ℃, adding 20 parts of silica sol and 1 part of alkaline catalyst into 70 parts of water, uniformly mixing, adding the active reactant, mixing for 15min, standing, preserving heat, aging for 48h, filtering and separating a product, and drying to obtain the white hollow organic silicon microspheres.
The acidity regulator is a carboxylic acid-water solution with the concentration of 0.5 wt%, and the carboxylic acid is acetic acid.
The organofunctional silane coupling agent is phenyl trimethoxysilane.
The hydrogen-containing silane coupling agent is trimethoxy silane.
The silica sol is ammonium silica sol AM 3010; the alkaline catalyst is sodium hydroxide.
The hollow organic silicon microspheres are applied to thermoplastic resin products and used as light diffusant.
Comparative example 1
This comparative example differs from example 1 in that:
the amount of the silica sol is 0 part by weight.
Comparative example 2
A preparation method of organic silicon powder comprises the following steps:
(S1) mixing 30 parts of organic functional silane coupling agent and 70 parts of hydrogen-containing silane coupling agent at the temperature of 50 ℃ to obtain a reaction body;
(S2), at the temperature of 30 ℃, adding 10 parts of silica sol and 0.5 part of alkaline catalyst into 70 parts of water, uniformly mixing, adding the reactant, mixing for 5min, standing, keeping the temperature for 25h, filtering and separating out a product, and drying to obtain the organic silicon powder.
The acidity regulator is acetic acid-water solution with the concentration of 0.5 wt%.
The organofunctional silane coupling agent is methyltrimethoxysilane.
The hydrogen-containing silane coupling agent is trimethoxy silane.
The silica sol is ammonium silica sol AM 3010; the alkaline catalyst is sodium hydroxide.
The organic silicon powder is applied to thermoplastic resin products and used as a light diffusant.
Comparative example 3
A light diffusion agent is silicon dioxide powder which is soaked in methyltrimethoxysilane for 24 hours, filtered and dried, and the particle size of the silicon dioxide powder is 3.5 mu m.
Performance testing
Taking the light diffusant of the embodiment 1, and scanning the light diffusant by adopting SEM (scanning Electron microscope) to obtain a result shown in figure 1, wherein the surface of a sphere is rough, a cavity is formed in the sphere, and the cavity is not obvious enough but still visible; the light diffusing agent of example 1 was observed with an optical microscope (eyepiece: 5 × objective lens: 10 times) and the result is shown in fig. 2, and it can be seen that the interior of the sphere has a cavity structure.
II, taking the light diffusion agents of the examples 1-4 and the comparative examples 1-3, and mixing the polycarbonate L-1250Y and the light diffusion agent according to the weight ratio of 99.7: 0.3, mixing, performing melt extrusion granulation by a double-screw extruder to obtain the light diffusion polycarbonate material, testing the light transmittance and the haze and observing the covering effect, wherein the testing method comprises the following steps:
injection molding a photodiffusive polycarbonate material into a 2.0mm thick, 100 x 100 square plaque using an injection molding machine, and measuring light transmittance and haze according to ASTM D1003-61(1997) standard;
the light diffusion polycarbonate material is injection molded into a square plate with the thickness of 2.0mm and the thickness of 100 x 100 by adopting an injection molding machine, the square plate is simultaneously taken and visually checked at the position 5cm away from a 3W LED light source to compare the covering effect, the test result shows that the square plate has the covering effect, and the x represents the non-covering effect.
The test results are shown in the following table:
light transmittance% Haze%) Covering effect
Example 1 82 98 √
Example 2 80 96 √
Example 3 86 95 √
Example 4 84 97 √
Comparative example 1 83 73 ×
Comparative example 2 84 77 ×
Comparative example 3 86 53 ×
From the above table, it can be seen that the hollow silicone microspheres of the present invention, when applied to polycarbonate as a light diffusing agent, can achieve higher light diffusion efficiency, and can soften light and reduce light loss.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.

Claims (10)

1. A preparation method of hollow organic silicon microspheres is characterized by comprising the following steps: the method comprises the following steps:
(S1) mixing an organic functional silane coupling agent and a hydrogen-containing silane coupling agent at a certain temperature, adding an acidic regulator to regulate the pH value to be acidic, and hydrolyzing for a certain time under an acidic condition to obtain an active reactant;
(S2), adding silica sol and an alkaline catalyst into water at a certain temperature, uniformly mixing, adding the active reactant, mixing for 1-30min, standing, preserving heat, aging for a certain time, filtering and separating a product, and drying to obtain the hollow organic silicon microspheres.
2. The preparation method of hollow organosilicon microspheres according to claim 1, characterized in that: the organic functional silane coupling agent, the hydrogen-containing silane coupling agent, the acidity regulator, the water, the silica sol and the alkaline catalyst are respectively used in the amount of 1-50 parts, 20-99 parts, 20-100 parts, 20-80 parts, 1-20 parts and 0.2-10 parts by weight.
3. The preparation method of hollow organosilicon microspheres according to claim 1, characterized in that: in the step (S1), the temperature condition is 20-70 ℃; in the step (S2), the temperature condition is 20 to 70 ℃.
4. The preparation method of hollow organosilicon microspheres according to claim 1, characterized in that: in the step (S1), the hydrolysis time is 1-8 h; in the step (S2), the heat preservation and aging time is 24-48 h.
5. The preparation method of hollow organosilicon microspheres according to claim 1, characterized in that: the acidity regulator is an inorganic acid-water solution or a carboxylic acid-water solution.
6. The preparation method of hollow organosilicon microspheres according to claim 1, characterized in that: the chemical general formula of the organic functional silane coupling agent is (R)xSi(OR)yWherein x is an integer of 0 to 3, y is an integer of 1 to 4, and x + y is 4, R is an alkyl group having 1 to 6 carbon atoms, a vinyl group having 1 to 6 carbon atoms, an aryl group having 6 to 20 carbon atoms, or an alkyl-substituted aryl group having 6 to 20 carbon atoms.
7. The preparation method of hollow organosilicon microspheres according to claim 1, characterized in that: the chemical general formula of the hydrosilane coupling agent is H (R)nSi(OR)mWherein n is an integer of 0 to 2, m is an integer of 1 to 3, and n + m is 3, R is an alkyl group having 1 to 6 carbon atoms, a vinyl group having 1 to 6 carbon atoms, an aryl group having 6 to 20 carbon atoms, or an alkyl-substituted aryl group having 6 to 20 carbon atoms.
8. The preparation method of hollow organosilicon microspheres according to claim 1, characterized in that: the silica sol is acidic silica sol or alkaline silica sol; the alkaline catalyst is inorganic alkali.
9. A hollow organic silicon microsphere is characterized in that: the hollow organic silicon microsphere is prepared by the preparation method of the hollow organic silicon microsphere as claimed in any one of claims 1 to 8.
10. Use of hollow silicone microspheres according to claim 9 wherein: the hollow organic silicon microspheres are applied to a thermoplastic resin product and used as a light diffusion agent, wherein the thermoplastic resin comprises at least one of polyvinyl chloride resin, styrene resin, SAN resin, acrylic-styrene resin, polyester resin, ABS resin or polycarbonate resin.
CN202111471524.5A 2021-12-06 2021-12-06 Hollow organic silicon microsphere, preparation method and application thereof Withdrawn CN113980279A (en)

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