CN111040173A - Preparation method and application of silicone rubber microsphere light diffusant - Google Patents
Preparation method and application of silicone rubber microsphere light diffusant Download PDFInfo
- Publication number
- CN111040173A CN111040173A CN201911364774.1A CN201911364774A CN111040173A CN 111040173 A CN111040173 A CN 111040173A CN 201911364774 A CN201911364774 A CN 201911364774A CN 111040173 A CN111040173 A CN 111040173A
- Authority
- CN
- China
- Prior art keywords
- mixture
- silicone oil
- weight ratio
- vinyl
- silicone rubber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to the technical field of polymer material photodiffusion, in particular to a preparation method and application of a silicone rubber microsphere photodiffusion agent, wherein a mixture consisting of vinyl silicone oil, mercaptopropyl silicone oil and a photoinitiator is dropwise added into a mixed solution of an emulsifier and water under stirring to form pre-emulsion; and (3) carrying out sulfydryl-alkene click chemical reaction on the pre-emulsion under the irradiation of ultraviolet light, and drying after separation to obtain the silicone rubber microsphere light diffusant. The invention has the advantages of high reaction speed, no need of heating, simple preparation steps, capability of obtaining the silicone rubber microsphere light diffusant with different particle sizes from 0.2 mu m to 50 mu m, and application in polycarbonate, polystyrene, polymethacrylate, polyester or LED.
Description
Technical Field
The invention relates to the technical field of polymer material photodiffusion, in particular to a preparation method and application of a silicone rubber microsphere photodiffusion agent.
Background
With the increasing optical demand of human, the lighting source becomes brighter and brighter, the problems of strong glare, uneven dispersion and the like become more and more obvious, and the light diffusant can well solve the problems. The light diffusion agent is a chemical auxiliary agent with light diffusion effect, is suitable for polycarbonate lampshades, polymethyl methacrylate lampshades, LEDs and the like, can uniformly refract and disperse strong light rays for many times, and can expand a point light source into a surface light source to enable the light to be very soft.
The light diffusing agent is generally of an inorganic material type and an organic material type, and is also specifically of an organic silicon type, and combines the advantages of the inorganic material and the organic material. The organic silicon type light diffusant comprises an organic silicon resin type and an organic silicon rubber type, and has the advantages of good temperature resistance, low addition amount and good light diffusion effect.
The patent of the invention with the publication number of CN106928476B discloses a preparation method of silicone rubber microspheres for light diffusant, which comprises the steps of uniformly mixing vinyl-terminated polydimethylsiloxane, simethicone, a mixed solvent, a crosslinking agent and a catalyst to obtain a silicone rubber solution, emulsifying in water, polymerizing to obtain a silicone rubber microsphere suspension, and separating and drying to obtain the silicone rubber microspheres. However, this method has the following disadvantages: (1) expensive noble metal catalysts need to be used, while the amount is not low. The method adopts emulsion polymerization, the polymerization temperature is generally not more than 80 ℃, in order to accelerate the reaction rate, more noble metal catalysts are required to be added, and the cost is increased; meanwhile, the noble metal catalyst is easy to be poisoned to cause the effect failure; (2) a long-time heating reaction is needed, so that the production efficiency is reduced; (3) the dimethyl silicone oil added into the raw material is difficult to volatilize, and can be separated out into a polymer base material when the light diffusant is used, so that the base material is polluted.
The sulfydryl-alkene click chemistry is a green chemical reaction, has the advantages of high reaction rate, high conversion rate, high product purity, no need of heating and the like, and has wide application in the fields of material modification, biological medicine and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a silicone rubber microsphere light diffusant.
Another purpose of the invention is to provide a silicone rubber microsphere light diffusant.
The invention also aims to provide application of the silicone rubber microsphere light diffusant.
The invention adopts the following technical scheme:
a preparation method of a silicone rubber microsphere light diffusant comprises the following steps,
s1, uniformly mixing the composite emulsifier and deionized water, dropwise adding a mixture consisting of vinyl silicone oil, mercaptopropyl silicone oil and benzoin dimethyl ether while stirring, and continuously stirring for 10-30 minutes after dropwise adding to obtain a pre-emulsion;
s2, stirring, and mixing the pre-emulsion obtained in the step S1 at a dominant wavelength of 365nm and a light intensity of 1-10mW/cm2Irradiating for 3-20 minutes under ultraviolet light, separating and drying to obtain the silicon rubber microspheres.
In the step S1, the stirring speed of the stirrer is controlled at 600rpm, 300rpm and 80-120 rpm.
The stirring speed of the stirrer during the ultraviolet irradiation in step S2 is 80-200 rpm.
Preferably, the complex emulsifier in step S1 comprises two emulsifiers, wherein one emulsifier is selected from one of the tween series of emulsifiers and the other emulsifier is selected from one of the span series of emulsifiers. The Tween series emulsifiers may be selected from Tween20, Tween40, Tween60 or Tween 80; the span series emulsifier can be selected from span20, span40, span60, span65, span80, or span 85. The HLB value of the compound emulsifier is 8.5-11.0, and the weight ratio of the tween series emulsifier to the span series emulsifier is 1:9-9: 1.
In a more preferred embodiment, the complex emulsifier is selected from the group consisting of a mixture of tween20 and span20 at a weight ratio of 1:5, a mixture of tween20 and span40 at a weight ratio of 1:3, a mixture of tween20 and span60 at a weight ratio of 1:1.5, a mixture of tween20 and span80 at a weight ratio of 1:1.3, a mixture of tween20 and span65 at a weight ratio of 1:1, a mixture of tween 65 and span65 at a weight ratio of 1.2:1, a mixture of tween 65 and span65 at a weight ratio of 1:4.4, a mixture of tween 65 and span65 at a weight ratio of 1:2.8, a mixture of tween 65 and span65 at a weight ratio of 1:1.5, a mixture of tween 65 and span65 at a weight ratio of 1: 2.72, a mixture of tween 65 and a mixture of 65 at a weight ratio of 65, a mixture of 65 and span65 at a weight ratio of 1:3, a mixture of 65 and a mixture of 65 at a weight ratio of 65, a mixture of 65 and a mixture of 65 at a weight ratio of 361: 1:3, a mixture of 65 and a mixture of 65 at a weight ratio of 65, a mixture of 65 at a weight ratio of 65 and a mixture of 65 at a weight ratio, A mixture of tween60 and span80 at a weight ratio of 1.1:1, a mixture of tween60 and span65 at a weight ratio of 1.3:1, a mixture of tween60 and span85 at a weight ratio of 1.4:1, a mixture of tween80 and span20 at a weight ratio of 1:4, a mixture of tween80 and span40 at a weight ratio of 1:2.5, a mixture of tween80 and span60 at a weight ratio of 1:1.2, a mixture of tween80 and span80 at a weight ratio of 1:1, a mixture of tween80 and span65 at a weight ratio of 1.3:1 or a mixture of tween80 and span20 at a weight ratio of 1.4: 1.
Preferably, the weight ratio of the composite emulsifier to the deionized water in the step S1 is 1:20-5: 10. More preferably, the weight ratio of the composite emulsifier to the deionized water is 1:10-3: 10.
Preferably, the weight ratio of the deionized water to the mixture in the step S1 is 10: 1-10. More preferably, the weight ratio of deionized water to the mixture is 10: 3-8.
Preferably, the viscosity (25 ℃) of the vinyl silicone oil in the step S1 is 100-2000 mPas, the mass percentage content of the vinyl is 0.05-5%, the chemical structural formula is shown as (I),
wherein R is1And R2Independently selected from methyl or vinyl, n and m are both positive numbers. The viscosity and the mass percentage content of the vinyl silicone oil determine the specific values of n and m in the chemical structural formula (I).
More preferably, the vinyl silicone oil has a viscosity (25 ℃) of 200-1400 mPas. In a further preferred embodiment, the vinyl silicone oil may have a viscosity (25 ℃) of 250 mPas, 400 mPas, 500 mPas, 700 mPas, 900 mPas, 1000 mPas, 1100 mPas or 1250 mPas.
More preferably, the vinyl silicone oil contains 0.2 to 3 mass percent of vinyl. In a more preferred embodiment, the vinyl silicone oil may contain 0.25%, 0.4%, 0.5%, 0.65%, 0.8%, 1.0%, 1.2%, 1.5%, 1.7%, or 1.9% by mass of vinyl groups.
Preferably, the viscosity (25 ℃) of the mercaptopropyl silicone oil in the step S1 is 50-3000 mPa.s, the mass percentage content of the mercapto group is 0.2-3%, the chemical structural formula is shown as the formula (II),
wherein R is3And R4Independently selected from methyl or 3-mercaptopropyl, x and y are both positive numbers. The viscosity and the mass percentage of sulfydryl of the mercaptopropyl silicone oil determine the specific values of x and y in the chemical structural formula (II).
More preferably, the mercaptopropyl silicone oil has a viscosity (25 ℃) of 150-2000 mPas. In a more preferred embodiment, the mercaptopropyl silicone oil has a viscosity (at 25 ℃) of 200 mPas, 350 mPas, 500 mPas, 700 mPas, 900 mPas, 1050 mPas, 1200 mPas, 1400 mPas, 1500 mPas, 1700 mPas or 1800 mPas.
More preferably, the mass percentage of the mercapto in the mercaptopropyl silicone oil is 0.5-2.5%. In a further preferred embodiment, the mercaptopropyl silicone oil may have a mercapto group content of 0.5%, 0.7%, 0.85%, 0.9%, 1.0%, 1.3%, 1.5%, 1.8%, 2.0%, or 2.2% by mass.
Preferably, the ratio of the mole number of vinyl groups in the vinyl silicone oil to the mole number of mercapto groups in the mercaptopropyl silicone oil in step S1 is 1: 0.7-2. More preferably, the ratio of the number of moles of vinyl groups in the vinyl silicone oil to the number of moles of mercapto groups in the mercaptopropyl silicone oil is 1:0.8 to 1.8, and further preferably, the ratio may be 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, or 1.5.
Preferably, the weight of benzoin dimethyl ether in step S1 is 2-5% of the weight of the mixture.
A silicone rubber microsphere light diffusant prepared by the preparation method of any one of the embodiments.
The application of the silicone rubber microsphere light diffusant in the embodiment in polycarbonate, polystyrene, polymethacrylate, polyester or LED.
The pre-emulsion of the invention can also be prepared as follows: uniformly mixing vinyl silicone oil, mercaptopropyl silicone oil and benzoin dimethyl ether, adding the composite emulsifier, continuously stirring for 5-10 minutes, increasing the stirring speed to 1500-4000rpm, dropwise adding deionized water, reducing the stirring speed to 80-150rpm after the deionized water is added, and stirring for 20-30 minutes to obtain the pre-emulsion.
The invention has the beneficial effects that: (1) the method does not need to use expensive noble metal catalysts like hydrosilylation reaction (the cost of the hydrosilylation catalyst is calculated by Pt, each 1ppm is added by about 0.5-1 yuan, the addition amount is generally 5-100ppm, the lower the reaction temperature is, the larger the addition amount of the catalyst is, the higher the cost is, the reaction temperature is about 130 ℃, the addition amount of the hydrosilylation catalyst (calculated by Pt) is generally 5-10ppm, the reaction temperature is about 50 ℃, the addition amount of the hydrosilylation catalyst (calculated by Pt) is generally 100ppm or more, the cost of the single catalyst is 50-100 yuan/Kg, and the cost is reduced; (2) heating is not needed, the requirement on production equipment is reduced, and meanwhile, the safety is improved; (3) the reaction time is short and is one sixth to one tenth of the hydrosilylation reaction time, so that the production efficiency is improved; (4) the silicone rubber microspheres with different particle diameters can be obtained by controlling different weight proportions of the composite emulsifier, water and silicone oil (mixture of vinyl silicone oil and mercaptopropyl silicone oil).
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Unless otherwise specified, the parts in the following embodiments are parts by weight.
Detailed description of the preferred embodiments
A preparation method of a silicone rubber microsphere light diffusant comprises the following steps: uniformly mixing the composite emulsifier and deionized water, dropwise adding a mixture of vinyl silicone oil, mercaptopropyl silicone oil and benzoin dimethyl ether while stirring, and continuously stirring for 10-30 minutes after dropwise adding to obtain a pre-emulsion; stirring, and adding the pre-emulsion at dominant wavelength of 365nm and light intensity of 1-10mW/cm2Irradiating for 3-20 minutes under ultraviolet light, separating and drying,obtaining the silicon rubber microsphere light diffusant.
The composite emulsifier is selected from a mixture consisting of tween20 and span20 in a weight ratio of 1:5, a mixture consisting of tween20 and span40 in a weight ratio of 1:3, a mixture consisting of tween20 and span60 in a weight ratio of 1:1.5, a mixture consisting of tween20 and span80 in a weight ratio of 1:1.3, a mixture consisting of tween20 and span65 in a weight ratio of 1:1, a mixture consisting of tween 65 and span65 in a weight ratio of 1.2:1, a mixture consisting of tween 65 and span65 in a weight ratio of 1:4.4, a mixture consisting of tween 65 and span 72 in a weight ratio of 1:2.8, a mixture consisting of tween 65 and span65 in a weight ratio of 1:1.5, a mixture consisting of tween 65 and span65 in a weight ratio of 1:5, a mixture consisting of tween 65 and a mixture consisting of 70.72 in a weight ratio of 1: 72, a mixture consisting of tween 65 and a mixture consisting of 65 in a weight ratio of 1:3, a mixture consisting of tween 65 and a mixture consisting of 65 in a weight ratio of 65, a mixture consisting of 65 in a weight ratio of 1:3, a mixture consisting of 65 and a mixture consisting of 65 in a weight ratio of 65 and a mixture of 65 in a weight ratio of 65, a mixture, A mixture of tween60 and span80 at a weight ratio of 1.1:1, a mixture of tween60 and span65 at a weight ratio of 1.3:1, a mixture of tween60 and span85 at a weight ratio of 1.4:1, a mixture of tween80 and span20 at a weight ratio of 1:4, a mixture of tween80 and span40 at a weight ratio of 1:2.5, a mixture of tween80 and span60 at a weight ratio of 1:1.2, a mixture of tween80 and span80 at a weight ratio of 1:1, a mixture of tween80 and span65 at a weight ratio of 1.3:1 or a mixture of tween80 and span20 at a weight ratio of 1.4: 1.
The weight ratio of the composite emulsifier to the deionized water is 1:20-5: 10; the weight ratio of the deionized water to the mixture is 10: 1-10; the viscosity (25 ℃) of the vinyl silicone oil is 100-2000 mPas, and the mass percentage of the vinyl is 0.05-5%; the viscosity (25 ℃) of the mercaptopropyl silicone oil is 50-3000 mPa.s, and the mass percentage content of the mercapto group is 0.2-3%; the ratio of the mol number of vinyl in the vinyl silicone oil to the mol number of sulfydryl in the mercaptopropyl silicone oil is 1: 0.7-2; the weight of benzoin dimethyl ether is 2-5% of the weight of the mixture.
Example 1
100 parts of vinyl silicone oil having a vinyl content of 0.25% by mass and a viscosity (25 ℃) of 250 mPas, 49 parts of mercaptopropyl silicone oil having a mercapto content of 0.5% by mass and a viscosity (25 ℃) of 1700 mPas, and 3.2 parts of benzoin dimethyl ether were combined to prepare a mixture 1.
Uniformly mixing 10 parts of tween20 and span60, namely, 100 parts of deionized water, according to a weight ratio of 1:1.5, dropwise adding 35 parts of the mixture 1 while stirring at a rotating speed of 600rpm, and continuously stirring for 10 minutes at a rotating speed of 300rpm after dropwise adding to obtain a pre-emulsion 1; stirring at 150rpm, and mixing the pre-emulsion 1 at dominant wavelength of 365nm and light intensity of 5mW/cm2Irradiating for 15 minutes under ultraviolet light, separating and drying to obtain the silicon rubber microsphere light diffusant 1. The D50, D90 and D10 of the silicone rubber microsphere light diffusant 1 are measured to be 4.5 microns, 7.0 microns and 1.3 microns by a laser particle size analyzer.
Example 2
100 parts of vinyl silicone oil having a vinyl content of 0.4% by mass and a viscosity (25 ℃ C.) of 400 mPas, 70 parts of mercaptopropyl silicone oil having a mercapto content of 0.7% by mass and a viscosity (25 ℃ C.) of 1200 mPas, and 7 parts of benzoin dimethyl ether were combined to form a mixture 2.
Uniformly mixing 10 parts of tween40 and span80, namely, a composite emulsifier consisting of 1:1 parts by weight and 60 parts of deionized water, dropwise adding 12 parts of the mixture 2 while stirring at the rotation speed of 600rpm, and continuously stirring for 12 minutes at the rotation speed of 250rpm after the dropwise adding is finished to obtain a pre-emulsion 2; stirring at 120rpm, and mixing the pre-emulsion 2 at dominant wavelength of 365nm and light intensity of 3mW/cm2Irradiating for 12 minutes under ultraviolet light, separating and drying to obtain the silicon rubber microsphere light diffusant 2. The D50, D90 and D10 of the silicone rubber microsphere light diffusant 2 were measured to be 2.1 μm, 5.6 μm and 0.9 μm by a laser particle size analyzer.
Example 3
100 parts of vinyl silicone oil having a vinyl content of 0.65% by mass and a viscosity (25 ℃) of 1000 mPas, 80 parts of mercaptopropyl silicone oil having a mercapto content of 1.0% by mass and a viscosity (25 ℃) of 500 mPas, and 6.5 parts of benzoin dimethyl ether were combined to prepare a mixture 3.
Uniformly mixing 10 parts of tween80 and span65, namely, a composite emulsifier consisting of 80 parts of deionized water and 1.3:1 in weight ratio, dropwise adding 32 parts of the mixture 3 while stirring at the rotation speed of 650rpm, and continuously stirring for 15 minutes at the rotation speed of 200rpm after dropwise adding to obtain a pre-emulsion 3; stirring at 120rpm to obtain pre-emulsion 3 with dominant wavelength of 365nmLight intensity of 1mW/cm2Irradiating for 17 minutes under ultraviolet light, separating and drying to obtain the silicon rubber microsphere light diffusant 3. The D50, D90 and D10 of the silicone rubber microsphere light diffusant 3 were measured to be 6.2 μm, 8.9 μm and 2.5 μm by a laser particle size analyzer.
Example 4
100 parts of vinyl silicone oil having a vinyl content of 0.8% by mass and a viscosity (25 ℃ C.) of 1250 mPas, 138 parts of mercaptopropyl silicone oil having a mercapto content of 0.85% by mass and a viscosity (25 ℃ C.) of 200 mPas, and 10 parts of benzoin dimethyl ether were combined to form a mixture 4.
Uniformly mixing 10 parts of tween80 and span60, namely, a composite emulsifier consisting of 130 parts of deionized water and 130 parts of deionized water according to a weight ratio of 1:1.2, dropwise adding 70 parts of mixture 4 while stirring at a rotating speed of 650rpm, and continuously stirring for 25 minutes at a rotating speed of 200rpm after dropwise adding to obtain a pre-emulsion 4; stirring at 150rpm, and mixing the pre-emulsion 4 at dominant wavelength of 365nm and light intensity of 5mW/cm2Irradiating for 20 minutes under ultraviolet light, separating and drying to obtain the silicon rubber microsphere light diffusant 4. The D50, D90 and D10 of the silicone rubber microsphere light diffusant 4 were measured to be 8.4 μm, 11.3 μm and 3.7 μm by a laser particle size analyzer.
Example 5
100 parts of vinyl silicone oil having a vinyl content of 0.8% by mass and a viscosity (25 ℃) of 1250 mPas, 140 parts of mercaptopropyl silicone oil having a mercapto content of 0.7% by mass and a viscosity (25 ℃) of 1200 mPas, and 10 parts of benzoin dimethyl ether were combined to form a mixture 5.
Uniformly mixing 10 parts of tween80 and span60, namely, a composite emulsifier consisting of 160 parts of deionized water according to a weight ratio of 1:1.2, dropwise adding 40 parts of the mixture 5 while stirring at a rotation speed of 650rpm, and continuously stirring for 20 minutes at a rotation speed of 200rpm after dropwise adding to obtain a pre-emulsion 5; stirring at 120rpm, and allowing the pre-emulsion 5 to stand at a dominant wavelength of 365nm and a light intensity of 5mW/cm2Irradiating for 20 minutes under ultraviolet light, separating and drying to obtain the silicon rubber microsphere light diffusant 5. The D50, D90 and D10 of the silicone rubber microsphere light diffusant 5 were measured to be 6.6 μm, 8.2 μm and 2.7 μm by a laser particle size analyzer.
Example 6
100 parts of vinyl silicone oil having a vinyl content of 0.8% by mass and a viscosity (25 ℃) of 1250 mPas, 140 parts of mercaptopropyl silicone oil having a mercapto content of 0.7% by mass and a viscosity (25 ℃) of 1200 mPas, and 10 parts of benzoin dimethyl ether were combined to form a mixture 6.
And adding 10 parts of tween80 and span60 into 30 parts of the mixture 6, stirring at the rotating speed of 300rpm for 5-10 minutes, increasing the stirring rotating speed to 2500rpm, dropwise adding 90 parts of deionized water, reducing the stirring rotating speed to 150rpm, and stirring for 30 minutes to obtain the pre-emulsion 6, wherein the weight ratio of the tween80 to the span60 is 1: 1.2. Stirring at 120rpm, and mixing the pre-emulsion 6 at dominant wavelength of 365nm and light intensity of 5mW/cm2Irradiating for 20 minutes under ultraviolet light, separating and drying to obtain the silicon rubber microsphere light diffusant 6. The D50, D90 and D10 of the silicone rubber microsphere light diffusant 6 were measured to be 0.3 μm, 0.5 μm and 0.09 μm by a laser particle size analyzer.
Application testing
0.2 part, 0.4 part and 0.6 part of the silicone rubber microsphere light diffusant 1-6 of examples 1-6 are respectively added into 100 parts of polycarbonate, and after mixing and melt extrusion under other process conditions, the mixture is molded into a sheet with the thickness of 2mm according to a conventional process in the field, and the haze and the light transmittance are respectively measured, and the results are shown in table 1.
TABLE 1
As can be seen from the data in Table 1, the light diffusion performance of the polycarbonate can be effectively improved by adding 0.2-0.6 part (per 100 parts of polycarbonate) of the silicone rubber microsphere light diffusion agent.
The invention provides a preparation method of a silicone rubber microsphere light diffusant, which has the characteristics of low cost, short reaction time, mild reaction conditions and the like, and the obtained silicone rubber microsphere light diffusant can be added into a polymer to improve the light diffusant performance of the polymer.
The foregoing has shown and described the fundamental principles, major features and advantages of the invention. It should be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, which are merely preferred embodiments of the present invention, and the scope of the present invention should not be limited thereby, and that equivalent changes and modifications made within the scope of the present invention and the specification should be covered thereby. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A preparation method of a silicone rubber microsphere light diffusant is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
s1, uniformly mixing the composite emulsifier and deionized water, dropwise adding a mixture consisting of vinyl silicone oil, mercaptopropyl silicone oil and benzoin dimethyl ether while stirring, and continuously stirring for 10-30 minutes after dropwise adding to obtain a pre-emulsion;
s2, stirring, and mixing the pre-emulsion obtained in the step S1 at a dominant wavelength of 365nm and a light intensity of 1-10mW/cm2Irradiating for 3-20 minutes under ultraviolet light, separating and drying to obtain the silicon rubber microsphere light diffusant.
2. The method of claim 1, wherein: the compound emulsifier in the step S1 comprises two emulsifiers, wherein one emulsifier is selected from one of tween series emulsifiers, and the other emulsifier is selected from one of span series emulsifiers.
3. The method of claim 1, wherein: the weight ratio of the composite emulsifier to the deionized water in the step S1 is 1:20-5: 10.
4. The method of claim 1, wherein: the weight ratio of the deionized water to the mixture in the step S1 is 10: 1-10.
5. The method of claim 1, wherein: in the step S1, the viscosity (25 ℃) of the vinyl silicone oil is 100-2000 mPas, the mass percentage of the vinyl is 0.05-5%, the chemical structural formula is shown as (I),
wherein R is1And R2Independently selected from methyl or vinyl, n and m are both positive numbers.
6. The method of claim 1, wherein: in the step S1, the viscosity (25 ℃) of the mercaptopropyl silicone oil is 50-3000 mPa.s, the mass percentage content of the mercapto group is 0.2-3%, the chemical structural formula is shown as (II),
wherein R is3And R4Independently selected from methyl or 3-mercaptopropyl, x and y are both positive numbers.
7. The method of claim 1, wherein: the ratio of the mole number of the vinyl groups in the vinyl silicone oil to the mole number of the mercapto groups in the mercaptopropyl silicone oil in the step S1 is 1: 0.7-2.
8. The method of claim 1, wherein: the weight of the benzoin dimethyl ether in the step S1 is 2-5% of the weight of the mixture.
9. A silicone rubber microsphere light diffusant prepared by the preparation method of any one of claims 1 to 8.
10. Use of the silicone rubber microsphere light diffuser of claim 9 in polycarbonate, polystyrene, polymethacrylate, polyester or LED.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911364774.1A CN111040173A (en) | 2019-12-26 | 2019-12-26 | Preparation method and application of silicone rubber microsphere light diffusant |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911364774.1A CN111040173A (en) | 2019-12-26 | 2019-12-26 | Preparation method and application of silicone rubber microsphere light diffusant |
Publications (1)
Publication Number | Publication Date |
---|---|
CN111040173A true CN111040173A (en) | 2020-04-21 |
Family
ID=70240176
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201911364774.1A Pending CN111040173A (en) | 2019-12-26 | 2019-12-26 | Preparation method and application of silicone rubber microsphere light diffusant |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111040173A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112731573A (en) * | 2020-12-30 | 2021-04-30 | 宁波长阳科技股份有限公司 | Diffusion film and preparation method thereof, backlight module and display device |
CN116462948A (en) * | 2023-03-16 | 2023-07-21 | 广东壹诺科技股份有限公司 | Glass fiber reinforced plastic diffusion plate for lighting of factory buildings in high-temperature areas and preparation method thereof |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20040120910A1 (en) * | 2002-04-10 | 2004-06-24 | Dyke Mark Van | Methods for producing, films comprising, and methods for using heterogeneous crosslinked protein networks |
CN102134383A (en) * | 2011-01-28 | 2011-07-27 | 暨南大学 | Light scattering polycarbonate composition for light emitting diode (LED) lighting and use thereof |
CN102321355A (en) * | 2011-07-07 | 2012-01-18 | 苏州奥美材料科技有限公司 | Method for manufacturing light diffusion polycarbonate sheet materials with adjustable light transmittance |
CN102417708A (en) * | 2011-11-23 | 2012-04-18 | 金发科技股份有限公司 | Halogen-free flame-retardant polycarbonate composition of light-emitting diode (LED) lamp shade and its preparation method and use |
CN102604100A (en) * | 2012-01-19 | 2012-07-25 | 华南理工大学 | Preparation method of monodispersity micron-sized polysilicon microspheres |
CN102786690A (en) * | 2012-06-13 | 2012-11-21 | 华南理工大学 | Light scattering microsphere containing benzoate polysilsesquioxane, and preparation method and application thereof |
CN103122070A (en) * | 2011-10-14 | 2013-05-29 | 信越化学工业株式会社 | Silicone fine particles and production method thereof |
CN106188582A (en) * | 2016-08-12 | 2016-12-07 | 四川大学 | Surface has the preparation method of the polydimethylsiloxane microsphere of pleated structure |
CN108359106A (en) * | 2018-03-26 | 2018-08-03 | 浙江新安化工集团股份有限公司 | A kind of preparation method of silicones microballoon lotion |
-
2019
- 2019-12-26 CN CN201911364774.1A patent/CN111040173A/en active Pending
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20040120910A1 (en) * | 2002-04-10 | 2004-06-24 | Dyke Mark Van | Methods for producing, films comprising, and methods for using heterogeneous crosslinked protein networks |
CN102134383A (en) * | 2011-01-28 | 2011-07-27 | 暨南大学 | Light scattering polycarbonate composition for light emitting diode (LED) lighting and use thereof |
CN102321355A (en) * | 2011-07-07 | 2012-01-18 | 苏州奥美材料科技有限公司 | Method for manufacturing light diffusion polycarbonate sheet materials with adjustable light transmittance |
CN103122070A (en) * | 2011-10-14 | 2013-05-29 | 信越化学工业株式会社 | Silicone fine particles and production method thereof |
CN102417708A (en) * | 2011-11-23 | 2012-04-18 | 金发科技股份有限公司 | Halogen-free flame-retardant polycarbonate composition of light-emitting diode (LED) lamp shade and its preparation method and use |
CN102604100A (en) * | 2012-01-19 | 2012-07-25 | 华南理工大学 | Preparation method of monodispersity micron-sized polysilicon microspheres |
CN102786690A (en) * | 2012-06-13 | 2012-11-21 | 华南理工大学 | Light scattering microsphere containing benzoate polysilsesquioxane, and preparation method and application thereof |
CN106188582A (en) * | 2016-08-12 | 2016-12-07 | 四川大学 | Surface has the preparation method of the polydimethylsiloxane microsphere of pleated structure |
CN108359106A (en) * | 2018-03-26 | 2018-08-03 | 浙江新安化工集团股份有限公司 | A kind of preparation method of silicones microballoon lotion |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112731573A (en) * | 2020-12-30 | 2021-04-30 | 宁波长阳科技股份有限公司 | Diffusion film and preparation method thereof, backlight module and display device |
CN112731573B (en) * | 2020-12-30 | 2022-08-05 | 宁波长阳科技股份有限公司 | Diffusion film and preparation method thereof, backlight module and display device |
CN116462948A (en) * | 2023-03-16 | 2023-07-21 | 广东壹诺科技股份有限公司 | Glass fiber reinforced plastic diffusion plate for lighting of factory buildings in high-temperature areas and preparation method thereof |
CN116462948B (en) * | 2023-03-16 | 2023-12-22 | 广东壹诺科技股份有限公司 | Glass fiber reinforced plastic diffusion plate for lighting of factory buildings in high-temperature areas and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101608068B (en) | Organ silicon material for encapsulating power-type LED and synthetic method thereof | |
CN110055027B (en) | Middle-folding refractive index LED packaging silicone rubber material and preparation method thereof | |
CN111040173A (en) | Preparation method and application of silicone rubber microsphere light diffusant | |
CN103467962A (en) | Photodiffusion film and preparation method thereof | |
TW200946583A (en) | Light-scattering compositions | |
CN106674852A (en) | Blue-ray-proof lens and resin raw material thereof | |
TW201704337A (en) | Resin Composition Having Improved Haze and Light Transmittance and Process for Preparing the Same | |
CN102656705A (en) | Fluorescent material for converting wavelengths, resin composition for converting wavelengths , solar cell module, process for producing resin composition for converting wavelengths, and process for producing solar cell module | |
CN102504733A (en) | Water-blush-resistant fluoride and siloxane modified waterborne pressure-sensitive adhesive and polyethylene protective film | |
CN108641031B (en) | Hindered phenol/styrene-acrylic composite emulsion and preparation method thereof | |
CN108276750B (en) | Light diffusion master batch, PET film and preparation method | |
CN114889268A (en) | Quantum dot light diffusion plate and preparation method and application thereof | |
CN103193914A (en) | Optical diffusion agent for acrylic optical diffusion board and preparation method of optical diffusion board | |
CN103936935A (en) | Method for preparing polymethylsilsesquioxane light scattering microspheres | |
CN113789133A (en) | Double-layer antistatic acrylic protective film and preparation method thereof | |
CN114854312B (en) | Ultraviolet light curing adhesive with high temperature resistance and preparation method thereof | |
CN108646327B (en) | Water-based quantum dot microcrystalline diffusion plate and preparation method thereof | |
CN1244602C (en) | High performance silicon emulsion and its preparation | |
CN103044887A (en) | PC composite material, as well as preparation method and application thereof | |
CN114058169B (en) | Light diffusing agent and preparation method and application thereof | |
CN112029259B (en) | Dynamic vulcanized organic silicon photodiffusion master batch and preparation method thereof | |
CN109265595A (en) | A kind of porous crosslinked polystyrene light diffusing agent and PC light diffusing sheet and preparation method thereof | |
TW201538576A (en) | Polysiloxane core-shell microspheres and preparation method thereof | |
CN110372901B (en) | High-haze polyimide film and preparation method thereof | |
CN1597720A (en) | Fine emulsion polymerization method of polyurethane acrylic ester compound emulsion |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |