CN105131197B - A kind of preparation method of makrolon photodiffusion material - Google Patents
A kind of preparation method of makrolon photodiffusion material Download PDFInfo
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- CN105131197B CN105131197B CN201510628803.6A CN201510628803A CN105131197B CN 105131197 B CN105131197 B CN 105131197B CN 201510628803 A CN201510628803 A CN 201510628803A CN 105131197 B CN105131197 B CN 105131197B
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Abstract
The invention provides a kind of preparation method of makrolon photodiffusion material：In a kettle., a certain amount of dispersant, initiator are added, polycarbonate resin lipid microspheres, polycarbonate acrylic hexafluoro butyl ester, γ (methacryloxypropyl) propyl trimethoxy silicane (KH 570) carries out polymerisation, obtains modified makrolon microballoon.
Description
Technical field
The present invention relates to a kind of preparation method of light diffusing agent, particularly a kind of preparation side of makrolon photodiffusion material
Method.
Background technology
Photodiffusion material is used widely in illuminating industry especially field of LED illumination.Traditional photodiffusion material is main
By adding the inorganic or organic diffusion particle with different refractivity, including SiO in transparent plastic base-material2、TiO2、
CaCO3、BaSO4With the inorganic particles such as glass microballoon, and the organic polymer such as polymethyl methacrylate, polystyrene, silicones
Thing particulate, reaches the purpose for improving material mist degree, point, line source is converted into line, area source.
CN103951847 is related to a kind of light diffusing agent with blue light shielding action and preparation method.The light diffusing agent with
Silicon microballoon is core, a diameter of 30~50nm of its Surface coating oxide nano rare earth particle, and the particle diameter of wherein silicon microballoon is：1
~5 μm, the mass ratio of silicon microballoon and oxide nano rare earth is：1: 1~1: 10.Prepared by the present invention is nano rare earth oxidation
Thing is attached to the surface of silicon microballoon, and it is spherical that compound particle is remained intact, its light diffusing can compared with silicon microballoon indifference.
CN102634067 is related to a kind of light diffusing agent, light dispersion and preparation method thereof.The light dispersant is with silicon microballoon
The porous nano titanic oxide hollow microballoon for coating a diameter of 30-70nm for core, its table, wherein silicon microballoon and porous hollow is received
Rice titanium dioxide mass ratio be：4∶1-1∶1.The composition and weight/mass percentage composition of the light dispersion be：Makrolon 97-
99%；Light scattering agent 0.5-1.5%；Fire retardant 0.3~1.5%；The weight/mass percentage composition sum of above each component is 100%.
CN103193915 is related to a kind of light diffusing agent, PMMA light diffusing sheets and preparation method thereof.The light diffusing agent is benzene second
Its random polymers of alkene and methacryloxypropyl isobutyl group polyhedral oligomeric silsesquioxane (MAiBuPOSS).PMMA light expands
The composition and weight/mass percentage composition fallen apart be：Polymethyl methacrylate 97.0~99.5%, light diffusing agent 0.5~3.0%, with
The weight/mass percentage composition of upper each component is 100%.The refractive index of styrene content in light diffusing agent and MAiBuPOSS compositions with
PMMA refractive index is different, when light passes through material, and light can become light by repeatedly refraction finally by the light of base material
It is bright soft.
The light diffusing agent of existing known technology disperses bad in the base, there is agglomeration.Need to be surface-treated with
Guarantee is uniformly dispersed, to improve light dispersiveness.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of preparation method of makrolon photodiffusion material.
In a kettle., pure water is squeezed into, polymerization inhibitor adds a certain amount of dispersant, initiator, polycarbonate acrylic six
Fluorine butyl ester, γ-(methacryloxypropyl) propyl trimethoxy silicane (KH-570), is warming up to reaction temperature, question response terminates, from
The heart, is dried.Obtain product of the present invention.
The present invention provides a kind of preparation method of makrolon photodiffusion material, is realized by following steps：
The preparation of step 1. aqueous phase
By weight, 1000 parts of water are added in a kettle., and 0.5-2 parts of emulsifying agents (preferably 1 part) stir；
The preparation of step 2. oil phase
By weight, by 100 parts of makrolon powders, 0.5-3 parts of KH570 monomers, 0.5-3 parts of hexafluorobutyl acrylates
Mixing, adds 0.05-0.5 parts of initiators, stirs；
Step 3. polymerisation
The oil-phase solution prepared in step 2 is added in step 1 equipped with the reactor for having prepared aqueous phase, is passed through, then
From 70-100 DEG C (preferably 90 DEG C) reaction 8-20h (preferably 10h), reaction is centrifuged after terminating, and is dried to obtain product.
The chemical dispersant includes anion emulsifier, is ammonium lauryl sulfate, neopelex, 16
The chain alkyl types such as sodium alkyl benzene sulfonate, B-53, polyoxyethylene alkyl ether sodium sulphate and paraffin sulfonate are cloudy
Any one in ionic emulsifying agent, perfluoro caprylic acid sylvite or ammonium salt and the pungent sulfonate sodium of perfluor alkane or ammonium salt.It is preferred that 12
Alkylsurfuric acid ammonium.
The preferred potassium peroxydisulfate of initiator, dredges sour ammonium excessively.
The γ-(methacryloxypropyl) propyl trimethoxy silicane (KH-570), hexafluorobutyl acrylate, makrolon
Resin microsphere is commercially available prod.
Beneficial effects of the present invention：
Existing light diffusing agent disperses bad in the base, there is agglomeration.Need to be surface-treated to ensure to disperse
Uniformly, it is dispersed to improve light.The light diffusing particles being modified by surface aggregate are without the shortcomings of inequality, reunion is disperseed, thoroughly
Light rate is higher.
Embodiment
Following examples are only to further illustrate the present invention, are not limitation the scope of protection of the invention.
The present invention provides a kind of preparation method of makrolon photodiffusion material, is realized by following steps：
Embodiment 1
The preparation of step 1. aqueous phase
1000kg water is added in 2000L autoclaves, 1kg ammonium lauryl sulfates stir；
The preparation of step 2. oil phase
In 200L reactors, by 100kg makrolon (Japanese Supreme Being people, L-1250WP types, 100 mesh powders), 1kg propylene
Sour hexafluoro butyl ester, 1kg γ-(methacryloxypropyl) propyl trimethoxy silicane (KH-570), adds 0.08kg potassium peroxydisulfates
Initiator, stir：
Step 3. polymerisation
The oil-phase solution prepared in step 2 is added in step 1 equipped with the reactor for having prepared aqueous phase, then from 90 DEG C
14h is reacted, reaction is centrifuged after terminating, and is dried to obtain product.Numbering is SX-1.
Embodiment 2
The preparation of step 1. aqueous phase
1000kg water is added in 2000L autoclaves, 0.5kg ammonium lauryl sulfates stir；
The preparation of step 2. oil phase
In 200L reactors, by 100kg makrolon (Japanese Supreme Being people, L-1250WP types, 200 mesh powders), 0.5kg third
Olefin(e) acid hexafluoro butyl ester, 0.5kg γ-(methacryloxypropyl) propyl trimethoxy silicane (KH-570) monomer mixing, is added
0.05kg potassium peroxydisulfate initiators, stir；
Step 3. polymerisation
The oil-phase solution prepared in step 2 is added in step 1 equipped with the reactor for having prepared aqueous phase, then from 70 DEG C
20h is reacted, reaction is centrifuged after terminating, and is dried to obtain product.Numbering is SX-2.
Embodiment 3
The preparation of step 1. aqueous phase
1000kg water is added in 2000L autoclaves, 2kg cetyl benzenesulfonic acid sodiums stir；
The preparation of step 2. oil phase
In 200L reactors, by 100kg makrolon (Japanese Supreme Being people, L-1250WP types, 100 mesh powders), 32kg third
Olefin(e) acid hexafluoro butyl ester, 3kg γ-(methacryloxypropyl) propyl trimethoxy silicane (KH-570) monomer mixing, adds 0.5kg
Ammonium persulfate initiator, stir；
Step 3. polymerisation
The oil-phase solution prepared in step 2 is added in step 1 equipped with the reactor for having prepared aqueous phase, then from 100
DEG C reaction 10h, reaction terminate after centrifuge, be dried to obtain product.Numbering is SX-3.
Comparative example 1
It is one-component only with makrolon, production code member is SX-4.
Embodiment 4
Obtained 1 part of light diffusing particles in embodiment 1-3 and comparative example 1,0.3 part of antioxidant is divided in advance with diffusant
Dissipate, add after 100 parts of polymethyl methacrylate, be transferred in low speed mixer and stir, twin-screw extrusion is used after being well mixed
Machine melt blending, granulation, most afterwards through injection machine injection molding light diffusing sheet.
Optic test
Using light transmittance/mist degree tester (EEL57D, Shanghai precision instrument Co., Ltd), surveyed by GB/T2410-2008
Examination.
| Sample number into spectrum | Light transmittance % |
| SX-1 | 85 |
| SX-2 | 82 |
| SX-3 | 85 |
| SX-4 | 71 |
It can be seen that, because SX-4 is without surface treatment, disperses uneven in PC plate, cause light transmittance low.And pass through table
The light diffusing particles of face polymeric modification are then without the shortcomings of inequality, reunion is disperseed, and light transmittance is higher.
Claims (2)
1. a kind of preparation method of makrolon photodiffusion material, it is characterised in that comprise the following steps：
The preparation of step 1. aqueous phase
By weight, 1000 parts of water are added in a kettle., and 0.5-2 parts of emulsifying agents stir；
The preparation of step 2. oil phase
By weight, by 100 parts of makrolon powders, 0.5-3 parts of KH570 monomers, 0.5-3 parts of hexafluorobutyl acrylates are mixed
Close, add 0.05-0.5 parts of initiators, stir；
Step 3. polymerisation
The oil-phase solution prepared in step 2 is added in step 1 equipped with the reactor for having prepared aqueous phase, then from 70-100 DEG C
8-20h is reacted, reaction is centrifuged after terminating, and is dried to obtain product.
2. the preparation method according to claim 1, it is characterised in that KH570 monomers, acrylic acid hexafluoro are used in step 2
Butyl ester, surface aggregate is carried out to polycarbonate resin powder.
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| CN105504129B (en) * | 2015-12-18 | 2018-05-15 | 王金明 | A kind of preparation of polystyrene light diffusing agent |
| CN105461864A (en) * | 2015-12-18 | 2016-04-06 | 王金明 | Preparation of polycarbonate photodiffusion agent |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1898348A (en) * | 2003-12-23 | 2007-01-17 | 3M创新有限公司 | Aqueous composition of an oligomeric fluorosilane and use thereof for surface treatment of optical elements |
| CN103030752A (en) * | 2011-09-29 | 2013-04-10 | 比亚迪股份有限公司 | Polymer microsphere, preparation method and application of polymer microsphere, composition, light diffusion plate or light diffusion film, lamp and backlight module |
| CN103937267A (en) * | 2014-04-11 | 2014-07-23 | 东南大学 | Core-shell-type optical diffusion hybrid microsphere and preparation method thereof |
| CN104830025A (en) * | 2015-04-28 | 2015-08-12 | 中科院广州化学有限公司 | LED inorganic-organic hybrid composite encapsulation material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090202838A1 (en) * | 2008-02-13 | 2009-08-13 | Chun-Fa Chen | Self-assembling optical film and a method of manufacturing the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1898348A (en) * | 2003-12-23 | 2007-01-17 | 3M创新有限公司 | Aqueous composition of an oligomeric fluorosilane and use thereof for surface treatment of optical elements |
| CN103030752A (en) * | 2011-09-29 | 2013-04-10 | 比亚迪股份有限公司 | Polymer microsphere, preparation method and application of polymer microsphere, composition, light diffusion plate or light diffusion film, lamp and backlight module |
| CN103937267A (en) * | 2014-04-11 | 2014-07-23 | 东南大学 | Core-shell-type optical diffusion hybrid microsphere and preparation method thereof |
| CN104830025A (en) * | 2015-04-28 | 2015-08-12 | 中科院广州化学有限公司 | LED inorganic-organic hybrid composite encapsulation material and preparation method thereof |
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