CN105254823B - A kind of organosilicon light spreads the preparation method of microballoon - Google Patents
A kind of organosilicon light spreads the preparation method of microballoon Download PDFInfo
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- CN105254823B CN105254823B CN201510628804.0A CN201510628804A CN105254823B CN 105254823 B CN105254823 B CN 105254823B CN 201510628804 A CN201510628804 A CN 201510628804A CN 105254823 B CN105254823 B CN 105254823B
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Abstract
The invention provides the preparation method that a kind of organosilicon light spreads microballoon：In a kettle., a certain amount of dispersant is added, initiator, organic siliconresin microballoon, perfluorobutyl ethylene, 4 vinylpyridines carry out polymerisation, obtain modified organic siliconresin microballoon.
Description
Technical field
The present invention relates to a kind of preparation method of light diffusing agent, particularly a kind of organosilicon light spreads the preparation side of microballoon
Method.
Background technology
Photodiffusion material refers to the optical material with certain light transmittance and mist degree, can be converted into spot light and line source
Line source and area source, reaching makes the effect of incident beam optical power detection, is widely used in FPD, illuminating engineering,
Laser, the technical field such as projection imaging.Nowadays, with the maturation of high power LED chip manufacturing technology, and its in vapour
The fields such as licence is bright, signal lamp, outdoor display screen and indoor and outdoor lighting are used widely, the need of LED light diffusion particle
The amount of asking increases sharply.
CN101849201 can assign the light diffusing and light transmission better than existing spherical resin particle there is provided a kind of
Property, improve the light diffusing agent of the performance of final products such as screen.The light diffusing agent of the present invention, which is included in surface, has multiple pits
Spherical resin particle, the transparency, optics physical property are excellent, so using the optical diffusion film of the light diffusing agent there is excellent light to expand
Dissipate property and total light transmission.So being to expand even in some position it was observed that also evenly meeting good light in the case of scattered light
The optical diffusion film of property and total light transmission is dissipated, the backlight of liquid crystal display, rear projection screen, ligthing paraphernalia, lamp decoration is can be widely applied for
Billboard etc..
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
The random copolymer 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 organosilicon light diffusion microballoon and preparation method thereof.
In a kettle., pure water is squeezed into, polymerization inhibitor adds a certain amount of dispersant, initiator, organic siliconresin microballoon,
Perfluorobutyl ethylene, 4-vinylpridine is warming up to reaction temperature, and question response terminates, and centrifuges, and dries.Obtain surface aggregate
Organic siliconresin microballoon, that is, obtain product of the present invention.
The present invention provides a kind of organosilicon light diffusion microballoon, is realized by following steps：
The preparation of step 1. aqueous phase
By weight, 1000 parts of water are added in a kettle., and 0.5-4 parts of emulsifying agents (preferably 2 parts) stir；
The preparation of step 2. oil phase
By weight, by 100 parts of organic siliconresin microballoons, 0.5-5 parts of (preferably 3 parts) 4-vinylpridine monomers are mixed
Close, add 0.05-0.1 parts of initiators (preferably 0.2 part), stir；
Step 3. suspension polymerization
The oil-phase solution prepared in step 2 is added in step 1 equipped with the autoclave for having prepared aqueous phase, is passed through
0.5-5 parts of (preferably 2 parts) perfluorobutyl ethylenes, then from 70-100 DEG C (preferably 90 DEG C) reaction 8-20h (preferably 10h), reaction
Centrifuged after end, be 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 dioxane
Base sodium succinate.
The preferred potassium peroxydisulfate of initiator, ammonium persulfate.The perfluorobutyl ethylene is commercially available prod, and such as Wuhan match is fertile
The product of your Chemical Co., Ltd.'s production.The 4-vinylpridine is commercially available prod, and such as Suzhou City four is limited with medical sci-tech
The product of company's production.The organic siliconresin microballoon is commercially available prod, and such as Dongguan City three closes having for Chemical Co., Ltd.'s production
Machine silicones microspheres product.
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 light diffusion microballoon, is realized by following steps：
Embodiment 1
The preparation of step 1. aqueous phase
1000kg water is added in 2000L autoclaves, 4kg B-53s stir；
The preparation of step 2. oil phase
In 200L reactors, by 100kgTM520 type organic siliconresin microballoons, the mixing of 5kg4- vinylpyridines, then add
Enter 0.2kg potassium peroxydisulfate initiators, stir；
Step 3. suspension polymerization
The oil-phase solution prepared in step 2 is added in step 1 equipped with the reactor for having prepared aqueous phase, 2kg is passed through complete
Fluorine butylethylene gas, then from 90 DEG C of reaction 14h, 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 TM540 type organic siliconresin microballoons, 0.5kg4- vinylpyridine monomers are mixed
Close, add 0.05kg potassium peroxydisulfate initiators, stir：
Step 3. suspension polymerization
The oil-phase solution prepared in step 2 beaker is added in step 1 equipped with the reactor for having prepared aqueous phase, is passed through
0.5kg perfluorobutyl ethylene gases, then from 70 DEG C of reaction 20h, reaction is centrifuged after terminating, and is dried to obtain product.Numbering is SX-
2。
Embodiment 3
The preparation of few rapid 1. aqueous phase
1000kg water is added in 2000L autoclaves, 4kg cetyl benzenesulfonic acid sodiums stir；
The preparation of step 2. oil phase
In 200L reactors, by 100kg TM580 type organic siliconresin microballoons, 5kg4- vinylpyridine monomers are mixed,
Add 0.1kg ammonium persulfate initiators, stir；
Step 3. suspension polymerization
The oil-phase solution prepared in step 2 is added in step 1 equipped with the reactor for having prepared aqueous phase, 5kg is passed through complete
Fluorine butylethylene gas, then from 100 DEG C of reaction 8h, reaction is centrifuged after terminating, and is dried to obtain product.Numbering is SX-3.
Comparative example 1
Organic siliconresin microballoon powder is without grafting, and 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 PC particles, be transferred in low speed mixer and stir, after being well mixed with double screw extruder 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 | 86 |
| SX-2 | 84 |
| SX-3 | 89 |
| SX-4 | 76 |
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 organosilicon light spreads the preparation method of microballoon, 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 0.5-4 parts of emulsifying agents stir；
The preparation of step 2. oil phase
By weight, by 100 parts of organic siliconresin microballoons, 0.5-5 parts of 4-vinylpridine monomer mixing add 0.05-
0.1 part of initiator, stir；
Step 3. suspension polymerization
The oil-phase solution prepared in step 2 is added in step 1 equipped with the autoclave for having prepared aqueous phase, 0.5-5 is passed through
Part perfluorobutyl ethylene, then from 70-100 DEG C of reaction 8-20h, reaction is centrifuged after terminating, and is dried to obtain product.
2. preparation method according to claim 1, it is characterised in that perfluorobutyl ethylene, 4- vinyl are used in step 2
Pyridine monomer, surface aggregate is carried out to organic siliconresin microballoon.
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| CN201510628804.0A CN105254823B (en) | 2015-09-24 | 2015-09-24 | A kind of organosilicon light spreads the preparation method of microballoon |
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| CN105254823B true CN105254823B (en) | 2017-08-22 |
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| CN107903363B (en) * | 2017-11-21 | 2020-07-28 | 天津工业大学 | Polydimethylsiloxane hollow nano-microsphere and preparation method and application thereof |
| CN111234231A (en) * | 2020-03-19 | 2020-06-05 | 衢州市中通化工有限公司 | Preparation method of copolymerized organic silicon resin microspheres |
| CN112143199B (en) * | 2020-09-18 | 2022-07-22 | 宁波工程学院 | Preparation method of polyester light diffusion plate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009122919A2 (en) * | 2008-03-31 | 2009-10-08 | Daikin Industries, Ltd. | Dispersion of fluorosilicones and fluorine- and silicon-containing surface treatment agent |
| CN101824238A (en) * | 2009-12-09 | 2010-09-08 | 广州市创至峰塑料制品科技有限公司 | Surface treatment method for powder composition of optical diffusion plastic |
| CN103275321A (en) * | 2013-05-17 | 2013-09-04 | 涌奇材料技术（上海）有限公司 | Preparation method and application of organosilicon photo-diffusion particle |
| CN104356274A (en) * | 2014-10-29 | 2015-02-18 | 上海大学 | Method for preparing silicon-acrylate core-shell light diffusion agent with super concentrated emulsion |
-
2015
- 2015-09-24 CN CN201510628804.0A patent/CN105254823B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009122919A2 (en) * | 2008-03-31 | 2009-10-08 | Daikin Industries, Ltd. | Dispersion of fluorosilicones and fluorine- and silicon-containing surface treatment agent |
| CN101824238A (en) * | 2009-12-09 | 2010-09-08 | 广州市创至峰塑料制品科技有限公司 | Surface treatment method for powder composition of optical diffusion plastic |
| CN103275321A (en) * | 2013-05-17 | 2013-09-04 | 涌奇材料技术（上海）有限公司 | Preparation method and application of organosilicon photo-diffusion particle |
| CN104356274A (en) * | 2014-10-29 | 2015-02-18 | 上海大学 | Method for preparing silicon-acrylate core-shell light diffusion agent with super concentrated emulsion |
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