CN105754039B - A kind of poly(4-methyl-1-pentene) light diffusing agent and preparation method thereof - Google Patents

A kind of poly(4-methyl-1-pentene) light diffusing agent and preparation method thereof Download PDF

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Publication number
CN105754039B
CN105754039B CN201610105627.2A CN201610105627A CN105754039B CN 105754039 B CN105754039 B CN 105754039B CN 201610105627 A CN201610105627 A CN 201610105627A CN 105754039 B CN105754039 B CN 105754039B
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methyl
poly
pentene
preparation
light diffusing
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CN105754039A (en
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王琪宇
马骏
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Chongqing Chemical Research Institute Co., Ltd
Chongqing Chemical Research Institute Material Technology Co., Ltd
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王金明
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F255/00Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
    • C08F255/08Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having four or more carbon atoms

Abstract

The present invention provides a kind of poly- 4 methyl, 1 amylene light diffusing agents and preparation method thereof.In poly- 4 methyl, 1 amylene particle surface, 1,2 epoxy group, 5 hexene, 3,4 epoxy, 1 butylene are introduced, allyl glycidyl ether participates in polymerization, is warming up to reaction temperature, to the end of reaction, centrifuges, dry.Obtain light diffusing agent product.

Description

A kind of poly(4-methyl-1-pentene) light diffusing agent and preparation method thereof
Technical field
The present invention relates to a kind of preparation method of light diffusing agent, particularly a kind of poly(4-methyl-1-pentene) light diffusing agent and Preparation method.
Background technology
The fields such as light diffusion is widely used in illuminating, show, projection imaging, laser, mainly have inorganic type light diffusing agent and Organic type light is spread:Inorganic light diffusing agent mainly has:Nano barium sulfate, calcium carbonate, silica etc., the diffusion of these inorganic type light Agent, inorganic type light diffusing agent are a solid microbeads balls from microcosmic angle, and light can not penetrate this solid sphere, can influence The transmission of many light, only some light pass through through refraction, therefore influence brightness or light transmission.Do fluorescent tube lampshade requirement light transmission Inorganic light diffusing agent cannot be all selected on rate 50%;Organic light diffusing agent mainly has acryl type, styrene type, acrylic acid Resin type etc., these resins are transparent or semitransparent in itself, and light can largely pass through, using these light diffusing agents in itself The difference of the refractive index of material and the refractive index of base material, light repeatedly after refraction, become bright soft by the light of base material, and It is smaller on the light transmittance influence of material, it is to do the optical materials such as fluorescent tube lampshade to select well.
CN104059246 discloses a kind of inorganic light diffusing agent of light transmission, it is characterized in that:The each component weight percent of composition For:Ice crystal 85-94%, pyrophillite 3-8%, kaolin 2-5%, potassium feldspar 0.5-1%, shepardite 0.2-1% utilize fluidisation Bed cladding ice crystal, by mixing granular material with the hot-air heated in circulation flow dynamic furnace, specific surface reaches moment Igneous fusion, spheroidization coat one layer of reflective layer on ice crystal surface, so as to which ice crystal be made to have good translucency and reflective Property.
CN102101971 discloses a kind of light diffusing agent, which contains urethane acrylate, polymerisable monomer And organic filler, the number-average molecular weight of the urethane acrylate is 1000-10000, and the polymerisable monomer is at least two The acrylate monomer of kind multiple functional radical, the average particle diameter of the organic filler is 1.8-30 microns.
The light diffusing agent of existing known technology is easy to aging under long-time illumination, decomposes.It is surface-treated to protect Inoxidizability is demonstrate,proved, to improve light dispersibility.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of poly(4-methyl-1-pentene) light diffusing agent and its preparation sides Method.
In poly(4-methyl-1-pentene) particle surface, 1,2- epoxy group -5- hexenes, 3,4- epoxy-1-butylenes, allyl are introduced Base glycidol ether participates in polymerization, is warming up to reaction temperature, to the end of reaction, centrifuges, dry.Obtain light diffusing agent product.
The present invention provides a kind of 4-methyl-1-pentene light diffusing agent and preparation method thereof, is realized by following steps:
The preparation of step 1 water phase:
By weight, 1000 parts of water of interior addition, 0.5-2 parts of neopelexes stir evenly in a kettle.
The preparation of step 2 oil phase:
By weight, in 100 parts of poly(4-methyl-1-pentene)s, the 1,2- of monomer total amount degree 0.05~0.5 is accounted for Epoxy group -5- hexenes account for 3, the 4- epoxy-1-butylenes of monomer total amount degree 0.05~0.5, participate in polymerization, add 0.2-0.6 parts of cumyl hydroperoxides, 0.05-0.2 parts of niter cakes are added in, are stirred evenly;
Step 3 polymerisation:
Oil-phase solution is added in step 1 equipped in the reaction kettle for having prepared water phase, addition accounts for monomer total amount percentage and contains The allyl glycidyl ether of amount 0.1~0.5 then at 50-80 DEG C, reacts 1-4h, filters after reaction, and drying is produced Product.
The poly(4-methyl-1-pentene) is commercial product, such as the product of Mitsui Chemical Co., Ltd. production.Described 3, 4- epoxy-1-butylenes are commercial product, such as the product of Shanghai Hu Zhen Industrial Co., Ltd.s production.1, the 2- epoxy groups -5- oneself Alkene is commercial product.The product produced such as Shanghai to prosperous Chemical Co., Ltd..The allyl glycidyl ether is commercial product. The product produced such as Jinan Zhong Wei Chemical Co., Ltd.s.
Beneficial effects of the present invention:
Existing light diffusing agent.It is surface-treated to ensure to be uniformly dispersed, to improve light dispersibility.By in bone Oxygen-containing functional group is introduced on frame, light diffusing particles oxidation resistent susceptibility is improved, should not decompose, aging improves light transmittance.
Specific embodiment
Following embodiment is only to further illustrate the present invention, and is not limitation the scope of protection of the invention.
The present invention provides a kind of poly(4-methyl-1-pentene) light diffusing agent and preparation method thereof, is realized by following steps:
Embodiment 1:
The preparation of step 1. water phase
Interior addition 1000Kg water, 1Kg cetyl benzenesulfonic acid sodiums stir evenly in 2000L autoclaves.
The preparation of step 2. oil phase
In 500L reaction kettles, by 100Kg poly(4-methyl-1-pentene)s, 0.3Kg1,2- epoxy group -5- hexenes, 0.3Kg3, 4- epoxy-1-butylenes add in 0.4Kg cumyl hydroperoxides, 0.1Kg niter cakes stir evenly.
Step 3. polymerisation
Oil-phase solution is added in the autoclave for being equipped in step 1 and having prepared water phase, is passed through the contracting of 0.25Kg pi-allyls Water glycerin ether then from 70 DEG C of reaction 2h, centrifuges, is dried to obtain product after reaction.Number is T-1.
Embodiment 2
The preparation of step 1. water phase
Interior addition 1000Kg water, 0.5Kg cetyl benzenesulfonic acid sodiums stir evenly in 2000L autoclaves.
The preparation of step 2. oil phase
In 500L reaction kettles, by 100Kg poly(4-methyl-1-pentene)s, 0.05Kg1,2- epoxy group -5- hexenes, 0.05Kg3,4- epoxy-1-butylene add in 0.2Kg cumyl hydroperoxides, 0.05Kg niter cakes, stir evenly.
Step 3. polymerisation
Oil-phase solution is added in step 1 equipped in the autoclave for having prepared water phase, is passed through 0.1Kg allyl glycidyls Glycerin ether then from 50 DEG C of reaction 4h, centrifuges, is dried to obtain product after reaction.Number is T-2.
Embodiment 3
The preparation of step 1. water phase
Interior addition 1000Kg water, 2Kg cetyl benzenesulfonic acid sodiums stir evenly in 2000L autoclaves.
The preparation of step 2. oil phase
In 500L reaction kettles, by 100Kg poly(4-methyl-1-pentene)s, 0.5Kg1,2- epoxy group -5- hexenes, 0.5Kg3, 4- epoxy-1-butylenes add in 0.6Kg cumyl hydroperoxides, 0.2Kg niter cakes, stir evenly.
Step 3. polymerisation
Oil-phase solution is added in step 1 equipped in the autoclave for having prepared water phase, is passed through 0.5Kg allyl glycidyls Glycerin ether then from 80 DEG C of reaction 1h, centrifuges, is dried to obtain product after reaction.Number is T-3.
Comparative example 1
1,2- epoxy group -5- hexenes are added without, other are the same as embodiment 1, product identification T-4.
Comparative example 2
Allyl glycidyl ether is added without, other are the same as embodiment 1, product identification T-5.
Comparative example 3
3,4- epoxy-1-butylenes are added without, other are the same as embodiment 1, product identification T-6.
Embodiment 4
Light diffusing particles 1Kg, antioxidant 0.3Kg obtained in embodiment 1-3 and comparative example 1-3 are carried out pre- with diffusant Dispersion after adding in PC particles 100Kg, is transferred in low speed mixer and stirs, and is melted altogether with double screw extruder after mixing Mixed, granulation, most afterwards through injection molding 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 %
T-1 85
T-2 79
T-3 88
T-4 73
T-5 71
T-6 67

Claims (1)

1. a kind of preparation method of poly(4-methyl-1-pentene) light diffusing agent, it is characterised in that include the following steps:
The preparation of step 1 water phase:
By weight, 1000 parts of water are added in a kettle, and 0.5-2 parts of dispersants stir evenly;
The preparation of step 2 oil phase:
By weight, 100 parts of poly(4-methyl-1-pentene)s account for poly(4-methyl-1-pentene) total amount degree 0.05~0.5 1,2- epoxy group -5- hexenes, account for 3, the 4- epoxy -1- fourths of poly(4-methyl-1-pentene) total amount degree 0.05~0.5 Alkene participates in polymerization, adds 0.2-0.6 parts of cumyl hydroperoxides and 0.05~0.2 part of niter cake stirs evenly;
Step 3 polymerisation:
By weight, oil-phase solution is added in step 1 equipped with having prepared in the reaction kettle of water phase, addition account for poly- 4- methyl- The allyl glycidyl ether of 1- amylene total amounts degree 0.1~0.5 then at 50-80 DEG C, reacts 1-4h, reaction knot It is filtered after beam, drying obtains product.
CN201610105627.2A 2016-02-26 2016-02-26 A kind of poly(4-methyl-1-pentene) light diffusing agent and preparation method thereof Active CN105754039B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101230179A (en) * 2007-01-26 2008-07-30 罗门哈斯公司 Light-scattering compositions
CN102089379A (en) * 2008-08-01 2011-06-08 三井化学株式会社 Poly(4-methyl-1-pentene) resin composition, film containing same, microporous film, battery separator and lithium ion battery
CN103293575A (en) * 2013-05-10 2013-09-11 张家港康得新光电材料有限公司 Diffusion and brightness enhancement film and method for manufacturing same
CN103552329A (en) * 2013-10-10 2014-02-05 宁波东旭成新材料科技有限公司 High-performance reflective film and its preparation method

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JPH0653406B2 (en) * 1986-06-18 1994-07-20 三井石油化学工業株式会社 Laminate
JP5019746B2 (en) * 2005-12-28 2012-09-05 タキロン株式会社 Direct light type backlight unit
US20140355122A1 (en) * 2013-05-28 2014-12-04 Tredegar Film Products Corporation Polyolefin Volumetric Diffuser

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101230179A (en) * 2007-01-26 2008-07-30 罗门哈斯公司 Light-scattering compositions
CN102089379A (en) * 2008-08-01 2011-06-08 三井化学株式会社 Poly(4-methyl-1-pentene) resin composition, film containing same, microporous film, battery separator and lithium ion battery
CN103293575A (en) * 2013-05-10 2013-09-11 张家港康得新光电材料有限公司 Diffusion and brightness enhancement film and method for manufacturing same
CN103552329A (en) * 2013-10-10 2014-02-05 宁波东旭成新材料科技有限公司 High-performance reflective film and its preparation method

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