CN105566568B - A kind of preparation method of silicon light diffusing agent - Google Patents

A kind of preparation method of silicon light diffusing agent Download PDF

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Publication number
CN105566568B
CN105566568B CN201510943508.XA CN201510943508A CN105566568B CN 105566568 B CN105566568 B CN 105566568B CN 201510943508 A CN201510943508 A CN 201510943508A CN 105566568 B CN105566568 B CN 105566568B
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preparation
light diffusing
diffusing agent
sodium
methyl
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CN105566568A (en
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马骏
王琪宇
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Dongguan Moneng Chemical Co ltd
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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
    • C08F230/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
    • C08F230/04Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
    • C08F230/08Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
    • 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
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/12Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
    • C08F283/126Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes being the result of polycondensation and radical polymerisation reactions

Abstract

The invention provides a kind of preparation method of silicon light diffusing agent, preparation method is as follows:In a kettle., pure water, polymerization inhibitor are squeezed into, add a certain amount of dispersant, initiator, (3 mercaptopropyi) trimethoxy silane (MPTS), the acrylic acid epoxy methyl esters of 2 methyl 2, N (isobutoxy) Methacrylamide, tetramethyl tetravinyl siloxanes participates in polymerization, is warming up to reaction temperature, and question response terminates, centrifugation, dries.Obtain this patent product.

Description

A kind of preparation method of silicon light diffusing agent
Technical field
The present invention relates to a kind of light diffusing agent, particularly a kind of preparation method of silicon light diffusing agent.
Background technology
Inorganic particulate, including glass microballoon, SiO, TiO, CaCO3, MgSiO3, BaSO4 and vulcanization are used light diffusing agent more Thing ZnS, BaS etc..These inorganic particulates are typically hard, irregular, easily worn and torn process equipment during processing, dispersed phase Grain size is extremely difficult to uniformly decline the mechanical property of polymeric matrix, and these particles are to hot, oxygen and ultraviolet photosensitive Sense, if the excessive uneven surface for also resulting in material of dispersed particle, and, the addition of inorganic particulate can have a strong impact on printing opacity Rate, seriously limits application of the inorganic particulate in photodiffusion material.In recent years, organic polymer particle is used as light diffusing agent Using also more, mainly there are polymethyl methacrylate, polystyrene, silicones, acrylic resin, methyl methacrylate One styrene copolymerzation with cross-linking microballoon 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 (St) and methacryloxypropyl isobutyl group polyhedral oligomeric silsesquioxane (MAiBuPOSS).PMMA The composition and weight/mass percentage composition of light diffusing sheet be:Polymethyl methacrylate 97.0~99.5%, light diffusing agent 0.5~ 3.0%, the weight/mass percentage composition of above each component is 100%.Styrene content and MAiBuPOSS compositions in light diffusing agent Refractive index is different from the refractive index of PMMA, and when light is by material, light can be by repeatedly refraction, finally by the light of base material It is soft that line becomes light.MAiBuPOSS compositions cause that dispersiveness liftings of the PS in PMMA is notable simultaneously, obtain excellent saturating Photosensitiveness and light scattering, optical performance is high.
CN101849201 provides a kind of light diffusing and light transmission that can be assigned better than existing spherical resin particle Property, improve the light diffusing agent of the performance of final products such as screen.Light diffusing agent of the invention 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.
The light diffusing agent of existing known technology disperses bad in the base, there is agglomeration.Needs 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 discloses a kind of preparation method of silicon light diffusing agent, preparation method is such as Under:
In a kettle., pure water is squeezed into, polymerization inhibitor adds a certain amount of dispersant, initiator, (3- mercaptopropyis) front three TMOS (MPTS), 2- methyl -2- acrylic acid epoxy methyl esters, N- (isobutoxy) Methacrylamide, tetramethyl tetrem Alkenyl siloxane participates in polymerization, is warming up to reaction temperature, and question response terminates, centrifugation, dries.Obtain this patent product.
The present invention provides a kind of preparation method of silicon light diffusing agent, is realized by following steps:
Step 1) water phase preparation:
By weight, it is interior in a kettle. to add 1000 parts of water, 0.5-2 parts of dispersant to stir.
Step 2) oil phase preparation:
By weight, in 100 parts of (3- mercaptopropyis) trimethoxy silanes (MPTS), monomer total amount degree is accounted for 0.5~5% 2- methyl -2- acrylic acid epoxy methyl esters, accounts for N- (the isobutyl oxygen of monomer total amount degree 0.5~5% Base) Methacrylamide, the tetramethyl tetravinyl siloxanes participation polymerization of monomer total amount degree 0.5~5% is accounted for, then 0.5~2 part of sodium peroxydisulfate is added to stir;
Step 3) polymerisation:
The oil-phase solution that will be prepared is added to step 1) in equipped with having prepared the reactor of water phase, then in 70-90 DEG C, 1-4h is reacted, reaction is filtered after terminating, and drying obtains product.
The preferred sodium peroxydisulfate of initiator.
(3- mercaptopropyis) trimethoxy silane (MPTS) is commercially available prod, such as Hubei Ju Sheng Science and Technology Ltd.s life The product of product;2- methyl -2- acrylic acid epoxies the methyl esters is commercially available prod, such as Shanghai Yan Jing bio tech ltd pin The product sold;N- (isobutoxy) Methacrylamide is commercially available prod.Such as Nanjing Kang Manlin chemical industry Industrial Co., Ltd. The product of production;The tetramethyl tetravinyl siloxanes is commercially available prod.Such as the product of Hubei Ju Sheng Science and Technology Ltd.s production Product.
The dispersant includes anion emulsifier, is ammonium lauryl sulfate, neopelex, cetyl The chain alkyl type anion such as benzene sulfonic acid sodium salt, B-53, polyoxyethylene alkyl ether sodium sulphate and paraffin sulfonate Any one in type emulsifying agent, perfluoro caprylic acid sylvite or ammonium salt and the pungent sulfonate sodium of perfluor alkane or ammonium salt.It is preferred that dodecyl Benzene sulfonic acid sodium salt.
Beneficial effects of the present invention:
Existing light diffusing agent.Needs are surface-treated to ensure to be uniformly dispersed, to improve light dispersiveness.By The functional groups such as epoxy radicals, isobutoxy, silica group are introduced on skeleton, makes resistance to oxidation in light diffusing particles matrix material, it is unsuitable Translucency is influenceed because of degraded, makes light transmittance higher.
Specific 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 silicon light diffusing agent, is realized by following steps:
Embodiment 1:
The preparation of step 1. water phase
The interior addition 1000Kg water in 2000L autoclaves, 1Kg neopelexes stir.
The preparation of step 2. oil phase
In 500L reactors, by 100Kg (3- mercaptopropyis) trimethoxy silane (MPTS), 1Kg2- methyl -2- third Olefin(e) acid epoxidation methyl esters, 1KgN- (isobutoxy) Methacrylamide, 2Kg tetramethyl tetravinyls siloxanes adds 1Kg over cures Sour sodium, stirs.
Step 3. polymerisation
The oil-phase solution that will be prepared is equipped with the autoclave for having prepared water phase in being added to step 1, then anti-from 80 DEG C Answer 14h, reaction to be centrifuged after terminating, be dried to obtain product.Numbering is SX-1.
Embodiment 2
The preparation of step 1. water phase
The interior addition 1000Kg water in 2000L autoclaves, 0.5Kg neopelexes stir.
The preparation of step 2. oil phase
In 500L reactors, by 100Kg (3- mercaptopropyis) trimethoxy silane (MPTS), 0.5Kg2- methyl -2- Acrylic acid epoxy methyl esters, 0.5KgN- (isobutoxy) Methacrylamide, 0.5Kg tetramethyl tetravinyl siloxanes is added 0.1Kg sodium peroxydisulfates, stir.
Step 3. polymerisation
The oil-phase solution that will be prepared is equipped with the autoclave for having prepared water phase in being added to step 1, then anti-from 70 DEG C Answer 2h, reaction to be centrifuged after terminating, be dried to obtain product.Numbering is SX-2.
Embodiment 3
The preparation of step 1. water phase
The interior addition 1000Kg water in 2000L autoclaves, 2Kg neopelexes stir.
The preparation of step 2. oil phase
In 500L reactors, by 100Kg (3- mercaptopropyis) trimethoxy silane (MPTS), 5Kg2- methyl -2- third Olefin(e) acid epoxidation methyl esters, 5KgN- (isobutoxy) Methacrylamide, 5Kg tetramethyl tetravinyl siloxanes adds 0.5Kg Sodium peroxydisulfate, stirs.
Step 3. polymerisation
The oil-phase solution that will be prepared is equipped with the autoclave for having prepared water phase in being added to step 1, then anti-from 90 DEG C Answer 1h, reaction to be centrifuged after terminating, be dried to obtain product.Numbering is SX-3.
Comparative example 1
2- methyl -2- acrylic acid epoxy methyl esters is added without, production code member is SX-4.
Comparative example 2
N- (isobutoxy) Methacrylamide is added without, production code member is SX-5.
Comparative example 3
Tetramethyl tetravinyl siloxanes is added without, production code member is SX-6.
Comparative example 4
It is added without tetramethyl tetravinyl siloxanes, N- (isobutoxy) Methacrylamide, 2- methyl -2- acrylic acid Epoxidation methyl esters production code member is SX-7.
Embodiment 4
1 part of obtained light diffusing particles in embodiment 1-3 and comparative example 1-3,0.3 part of antioxidant is carried out pre- with diffusant Dispersion, after adding 100 parts of PC particles, is transferred to stirring in low speed mixer, is melted altogether with double screw extruder after being well mixed Mixed, granulation, most afterwards through injection machine injection moulding light diffusing sheet.
Optic test
Using light transmittance/mist degree tester (EEL57D, Shanghai precision instrument Co., Ltd), surveyed by GB/T2410-2008 Examination.

Claims (1)

1. a kind of preparation method of silicon light diffusing agent, it is characterised in that comprise the following steps:
Step 1) water phase preparation:
By weight, it is interior in a kettle. to add 1000 parts of water, 0.5-2 parts of dispersant to stir;
The dispersant includes ammonium lauryl sulfate, neopelex, cetyl benzenesulfonic acid sodium, dialkyl group amber Sour sodium, polyoxyethylene alkyl ether sodium sulphate and paraffin sulfonate, perfluoro caprylic acid sylvite or ammonium salt and the pungent sulfonate of perfluor alkane;
Step 2) oil phase preparation:
By weight, in 100 parts of (3- mercaptopropyis) trimethoxy silanes (MPTS), 0.5~5 part of 2- methyl -2- propylene Sour epoxidation methyl esters, 0.5~5 part N- (isobutoxy) Methacrylamide, 0.5~5 part of tetramethyl tetravinyl silicon Oxygen alkane participates in polymerization, adds 0.5~2 part of sodium peroxydisulfate and stirs;
Step 3) polymerisation:
By step 2) in the oil-phase solution for preparing be added to step 1) in equipped with the reactor for having prepared water phase, then in 70- 90 DEG C, 1-4h is reacted, reaction is filtered after terminating, and drying obtains product.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102037059A (en) * 2008-05-21 2011-04-27 住友精化株式会社 Resin particle having many recesses on surface thereof
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
CN105131183A (en) * 2015-09-24 2015-12-09 衢州市中通化工有限公司 Preparation method of fluorosilicone optical diffusing agent

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5860689B2 (en) * 2011-12-20 2016-02-16 株式会社日本触媒 Organic particles for light diffusion media

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102037059A (en) * 2008-05-21 2011-04-27 住友精化株式会社 Resin particle having many recesses on surface thereof
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
CN105131183A (en) * 2015-09-24 2015-12-09 衢州市中通化工有限公司 Preparation method of fluorosilicone optical diffusing agent

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