CN106832354A - A kind of preparation method for optical thin film hardening wear-resistant plastic particle - Google Patents
A kind of preparation method for optical thin film hardening wear-resistant plastic particle Download PDFInfo
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- CN106832354A CN106832354A CN201710103580.0A CN201710103580A CN106832354A CN 106832354 A CN106832354 A CN 106832354A CN 201710103580 A CN201710103580 A CN 201710103580A CN 106832354 A CN106832354 A CN 106832354A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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- 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
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
The invention discloses a kind of preparation method for optical thin film hardening wear-resistant plastic particle, comprise the following steps:(1), the inorganic nanometer powder with high rigidity is prepared into the nano color paste of good dispersion;(2), dispersion will at high temperature be melted with the above-mentioned inorganic nano mill base for preparing and organic polymer plastic master batch;(3) after, miscible compound system is well mixed by twin-screw, extrusion, pelletizing obtain the plastic pellet of wear-resisting hardening.It is of the invention that multi-functional inorganic nano-particle is directly aggregated in high-molecular organic material the inside, on the one hand can so keep the feature and stability of inorganic material, on the other hand can also modified organic polymer device for Optical Properties of Materials, mechanical performance, chemical stability etc., and the composite master batch prepared can be used to easily produce plastic plate or film, and this plastic products have the advantages that mist degree is low, good weatherability, can be widely applied to the fields such as building, automobile, ship.
Description
Technical field
The present invention relates to a kind of preparation method for optical thin film hardening wear-resistant plastic particle, particularly relate to a kind of organic
The preparation method and purposes of inorganic compounding master batch.
Background technology
It is always field of compound material that will be uniformly combined with functional inorganic nano material and high-molecular organic material
The focus of research.Because general high-molecular organic material has, production is simple, easy processing is molded, transparency is high, cost is low
Advantage, but also have the shortcomings that weatherability is poor, feature is weak;And inorganic material have great thermotolerance, it is multi-functional (antistatic, uvioresistant,
Antifouling, antistatic, hardness are high, wearability is good) the advantages of, but have the disadvantage to be not easy machine-shaping, particularly non-geometric rule is difficult
Its large-scale use in daily life is restricted with the shortcoming processed.Therefore, homogenous material constrains organic material and inorganic
Application of the material during industrial upgrading.
If inorganic material, particularly inorganic nanoparticles can be homogeneously dispersed in high-molecular organic material, not only may be used
To prepare multi-functional composite, while also have the advantage of organic material and inorganic material concurrently, such as organic material easily into
Type is processed, and inorganic material can also improve the wearability of organic material, improves weatherability of organic material etc..At present, this
Planting organic/inorganic composite material will progressively be applied in our daily life, and such as organic-inorganic thermal isolation film, organic-inorganic are prevented
Electrostatic film, organic-inorganic insulation film, organic-inorganic anti-soil film etc..
At present, the extensive patent prepared in terms of the low organic/inorganic composite material of transparent good, mist degree rarely has and is related to, greatly
Part is all directly to add or coupling agent modified, is all opaque product, and inorganic material is in organic system
The development trend of high dispersive this composite has obtained being widely recognized as academia and industrial quarters.Therefore, one kind is disclosed herein
The preparation method of organic-inorganic ultraviolet isolating composite master batch, can just be prepared by simple following process and contain ultraviolet resistance
Every the plastic plate and optical thin film of function, the plastic plate or film prepared by the composite master batch have mist degree low, weather-proof
Property it is good the advantages of, this for conventional plastic industry industrial upgrading open up a good road.
The content of the invention
The invention aims to provide a kind of preparation method for optical thin film hardening wear-resistant plastic particle, to solve
The certainly above mentioned problem of prior art.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method for optical thin film hardening wear-resistant plastic particle, comprises the following steps:
(1), the inorganic nanometer powder with high rigidity is prepared into the nano color paste of good dispersion;
(2), will at high temperature be melted point with the above-mentioned inorganic nano mill base for preparing and organic polymer plastic master batch
Dissipate;
(3) after, miscible compound system is well mixed by twin-screw, extrusion, pelletizing obtain the plastics of wear-resisting hardening
Particle, extrusion temperature is the melt temperature of plastic pellet, and usually 280-285 DEG C, water-cooled pelletizing afterwards, the selection of twin-screw is long
Footpath than larger, generally between 40-48;
Wherein, in step (1), the preparation method of the inorganic nano mill base of high rigidity is realized, its step is:
B () mixes:By the inorganic nanometer powder with high rigidity, organic dispersing agent and organic solvent three in mass ratio
(10-30):(1-3):(67-89) is well mixed;
B () disperses:By mixture in high speed shear decentralized medium high speed shearing dispersion 30-60 minutes, the speed of mixer
Degree is controlled at 1000-3000 rpms to obtain slurry;
C () grinds:Put the scattered slurry of high speed shear into jar mill, ball mill or grinding distribution is obtained in sand mill
Mill base;
D () is sieved:Ground mill base is sieved with the gauze of 400 mesh, to remove big particle, high hardness nanocomposite is obtained
Mill base.
In step (a), the three-dimensional dimension of the inorganic nanometer powder of described high rigidity is no more than 100 nanometers.Described
The inorganic nanometer powder of high rigidity is nano silicon oxide, nano aluminium oxide, nano zircite, nano zirconium nitride, nano-titanium oxide
In one or more.
In step (a), described organic dispersing aid is the dispersant containing high polymer long chain, such as organic high containing hydroxyl
Molecule long-chain, carboxyl organic polymer long-chain, epoxy radicals organic polymer long-chain or the organic polymer long-chain containing amino;
It is preferred that polyethylene glycols, polyacrylic, polyvinylpyrrolidone class, polyurethanes dispersant.The addition of organic dispersing aid
Amount should be 0.5-15% of inorganic nanometer powder or so, preferably 5-8%
In step (a), described organic solvent is selected from alcohols, esters, the one kind in benzene class, ketone, ethers.Wherein, alcohol
Class is the one kind in methyl alcohol, ethanol, propyl alcohol, butanol, and esters are the one kind in methyl acetate, ethyl acetate, butyl acetate;Benzene class
It is the one kind in toluene, dimethylbenzene.
In step (b), the decentralized medium is generally atent solvent, carried out in inert media it is organically-modified, can be with
The denaturation of inorganic nanometer powder is prevented, the chemical stability of powder is improved.
In step (2), described organic polymer plastic master batch is the conventional organic polymer for preparing plastic material modeling
Material master batch, preferably PE master batches, PET master batch, PVC master batches, PP master batches, PC master batches, PVA master batches, ABS masterbatch etc..
In step (2), described high temperature is generally referred near the softening point temperature of organic polymer plastic master batch, wherein,
PET is 260-300 DEG C, and PC is 280-300 DEG C.
The plastic pellet of this wear-resisting hardening is during the optical thin film for preparing scratch resistant, and addition is typically less, should
No more than 20%, preferably more than 15%, more preferably no more than 10%, it is possible to obtain the wear-resisting optical thin film of hardening.
Beneficial effects of the present invention are:The present invention inorganic nanometer powder and organic polymer plastics of the application with high rigidity
Master batch is blended, and multi-functional inorganic nano-particle directly is aggregated in into high-molecular organic material the inside, on the one hand can so be protected
Hold the feature and stability of inorganic material, on the other hand can also modified organic polymer device for Optical Properties of Materials, mechanical performance,
Chemical stability etc., and the composite master batch prepared can be used to easily produce plastic plate or film, and this plastics
Product has the advantages that mist degree is low, good weatherability, can be widely applied to the fields such as building, automobile, ship.
Specific embodiment
Technical scheme is described in more details below by embodiment.
Embodiment 1
Step (1) prepares the inorganic nano dispersion mill base with high rigidity
10 parts of nano silicon oxide is taken, 89 parts of isopropanol, 1 part of PEG dispersants are put into rustless steel container, in high speed shear
Carried out pre-dispersed 30 minutes with 1500r/min in dispersion machine;Ball milling 24 hours in high speed ball mill, sieving removal are put into afterwards
Bulky grain, obtains dispersed nano silicon oxide mill base.
Step (2)
The above-mentioned nano color paste for preparing and PET master batch are blended, heating stirring dispersion, squeezes afterwards in screw pelletizer
Go out, cool down, granulating the organic-inorganic PET composite master batch obtained with high rigidity.
The PET master batch of organo-mineral complexing is melted, is cast, slab, membrane, test finds that the hardness of film can be with
2H is reached, is had than the hardness 5B of normal PET film and is significantly lifted, it is possible to reduce follow-up increase coating process is thin in raising PET
The case hardness of film.
Embodiment 2
Step (1) prepares the inorganic nano dispersion mill base with high rigidity
10 parts of nano aluminium oxide is taken, 89 parts of isopropanol, 1 part of PVP dispersants are put into rustless steel container, in high speed shear
Carried out pre-dispersed 30 minutes with 1500r/min in dispersion machine;Ball milling 24 hours in high speed ball mill, sieving removal are put into afterwards
Bulky grain, obtains dispersed nano aluminium oxide mill base.
Step (2)
The above-mentioned nano color paste for preparing and PET master batch are blended, heating stirring dispersion, squeezes afterwards in screw pelletizer
Go out, cool down, granulating the organic-inorganic PET composite master batch obtained with high rigidity.
The PET master batch of organo-mineral complexing is melted, is cast, slab, membrane, test finds that the hardness of film can be with
2H is reached, is had than the hardness 5B of normal PET film and is significantly lifted, it is possible to reduce follow-up increase coating process is thin in raising PET
The case hardness of film.
Embodiment 3
Step (1) prepares the inorganic nano dispersion mill base with high rigidity
10 parts of nano zircite is taken, 89 parts of ethyl acetate, 1 part of solvent borne polyurethane class dispersant puts into rustless steel container
In, carried out pre-dispersed 30 minutes with 1500r/min in high speed shear dispersion machine;Ball milling 24 in high speed ball mill are put into afterwards
Hour, sieving removal bulky grain obtains dispersed nano zircite mill base.
Step (2)
The above-mentioned nano color paste for preparing and PET master batch are blended, heating stirring dispersion, squeezes afterwards in screw pelletizer
Go out, cool down, granulating the organic-inorganic PET composite master batch obtained with high rigidity.
The PET master batch of organo-mineral complexing is melted, is cast, slab, membrane, test finds that the hardness of film can be with
2H is reached, is had than the hardness 5B of normal PET film and is significantly lifted, it is possible to reduce follow-up increase coating process is thin in raising PET
The case hardness of film.
In a word, the organo-mineral complexing master batch that prepared by the method, because inorganic nanometer powder entered organic polymer dispersion
After agent is modified, can be compatible with organic polymer plastic master batch well.Additionally, high-molecular organic material is used as protective layer,
The stability of inorganic nanometer powder can well be protected.The present invention prepares organo-mineral complexing master batch, and to can be applied to function thin
The composites such as film, function sheet material, insulation fibre, antistatic fiber, the film or sheet material transparency of preparation is high, and mist degree is low, resistance to old
The advantages of change ability is strong, wearability is good.The preparation method of the organic-inorganic hardening wear-resistant masterbatch that the present invention is provided is simple, prepares work
Skill is innovated, and following process is application one new road of developing of inorganic nanometer functional powder easily.
Claims (13)
1. a kind of preparation method for optical thin film hardening wear-resistant plastic particle, it is characterised in that:Comprise the following steps:
(1), the inorganic nanometer powder with high rigidity is prepared into the nano color paste of good dispersion;
(2), dispersion will at high temperature be melted with the above-mentioned inorganic nano mill base for preparing and organic polymer plastic master batch;
(3) after, miscible compound system is well mixed by twin-screw, extrusion, pelletizing obtain the plastic pellet of wear-resisting hardening,
Extrusion temperature is the melt temperature of plastic pellet, usually 280-285 DEG C, water-cooled pelletizing afterwards, the selection draw ratio of twin-screw
Larger, generally between 40-48;
Wherein, in step (1), the preparation method of the inorganic nano mill base of high rigidity is realized, its step is:
A () mixes:By the inorganic nanometer powder with high rigidity, organic dispersing agent and organic solvent three (10- in mass ratio
30):(1-3):(67-89) is well mixed;
B () disperses:By mixture in high speed shear decentralized medium high speed shearing dispersion 30-60 minutes, the speed control of mixer
Make at 1000-3000 rpms to obtain slurry;
C () grinds:Put the scattered slurry of high speed shear into jar mill, ball mill or grinding distribution obtains color in sand mill
Slurry;
D () is sieved:Ground mill base is sieved with the gauze of 400 mesh, to remove big particle, high hardness nanocomposite color is obtained
Slurry.
2. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 1, its feature exists
In:In step (a), the three-dimensional dimension of the inorganic nanometer powder of described high rigidity is no more than 100 nanometers;Described high rigidity
Inorganic nanometer powder be in nano silicon oxide, nano aluminium oxide, nano zircite, nano zirconium nitride, nano-titanium oxide
Plant or several.
3. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 1, its feature exists
In:In step (a), described organic dispersing aid be selected from containing hydroxyl organic polymer long-chain, carboxyl organic polymer long-chain,
One kind in epoxy radicals organic polymer long-chain and the organic polymer long-chain containing amino.
4. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 3, its feature exists
In:Described organic dispersing aid is selected from polyethylene glycols, polyacrylic, polyvinylpyrrolidone class, polyurethanes dispersion
Agent.
5. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 1, its feature exists
In:The addition of described organic dispersing aid is the 0.5-15% of inorganic nanometer powder.
6. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 5, its feature exists
In:The addition of described organic dispersing aid is the 5-8% of inorganic nanometer powder.
7. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 1, its feature exists
In:In step (a), described organic solvent is selected from alcohols, esters, the one kind in benzene class, ketone, ethers.
8. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 7, its feature exists
In:Alcohols is the one kind in methyl alcohol, ethanol, propyl alcohol, butanol, and esters are in methyl acetate, ethyl acetate, butyl acetate
Kind;Benzene class is the one kind in toluene, dimethylbenzene.
9. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 1, its feature exists
In:In step (2), it is female that described organic polymer plastic master batch is selected from PE master batches, PET master batch, PVC master batches, PP master batches, PC
One kind in grain, PVA master batches, ABS masterbatch.
10. a kind of preparation method for optical thin film hardening wear-resistant plastic particle according to claim 1, its feature exists
In:In step (2), described high temperature refers to:PET is 260-300 DEG C, and PC is 280-300 DEG C.
The optical thin film of plastic pellet prepared by a kind of 11. preparation methods containing described in claim 1, it is characterised in that:Institute
In the optical thin film stated, the plastic pellet addition of wear-resisting hardening is no more than 20%.
12. optical thin films according to claim 11, it is characterised in that:The plastic pellet addition of wear-resisting hardening does not surpass
Cross no more than 15%.
13. optical thin films according to claim 11, it is characterised in that:The plastic pellet addition of wear-resisting hardening does not surpass
Cross 10%.
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CN107365493A (en) * | 2017-07-31 | 2017-11-21 | 湖州裕宇塑料有限公司 | Wear-resistant plastic particle and preparation method thereof |
CN108145988A (en) * | 2017-12-20 | 2018-06-12 | 江苏斯瑞达新材料科技有限公司 | The production method of the antistatic scratch resistant polyester film of display screen |
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CN110229474B (en) * | 2018-03-06 | 2021-01-26 | 中国科学院化学研究所 | PBT (polybutylene terephthalate) nano composite material and preparation method thereof |
CN110229484B (en) * | 2018-03-06 | 2021-01-26 | 中国科学院化学研究所 | PLA (polylactic acid) nano composite material and preparation method thereof |
CN110229490B (en) * | 2018-03-06 | 2021-02-02 | 中国科学院化学研究所 | PC (polycarbonate) nano composite material and preparation method thereof |
CN110229494B (en) * | 2018-03-06 | 2021-02-26 | 中国科学院化学研究所 | PPO (Poly-p-phenylene oxide) nano composite material and preparation method thereof |
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