CN101921470B - Special master batch for PC (Polycarbonate) sunlight board and application thereof - Google Patents
Special master batch for PC (Polycarbonate) sunlight board and application thereof Download PDFInfo
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- CN101921470B CN101921470B CN2010102382958A CN201010238295A CN101921470B CN 101921470 B CN101921470 B CN 101921470B CN 2010102382958 A CN2010102382958 A CN 2010102382958A CN 201010238295 A CN201010238295 A CN 201010238295A CN 101921470 B CN101921470 B CN 101921470B
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 6
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- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 abstract 7
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 abstract 7
- 235000021355 Stearic acid Nutrition 0.000 abstract 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 abstract 1
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Images
Abstract
The invention discloses a special master batch for a PC (Polycarbonate) sunlight board and application thereof. The preparation method of the special master batch for PC sunlight board comprises the following steps of: (1) carrying out nano dispersion and modification to dispersing agent, the ATO (Arsenic Trioxide) content of which accounts for 0.1%-10% of the mass of the ATO to obtain ATO nanoparticles, wherein the dispersing agent is a silane coupling agent or stearic acid, and the ATO is stibium-doped stannic oxide; and (2) fusing and mixing the ATO nanoparticles in PC resins to prepare the special master batch for PC sunlight board, wherein the mass fraction of the ATO is 1%-50%. The master batch has high processing fluidity and is suitable for preparing the PC sunlight board with higher transparence and good heat-insulation effect.
Description
(1) technical field
The present invention relates to the preparation method of a kind of PC sunlight board dedicated parent material and PC sunlight board.
(2) background technology
The PC sunlight board is a kind of New Building Materials, has transparent, light weight, inexpensive advantage.But it is when putting visible light into, is that main thermal source light in the sunlight has also been put to infrared light, and promptly its heat-proof quality is relatively poor.
ATO (stibium doping stannic oxide) is the material with special light electrical property, with nano ATO all be distributed among the PC (polycarbonate), can let the PC sunlight board have good transparent heat-insulated effect.Patented claim CN101421353A obtains modification ATO particle with the macromolecule dispersing agent modification earlier with ATO, mixes with PC, and will add micromolecular auxiliary agent, extrudes and obtains the PC matrix material.Though make ATO to be scattered in preferably among the PC, this technology relative complex, and introduced another kind of macromolecular material will cause the compatibility problem with the PC resin, causes that interfacial effect causes transparency degradation down.And well-known pure PC Resin Flow is poor, cause relatively difficulty of processing, and aforesaid method is produced and still had problem of difficult processing.Therefore, how to find and a kind of ATO can evenly be sneaked in the PC sunlight board with the nano-dispersed mode, reduce to cause the PC sunlight board transparency, can improve mobilely simultaneously, be badly in need of to be easy to method for processing but do not introduce other polymkeric substance.
(3) summary of the invention
The primary technical problem that the present invention will solve is to provide a kind of PC sunlight board dedicated parent material, and this masterbatch has high processing fluidity, is applicable to that the preparation transparency is higher, the PC sunlight board of good heat-insulation effect.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of PC sunlight board dedicated parent material, its preparation method may further comprise the steps:
(1) using quality to carry out nanometer as 0.1～10% dispersion agent of ATO quality the ATO powder disperses and modification, obtains the ATO nano particle; Described dispersion agent is silane coupling agent or Triple Pressed Stearic Acid;
(2) the ATO nano particle is melt blended into processes the ATO massfraction in the PC resin at 1%～50% PC sunlight board dedicated parent material.
ATO powder of the present invention; Be stibium doping stannic oxide, be light blue, can use the commercial goods; As buying to companies such as the positive nanometer in Shanghai, Shanghai ltd, Wen County, Gansu Mei Dilin nano material development corporation, Ltd., Shandong Origine Nanomaterial Engineering Co., Ltd.; Also can be according to relevant document like [" University Of Science and Technology Of Hunan's journal " 2005,20, (3) 71], [" sufacing " 2005; 34; (4) 6], preparations voluntarily such as the method for introductions such as [" silicate journal " 2006,34 (4), 417] and publication such as CN1317803A, CN101597022, CN101468397, CN101428849 such as chemical coprecipitation, hydrothermal synthesis method, combustion synthesis method.The antimony doping is 1～30mol% in the ATO powder that the present invention uses, preferred 8～10mol%.
Further, in the step of the present invention (1), the adding quality optimization of said dispersion agent is 0.5～5% of an ATO quality, most preferably is about 1.0%.
Said nanometer dispersion and modification are meant that utilizing dispersion agent that ATO is carried out nano modification earlier makes better, the stable slurries of dispersion in the step of the present invention (1), and the ATO particle diameter is below 100nm in the slurries.Again ATO slurries evaporate to dryness and grinding are obtained the ATO nano particle.
Further, the present invention recommends described step (1) specifically to adopt following method: silane coupling agent and ATO powder are added to stir in the entry obtain solid content at 15～55% suspension-s, regulate pH of suspension value to 9～11; Gained suspension-s is carried out ball-milling processing, obtain slurries, regulate pH value to 6～8 rapidly; Again slurries evaporate to dryness and grinding are obtained the ATO nano particle.
Silane coupling agent of the present invention is meant the silane of the Si-O-R structure that contains facile hydrolysis, as using the silane coupling agent of models such as KH550, KH560, KH570.The silane coupling agent that the present invention uses in water hydrolysis or with the optimal ph of particle surface generation surface reaction be～4.0.But contain easy dissociated Cl ion among the ATO usually; Causing its suspension-s original ph is 2～3; Drop to 1～2 (being the ATO suspension solid content is) after " mill leaves " at 15～55% o'clock, its pH value is adjusted to 9～11 could realizes that the pH value maintains about 4.0 in the mechanical milling process so have only before the ball milling, thereby accelerate surface reaction speed greatly; Significantly reduce the Ball milling time, realize quick, efficient, stabilized nano dispersion.Regulate suspension-s and slurry pH value and can use alkali lye, like sodium hydroxide solution commonly used, its concentration is recommended as 0.5～2mol/L, also can use alkali lye commonly used such as ammoniacal liquor.
Further, ball-milling processing of the present invention is specially: with the zirconium pearl is the ball milling pearl, and gained suspension-s was put into the ball mill ball milling 0.5-7.5 hour, removes the ball milling pearl then, obtains slurries.
Further again; We find, in mechanical milling process, it is thin more to have a ball milling pearl; The tonburden of ATO powder is just bigger, efficient is just high more, the particle diameter of gained slurries is also with regard to more little rule; So the present invention preferably uses the diameter 0.1～1.5mm zirconium pearl with high-ratio surface as the ball milling pearl, thereby the ATO powder is mountable to ball milling pearl volume 1/3 to 1/2, be higher than 1/6 to 1/4 in the existing ball-milling technology.Simultaneously, the average diameter of particles of gained slurries is also less, between 25～50nm.Further again, among the present invention, the rotating speed of balls grinding machine is between 180～580rpm.
Further again, the preferred spheres time consuming is 2.5～7.5 hours.
Further, the present invention recommends described step (1) specifically to adopt following method: Triple Pressed Stearic Acid and ATO powder are added to stir in the absolute ethyl alcohol obtain solid content at 15～30% suspension-s; Gained suspension-s is carried out ball-milling processing, obtain slurries; Again slurries evaporate to dryness and grinding are obtained the ATO nano particle.The concrete operations and the condition setting of described ball-milling processing are the same, repeat no more.
In the step of the present invention (2), described melt blending is meant: ATO nano particle and PC resin particle are pressed the certain mass mixed, and blend is extruded under 220～280 ℃ temperature condition, makes the ATO massfraction at 1%～50% PC sunlight board dedicated parent material.
Further, the ATO massfraction is 10%～30% in the preferred described PC sunlight board dedicated parent material.
The PC sunlight board dedicated parent material that the present invention makes has the characteristics of high workability; Said high workability is meant than unmanageable pure PC resin; The steady periodic processing moment of torsion of masterbatch according to the invention has reduced more than 50%; And along with the increase of ATO content in the masterbatch, its processing flowability is better, thereby makes difficulty of processing reduce greatly.Simultaneously, the ATO particulate size of the present invention after dispersion agent is handled be at nano level, even average diameter of particles can reach 25-50nm, makes that its dispersion effect in PC sunlight board masterbatch is better.
Second technical problem that the present invention will solve is the PC sunlight board masterbatch that the present invention makes to be used to prepare the transparency is higher, the PC sunlight board of good heat-insulation effect.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of preparation method of PC sunlight board; Comprise the steps: the blend dilution in the PC resin of PC sunlight board dedicated parent material; And extrude or be hot pressed into the sheet material (like 0.1mm, 0.2mm, 0.5mm etc.) of different thickness with molten state, can obtain described PC sunlight board.
The said blend dilution of the present invention is meant that the PC sunlight board masterbatch with relative high density mixes with the PC resin particle according to a certain percentage, and the ATO-PC matrix material of preparation low concentration is to be used to prepare transparent heat-insulated PC sunlight board.
The present invention said transparent heat-insulated be meant sunlight board to the rejection rate of infrared light (wavelength 760-2600nm) greater than 60%, and to the transmitance of visible light (wavelength 400-760nm) greater than 70%.
The said PC sunlight board of the present invention is meant the clear sheet that is obtained through machine-shaping by polycarbonate (PC) resin.
The dispersion state of ATO in the PC sunlight board masterbatch that the present invention makes, available TEM is that transmission electron microscope detects; The transparent heat-insulated performance of masterbatch, can through with pure PC blend dilution after the effect of heat insulation or the spectral response of the transparent heat-insulated sheet material that obtains detect.To the former, sheet material is covered on the uncovered polystyrene foamed plastics case, place a distance acceptance irradiation (see figure 1) under the ir lamp.If the surface temperature of the purer PC sheet material of plate surface temperature obviously raises, the temperature inside the box that the temperature inside the box that perhaps is coated with the plastic box of ATO-PC sheet material is coated with the plastic box of pure PC sheet material obviously reduces, and proves that promptly the effect of heat insulation of ATO-PC sheet material is good.To the latter, be that sheet material is done the ultraviolet-visible-near-infrared spectrum performance test.
Compared with prior art, beneficial effect of the present invention is:
A) ATO content is higher in the PC sunlight board masterbatch, has the high workability ability, is easy to processing.
B) the ATO slurries that make of the present invention have nano level and disperse, and the ATO particle that makes with it can reach nano level in the PC resin disperses, thereby obtains good dispersion effect.
C) the present invention is through making PC sunlight board masterbatch earlier; And then gained masterbatch and PC resin mixed in varing proportions the PC sunlight board of producing different content; Because the high workability of PC sunlight board ability and good dispersiveness; Make that processing is fairly simple, ATO good dispersivity in the PC sunlight board that makes, thus make that the transparency is better, good heat-insulation effect.
(4) description of drawings
Fig. 1 is the device of test sheet material effect of heat insulation among the present invention; Wherein: the 1-ir lamp; 2-ATO-PC sheet material; The 3-foam plastic reservoir; 4-tin platinum paper baffle plate; The 5-mercurythermometer;
A and b are respectively embodiment 1 and embodiment 2 gained ATO particulate diameter and distributions among Fig. 2;
The TEM figure of the ATO-PC nano composite material that Fig. 3 makes for embodiment 4, its right-of-center in political views figure is the amplification of left figure;
Fig. 4 is the effect of heat insulation of the thick ATO-PC sheet material of the 1mm that obtains among the embodiment 4;
Fig. 5 is the spectral response figure of the sheet material that obtains among embodiment 4 and the embodiment 5;
Fig. 6 is the stress-strain curve of different ATO content masterbatch;
Fig. 7 is a processing fluidity for the processing moment of torsion of different ATO content masterbatch.
(5) embodiment
Following instance further specifies the present invention, but these instances are not used for limiting the present invention.
The ATO modification: the dispersion agent KH570 (Chemical Reagent Co., Ltd., Sinopharm Group) that will account for ATO (the positive nanometer in Shanghai, Shanghai ltd) quality 1.0% joins in the zero(ppm) water and stirring; Adding ATO again, to be configured to solid content be 30% suspension-s; NaOH solution with 1M is regulated pH of suspension to 10; Obtain slurries with ball milled modification ATO (ball mill model QM-2SP12, ball milling pearl are zirconium pearl, drum's speed of rotation 380rpm, the ball milling time 7.5h of particle diameter 1mm), regulate pH and transfer to that (particle diameter of ATO is seen Fig. 2 a) in the slurries about 8.0.ATO slurries with nano-dispersed obtain the ATO nano particle to grind behind 45 ℃ of left and right sides evaporates to dryness in Rotary Evaporators again.
Change dispersion agent KH570 into KH560 (Chemical Reagent Co., Ltd., Sinopharm Group), usage quantity changes 1.8% of ATO quality into simultaneously, and other obtains slurries adjusting pH and transfer to (particle diameter of ATO is seen Fig. 2 b in the slurries) about 8.0 with embodiment 1.
Add in the 80g absolute ethyl alcohol dispersion agent Triple Pressed Stearic Acid of 0.2g and stirring; The ATO (the positive nanometer in Shanghai, Shanghai ltd) that adds 20g again obtains the absolute ethyl alcohol slurries of ATO with ball milled modification ATO (ball mill model QM-2SP12, ball milling pearl are zirconium pearl, drum's speed of rotation 380rpm, the ball milling time 2.5h of particle diameter 1mm).ATO slurries with nano-dispersed obtain the ATO nano particle with 30 ℃ of left and right sides evaporates to dryness grindings in Rotary Evaporators again.
The mass ratio of the ATO nano particle that obtains among the embodiment 1 with 1: 4 mixed with pure PC resin particle; And at plastics twin screw extruder (TE-35; Inferior chemical equipment ltd of Nanjing section) blend is extruded in; Extruder temperature is set in 240 ℃ to 280 ℃, is uniformly mixed after the water-cooled granulation and ATO disperses masterbatch preferably, and ATO content is 20%.Again masterbatch being diluted blend with 1: 19 mass ratio and pure PC particle in forcing machine, to obtain ATO content be 1.0% ATO-PC matrix material (branch of ATO in PC sporadically appear Fig. 3); Through hot-forming 0.4mm and the thick ATO-PC sheet material of 1mm of obtaining; Its actual effect of heat insulation is seen Fig. 4, and spectral response is seen Fig. 5.It is thus clear that masterbatch has given PC sheet material transparent heat-insulated function really.
Other is with embodiment 4, and to obtain ATO content be 2.0% ATO-PC matrix material but masterbatch is diluted blend with 1: 9 mass ratio and pure PC particle in forcing machine, and through hot-forming 0.4mm and the thick ATO-PC sheet material of 1mm of obtaining, its spectral response is seen Fig. 5.
The ATO nano particle that respectively embodiment 1 is made mixes with 1: 99,1: 19,1: 9,1: 4 mass ratio and pure PC resin particle and is incorporated in the forcing machine blend and extrudes, and obtains ATO content and be 1.0%, 5%, 10% and 20% masterbatch.(RH7, Britain BOHLIN company) surveys its stress strain relationship with capillary rheometer, finds that ATO content is many more, the good more (see figure 6) of its processing flowability.HAKKE torque rheometer test also obtains similar conclusion, and promptly processing flowability increases with ATO content and improve (Fig. 7).The matrix material processing characteristics improves after adding ATO; Has significant application value; This means that we can make ultra-thin transparent heat-insulated coextruded layer with the coextruded layer (thick～50 μ m) of the direct Using P C sunlight board of masterbatch, can give the PC sunlight board transparent heat-insulated effect equally.
Claims (7)
1. PC sunlight board dedicated parent material, the preparation of described PC sunlight board dedicated parent material may further comprise the steps:
(1) using quality to carry out nanometer as 0.1～10% dispersion agent of ATO quality the ATO powder disperses and modification, obtains the ATO nano particle;
Described dispersion agent is a silane coupling agent, and described nanometer disperses to adopt following method with modification is concrete: silane coupling agent and ATO powder are added stirring in the entry obtain solid content in 15～55% suspension-s, adjusting pH of suspension value to 9～11; Gained suspension-s is carried out ball-milling processing, obtain slurries, regulate pH value to 6～8 rapidly; Again slurries evaporate to dryness and grinding are obtained the ATO nano particle;
Perhaps described dispersion agent is a Triple Pressed Stearic Acid, and described nanometer disperses and modification is concrete adopts following method: stirring in Triple Pressed Stearic Acid and the ATO powder adding absolute ethyl alcohol is obtained solid content at 15～30% suspension-s; Gained suspension-s is carried out ball-milling processing, obtain slurries; Again slurries evaporate to dryness and grinding are obtained the ATO nano particle;
(2) the ATO nano particle is melt blended into processes the ATO massfraction in the PC resin at 1%～50% PC sunlight board dedicated parent material.
2. by the described PC sunlight board of claim 1 dedicated parent material, it is characterized in that described ball-milling processing is specially: with the zirconium pearl is the ball milling pearl, and gained suspension-s was put into the ball mill ball milling 0.5-7.5 hour, removes the ball milling pearl then, obtains slurries.
3. by the described PC sunlight board of claim 2 dedicated parent material, it is characterized in that said zirconium pearl diameter is 0.1～1.5mm.
4. by the described PC sunlight board of claim 1 dedicated parent material, the adding quality that it is characterized in that said dispersion agent is 0.5～5% of an ATO quality.
5. by the described PC sunlight board of claim 1 dedicated parent material; It is characterized in that the described melt blending of step (2) is meant: ATO nano particle and PC resin particle are pressed the certain mass mixed; Blend is extruded under 220～280 ℃ temperature condition, makes the ATO massfraction at 1%～50% PC sunlight board dedicated parent material.
6. by claim 1 or 5 described PC sunlight board dedicated parent materials, it is characterized in that the ATO massfraction is 10%～30% in the described PC sunlight board dedicated parent material.
7. the application of PC sunlight board masterbatch as claimed in claim 1 in preparation PC sunlight board; The preparation method of said PC sunlight board comprises: with the blend dilution in the PC resin of PC sunlight board dedicated parent material; And extrude or be hot pressed into sheet material with molten state, obtain described PC sunlight board.
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| CN2010102382958A CN101921470B (en) | 2010-07-28 | 2010-07-28 | Special master batch for PC (Polycarbonate) sunlight board and application thereof |
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