CN110229433A - A kind of PS nanocomposite and preparation method thereof - Google Patents
A kind of PS nanocomposite and preparation method thereof Download PDFInfo
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- CN110229433A CN110229433A CN201810183215.XA CN201810183215A CN110229433A CN 110229433 A CN110229433 A CN 110229433A CN 201810183215 A CN201810183215 A CN 201810183215A CN 110229433 A CN110229433 A CN 110229433A
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- liquid medium
- paste
- mixing
- nano material
- nanocomposite
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000002086 nanomaterial Substances 0.000 claims abstract description 101
- 238000002156 mixing Methods 0.000 claims abstract description 87
- 239000007788 liquid Substances 0.000 claims abstract description 78
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 13
- 239000012752 auxiliary agent Substances 0.000 claims description 50
- -1 esters salt Chemical class 0.000 claims description 21
- 229920001169 thermoplastic Polymers 0.000 claims description 20
- 239000011229 interlayer Substances 0.000 claims description 16
- 239000004094 surface-active agent Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000002309 gasification Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 241000446313 Lamella Species 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 239000010410 layer Substances 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 229910052976 metal sulfide Inorganic materials 0.000 claims description 5
- 230000001052 transient effect Effects 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 238000005253 cladding Methods 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 3
- 125000000623 heterocyclic group Chemical group 0.000 claims description 3
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- 238000002604 ultrasonography Methods 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 239000008239 natural water Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
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- 239000011574 phosphorus Substances 0.000 claims 1
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- 238000012545 processing Methods 0.000 abstract description 6
- 238000002474 experimental method Methods 0.000 abstract description 4
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- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
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- 239000005995 Aluminium silicate Substances 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 3
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 3
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- 239000004594 Masterbatch (MB) Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 235000012211 aluminium silicate Nutrition 0.000 description 3
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- 238000006243 chemical reaction Methods 0.000 description 3
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
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- 239000000203 mixture Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
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- XYXJKPCGSGVSBO-UHFFFAOYSA-N 1,3,5-tris[(4-tert-butyl-3-hydroxy-2,6-dimethylphenyl)methyl]-1,3,5-triazinane-2,4,6-trione Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C)=C1CN1C(=O)N(CC=2C(=C(O)C(=CC=2C)C(C)(C)C)C)C(=O)N(CC=2C(=C(O)C(=CC=2C)C(C)(C)C)C)C1=O XYXJKPCGSGVSBO-UHFFFAOYSA-N 0.000 description 2
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- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229950008882 polysorbate Drugs 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- GGHPAKFFUZUEKL-UHFFFAOYSA-M sodium;hexadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCOS([O-])(=O)=O GGHPAKFFUZUEKL-UHFFFAOYSA-M 0.000 description 1
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000011115 styrene butadiene Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 1
- 229960002415 trichloroethylene Drugs 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- FLTJDUOFAQWHDF-UHFFFAOYSA-N trimethyl pentane Natural products CCCCC(C)(C)C FLTJDUOFAQWHDF-UHFFFAOYSA-N 0.000 description 1
- 239000004846 water-soluble epoxy resin Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- 239000002888 zwitterionic surfactant Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to field of nanocomposite materials, specifically, being related to a kind of PS nanocomposite, PS nanocomposite is to be made by mixing through melt blending;Mixing includes PS, is combined with nano material and liquid medium on PS particle.Further relate to a kind of preparation method of PS nanocomposite, comprising: (1) nano material, liquid medium are mixed, paste is made;(2) paste and PS are mixed, covers paste in PS particle surface, mixing is made;(3) by mixing melt blending, nanocomposite is made.Mixing of the invention will not skid after being added in the equipment such as extruder, nanocomposite can directly be prepared, it is not necessary that other materials are added during the preparation process, processing easy to produce, and avoid the problem that nanocomposite performance is poor caused by liquid medium in the prior art gasifies too early, through experiments, it was found that compared with the prior art, nanocomposite performance made from mixing of the invention is more superior.
Description
Technical field
The present invention relates to field of nanocomposite materials, specifically, being related to a kind of using PS as the nanocomposite of base-material
And preparation method thereof.
Background technique
It is squeezed out in existing technology frequently with stratified nano materials and mixed with polymers, forms composite material, although such
The tensile strength of composite material is promoted, but the problems such as due to the poor compatibility of stratified nano materials and polymer, is caused
The impact resistance of such material is not generally high.
To solve the above problems, enabling polymer in the interlayer of stratified nano materials frequently with modes such as intercalation in-situ polymerizations
It reacts to improve the impact resistance of composite material, but the process is time-consuming longer, polymeric reaction condition is harsh, and molten
Agent is not easily recycled, and can bring the variations such as environmental pollution.
Patent No. CN101081928A proposes a kind of preparation method of polyamide/nano montmorillonite masterbatch, auxiliary using water
Help method to prepare polyamide/nano montmorillonite masterbatch, it is intercalator that preparation method, which is with deionized water, by the montmorillonite of purifying and
Mud is added step-wise to the polyamide that prescription amount melts completely by deionized water mixing, fully dispersed obtained montmorillonite mud, then
Polyamide/nano montmorillonite masterbatch is obtained through extruding pelletization.Preparation method is simple, and production cost is low, but this method is poly-
Montmorillonite mud is added after amide melting, montmorillonite mud is will lead to and has not enough time to be thoroughly mixed with copolymer, interlayer
Water just because of high-temperature gasification, causes polyamide to fail to timely enter interlayer, meanwhile, it is insufficient only by the energy of water generation
Will be completely exfoliated between cheating engaging layer thus cannot obtain the composite material that type is completely exfoliated, properties of product are also received greatly
Influence.
In view of this, the present invention is specifically proposed.
Summary of the invention
In order to solve the problems existing in the prior art, the present invention provides a kind of PS nanocomposite, properties of product are more
Add superior.
In order to achieve the above objectives, the present invention specifically adopts the following technical scheme that
A kind of PS nanocomposite, PS nanocomposite are to be made by mixing through melt blending;
Mixing includes PS, is combined with nano material and liquid medium on PS particle.
Mixing of the invention will not skid after being added in the equipment such as extruder, can directly prepare nanocomposite, nothing
Other materials, processing easy to produce need to be added during the preparation process, and avoid liquid medium in the prior art and gasify too early and lead
The poor problem of the nanocomposite performance of cause, through experiments, it was found that, compared with the prior art, received made from mixing of the invention
Nano composite material performance is more superior.
The paste that PS particle surface covers nano material and liquid medium is mixed to form.
Mud made from the prior art is semiliquid, in the preparation process of nanocomposite, is needed in a high voltage state
It is added into reaction system, makes troubles to production and processing, to solve the above problems, the present invention provides a kind of paste, institute
Stating paste is semisolid, can be added under passive state into reaction system, processing easy to produce, which can be mixed with PS
It closes, and covers in PS particle surface, obtain mixing.
Preferably, also contain auxiliary agent in paste.
Specifically, the mixture of nano material and liquid medium viscosity under the action of auxiliary agent increases to form paste, this hair
Bright auxiliary agent also improves the boiling point of liquid medium, further avoids liquid medium in the prior art and receives caused by gasifying too early
The poor problem of nano composite material performance.
Paste includes: 1 parts by weight of nano material, liquid medium 5-100 parts by weight, auxiliary agent 0-50 parts by weight, but is not
0。
Preferably, paste includes: 1 parts by weight of nano material, liquid medium 5-20 parts by weight, auxiliary agent 2-10 parts by weight,
It but is not 0;
It is furthermore preferred that paste includes: 1 parts by weight of nano material, 10 parts by weight of liquid medium, 5 parts by weight of auxiliary agent, but not
It is 0.
The consistency of paste is 0-100mm, but is not 0.Consistency corresponds to standard JBJ/T70-2009.
The mass ratio of nano material and PS are 0.1-20:100;It is preferred that 1-10:100;More preferable 4:100.
Also incorporate age resister on PS particle, the mass ratio of age resister and PS are 0.1:100~1:100;It is preferred that
0.3:100;
Nano material is stratified nano materials;In the composite material, stratified nano materials are at least partly in interlayer stripping
From.
Nano material is phyllosilicate, layered titanate, layer dress phosphate, layered metal hydroxides, transition metal
Oxyhalide, lamellar graphite, transient metal sulfide, layered metal oxide, laminated metal nitride, laminated metal carbonization
Object, the mixing of two-dimensional metallic organic frame one or more.
When nano material is ionic stratified nano materials, nanocomposite XRD diffraction pattern is within the scope of 2 2-10 ° of the angles θ
Without interlamellar spacing characteristic peak.
Auxiliary agent includes carboxylate surface active agent, sulfate salt surfactant, sulfosalt surfactant, phosphate ester salt
Surfactant, amine salt surfactant, quaternary surfactant, heterocyclic type surfactant, nonionic surfactant,
Natural water soluble high molecular, synthetic water soluble high molecular;
The boiling point of liquid medium is lower than the plasticization temperature of PS, and preferably shorter than 180 DEG C, liquid medium includes water.
Specifically, stratified nano materials include ionic stratified nano materials, non-ionic stratified nano materials.
One, ionic stratified nano materials include:
Cationic nano lamellar material include: montmorillonite, inorganic phosphate, phyllosilicate, kaolin, sepiolite,
Titanate;
Anionic nano lamellar material includes: hydrotalcite (LDHs)
Two, non-ionic nano lamellar material includes:
1. carbon material: graphene.
2. graphene analog: the element of the 4th main group of the periodic table of elements, such as silene, germanium alkene, boron alkene, arsenic alkene, black phosphorus.
3. transient metal sulfide (TMDs): coordination environment and oxidation state based on metallic atom, transient metal sulfide
(TMDs) insulator (HfS2), semiconductor (MoS2), semimetal (TiSe2) and all-metal (NbSe2) can be formed, or even low
Transient metal sulfide (TMDs) can show superconductivity under the conditions of temperature.It is reported in the literature at present to have more than 40 laminate transition
Metal sulfide.
4. layered metal oxide: MoO3, V2O3, V2O5, Al2O3, chromium oxide, TiO2, BiOCl, MnO2.
5. the oxide of layered metal hydroxides, perovskite.
6. metal nitride, carbide: h-BN, nitrogen carbide (g-C3N4).
7. two-dimensional metallic organic framework materials: the MOF for having been carried out removing includes: [Cu2Br (IN) 2] n (different cigarette of IN=
Acid), Zn-BDC (BDC=terephthalic acid (TPA)), it is brilliant to remove manganese -2,2- dimethyl succinate (MnDMS) block in ethanol, in methanol
[Zn2 (bim) 4] (bim=benzimidazole) is removed with the in the mixed solvent of propyl alcohol, in the mixed of n,N-Dimethylformamide and acetonitrile
It grows to obtain ultra-thin 2D CuBDC and ZnBDC MOF material by diffusion control MOF in bonding solvent.M-TCPP ultrathin nanometer piece (M
=Zn, Cu, Cd, Co;TCPP=5,10,15,20- tetra- (4- carboxyl phenyl) porphines).
8. transition metal oxyhalide: LiCoO2, FeOCl etc..
Auxiliary agent includes surfactant, water soluble polymer.
Specifically, surfactant includes:
1, anionic surfactant: it is divided into carboxylate, sulfuric acid, sulfonate and phosphate ester salt.
(1) soap kind is higher fatty acid salt, and general formula of molecular structure is (RCOO)-nMn+.With stearic acid, oleic acid, laurel
Acid etc. is more common.According to the difference of its metal ion (Mn+), there are alkali metal soap, alkaling earth metal base and organic amine soap etc..
(2) hydrosulphate is mainly the sulfuric acid ester of sulfated oil and higher aliphatic, general formula of molecular structure ROSO3-M
+, there are commonly lauryl sodium sulfate (also known as " sldium lauryl sulfate "), sodium hexadecyl sulfate (also known as " cetanol sulfuric acid
Sodium "), sodium stearyl sulfate (also known as " stearyl alcohol sodium sulphate ") etc..
(3) sulphonic acid compound mainly has aliphatic sulfonic compound, sulfo group aryl sulfonic acid compound, sulfo group naphthalene sulfonic acids compound etc.
2, cationic surfactant: containing nitrogen-atoms in the hydrophilic group ion of cationic surfactant, according to nitrogen original
The position difference of son in the molecule is divided into amine salt, quaternary ammonium salt and heterocyclic type three classes.Such as benzalkonium chloride (trade name " geramine "), benzene
Prick bromine ammonium (trade name " bromogeramine "), chlorination (bromination) cetyl pyridinium (trade name " Xi Bailin ") etc.
3, zwitterionic surfactant: lecithin, amino acid pattern, betaine type
4, nonionic surfactant: fatty glyceride, fatty acid sorbitan (sapn), polysorbate (tween), alkane
Base phenol polyethenoxy ether, fatty alcohol polyoxyethylene ether, fatty acid methyl ester APEO, detergent series.
Water soluble polymer includes:
1, natural class macromolecule
Starch
Seaweeds: sodium alginate, agar-agar.
Natural plant gum class: Arabic gum, tragacanth gum, locust bean gum, tamarind seed polysaccharide glue, sesbania gum, carrageenan, guar gum, fruit
Glue.
Animal glue class: gelatin, casein, chitosan.
Microbiological gum: xanthan gum, gellan gum, hyaluronic acid.
2, class organic polymer and its prepolymer are synthesized
(1) polymeric type water soluble polymer
Polyacrylamide, polyacrylic acid, polymethylacrylic acid and its copolymer, polyvinyl alcohol, polyethylene glycol, polyoxyethylene
Alkene, polyvinylpyrrolidone, polymaleic anhydride, polydimethyl diallyl ammonium chloride, polyvinylamine, poly- divinyl imidazoles
Quinoline, sulfonate styrene maleic anhydride copolymer, opens Pu Shi resin at kayexalate.
(2) polycondensation class water soluble polymer
Water soluble amino resin, water soluble phenol resin, water soluble alkyd resin, water-soluble epoxy resin, water-soluble poly
Urethane resin, polyethylene imine, poly-aspartate, poly-epoxy succinic acid, polyamine epichlorohydrin resin, polyamide second two
Urea formaldehyde, ammonia-epichlorohydrin resin, heavy polyamine epichlorohydrin resin, ammonia-dimethylamine-epichlorohydrin resin, N, N-
Dimethyl 1,3- propane diamine and epichlorohydrin resin.
(3) other
Water Soluble Maleic Anhydride oil, dicyandiamide formaldehyde resin, rosin amine-ethylene oxide condensate, poly N-ethylene yl acetamide, water
Dissolubility ficoll.
3, semi-synthetic class macromolecule
Modified cellulose and converted starch.
Liquid medium includes: isopentane, pentane, petroleum ether, hexane, hexamethylene, isooctane, trifluoroacetic acid, trimethyl
Pentane, pentamethylene, heptane, butyl chloride, trichloro ethylene, carbon tetrachloride, chlorotrifluoroethane, propyl ether, toluene, paraxylene,
Chlorobenzene, o-dichlorohenzene, diethyl ether, benzene, isobutanol, ethylene dichloride, n-butanol, butyl acetate, propyl alcohol, methylisobutylketone, four
Hydrogen furans, ethyl acetate, isopropanol, ethyl alcohol, chloroform, methyl ethyl ketone, dioxane, pyridine, acetone, nitromethane,
Acetic acid, acetonitrile, dimethylformamide, methanol, water, methylamine, dimethylamine, ether, pentane, methylene chloride, carbon disulfide, 1,1- bis-
Chloroethanes, trifluoroacetic acid, 1,1,1- trichloroethanes, ethyl alcohol, butanone, 1,2- dichloroethanes, glycol dimethyl ether, triethylamine,
Propionitrile, 4-methyl-2 pentanone, ethylenediamine, butanol, acetic acid, glycol monomethyl ether, octane, morpholine, ethylene glycol monoethyl ether, diformazan
Benzene, meta-xylene, acetic anhydride, ortho-xylene, N,N-dimethylformamide, cyclohexanone, cyclohexanol, furfural, N-METHYLFORMAMIDE.
Age resister includes:
Antioxidant:
Amine antioxidants have ketoamine condensation product, secondary diarylamine, substituted p-phenylenediamine, hindered amine.
Phenolic antioxidant, phenolic antioxidant can be divided into alkylation monophenols, alkylation polyphenol, thiobisphenol and polyphenol.Alkane
Base single phenol and polyphenol antioxidant principal item have antioxidant 264,1076,2246,1035,1010,3114 and 1790.Thiobis
The principal item of phenol has antioxidant 2246 and 300.Polyatomic phenol antioxidant principal item has 2,5 1 di-t-butyl hydroquinones and 2,5
One or two amyl hydroquinones.
Thio-2 acid vinegar and phosphorous vinegar kind antioxidant, principal item have anti-aging agent TNP, Ultranox624 and Asia
Tricresyl phosphate (2, the tertiary T base phenyl of soul one or two) ester.
Other type antioxidants, 2 one coloured glaze base benzo miaow trade name antioxidant MBs, nickel dibutyl dithiocarbamate
Trade name antioxidant NBC, there are also zinc dialkyl dithiophosphates.
Primary anti-oxidant has: anti-aging agent RD, antioxidant A W, antioxidant BLE, antioxidant A, anti-aging agent OD, 4,4 '-bis- (α-
Methylbenzyl) diphenylamines, 4,4 '-bis- (α, α-methylbenzyl) diphenylamines, N, N ,-di-sec-butyl-p-phenyl enediamine, anti-aging agent 4030,
Antioxidant 4010, antioxidant 4010NA, antioxidant 4020, antioxidant 264, antioxidant 1076, antioxidant 2216, antioxidant
1035, antioxidant 1010, antioxidant 3114, antioxidant 1790, antioxidant 2246, DBH 2,5 di tert butylhydroquinone, anti-oxidant DLTP,
Antioxidant TNP, Ultranox624, phosphorous acid three (the tertiary T base phenyl of 2,4- bis-) ester, antioxidant MB, antioxidant NBC, dialkyl group two
Thiophosphoric acid zinc.
The present invention also provides a kind of mixings, comprising: paste and PS;Paste includes: 1 parts by weight of nano material, liquid
Body medium 5-100 parts by weight, auxiliary agent 0-50 parts by weight, but be not 0;Paste, which is covered, forms mixing in PS particle surface;
Preferably, during preparing paste, successively nano material and auxiliary agent are added into liquid medium and are divided
It dissipates;
It is furthermore preferred that dispersing mode includes ultrasound, shearing, stirring, ball milling, colloid mill;
It is further preferred that nano material and the adding manner of auxiliary agent include being added at one time and being added in batches.
The present invention also provides a kind of preparation methods of PS nanocomposite, comprising:
(1) nano material, liquid medium are mixed, paste is made;
(2) paste and PS are mixed, covers paste in PS particle surface, mixing is made;
(3) by mixing melt blending, nanocomposite is made.
In the preparation process of nanocomposite, mixing will not skid after being added in the equipment such as extruder, can be direct
Nanocomposite is prepared, it is not necessary that other materials, processing easy to produce are added during the preparation process, and is avoided in the prior art
The poor problem of nanocomposite performance caused by liquid medium gasifies too early, through experiments, it was found that, compared with the prior art, this
Nanocomposite performance made from the mixing of invention is more superior.
Step is additionally added auxiliary agent in (1).
During the melt blending of paste and PS, all hot melt processing technologies can be used, such as mixing, mill, screw rod
(parallel/taper/mono-/bis -/tri- screw rods).
In step (1), nano material is stratified nano materials, and liquid medium enters stratified nano materials interlayer.Auxiliary agent makes
More liquid mediums enter stratified nano materials interlayer, form paste.
In step (1), successively nano material and auxiliary agent are added into liquid medium and are dispersed, paste is made.
Dispersing mode includes ultrasound, shearing, stirring, ball milling, colloid mill.Nearly all dispersing mode can be used.It is described super
The frequency of sound is 800~1000Hz, and power is 200~1000W.
Nano material and the adding manner of auxiliary agent include being added at one time and being added in batches.
Nano material and the addition speed of auxiliary agent are respectively 0.01-100g/min, preferably 5-10g/min, more preferable 7g/
min。
In step (3), comprising:
(1) heat temperature raising, PS are mixed under the first stirring with the liquid medium in paste, nano material, soften
And the cladding that interpenetrates;
(2) after the boiling point that temperature is greater than liquid medium, liquid medium portion gasification, the gasification carries out the to mixing
Two stirrings.
In the preparation process of nanocomposite, there are the heat temperature raising stages, and at this stage, PS gradually softens and stirring
The effect of mixing is lower to be interpenetrated with paste, and PS and liquid medium and nano material is made to contact with each other cladding.
Liquid in step (3), when mixing melt blending, when temperature is greater than or equal to PS plasticization temperature, in paste
Medium further gasifies, and the nano material of reunion is separated.
In the melt blending stage, PS is in molten condition, at this point, liquid medium gasifies, divides the nano material reunited mutually
From PS is flow between nano material, to improve dispersion effect of the nano material in PS.
In step (3), when mixing melt blending, liquid medium gasification promotes the mobility of the mixing and promotes heat
Conduction, liquid medium gasification will be helpful to PS softening.
Nano material is stratified nano materials, and liquid medium enters stratified nano materials interlayer, step (3) in step (1)
When temperature is higher than polymer plasticization temperature, liquid medium gasification separates lamella.
When nano material in paste is stratified nano materials, liquid medium enters stratified nano materials in step (1)
Interlayer, in the melt blending stage, the liquid medium of stratified nano materials interlayer gasifies, and makes at least partly lamella separation, molten
The PS of state is flowed between isolated lamella, to improve dispersion effect of the nano material in PS.The unsegregated stratiform of lamella is received
Rice material interlamellar spacing increases, and the PS of molten condition flows into interlayer, to improve the compatibility of PS and stratified nano materials.
Step is additionally added age resister in (1).
When nano material in paste is stratified nano materials, auxiliary agent makes more liquid mediums enter laminar nano material
Between the bed of material, to further improve the interlamellar spacing of stratified nano materials.
When nano material is ionic stratified material, nanocomposite XRD diffraction pattern is within the scope of 2 2-10 ° of the angles θ without layer
Pitch characteristics peak.
In an embodiment of the present invention, double screw extruder includes solid conveying zone, melting zone and melt delivery area, mixing
It being added from barrel to solid conveying zone, the engine speed of double screw extruder is 30~80Hz, main feeding hopper revolving speed is 10~
30Hz, extrusion temperature be 150~200 DEG C of an area, two 230~280 DEG C of areas, three 230~280 DEG C of areas, four 230~280 DEG C of areas, five
230~280 DEG C of area;It is preferred that engine speed is 60Hz, main feeding hopper revolving speed is 20Hz, and extrusion temperature is 150~180 DEG C of an area,
Two 245~260 DEG C of areas, three 245~255 DEG C of areas, four 240~250 DEG C of areas, five 240~260 DEG C of areas.The linear velocity of screw speed
For 0.6~1m/s.
In mixing before melt blending, PS coats nano material and liquid medium, obtains mixture, molten
When melting blending, while mixture is by external shear action, also mixed under the two effect by the gasification of internal liquid medium
It closes object and explosion occurs, while liquid medium escapes, the PS of molten condition enters between nano material;When nano material is stratiform
When nano material, explosion also occurs for the interlayer of stratified nano materials, makes at least partly lamella separation, and the PS of molten condition, which enters, to be divided
From lamella between, the unsegregated stratified nano materials interlamellar spacing of lamella increases, and the PS of molten condition enters interlayer.It is quick-fried to realize
Broken, the melt pressure of PS should be greater than the vapour pressure of liquid medium.The present invention is also possible that and first coats to paste, then will coat
Paste mixed with thermoplastic elastomer (TPE), coating includes: styrene-acrylic emulsion, acrylic acid ester emulsion, acrylic emulsion, the third cream of silicon
Liquid, aqueous polyurethane emulsion, fluorine carbon emulsion, rosin resin lotion, terpinol, acrylate and vinyl acetate emulsion, aqueous epoxy resin emulsion, butylbenzene
Latex, Heveatex, white glue cream, polychloroprene latex, pure C latex, carboxylic styrene butadiene latex, styrene-acrylic latex.Above-mentioned cladding is greatly prolonged
Delay interlayer liquid medium in the release rate in melt blending stage, effectively prevent liquid medium that phase transformation, another party occurs to early
Face, the scale of the expansion of interlayer when further improving liquid medium phase transformation are conducive to polymer and travel further into interlayer reality
Now fill.
Compared with prior art, the invention has the following beneficial effects:
Mixing of the invention will not skid after being added in the equipment such as extruder, can directly prepare nanocomposite, nothing
Other materials, processing easy to produce need to be added during the preparation process, and avoid liquid medium in the prior art and gasify too early and lead
The poor problem of the nanocomposite performance of cause, through experiments, it was found that, compared with the prior art, received made from mixing of the invention
Nano composite material performance is more superior.
Detailed description of the invention
Fig. 1 is the SEM figure of graphene in paste of the invention.
Fig. 2 is the TEM figure of graphene in paste of the invention.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below to the technical side in embodiment
Case is clearly and completely described, and the following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
One, the preparation of paste
Nano material is montmorillonite, and liquid medium is water, and auxiliary agent is pectin, thermoplastic polymer PS, and age resister is
Antioxidant 264.
1 parts by weight of nano material
10 parts by weight of liquid medium
0.01 parts by weight of auxiliary agent
Successively nano material and auxiliary agent are added into liquid medium and are dispersed, wherein the addition of nano material and auxiliary agent
Speed is respectively 0.01g/min, and paste is made, and paste consistency is 2mm.
Two, the preparation of mixing
5 parts by weight of thermoplastic polymer
0.005 parts by weight of age resister
Paste, age resister are mixed with thermoplastic polymer, obtain mixing.
Three, the preparation of nanocomposite
By mixing melt blending, wherein mixing is added to double screw extruder solid conveying zone, double screw extruder
Engine speed is 30Hz, and main feeding hopper revolving speed is 10Hz, and extrusion temperature is 150 DEG C of an area, two 230 DEG C of areas, three 230 DEG C of areas, four
The linear velocity in 230 DEG C of area, five 230 DEG C of areas, screw speed is 0.6m/s, obtains nanocomposite.
Embodiment 2
Nano material is kaolin, and liquid medium is isopentane, and auxiliary agent is chitosan, thermoplastic polymer PS, anti-ageing
Agent is antioxidant TNP.
One, the preparation of paste
1 parts by weight of nano material
5 parts by weight of liquid medium
1.5 parts by weight of auxiliary agent
Successively nano material and auxiliary agent are added into liquid medium and are dispersed, wherein the addition of nano material and auxiliary agent
Speed is respectively 1g/min, and paste is made, and paste consistency is 10mm.
Two, the preparation of mixing
50 parts by weight of thermoplastic polymer
0.1 parts by weight of age resister
Paste, age resister are mixed with thermoplastic polymer, obtain mixing.
Three, the preparation of nanocomposite
By mixing melt blending, wherein mixing is added to double screw extruder solid conveying zone, double screw extruder
Engine speed is 60Hz, and main feeding hopper revolving speed is 20Hz, and extrusion temperature is 180 DEG C of an area, two 230 DEG C of areas, three 230 DEG C of areas, four
The linear velocity in 250 DEG C of area, five 250 DEG C of areas, screw speed is 0.8m/s, obtains nanocomposite.
Embodiment 3
Nano material is graphene, and liquid medium is dimethylamine, and auxiliary agent is xanthan gum, thermoplastic polymer PS, anti-ageing
Agent is antioxidant 3114.
One, the preparation of paste
1 parts by weight of nano material
30 parts by weight of liquid medium
5 parts by weight of auxiliary agent
Successively nano material and auxiliary agent are added into liquid medium and are dispersed, wherein the addition of nano material and auxiliary agent
Speed is respectively 10g/min, and paste is made, and paste consistency is 30mm.
Two, the preparation of mixing
100 parts by weight of thermoplastic polymer
1 parts by weight of age resister
Paste, age resister are mixed with thermoplastic polymer, obtain mixing.
Three, the preparation of nanocomposite
By mixing melt blending, wherein mixing is added to double screw extruder solid conveying zone, double screw extruder
Engine speed is 80Hz, and main feeding hopper revolving speed is 30Hz, and extrusion temperature is 200 DEG C of an area, two 250 DEG C of areas, three 250 DEG C of areas, four
The linear velocity in 280 DEG C of area, five 280 DEG C of areas, screw speed is 1m/s, obtains nanocomposite.
Embodiment 4
Nano material is montmorillonite, and liquid medium is acetonitrile, and auxiliary agent is polyacrylic acid, thermoplastic polymer PS, anti-ageing
Agent is antioxidant 1790.
One, the preparation of paste
1 parts by weight of nano material
50 parts by weight of liquid medium
10 parts by weight of auxiliary agent
Successively nano material and auxiliary agent are added into liquid medium and are dispersed, wherein the addition of nano material and auxiliary agent
Speed is respectively 30g/min, and paste is made, and paste consistency is 80mm.
Two, the preparation of mixing
500 parts by weight of thermoplastic polymer
5 parts by weight of age resister
Paste, age resister are mixed with thermoplastic polymer, obtain mixing.
Three, the preparation of nanocomposite
By mixing melt blending, wherein mixing is added to double screw extruder solid conveying zone, double screw extruder
Engine speed is 60Hz, and main feeding hopper revolving speed is 20Hz, and extrusion temperature is 150 DEG C of an area, two 260 DEG C of areas, three 245 DEG C of areas, four
The linear velocity in 240 DEG C of area, five 240 DEG C of areas, screw speed is 0.6m/s, obtains nanocomposite.
Embodiment 5
Nano material is kaolin, and liquid medium is chloroform, and auxiliary agent is poly-aspartate, and thermoplastic polymer PS resists
Aging agent is antioxidant 4020.
One, the preparation of paste
1 parts by weight of nano material
100 parts by weight of liquid medium
50 parts by weight of auxiliary agent
Successively nano material and auxiliary agent are added into liquid medium and are dispersed, wherein the addition of nano material and auxiliary agent
Speed is respectively 100g/min, and paste is made, and paste consistency is 100mm.
Two, the preparation of mixing
1000 parts by weight of thermoplastic polymer
10 parts by weight of age resister
Paste, age resister are mixed with thermoplastic polymer, obtain mixing.
Three, the preparation of nanocomposite
By mixing melt blending, wherein mixing is added to double screw extruder solid conveying zone, double screw extruder
Engine speed is 60Hz, and main feeding hopper revolving speed is 20Hz, and extrusion temperature is 180 DEG C of an area, two 245 DEG C of areas, three 255 DEG C of areas, four
The linear velocity in 240 DEG C of area, five 260 DEG C of areas, screw speed is 1m/s, obtains nanocomposite.
Embodiment 6
Nano material is graphene, and liquid medium is carbon disulfide, and auxiliary agent is dicyandiamide formaldehyde resin, thermoplastic polymer
For PS, age resister is antioxidant 1035.
One, the preparation of paste
1 parts by weight of nano material
10 parts by weight of liquid medium
2 parts by weight of auxiliary agent
Successively nano material and auxiliary agent are added into liquid medium and are dispersed, wherein the addition of nano material and auxiliary agent
Speed is respectively 7g/min, and paste is made, and paste consistency is 20mm.
Two, the preparation of mixing
25 parts by weight of thermoplastic polymer
0.2 parts by weight of age resister
Paste, age resister are mixed with thermoplastic polymer, obtain mixing, paste consistency is 50mm.
Three, the preparation of nanocomposite
By mixing melt blending, wherein mixing is added to double screw extruder solid conveying zone, double screw extruder
Engine speed is 30Hz, and main feeding hopper revolving speed is 10Hz, and extrusion temperature is 200 DEG C of an area, two 280 DEG C of areas, three 260 DEG C of areas, four
The linear velocity in 250 DEG C of area, five 240 DEG C of areas, screw speed is 1m/s, obtains nanocomposite.
Comparative example 1
Difference with embodiment 2 is only that, in the preparation process of paste, is added without auxiliary agent.
Comparative example 2
Difference with embodiment 2 is only that paste melt blending is added after reaching molten condition in thermoplasticity.
Test example 1
This test detects the mechanical property of embodiment 1-6 and comparative example 1,2 gained nanocomposites, as a result sees
Table 1.
Table 1
As can be seen from Table 1,2 gained nanocomposite performance of embodiment is better than comparative example 1, it follows that of the invention
The performance for improving nanocomposite by the way that auxiliary agent is added in the preparation process of paste.2 gained of embodiment is nano combined
Material property be better than comparative example 2, it follows that the present invention by the way that paste is first mixed with thermoplastic polymer, it is remelted total
The mixed performance for improving nanocomposite.
As seen from Figure 1, the sample obtained is in relatively transparent state, illustrates that graphene sheet layer is relatively thin, and agglomeration is not
Obviously.
As seen from Figure 2, the sample lamella obtained is very thin, can be considered the single-layer graphene peeled away stack and
At the surface folding of sample is because the material of two-dimensional structure is not easy to stablize individualism, and fold is stablized conducive to graphene, goes forward side by side
The sample that one step demonstrates is single layer or few layer graphene.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any to be familiar with technology people of the invention
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompt make it is a little change or be modified to
The equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, it is right according to the technical essence of the invention
Any simple modification, equivalent change and modification made by above embodiments, in the range of still falling within the present invention program.
Claims (10)
1. a kind of PS nanocomposite, which is characterized in that PS nanocomposite is to be made by mixing through melt blending;
Mixing includes PS, is combined with nano material and liquid medium on PS particle.
2. a kind of PS nanocomposite according to claim 1, which is characterized in that PS particle surface has covered a nanometer material
The paste that material is mixed to form with liquid medium;
Preferably, also contain auxiliary agent in paste.
3. a kind of PS nanocomposite according to claim 1 or 2, which is characterized in that nano material is laminar nano
Material;In the composite material, stratified nano materials are at least partly in splitting;
Preferably, nano material is phyllosilicate, layered titanate, layer dress phosphate, layered metal hydroxides, transition gold
Belong to oxyhalide, lamellar graphite, transient metal sulfide, layered metal oxide, laminated metal nitride, laminated metal carbonization
Object, the mixing of two-dimensional metallic organic frame one or more;
It is furthermore preferred that nanocomposite XRD diffraction pattern is at 2 2-10 ° of the angles θ when nano material is ionic stratified nano materials
Without interlamellar spacing characteristic peak in range.
4. a kind of PS nanocomposite according to claim 1 to 3, which is characterized in that the consistency of paste is 0-
100mm, but be not 0;
Preferably, paste includes: 1 parts by weight of nano material, liquid medium 5-100 parts by weight, auxiliary agent 0-50 parts by weight, but not
It is 0.
5. a kind of PS nanocomposite according to claim 1 to 4, which is characterized in that the matter of nano material and PS
Amount is than being 0.1-20:100;It is preferred that 1-10:100;More preferable 4:100;
Preferably, age resister is also incorporated on PS particle, the mass ratio of age resister and PS are 0.1:100~1:100;It is preferred that
0.3:100;
It is furthermore preferred that auxiliary agent includes carboxylate surface active agent, sulfate salt surfactant, sulfosalt surfactant, phosphorus
Acid esters salt surfactant, amine salt surfactant, quaternary surfactant, heterocyclic type surfactant, non-ionic surface
Activating agent, natural water soluble high molecular, synthetic water soluble high molecular;
It is further preferred that the boiling point of liquid medium is lower than the plasticization temperature of thermoplastic polymer, liquid medium includes water.
6. a kind of preparation method of PS nanocomposite characterized by comprising
(1) nano material, liquid medium are mixed, paste is made;
(2) paste and PS are mixed, covers paste in PS particle surface, mixing is made;
(3) by mixing melt blending, nanocomposite is made.
7. preparation method according to claim 6, which is characterized in that step is additionally added auxiliary agent in (1).
8. preparation method according to claim 6, which is characterized in that in step (3), comprising:
(1) heat temperature raising, PS are mixed under the first stirring with the liquid medium in paste, nano material, soften and mutual
Mutually infiltration cladding;
(2) after the boiling point that temperature is greater than liquid medium, liquid medium portion gasification, the gasification carries out second to mixing and stirs
It mixes.
9. preparation method according to claim 6, which is characterized in that in step (3), when mixing melt blending, in temperature
When greater than or equal to PS plasticization temperature, the liquid medium in paste further gasifies, and the nano material of reunion is separated;
Preferably, in step (3), when mixing melt blending, liquid medium gasification promotes the mobility and promotion of the mixing
The conduction of heat, liquid medium gasification will be helpful to PS softening;
It is furthermore preferred that nano material is stratified nano materials, liquid medium enters stratified nano materials interlayer in step (1), walks
Suddenly (3) temperature be higher than polymer plasticization temperature when, liquid medium gasification, lamella is separated.
10. a kind of mixing characterized by comprising paste and PS;Paste includes: 1 parts by weight of nano material, liquid Jie
Matter 5-100 parts by weight, auxiliary agent 0-50 parts by weight, but be not 0;Paste, which is covered, forms mixing in PS particle surface;
Preferably, during preparing paste, successively nano material and auxiliary agent are added into liquid medium and are dispersed;
It is furthermore preferred that dispersing mode includes ultrasound, shearing, stirring, ball milling, colloid mill;
It is further preferred that nano material and the adding manner of auxiliary agent include being added at one time and being added in batches.
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CN1752112A (en) * | 2004-09-20 | 2006-03-29 | 中国科学院化学研究所 | Montmorillonoid in-situ organises and prepares the method for nano composite polymer-montmorillonoid material |
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CN1752112A (en) * | 2004-09-20 | 2006-03-29 | 中国科学院化学研究所 | Montmorillonoid in-situ organises and prepares the method for nano composite polymer-montmorillonoid material |
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