CN106519092B - The method for preparing polymer nanocomposites as the Pickering lotion of emulsifier using organically-modified magadiite - Google Patents
The method for preparing polymer nanocomposites as the Pickering lotion of emulsifier using organically-modified magadiite Download PDFInfo
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- CN106519092B CN106519092B CN201611019424.8A CN201611019424A CN106519092B CN 106519092 B CN106519092 B CN 106519092B CN 201611019424 A CN201611019424 A CN 201611019424A CN 106519092 B CN106519092 B CN 106519092B
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- pickering lotion
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- 239000006210 lotion Substances 0.000 title claims abstract description 37
- 239000003995 emulsifying agent Substances 0.000 title claims abstract description 35
- 229920000642 polymer Polymers 0.000 title claims abstract description 34
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000000178 monomer Substances 0.000 claims abstract description 15
- 239000007870 radical polymerization initiator Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 229940117958 vinyl acetate Drugs 0.000 claims description 3
- -1 methyl methacrylate Ester Chemical class 0.000 claims description 2
- 239000002861 polymer material Substances 0.000 claims description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 2
- 230000000717 retained effect Effects 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims 1
- 239000012966 redox initiator Substances 0.000 claims 1
- 238000007720 emulsion polymerization reaction Methods 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 3
- 238000004945 emulsification Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract 1
- 239000000839 emulsion Substances 0.000 description 10
- 239000004926 polymethyl methacrylate Substances 0.000 description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000004908 Emulsion polymer Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- JKMXKNVVELCAQT-UHFFFAOYSA-N O[Si][Na] Chemical compound O[Si][Na] JKMXKNVVELCAQT-UHFFFAOYSA-N 0.000 description 2
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 239000012874 anionic emulsifier Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000007762 w/o emulsion Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses the methods for preparing polymer nanocomposites as the Pickering lotion of emulsifier using organically-modified magadiite.For this method using organically-modified magadiite as emulsifier, polymerized monomer prepares stable Pickering lotion as oily phase, and water-soluble radical polymerization initiator is then added, and carries out emulsion polymerization, polymer nanocomposites are prepared.The present invention replaces traditional surfactant to play emulsification using organically-modified magadiite solid particle, substantially reduces the usage amount of emulsifier, and nontoxic, has many advantages, such as environmentally protective.Preparation method simple process of the present invention, easy to operate, polymerizate are without post-processing.
Description
Technical field
The present invention relates to emulsion polymerizing preparations to close object technical field of nano material, and in particular to one kind is with organically-modified wheat
Hydroxyl silicon sodium stone is the method that the Pickering lotion of emulsifier prepares polymer nanocomposites.
Background technique
Emulsion polymerization is that monomer polymerization synthesizes a kind of high molecular common polymerization, it is using water as solvent, to ring
Border is highly beneficial.Emulsion polymerization is monomer by emulsifier and mechanical stirring, makes monomer be dispersed in water to form lotion, adds
Initiator causes monomer polymerization.The beginning of the thirties, emulsion polymerisation process have already appeared in industrial production.Include in many polymer
Synthetic rubber, synthetic fibers, synthetic plastic, flocculant, adhesive, synthetic resin coating and impact copolymer production in,
Emulsion polymerization has become one of main method, and the polymer produced in the world by emulsion polymerisation process every year is thousands of,
Vinyl emulsion-polymer emulsion is fastest-rising type, and acrylic emulsion-polymer emulsion is the largest one kind.It is poly-
It is significant in the expansion of five annual capacity of past to close the manufacture of object lotion, the main application fields of polymer emulsion are transport, durable consumer goods
And building and construction industry, and market have very high annual compound growth rate.Emulsion polymerization technology has world economy great
Meaning.
Emulsifier belongs to surfactant, it is the substance that can form micella, plays in emulsion polymerization important
Effect.It is also widely used in other each technical fields and daily life simultaneously.In general, emulsifier is reacting
It does not participate in reaction, but its one of main component as emulsion polymerization in the process, plays very important effect.Traditional lotion
Cationic emulsifier, anionic emulsifier, amphoteric emulsifier and non-ionic emulsification can be divided by polymerizeing the emulsifier used
Agent, and the emulsifier of these types and its system studied it is more thorough.More importantly traditional emulsifier has centainly
Toxicity, the stability of emulsion of formation is poor, and after polymerisation, emulsifier remains in polymeric articles, influence the performance of product,
It needs to post-process product after polymerization reaction, post processing cost is high and cannot eliminate completely.
Solid particle can make water phase and an oil phase form stable oil-in-water or water-in-oil emulsion, and use solid particle now
Stable emulsion is polymerize less.It is poly- instead of traditional emulsifier that magadiite (magadiite) can be used as emulsifier
Macromolecule is closed, and mixes to form polymer nanocomposites with macromolecule, and dosage is conventional emulsifier dosage
Percent zero point several can reach good emulsifying effectiveness；Organically-modified magadiite is used to be made as emulsifier
Pickering type lotion, carries out emulsion polymerization, and the research for forming polymer nanocomposites does not have so far.
Summary of the invention
It is the Pickering lotion of emulsifier that the purpose of the present invention is to provide a kind of based on organically-modified magadiite
The method for preparing polymer nanocomposites.
Using organically-modified magadiite as emulsifier, polymerized monomer is prepared stable the method for the present invention as oily phase
Water-soluble radical polymerization initiator is then added in Pickering lotion, carries out emulsion polymerization, polymer nanocomposite is prepared
Composite material.
The present invention is achieved through the following technical solutions.
The side of polymer nanocomposites is prepared using organically-modified magadiite as the Pickering lotion of emulsifier
Method includes the following steps:
(1) organically-modified magadiite is added in deionized water, stirs and heat up, makes organically-modified magadiite
It is evenly dispersed in deionized water；Cool down after being uniformly dispersed, polymerized monomer is added, continues to stir, be formed uniform and stable
Pickering lotion；
(2) Pickering lotion is heated, water-soluble radical polymerization initiator is added dropwise；Heating carries out anti-after being added dropwise
It answers, cools down after reaction, stop stirring, discharging.
Further, in step (1), the deionized water is the 50wt%-90wt% of Pickering lotion.
Further, in step (1), the organically-modified magadiite is the 0.01wt%-1wt% of polymerized monomer.
Further, in step (1), the organically-modified magadiite is to change by quaternary ammonium salt, quaternary alkylphosphonium salt or silane
The magadiite of property.
Further, in step (1), the polymerized monomer includes styrene, methyl methacrylate or vinylacetate.
Further, in step (1), the heating is to be warming up to 60-80 DEG C.
Further, in step (1), the cooling is to be cooled to 40-60 DEG C.
Further, in step (2), the water-soluble radical polymerization initiator is the 0.1wt%- of polymerized monomer
0.5wt%。
Further, in step (2), the water-soluble radical polymerization initiator includes that persulfate and redox are drawn
One of hair system.
Further, in step (2), the heating is heated to 70-90 DEG C.
Further, in step (2), the reaction is in 80-90 DEG C of reaction 1-5h.
Further, in step (2), the cooling is to be cooled to 50 DEG C or less.
Further, organically-modified magadiite particle, which is retained in the polymer material of synthesis, constitutes the polymer
Nanocomposite.
Further, which stirs.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) present invention uses organically-modified magadiite as the emulsifying effectiveness of Pickering lotion made of emulsifier
Good, the dosage that the dosage of organically-modified magadiite compares conventional emulsifier significantly reduces, and substantially reduces the use of emulsifier
Amount, save the cost；
(2) organically-modified magadiite is a kind of mineral clay, nontoxic, not can cause environmental pollution, also not
The health of the mankind can be jeopardized；
(3) the organically-modified magadiite particle reservation of the present invention may make up polymer nanocomposites in the material,
Product does not need to post-process after polymerization, and economic benefit improves, environmentally friendly；
(4) present invention uses organically-modified magadiite strong as Pickering stability of emulsion made of emulsifier, no
Vulnerable to the influence of the external environments such as temperature, there are long-time stability；
(5) biocompatibility that organically-modified magadiite and organism have had, does not influence polymer nanocomposite composite wood
Material is in the daily lifes such as the industrial circles such as oil exploitation, cosmetics and food and the extensive use of field of medicaments；
(6) the method for the present invention simple process, it is easy to operate.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of polymer nanocomposites obtained in embodiment 1；
Fig. 2 is the infrared spectrogram of polymer nanocomposites obtained in embodiment 2；
Fig. 3 is the infrared spectrogram of polymer nanocomposites obtained in embodiment 3；
Fig. 4 is the X-ray diffractogram of polymer nanocomposites obtained in embodiment 3.
Specific embodiment
The present invention is described in further details with reference to the accompanying drawings and examples, but the present invention is not limited to following implementations
Example.
Embodiment 1
(1) it is sequentially added into three-necked flask and accounts for the deionized water of total emulsion quality 50%, accounts for polymerized monomer quality 0.01%
The modified magadiite of cetyl triphenyl quaternary alkylphosphonium salt, start stirring, be warming up to 60 DEG C, make organically-modified magadiite
It is evenly dispersed in water after, be cooled to 40 DEG C, methyl methacrylate monomer be then added, with oar propeller be stirred continuously mixing it is molten
Liquid makes mixed solution form uniform and stable Pickering lotion；It takes suitable lotion to finger bottle, divides before can be observed
The water-oil phase of layer becomes uniform milky milk, and by standing observation, lotion remains stable.
(2) heating Pickering lotion to 70 DEG C, account for methyl methacrylate monomer quality be 0.1% ammonium persulfate
It is added in three-necked flask by constant pressure funnel, the container of splendid attire is washed with deionized after being added dropwise, and be added to
In flask；80 DEG C are warming up to the reaction was continued 1h, starts to cool down later；When reaction mass temperature is down to 50 DEG C or less, stop stirring
It mixes, discharges.
The infrared spectrogram of obtained polymer nanocomposites by Fig. 1 as shown in Figure 1, shown, 1734 cm-1For C=O
The stretching vibration characteristic peak of double bond, and the intensity at peak is big；1488 cm-1With 1448 cm-1It is-CH2Bending vibration characteristic absorption
Peak；1281 cm-1With 1244 cm-1It is the asymmetric stretching vibration characteristic peak of-C-O-C-；It is found that obtained polymer is poly-
Methyl methacrylate；And it proves that magadiite is stayed by test and forms polymer nanocomposites in the polymer.
The measurement of molecular weight and its dispersibility, obtained knot are carried out to obtained product with gel permeation chromatography (GPC)
Fruit is as shown in table 1.
The molecular weight and its dispersibility of 1 polymethyl methacrylate of table (PMMA) nanocomposite
| Mn | Mw | Mz | Mz+1 | Polydispersity |
| 165639 | 435675 | 903508 | 1349719 | 2.630267 |
As shown in Table 1, the polymethyl methacrylate of higher molecular weight can be obtained by Pickering emulsion polymerization, number
Average molecular weight is 165639, and the polydispersity (Mw/Mn) of polymethyl methacrylate is about 2.63, and molecular weight distribution is wide.
Embodiment 2
(1) deionized water for accounting for lotion gross mass 70% is sequentially added into three-necked flask, accounting for polymerized monomer quality is 0.5%
The quaternary ammonium salt-modified magadiite of cetyl triphenyl, start stirring, be warming up to 70 DEG C, make organically-modified magadiite
It is evenly dispersed in water after, be cooled to 50 DEG C, styrene monomer be then added, be stirred continuously mixed solution with oar propeller, make to mix
It closes solution and forms uniform and stable Pickering lotion；
(2) heating Pickering lotion is led to 80 DEG C the cumyl peroxide that styrene monomer quality is 0.3% is accounted for
It crosses constant pressure funnel to be added in three-necked flask, the container of splendid attire is washed with deionized after being added dropwise, and be added to burning
In bottle；85 DEG C are warming up to the reaction was continued 3h, starts to cool down later；When reaction mass temperature is down to 50 DEG C or less, stop stirring,
Discharging.
The infrared spectrograms of obtained polymer nanocomposites is as shown in Fig. 2, Fig. 2 is shown, 3000-3100 cm-1It is
Phenyl ring=CH stretching vibration characteristic peak；2924 cm-1With 2851 cm-1It is CH respectively2Asymmetry and symmetrical stretching vibration it is special
Levy peak；Confirm that obtained polymer is polystyrene；And it proves that magadiite is stayed by test and forms polymer in the polymer
Nanocomposite.
Embodiment 3
(1) it is sequentially added into three-necked flask and accounts for the deionized water that lotion gross mass is 90%, accounting for polymerized monomer quality is 1%
The modified magadiite of gamma-aminopropyl-triethoxy-silane, start stirring, be warming up to 80 DEG C, make organically-modified wheat hydroxyl silicon sodium
Stone it is evenly dispersed in water after, be cooled to 60 DEG C, vinyl acetate monomer be then added, with oar propeller be stirred continuously mixing it is molten
Liquid makes mixed solution form uniform and stable Pickering lotion；
(2) heating Pickering lotion to 90 DEG C, then account for vinyl acetate monomer quality be 0.5% hydrogen peroxide
It is added in three-necked flask by constant pressure funnel, the container of splendid attire is washed with deionized after being added dropwise, and be added to
In flask；90 DEG C of the reaction was continued 5h of heat preservation, start to cool down later；When reaction mass temperature is down to 50 DEG C or less, stop stirring,
Discharging.
The infrared spectrogram of obtained polymer nanocomposites is as shown in figure 3, in 2925 cm-1Place is the flexible vibration of C-H
Dynamic characteristic peak；1739 cm-1Place is the stretching vibration characteristic peak of C=O, and intensity is larger；1443 cm-1Place is CH2 Bending vibration
Dynamic characteristic peak；It is found that obtained polymer is polyvinyl acetate.
X-ray diffraction test is carried out to product, test results are shown in figure 4: the characteristic diffraction peak in 2 θ=4.34 ° is poly-
The characteristic diffraction peak of vinyl acetate, 24.76 ° -28.60 ° be magadiite characteristic peak region；Illustrate magadiite conduct
Emulsifier successfully prepares polymer, and magadiite is stayed and formed polymer nanocomposites in the polymer.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (8)
1. preparing the side of polymer nanocomposites using organically-modified magadiite as the Pickering lotion of emulsifier
Method, which comprises the steps of:
(1) organically-modified magadiite is added in deionized water, stirs and heat up, keeps organically-modified magadiite uniform
Dispersion is in deionized water；Cool down after being uniformly dispersed, polymerized monomer is added, continues to stir, forms uniform and stable Pickering
Lotion；The deionized water is the 50wt%-90wt% of Pickering lotion；The organically-modified magadiite is that polymerization is single
The 0.01wt%-1wt% of body；
(2) Pickering lotion is heated, water-soluble radical polymerization initiator is added dropwise；Heating is reacted after being added dropwise, instead
Cool down after answering, stops stirring, discharging.
2. according to claim 1 prepare polymerization by the Pickering lotion of emulsifier of organically-modified magadiite
The method of object nanocomposite, which is characterized in that in step (1), the organically-modified magadiite be by quaternary ammonium salt,
Quaternary alkylphosphonium salt or silane-modified magadiite.
3. according to claim 1 prepare polymerization by the Pickering lotion of emulsifier of organically-modified magadiite
The method of object nanocomposite, which is characterized in that in step (1), the polymerized monomer includes styrene, methyl methacrylate
Ester or vinylacetate.
4. according to claim 1 prepare polymerization by the Pickering lotion of emulsifier of organically-modified magadiite
The method of object nanocomposite, which is characterized in that in step (1), the heating is to be warming up to 60-80 DEG C；The cooling is
It is cooled to 40-60 DEG C.
5. according to claim 1 prepare polymerization by the Pickering lotion of emulsifier of organically-modified magadiite
The method of object nanocomposite, which is characterized in that in step (2), the water-soluble radical polymerization initiator is that polymerization is single
The 0.1wt%-0.5wt% of body.
6. according to claim 1 prepare polymerization by the Pickering lotion of emulsifier of organically-modified magadiite
The method of object nanocomposite, which is characterized in that in step (2), the water-soluble radical polymerization initiator includes over cure
One of hydrochlorate and redox initiation system.
7. according to claim 1 prepare polymerization by the Pickering lotion of emulsifier of organically-modified magadiite
The method of object nanocomposite, which is characterized in that in step (2), the heating is heated to 70-90 DEG C；The reaction is
In 80-90 DEG C of reaction 1-5h；The cooling is to be cooled to 50 DEG C or less.
8. according to claim 1 prepare polymerization by the Pickering lotion of emulsifier of organically-modified magadiite
The method of object nanocomposite, which is characterized in that organically-modified magadiite particle is retained in the polymer material of synthesis
It is middle to constitute the polymer nanocomposites；Preparation process whole process stirring.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611019424.8A CN106519092B (en) | 2016-11-21 | 2016-11-21 | The method for preparing polymer nanocomposites as the Pickering lotion of emulsifier using organically-modified magadiite |
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|---|---|---|---|
| CN201611019424.8A CN106519092B (en) | 2016-11-21 | 2016-11-21 | The method for preparing polymer nanocomposites as the Pickering lotion of emulsifier using organically-modified magadiite |
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| Publication Number | Publication Date |
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| CN106519092A CN106519092A (en) | 2017-03-22 |
| CN106519092B true CN106519092B (en) | 2019-01-18 |
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| CN108641024B (en) * | 2018-05-15 | 2021-03-30 | 华南理工大学 | Method for synthesizing magadiite/PMMA (polymethyl methacrylate) nano composite microspheres in Pickering emulsion by utilizing pH value regulation |
| CN111087538B (en) * | 2020-01-02 | 2021-02-05 | 中国科学院长春应用化学研究所 | W/O emulsion and preparation method thereof, polymer particles and preparation method thereof |
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| WO2004101691A2 (en) * | 2003-05-02 | 2004-11-25 | Dow Global Technologies Inc. | Coating and filler compositions comprising platy layered silicate pigments |
| CN104558356A (en) * | 2014-12-25 | 2015-04-29 | 常州大学 | Method for synthesizing Pickering-type emulsion through semi-continuous polymerization |
| CN105496799A (en) * | 2015-12-28 | 2016-04-20 | 西北工业大学 | Stable photo-responsive Pickering emulsion with photosensitive POSS hybrid particles as emulsifying agent and preparation method |
| CN105858678A (en) * | 2016-02-29 | 2016-08-17 | 华南理工大学 | Preparation method of hybrid type interpenetrating-network-structure material based on magadiite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004101691A2 (en) * | 2003-05-02 | 2004-11-25 | Dow Global Technologies Inc. | Coating and filler compositions comprising platy layered silicate pigments |
| CN104558356A (en) * | 2014-12-25 | 2015-04-29 | 常州大学 | Method for synthesizing Pickering-type emulsion through semi-continuous polymerization |
| CN105496799A (en) * | 2015-12-28 | 2016-04-20 | 西北工业大学 | Stable photo-responsive Pickering emulsion with photosensitive POSS hybrid particles as emulsifying agent and preparation method |
| CN105858678A (en) * | 2016-02-29 | 2016-08-17 | 华南理工大学 | Preparation method of hybrid type interpenetrating-network-structure material based on magadiite |
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