CN1663969A - Process for preparing nano polymer with montmorillonite as template - Google Patents
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- CN1663969A CN1663969A CN 200510011348 CN200510011348A CN1663969A CN 1663969 A CN1663969 A CN 1663969A CN 200510011348 CN200510011348 CN 200510011348 CN 200510011348 A CN200510011348 A CN 200510011348A CN 1663969 A CN1663969 A CN 1663969A
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Abstract
The invention provides a method for preparing nanometer polymer with montmorillonite as mold, which comprises taking the MMT interlamination of the montmorillonite as monomer polymerization's reaction spacing, applying the intercalation character of the anion clay montmorillonite into the mold polymerization, plugging and assembling the polymeric monomer into the MMT interlamination, taking MMT as mold and the polymeric monomer generating polymerization in the mold, then separating the polymer. The invention is characterized in that the polymerization condition is easy to control, there are few influencing factors, and the prepared polymer is in nanometer size. Said polymer will have a broad application prospect in machinery, light, electricity, magnetism, micro processing unit, medicinal controlled release, environmental protection, body concealed material, high-performance coating material, nanometer reactor and biochemistry and so on.
Description
Affiliated field
The invention belongs to the nanometer polymer technical field, particularly providing a kind of is the method that template prepares nanometer polymer with the polynite.
Background technology
Nano material produces characteristics such as unusual mechanics, electronics, magnetics, calorifics, optics and chemically reactive owing to having surface effects, volume effect, quantum size effect and macro quanta tunnel effect, it be a kind of novel material be again the important source material that constitutes novel material.Therefore, the various countries scientist the exploitation of nano material and development as the field of new of giving priority to, Ri Ben " creating scientific and technical propelling cause ", the Star Wars Program of the U.S. and Eurika research programme in West Europe etc. for example.In recent years, the exploration of preparation of nanomaterials has become the focus of nano materials research.At present the method for the preparation of nanometer polymer material is a lot, and as molecule self-assembly, mechanical disintegration, organic synthesis, micro-emulsion polymerization, template polymerization or the like, wherein effectively the pattern of controlling polymers and particle diameter and cost are low for template, are easy to control.Template is meant selects a kind of material to grow in mould or grow around mould for " mould " impels component, and the geometric parameter of material will be subjected to the restriction of template.Therefore the shape and size that change template can realize that the expection of product structure is controlled.Employing has the film of nanometer micropore such as polycarbonate, Al
2O
3Films etc. or inorganic laminated clay be as template, makes monomer polymerization in these have the micropore of nanoscale or lamellar spacing, forms the material of nanometer polymer tubulose, wire or laminate structure.Template is more extensive and effective in the research work of preparation nanometer polymer.This work has adopted this layered inorganic material of polynite (montmorillonite is called for short MMT) as template, the polymkeric substance of preparation nano-scale special appearance in its confinement space.
Polynite is the layer stylolitization compound that the positively charged ion by silicon-oxy tetrahedron and alumina octahedral and interlayer filling tape positive charge constitutes, and belongs to anionic clay.But the constructional feature of polynite makes it have the performance of intercalation assembling, different monomer intercalations can be assembled between cheating engaging layer, and preparation has the functional materials of different qualities.
Summary of the invention
The object of the present invention is to provide a kind of is that template prepares nanometer polymer and preparation method thereof with polynite (MMT), realizes that the expection of product structure is controlled.
But the present invention is the intercalation property with the anionic clay polynite to be applied in the template polymerization reaction, promptly earlier the polymerization single polymerization monomer intercalation is assembled into the MMT interlayer, is template with MMT again, makes polymerization single polymerization monomer polymerization reaction take place in template.Owing to will be subjected to the restriction of template at the molecular chain structure of the confinement space of template interpolymer etc., therefore can prepare the polymkeric substance of nano-scale; Isolate polymkeric substance then.Concrete preparation process is as follows:
A splashes into polymerization single polymerization monomer (monomer) in the polynite aqueous solution, and solution quality concentration is generally 3-7%.Stirred 6～24 hours, whipping temp is 20～80 ℃, and decide on monomer solubleness size: solvability is stirring at room preferably, 60～80 ℃ of poorly soluble stirrings.Be washed to that polymeric monomer concentration reaches 1～9ppm (ppm is 1,000,000/order of magnitude) mol in the filtrate, 60～80 ℃ of dryings 18～25 hours, obtaining the interlayer object was the monomeric polynite template of institute's insertion polymerization then.With infrared spectra (IR), nuclear-magnetism (NMR), χ-ray diffraction (XRD) characterization method proof polymerization single polymerization monomer intercalation has been assembled into the interlayer of polynite.
B. the template MMT-polymerization single polymerization monomer (MMT-monomer) that steps A is obtained is dispersed in the aqueous solvent, looking the different weight ratios that add of template internal reaction polymerization single polymerization monomer is that (initiator is an ammonium persulphate for the initiator of 1-5%, Potassium Persulphate), reflux 6～25 hours, make the polymerization single polymerization monomer polymerization reaction take place in the template, filter then, wash,, obtain the polynite that the interlayer object is a polymkeric substance (MMT-polymer) 60～80 ℃ of dryings 20～25 hours.
The MMT-polymkeric substance (polymer) that obtains is carried out nuclear-magnetism characterize, can determine that monomer at interlayer polyreaction has taken place.
C. the laminate dissolving of the polynite that step B is obtained with hydrofluoric acid is separated polymkeric substance with separation method commonly used again.
Polynite of the present invention is the sodium base, the calcium base, and magnesium base etc.; Described polymerization single polymerization monomer is polymerizability quaternary ammonium salt or acid amides: wherein the polymerizability quaternary ammonium salt comprises: trimethylammonium allyl ammonium chloride, dimethyl diallyl ammonium chloride; Acid amides comprises: aniline, hexanolactam, acrylamide etc.The ion exchange capacity CEC of polynite (cationexchange capability) is 90～110 mmoles/100g (mmole mmol).
The invention has the advantages that: polymerizing condition is easy to control, and the polymerization influence factor is few, and the polymkeric substance of preparation has the nano-scale characteristics.This base polymer will have broad application prospects at aspects such as machinery, light, electricity, magnetic, microprogramming device, medicine controlled releasing, environment protection, stealth material, high-performance coating material, nano-reactor and biological chemistries.
Description of drawings
Fig. 1 is embodiment of the invention Na-MMT, DMDAAC-MMT, the XRD spectra of PDMDAAC-MMT.
Fig. 2 is the TEM photo of the Poly Dimethyl Diallyl Ammonium Chloride (PDMDAAC) of embodiment of the invention step C preparation.
Embodiment
Embodiment 1
A. 10g ion exchange capacity CEC=100mmol/100g sodium-based montmorillonite is added in the there-necked flask, to going into 200ml deionized water vigorous stirring 0.5 hour.Dimethyl diallyl ammonium chloride DMDAAC (dimethyl diallylammonium chloride) 16ml (0.05mol) is slowly splashed into stirring at room 24 hours.Centrifugal, wash to filtrate and splash into AgNO
3Do not produce till the white precipitate in the solution.70 ℃ of dryings 20 hours obtain the MMT-DMDAAC template.With characterization methods such as XRD and IR proofs monomer intercalation be assembled into the interlayer of polynite.Recording interlamellar spacing with XRD is 1.42nm.Molecular size and interlamellar spacing according to DMDAAC judge that monomer DMDAAC is in the interlayer monolayer alignment.
B takes by weighing polymerization single polymerization monomer dimethyl diallyl ammonium chloride initiator of polyreaction K
2S
2O
81.081g (0.004mol), be mixed with the aqueous solution of 0.016M with the 250ml deionized water; The template that step D is obtained is dispersed in this solution, reflux 20 hours, temperature of reaction is 60 ℃, make the monomer in the template carry out polymerization, filter, wash, 70 ℃ of dryings 20 hours, the polynite MMT-PDMDAAC. that obtains the interlayer object and be polymkeric substance with MMT-PDMDAAC carry out XRD, IR, NMR characterizes, and shows that DMDAAC at interlayer polymerization has taken place.
C. the laminate of the polynite that step B is obtained with hydrofluoric acid dissolves away, and obtains the clarifying aqueous solution, and this aqueous solution is dropwise joined in the acetone, after static 1 hour, faint yellow precipitation occurs, and centrifugal this turbid solution is separated bottom settlings absolute ethanol washing.At room temperature dry 24 hours.Obtain white powder PDMDAAC.This product is carried out NMR, TEM, IR test, and the result shows that product is the nanoscale polymkeric substance.
A. 10g CEC=93mmol/100g calcium-base montmorillonite is added in the there-necked flask, to going into 200ml deionized water vigorous stirring 0.5 hour.Dimethyl diallyl ammonium chloride DMDAAC (dimethyl diallyl ammoniumchloride) 14ml is slowly splashed into stirring at room 24 hours.Centrifugal, wash to filtrate splash into do not produce white precipitate in the AgNO3 solution till.70 ℃ of dryings 20 hours obtain the MMT-DMDAAC template.With characterization methods such as XRD and IR proofs monomer intercalation be assembled into the interlayer of polynite.Record interlamellar spacing with XRD and increased 0.46nm.Molecular size and interlamellar spacing according to DMDAAC judge that monomer DMDAAC is in the interlayer monolayer alignment.
B takes by weighing polymerization single polymerization monomer dimethyl diallyl ammonium chloride initiator of polyreaction K
2S
2O
81.081g (0.004mol), be mixed with the aqueous solution of 0.016M with the 250ml deionized water; The template that step D is obtained is dispersed in this solution, reflux 20 hours, temperature of reaction is 60 ℃, make the polymerization single polymerization monomer in the template carry out polymerization, filter, washing, 60 ℃ of dryings 24 hours, obtaining the interlayer object was the polynite MMT-PDMDAAC of polymkeric substance, MMT-PDMDAAC is carried out XRD, IR, NMR sign, show that DMDAAC at interlayer polymerization has taken place.
C. the laminate of the polynite that step B is obtained with hydrofluoric acid dissolves away, and obtains the clarifying aqueous solution, and this aqueous solution is dropwise joined in the acetone, after static 1 hour, faint yellow precipitation occurs, and centrifugal this turbid solution is separated bottom settlings absolute ethanol washing.At room temperature dry 24 hours.Obtain white powder PDMDAAC.This product is carried out NMR, TEM, IR test, and the result shows that product is the nanoscale polymkeric substance.
Embodiment 3
A. 10g CEC=100mmol/100g sodium-based montmorillonite is added in the there-necked flask, to going into 200ml deionized water vigorous stirring 0.5 hour.Dimethyl diallyl ammonium chloride DMDAAC (dimethyl diallyl ammoniumchloride) 22ml (0.07mol) is slowly splashed into, and 20 ℃ were stirred 24 hours.Centrifugal, wash to filtrate and splash into AgNO
3Do not produce till the white precipitate in the solution.70 ℃ of dryings 20 hours obtain the MMT-DMDAAC template.With characterization methods such as XRD and IR proofs monomer intercalation be assembled into the interlayer of polynite.Record interlamellar spacing with XRD and increase to 1.42nm by original 0.96nm.Molecular size and interlamellar spacing according to DMDAAC judge that monomer DMDAAC is in the interlayer monolayer alignment.
B takes by weighing polymerization single polymerization monomer dimethyl diallyl ammonium chloride initiator of polyreaction K
2S
2O
81.081g (0.004mol), be mixed with the aqueous solution of 0.016M with the 250ml deionized water; The template that step D is obtained is dispersed in this solution, reflux 20 hours, temperature of reaction is 60 ℃, make the monomer in the template carry out polymerization, filter, wash, 70 ℃ of dryings 18 hours, the polynite MMT-PDMDAAC. that obtains the interlayer object and be polymkeric substance with MMT-PDMDAAC carry out XRD, IR, NMR characterizes, and shows that DMDAAC at interlayer polymerization has taken place.
C. the laminate of the polynite that step B is obtained with hydrofluoric acid dissolves away, and obtains the clarifying aqueous solution, and this aqueous solution is dropwise joined in the acetone, after static 1 hour, faint yellow precipitation occurs, and centrifugal this turbid solution is separated bottom settlings absolute ethanol washing.50 ℃ of vacuum-drying 20h under the room temperature dry 24 hours again.Obtain white powder PDMDAAC.This product is carried out NMR, TEM, IR test, and the result shows that product is the nanoscale polymkeric substance.
Embodiment 4
A.50ml 1M HCl splashes into 3.56g (0.05mol) third rare acid amides AM (acrylamide) stirring 1 hour.10g CEC=100mmol/100g sodium-based montmorillonite is added in the there-necked flask, it was uniformly dispersed in 0.5 hour and is heated to 70 ℃, then third protonated rare amide solution is slowly splashed into 80 ℃ of stirring 6h to going into 200ml deionized water vigorous stirring.Centrifugal, wash to filtrate and splash into AgNO
3Do not produce till the white precipitate in the solution.70 ℃ of dry 20h obtain the MMT-AM template.With characterization methods such as XRD and IR proofs monomer intercalation be assembled into the interlayer of polynite.Recording interlamellar spacing with XRD is 2.15nm.Molecular size and interlamellar spacing according to AM judge that monomer A M is in the interlayer dual layer arrangement.
B takes by weighing polymerization single polymerization monomer third rare acid amides initiator of polyreaction (NH
4)
2S
2O
80.912g (0.004mol), be mixed with the aqueous solution of 0.016M with the 250ml deionized water; The template that steps A is obtained is dispersed in this solution, reflux 20 hours, temperature of reaction is 60 ℃, make the monomer in the template carry out polymerization, filter, wash, 70 ℃ of dryings 20 hours, the polynite MMT-PAM. that obtains the interlayer object and be polymkeric substance with MMT-PAM carry out XRD, IR, NMR characterizes, and shows that AM at interlayer polymerization has taken place.
C. the laminate of the polynite that step B is obtained with hydrofluoric acid dissolves away, and obtains the clarifying aqueous solution, and this aqueous solution is dropwise joined in the acetone, after static 1 hour, faint yellow precipitation occurs, and centrifugal this turbid solution is separated bottom settlings absolute ethanol washing.At room temperature dry 24h.Obtain yellow powder polyacrylamide (PAM).This product is carried out NMR, TEM, IR test, and the result shows that product is the nanoscale polymkeric substance.
Embodiment 5
A.50ml 1M HCl splashes into 3.31g (0.05mol) third rare acid amides AM (acrylamide) and stirs 1h.10g CEC=93mmol/100g calcium-base montmorillonite is added in the there-necked flask, it was uniformly dispersed in 0.5 hour and is heated to 70 ℃, then third protonated rare amide solution is slowly splashed into 80 ℃ of stirring 24h to going into 200ml deionized water vigorous stirring.Centrifugal, wash to filtrate and splash into AgNO
3Do not produce till the white precipitate in the solution.70 ℃ of dryings 20 hours obtain the MMT-AM template.With characterization methods such as XRD and IR proofs monomer intercalation be assembled into the interlayer of polynite.Record interlamellar spacing with XRD and increased 1.20nm.Molecular size and interlamellar spacing according to AM judge that monomer A M is in the interlayer dual layer arrangement.
B takes by weighing polymerization single polymerization monomer third rare acid amides initiator of polyreaction (NH
4)
2S
2O
80.912g (0.004mol), be mixed with the aqueous solution of 0.016M with the 250ml deionized water; The template that steps A is obtained is dispersed in this solution, reflux 20 hours, temperature of reaction is 60 ℃, make the monomer in the template carry out polymerization, filter, wash, at 70 ℃ of dry 20h, the polynite MMT-PAM. that obtains the interlayer object and be polymkeric substance with MMT-PAM carry out XRD, IR, NMR characterizes, and shows that AM at interlayer polymerization has taken place.
C. the laminate of the polynite that step B is obtained with hydrofluoric acid dissolves away, and obtains the clarifying aqueous solution, and this aqueous solution is dropwise joined in the acetone, after static 1 hour, faint yellow precipitation occurs, and centrifugal this turbid solution is separated bottom settlings absolute ethanol washing.50 ℃ of vacuum-drying 24h under the room temperature dry 24 hours again.Obtain yellow powder polyacrylamide (PAM).This product is carried out NMR, TEM, IR test, and the result shows that product is the nanoscale polymkeric substance.
Embodiment 6
A.30ml 1M HCl splashes into 2.14g (0.03mol) third rare acid amides AM (acrylamide) and stirs 1h.10g CEC=100mmol/100g sodium-based montmorillonite is added in the there-necked flask, it was uniformly dispersed in 0.5 hour and is heated to 70 ℃, then third protonated rare amide solution is slowly splashed into, 80 ℃ of stirrings 24 hours to going into 200ml deionized water vigorous stirring.Centrifugal, wash to filtrate and splash into AgNO
3Do not produce till the white precipitate in the solution.60 ℃ of dry 24h obtain the MMT-AM template.With characterization methods such as XRD and IR proofs monomer intercalation be assembled into the interlayer of polynite.Record interlamellar spacing with XRD and increase to 2.15nm by original 0.96nm.Molecular size and interlamellar spacing according to AM judge that monomer A M is in the interlayer dual layer arrangement.
B takes by weighing polymerization single polymerization monomer third rare acid amides initiator of polyreaction (NH
4)
2S
2O
80.912g (0.004mol), be mixed with the aqueous solution of 0.016M with the 250ml deionized water; The template that steps A is obtained is dispersed in this solution, reflux 20 hours, temperature of reaction is 55 ℃, make the monomer in the template carry out polymerization, filter, wash, 60 ℃ of dryings 24 hours, the polynite MMT-PAM. that obtains the interlayer object and be polymkeric substance with MMT-PAM carry out XRD, IR, NMR characterizes, and shows that AM at interlayer polymerization has taken place.
C. the laminate of the polynite that step B is obtained with hydrofluoric acid dissolves away, and obtains the clarifying aqueous solution, and this aqueous solution is dropwise joined in the acetone, after static 1 hour, faint yellow precipitation occurs, and centrifugal this turbid solution is separated bottom settlings absolute ethanol washing.Under 50 ℃ of vacuum-drying 20 hours and then the room temperature dry 24 hours.Obtain yellow powder polyacrylamide (PAM).This product is carried out NMR, TEM, IR test, and the result shows that product is the nanoscale polymkeric substance.
Claims (3)
1, a kind of is the method that template prepares nanometer polymer with the polynite, it is characterized in that: but the intercalation property of anionic clay polynite is applied in the template polymerization reaction, earlier the polymerization single polymerization monomer intercalation is assembled into polynite MMT interlayer, be template again with MMT, make polymerization single polymerization monomer polymerization reaction take place in template, isolate polymkeric substance then; Concrete preparation process is as follows:
A, polymerization single polymerization monomer is splashed in the polynite aqueous solution, solution quality concentration is 3-7%, stirred 6～24 hours, whipping temp is 20～80 ℃, be washed to that polymeric monomer concentration reaches 1～9ppm mol in the filtrate, 60～80 ℃ of dryings 18～25 hours, obtaining the interlayer object was the monomeric polynite template of institute's insertion polymerization then; Use infrared spectra IR, nuclear-magnetism NMR, X-ray diffraction XRD characterization method proof monomer intercalation has been assembled into the interlayer of polynite;
B, the template MMT-polymerization single polymerization monomer that step a is obtained are dispersed in the water solvent, looking the different adding of template internal reaction polymerization single polymerization monomer weight ratio is the initiator of 1-5 ‰, reflux 6～25 hours, make the polymerization single polymerization monomer polymerization reaction take place in the template, filter then, wash, 60～80 ℃ of dryings 20～25 hours, obtain the polynite that the interlayer object is a polymkeric substance;
The laminate dissolving of c, the polynite that step b obtained with hydrofluoric acid is separated polymkeric substance again.
2, in accordance with the method for claim 1, it is characterized in that: described polynite is the sodium base, the calcium base, magnesium base, described polymerization single polymerization monomer are polymerizability quaternary ammonium salt or acid amides: wherein the polymerizability quaternary ammonium salt comprises: trimethylammonium allyl ammonium chloride, dimethyl diallyl ammonium chloride; Acid amides comprises: aniline, hexanolactam, acrylamide; Described initiator is an ammonium persulphate, Potassium Persulphate.
3, according to claim 1 or 2 described methods, it is characterized in that: the ion exchange capacity CEC of described polynite is 90～110 mmoles/100g.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351279C (en) * | 2005-11-29 | 2007-11-28 | 天津理工大学 | Preparation of monodispersion high molecular nanometer sphere using envelop virus as template |
| CN102492090A (en) * | 2011-11-11 | 2012-06-13 | 广州大学 | Preparation method for montmorillonite intercalation cation flocculating agent emulsion |
| CN114702647A (en) * | 2022-04-27 | 2022-07-05 | 青岛科技大学 | Polyacenoquinone polymer and preparation method thereof |
-
2005
- 2005-02-24 CN CN 200510011348 patent/CN1281633C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351279C (en) * | 2005-11-29 | 2007-11-28 | 天津理工大学 | Preparation of monodispersion high molecular nanometer sphere using envelop virus as template |
| CN102492090A (en) * | 2011-11-11 | 2012-06-13 | 广州大学 | Preparation method for montmorillonite intercalation cation flocculating agent emulsion |
| CN102492090B (en) * | 2011-11-11 | 2014-07-02 | 广州大学 | Preparation method for montmorillonite intercalation cation flocculating agent emulsion |
| CN114702647A (en) * | 2022-04-27 | 2022-07-05 | 青岛科技大学 | Polyacenoquinone polymer and preparation method thereof |
| CN114702647B (en) * | 2022-04-27 | 2023-08-04 | 青岛科技大学 | Polymeroquinone polymer and preparation method thereof |
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