CN105801889A - Preparation method of polymethyl methacrylate macromolecule extended chain - Google Patents
Preparation method of polymethyl methacrylate macromolecule extended chain Download PDFInfo
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- CN105801889A CN105801889A CN201610183674.9A CN201610183674A CN105801889A CN 105801889 A CN105801889 A CN 105801889A CN 201610183674 A CN201610183674 A CN 201610183674A CN 105801889 A CN105801889 A CN 105801889A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/092—Hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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Abstract
The invention belongs to the technical field of macromolecular physics or condensed matter physics, and particularly relates to a preparation method of a polymethyl methacrylate macromolecule extended chain.A polystyrene- polymethyl methacrylate segmented copolymer is adopted as a raw material, dissolved into methylbenzene, repeatedly diluted to form a PS-b-PMMA extremely-low solution of the certain concentration, the rotating speed and time are controlled, then, the diluted solution is dropped on the surface of a newly-split mica substrate for spin-coating, a sample is taken out and dried at room temperature, and the PMMA extended chain can be observed under the atomic force microscope.The preparation method is simple and good in controllability; the prepared polymethyl methacrylate macromolecule extended chain is dispersed on the mica substrate uniformly, the extending degree is high, and the polymethyl methacrylate macromolecule extended chain is particularly applicable to research on conformation conversion and corresponding condensed characteristics.
Description
Technical field
The invention belongs to Polymer Physics or Condensed Matter Physics technical field, be specifically related to the preparation method of a kind of polymethyl methacrylate macromolecule extended chain.
Background technology
Macromolecule is to have many special form, structure and character in the presence of single stranded form.As the study hotspot of macromolecular condensed state, may there is intramolecular entanglement in macromolecular single-chain, but there is not the entanglement of molecule interchain, and the intersegmental existence of chain of strand necessarily attracts each other, and is totally different from molecule interchain intermeshing multichain condensed state.At present, use atomic force microscope (AFM) that the feature such as pattern and conformation transition thereof of macromolecule extended chain can be observed directly.
Application No. 200410013589.5, the Chinese patent of the preparation method of entitled a kind of macromolecular single-chain discloses the preparation method of a kind of macromolecular single-chain, specifically including: a. dissolves a polymer in and is made into polymer solution in low boiling point solvent, magnetic agitation solution makes polymer molecular chain be in isolated state each other in the solution；B. being added drop-wise in precipitation solvent by this solution, magnetic agitation mixed solution, control temperature is between low boiling point solvent boiling point and precipitation solvent boiling point, and constant temperature 0.5～1 hour, monochain polymer is deposited in precipitation solvent；C. centrifugation or filtration precipitation solvent, it is thus achieved that be collapsed into spherical single chain polymer granule.What above-mentioned patent was finally prepared is spherical single chain polymer granule rather than macromolecule extended chain.Using weak solution skin covering of the surface transfer method the preparation of existing macromolecule extended chain more.The weak solution of polystyrene-poly methyl methacrylate segmented copolymer (PS-b-PMMA) is dropped in the water surface of Langmuir-Blodgett (LB) tank by Japanese Scientists Hashimoto etc., then scattered strand is transferred to polymethyl methacrylate (PMMA) molecular chain structure obtaining assembling in mica substrate, by sample being made annealing treatment under control humidity, PMMA extended chain can be obtained.It is 9.2 × 10 that Kumaki etc. select isotaxy PMMA to be made into concentration-5 The chloroformic solution of g/mL, drops in the water surface of LB tank by solution, uses the mica sheet newly rived to be stained with in water and pulls out vertically upward, prepares PMMA extended chain by adjusting the surface pressing of LB tank.
In sum, the most authorized Chinese patent (200410013589.5) can only be prepared and be collapsed into spherical single chain polymer granule, and the existing method preparing macromolecule extended chain is the water surface using the mutually isolated extremely dilute solution existed of strand to be dropped in LB tank, making solution extend to rapidly on liquid surface to pick up with substrate more first to prepare monofilm, the post processing being then passed through complexity just can obtain macromolecule extended chain.Visible, the preparation process of existing PMMA extended chain is complicated, especially needs strictly controlled environment humidity and annealing time in last handling process, repeatable poor.
Summary of the invention
In order to solve the problem that above-mentioned prior art exists, the present invention provides the preparation method of a kind of polymethyl methacrylate (PMMA) macromolecule extended chain, purpose is as raw material with polystyrene-poly methyl methacrylate segmented copolymer (PS-b-PMMA), it is dissolved in toluene, repeatedly dilution is made into certain density PS-b-PMMA extremely dilute solution, then carries out spin-coating.Controlling rotary speed and after the time, weak solution drops in the mica substrate surface spin coating sample preparation newly rived, take out sample, under an atomic force microscope it is observed that PMMA extended chain after drying at room temperature, method is simple, and condition controllability is good.
The technical scheme realizing the object of the invention follows the steps below:
(1) preparation polystyrene-poly methyl methacrylate segmented copolymer (PS-b-PMMA) weak solution: first the PS-b-PMMA powder of certain mass is dissolved in toluene, it is made into the toluene solution that weight concentration is 0.1 wt% ~ 0.4wt%, add toluene repeatedly to dilute, be finally configured to the PS-b-PMMA extremely dilute solution that weight concentration is 0.0001wt% ~ 0.0006wt% standby；
(2) spin-coating method prepares macromolecule extended chain: be placed on whirler as substrate by the mica sheet newly rived, preset rotating speed and the time of whirler, PS-b-PMMA extremely dilute solution in step (1) is dripped to mica surface, close the lid, start whirler and carry out spin-coating, after terminating, take out sample.Room temperature is placed, and after vaporing away residual toluene, is adhered to by sample in circular gasket, uses atomic force microscope tapping-mode can observe directly polymethyl methacrylate extended chain.
Wherein, described polystyrene-poly methyl methacrylate segmented copolymer is business-like containing polystyrene with the di-block copolymer of polymethyl methacrylate, wherein the number-average molecular weight of polystyrene block is 50,000 ~ 200,000 g/mol, the number-average molecular weight of polymethylmethacrylablock block is 50,000 ~ 400,000 g/mol, the polydispersity index (Mw/Mn) of this block copolymer is 1.0 ~ 1.4.
The rotating speed of described whirler is 1000 rpm ~ 8000 rpm, and the spin-coating time is 10 s ~ 50 s.
Compared with prior art, the feature of the present invention and providing the benefit that:
(1) present invention uses polystyrene-poly methyl methacrylate segmented copolymer weak solution spin-coating method to prepare polymethyl methacrylate extended chain, the polymethyl methacrylate extended chain that spin-coating process can make weak solution camber stretch is caught rapidly in mica substrate surface, effectively prevents the reunion of polymethyl methacrylate strand.
(2) compared with the existing methods, the preparation process of the present invention is simple, controllability good；The polymethyl methacrylate extended chain of preparation is uniformly dispersed in mica substrate, and extension degree is high, is particularly suited for studying the conformation transition of macromolecule extended chain and corresponding condensed state feature.
Accompanying drawing explanation
Fig. 1 is the polymethyl methacrylate macromolecule extended chain prepared in the embodiment of the present invention 1 AFM figure under different resolution；
Fig. 2 is that the present invention uses AFM method of resection to measure the high-level schematic of PMMA extended chain.
Detailed description of the invention
The atomic force microscope used in the present embodiment is business-like atomic force microscope, and can operate at tapping-mode or noncontact mode, it addition, the needle point used by atomic force microscope is business-like silicon or nitride tips, force constant is 2.0 ~ 25.0 N/m.
The detailed description of the invention of this invention is described below in conjunction with embodiment, and embodiments of the present invention are not limited only to content described in embodiment.
Embodiment
1
The preparation method of the polymethyl methacrylate macromolecule extended chain of the present embodiment follows the steps below:
(1) preparation PS-b-PMMA weak solution: first the PS-b-PMMA powder of certain mass is dissolved in toluene, the PS-b-PMMA block copolymer amount wherein selected is 130,000-133,000, Mw/Mn=1.10, it is configured to the toluene solution that weight concentration is 0.1wt%, adds toluene and repeatedly dilute, be finally configured to the PS-b-PMMA extremely dilute solution that weight concentration is 0.0001wt% standby；
(2) spin-coating method prepares macromolecule extended chain: be placed on whirler as substrate by the mica sheet newly rived, the rotating speed of pre-set whirler and time, the rotating speed of whirler is 3000 rpm, the spin-coating time is 30 s, PS-b-PMMA extremely dilute solution in step (1) is dripped to mica surface, close the lid, start whirler and carry out spin-coating, sample is taken out after end, room temperature is placed and is vapored away residual toluene, sample is adhered in circular gasket, atomic force microscope tapping-mode is used directly to observe polymethyl methacrylate macromolecule extended chain, as shown in Figure 1, can be seen that between extended chain independent of one another, do not reunite.Use method of resection can measure average chain length and average height, as in figure 2 it is shown, concrete test result is as shown in table 1.
Embodiment
2
The preparation method of the polymethyl methacrylate macromolecule extended chain of the present embodiment follows the steps below:
(1) preparation PS-b-PMMA weak solution: first the PS-b-PMMA powder of certain mass is dissolved in toluene, the PS-b-PMMA block copolymer amount wherein selected is 130,000-360,000, Mw/Mn=1.09, it is configured to the toluene solution that weight concentration is 0.3wt%, adds toluene and repeatedly dilute, be finally configured to the PS-b-PMMA extremely dilute solution that weight concentration is 0.0003wt% standby；
(2) spin-coating method prepares macromolecule extended chain: be placed on whirler as substrate by the mica sheet newly rived, the rotating speed of pre-set whirler and time, the rotating speed of whirler is 4000 rpm, the spin-coating time is 20 s, PS-b-PMMA extremely dilute solution in step (1) is dripped to mica surface, close the lid, start whirler and carry out spin-coating, sample is taken out after end, room temperature is placed and is vapored away residual toluene, sample is adhered in circular gasket, atomic force microscope tapping-mode is used directly to observe polymethyl methacrylate macromolecule extended chain, use method of resection can measure average chain length and average height, concrete test result is as shown in table 1.
Embodiment
3
The preparation method of the polymethyl methacrylate macromolecule extended chain of the present embodiment follows the steps below:
(1) preparation PS-b-PMMA weak solution: first the PS-b-PMMA powder of certain mass is dissolved in toluene, the PS-b-PMMA block copolymer amount wherein selected is 140,000-65,000, Mw/Mn=1.09, it is configured to the toluene solution that weight concentration is 0.2wt%, adds toluene and repeatedly dilute, be finally configured to the PS-b-PMMA extremely dilute solution that weight concentration is 0.0002wt% standby；
(2) spin-coating method prepares macromolecule extended chain: be placed on whirler as substrate by the mica sheet newly rived, the rotating speed of pre-set whirler and time, the rotating speed of whirler is 2500 rpm, the spin-coating time is 40 s, PS-b-PMMA extremely dilute solution in step (1) is dripped to mica surface, close the lid, start whirler and carry out spin-coating, sample is taken out after end, room temperature is placed and is vapored away residual toluene, sample is adhered in circular gasket, atomic force microscope tapping-mode is used directly to observe polymethyl methacrylate macromolecule extended chain, use method of resection can measure average chain length and average height, concrete test result is as shown in table 1.
Embodiment
4
The preparation method of the polymethyl methacrylate macromolecule extended chain of the present embodiment follows the steps below:
(1) preparation PS-b-PMMA weak solution: first the PS-b-PMMA powder of certain mass is dissolved in toluene, the PS-b-PMMA block copolymer amount wherein selected is 130,000-133,000, Mw/Mn=1.10, it is configured to the toluene solution that weight concentration is 0.4wt%, adds toluene and repeatedly dilute, be finally configured to the PS-b-PMMA extremely dilute solution that weight concentration is 0.0004wt% standby；
(2) spin-coating method prepares macromolecule extended chain: be placed on whirler as substrate by the mica sheet newly rived, the rotating speed of pre-set whirler and time, the rotating speed of whirler is 5000 rpm, the spin-coating time is 20 s, PS-b-PMMA extremely dilute solution in step (1) is dripped to mica surface, close the lid, start whirler and carry out spin-coating, sample is taken out after end, room temperature is placed and is vapored away residual toluene, sample is adhered in circular gasket, atomic force microscope tapping-mode is used directly to observe polymethyl methacrylate macromolecule extended chain, use method of resection can measure average chain length and average height, concrete test result is as shown in table 1.
Claims (3)
1. the preparation method of a polymethyl methacrylate macromolecule extended chain, it is characterised in that follow the steps below:
(1) preparation polystyrene-poly methyl methacrylate segmented copolymer weak solution: first the PS-b-PMMA powder of certain mass is dissolved in toluene, it is made into the toluene solution that weight concentration is 0.1 wt% ~ 0.4wt%, add toluene repeatedly to dilute, be finally configured to the PS-b-PMMA extremely dilute solution that weight concentration is 0.0001wt% ~ 0.0006wt% standby；
(2) spin-coating method prepares macromolecule extended chain: be placed on whirler as substrate by the mica sheet newly rived, the rotating speed of pre-set whirler and time, PS-b-PMMA extremely dilute solution in step (1) is dripped to mica surface, close the lid, start whirler and carry out spin-coating, sample is taken out after end, room temperature is placed and is vapored away residual toluene, sample is adhered in circular gasket, use atomic force microscope tapping-mode can observe directly polymethyl methacrylate extended chain.
The preparation method of a kind of polymethyl methacrylate macromolecule extended chain the most according to claim 1, it is characterized in that described polystyrene-poly methyl methacrylate segmented copolymer is business-like containing polystyrene with the di-block copolymer of polymethyl methacrylate, wherein the number-average molecular weight of polystyrene block is 50,000 ~ 200,000 g/mol, the number-average molecular weight of polymethylmethacrylablock block is 50,000 ~ 400,000 g/mol, the polydispersity index (Mw/Mn) of this block copolymer is 1.0 ~ 1.4.
The preparation method of a kind of polymethyl methacrylate macromolecule extended chain the most according to claim 1, it is characterised in that the rotating speed of described whirler is 1000 rpm ~ 8000 rpm, the spin-coating time is 10 s ~ 50 s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610183674.9A CN105801889A (en) | 2016-03-28 | 2016-03-28 | Preparation method of polymethyl methacrylate macromolecule extended chain |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610183674.9A CN105801889A (en) | 2016-03-28 | 2016-03-28 | Preparation method of polymethyl methacrylate macromolecule extended chain |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432955A (en) * | 2011-07-27 | 2012-05-02 | 天津大学 | Polystyrene nanoparticle adsorbed on mica sheet surface and preparation method thereof |
| CN105384952A (en) * | 2015-09-15 | 2016-03-09 | 北京航空航天大学 | Method for adjusting and controlling block copolymer self-assembled orientation by using mechanical shearing force |
-
2016
- 2016-03-28 CN CN201610183674.9A patent/CN105801889A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432955A (en) * | 2011-07-27 | 2012-05-02 | 天津大学 | Polystyrene nanoparticle adsorbed on mica sheet surface and preparation method thereof |
| CN105384952A (en) * | 2015-09-15 | 2016-03-09 | 北京航空航天大学 | Method for adjusting and controlling block copolymer self-assembled orientation by using mechanical shearing force |
Non-Patent Citations (1)
| Title |
|---|
| JIRO KUMAKI等: "Conformational Change in an Isolated Single Synthetic Polymer Chain on a Mica Surface Observed by Atomic Force Microscopy", 《AMERICAN CHEMICAL SOCIETY》 * |
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Application publication date: 20160727 |