CN1563175A - Method for preparing functional gradient nano composite material of montmorillonite/polystyrene - Google Patents
Method for preparing functional gradient nano composite material of montmorillonite/polystyrene Download PDFInfo
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- CN1563175A CN1563175A CN 200410017015 CN200410017015A CN1563175A CN 1563175 A CN1563175 A CN 1563175A CN 200410017015 CN200410017015 CN 200410017015 CN 200410017015 A CN200410017015 A CN 200410017015A CN 1563175 A CN1563175 A CN 1563175A
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Abstract
A method for preparing nanofunctional gradient composite of imvite/polystyrene includes utilizing cation exchanging process to carry out decoration for layered inorganic nanoimvite with organic intercalator procesisng decorated imvite with dispersing agent to form uniform colloid solution of imvite and polystyrene, carrying out home position polymerization under action of parallel electric field for obtaining the nanofunctional gradient composite of imvite/polystyrene.
Description
Technical field
The present invention relates to the preparation method of a kind of polynite/pipe/polyhenylethylene nano functional gradient composite materials, the method that relates in particular to a kind of employing free radical mass polymerization under electric field is induced prepares the novel method of polynite/pipe/polyhenylethylene nano functional gradient composite materials.The invention belongs to field of compound material.
Background technology
Functionally Graded Materials is exactly in manufacturing processed, make the key element (composition, structure, porosity, concentration etc.) of constituent material prolong thickness direction and be continuous variation to opposite side by a side, feasible inside does not have sharp interface, thereby make material character and function also be a kind of novel material of continually varying, compare with matrix material, because composition is to change in gradient to opposite side from a side, and there is not specific interface, thereby make the smooth performance of this material change, therefore relaxed the stress between top layer and bottom, make performance better, and owing to make gradient, so can save material.The Functionally Graded Materials notion is in 1984, by geographic several material supply section scholar Xinye doctor, the horizontal wells just of Japanese celestial platform quick male professors with cross the limit dragon three religions and be beheaded and propose earlier, subsequently, just is subjected to the great attention of Japan and world's material circle.Functionally Graded Materials commonly used relates generally to ceramic/metal, has also related to each material field such as inorganics, metal, polymer, organism and living body.At present, gradient structure working method mainly contains gas phase control method, solid phase control method, liquid phase control method, compound control method, also have sol method, gel method, copolymerization method and hydrolysis method etc., wherein gas phase control method is to separate out the complex functionality key element and carry out the method for gradient distribution from gas phase, advantage can be made small-sized, also can make the material of large complicated shape, but needs adopt chemistry steaming or physics is steaming, device is complicated; Solid phase control method is that raw material powder is accumulated the method that is sintered to fix the gradient layered material by gradient, generally is used for materials such as pottery and metal more; Liquid phase control method is to solidify and separate out when solidifying functional imperative the method for gradient lamination on base material from liquid phase, generally will be with the molten method of penetrating of plasma body, and equipment is complicated and need plasma source; The mixture control method is with vapor phase process and liquid phase method, solid phase method and liquid phase method combination, makes full use of strong point separately and the produced with combination method that forms; Above method is used for preparing the gradient material of pottery, metal and inorganic materials more; Sol method, gel method, copolymerization method and hydrolysis method etc. can polymkeric substance and material such as biology, but selected materials must be easy to make collosol and gel or be easy to copolyreaction maybe hydrolysis reaction to take place, and has so just limited the kind of preparation gradient material more or less.Though gradient material has application promise in clinical practice, because at the early-stage, the domestic and international research exploitation is fewer, focuses mostly on the ceramic/metal material, so the kind of preparation Functionally Graded Materials and method are all not really ripe.
Summary of the invention
The objective of the invention is to kind and the less limitation of method at present preparation Functionally Graded Materials, a kind of preparation method who induces polynite down/pipe/polyhenylethylene nano functional gradient composite materials at electric field is proposed, preparation has the high barrier Functionally Graded Materials, has more Practical significance.
For realizing such purpose, in technical scheme of the present invention, at application for a patent for invention " preparation method of the in-situ inserted polymkeric substance of nano imvite-vinylbenzene " (application number: on the basis 03115777.7), adopt base exchange method earlier the layered inorganic polynite to be modified with organic intercalation agent, the polynite of modified is handled with dispersion agent again, be mixed and made into vinylbenzene/montmorillonite Composite colloid with vinylbenzene then, at last composite gel is carried out the preparation method of in-situ polymerization under the parallel electric field effect, thereby prepare polynite/pipe/polyhenylethylene nano functional gradient composite materials.
The inventive method is carried out as follows:
1, adopting base exchange method that organic intercalation agent is carried out in the inorganic nano polynite modifies, with nano imvite powder and solvent ratio high-speed stirring on high-speed mixer in 1: 1～500 (weight ratios), rotating speed is 500-4500 rev/min, makes to form stable montmorillonite suspension liquid; Other presses organic intercalation agent and solvent the mixed of 1: 1～100 (weight ratios), stirring makes it abundant dissolving, then with this solution by joining in the suspension of polynite with the weight ratio of montmorillonite suspension liquid 1: 1～300, under 20-300 ℃ of temperature vigorous stirring 0.5-80 hour.After the filtration throw out is washed with hot solvent, the hot solvent consumption is equivalent to 2-50 times of weight of precipitate, stirs 0.5-10 hour, filters.Washing process repeats 2-5 time, to remove wherein remaining organism, final product in 60 ℃ of following vacuum-dryings, is obtained organo montmorillonite.
2, be to mix 5-60 minute on 500-6000 rev/min the high-speed mixer with the dispersion agent of organo montmorillonite 80-99.9 part of obtaining in the step 1 and 0.1-20 part (by weight), thereby make the polynite that can form stable and uniform colloidal solution with vinylbenzene at 30-200 ℃, rotating speed.
3, in polymerization equipment, be that nano imvite material in the step 2 of 0.05%-40% and the weight percent styrene monomer that is 60%-99.95% is at room temperature even with magnetic stirrer with weight percent, add 0.5 ‰-15% the initiator be equivalent to styrene monomer weight again, under 0.001～100 voltaism field action, in 40-120 ℃ of following isothermal polymerization 4-100 hour, make nano imvite/pipe/polyhenylethylene nano functional gradient composite materials.
Inorganic nano polynite of the present invention is of a size of nano level at least on the one dimension direction, the disperse phase yardstick is the 1-100 nanometer.
Solvent of the present invention is toluene, dimethylbenzene, perhydronaphthalene, whiteruss, kerosene, water, ethanol, methyl alcohol, acetone, ethylene dichloride or sherwood oil.
Organic intercalation agent of the present invention is the hexadecyl brometo de amonio, the n-cetyltrimethyl ammonium, dimethyl benzene ethyl dodecyl chlorination ammonium, two octadecyl bromination ammoniums, octadecyl bromination ammonium, cetyl trimethylammonium bromide, methylacryoyloxyethyl-benzyl-alkyl dimethyl ammonium chloride, hexadecyl-phenyl-azo pyridine ammonium chloride, vinyl benzyl-dimethyl dodecyl chlorination ammonium, vinyl benzyl-dimethyl cetyl chloride ammonium, methylacryoyloxyethyl-benzyl-dimethyl brometo de amonio, the 3,5-dimethylphenyl octadecyl ammonium chloride, dimethyl stearyl ammonium chloride or vinyl benzyl-dimethyl dodecyl bromination ammonium, or the mixture of their compositions.
Dispersion agent agent of the present invention is whiteruss, Resins, epoxy, silane coupling agent, titanate coupling agent, silicone oil, vulcabond, glycerine, ethylene glycol, ethylene waxes, ethyl acetate or methyl methacrylate, or the mixture of their compositions.
Initiator of the present invention is azo-bis-isobutyl cyanide (AIBN), dicumyl peroxide (DCP), benzoyl peroxide (BPO), t-butyl peroxide (TBP), or the mixture of their compositions.
Electric field of the present invention is a parallel electric field, is alternating-electric field or DC electric field, and voltage is 0.001～100 volt.
The present invention has not only overcome vinylbenzene and polynite is difficult to the blended weakness, and has obtained polynite/pipe/polyhenylethylene nano functional gradient composite materials, and method is easy, and the gained material has barrier and thermostability preferably, is with a wide range of applications.
Embodiment
Following embodiment further specifies of the present invention, rather than limits the scope of the invention.
Embodiment 1
Add 25 gram methylacryoyloxyethyl-benzyl-dimethyl amine bromides in 500 milliliters beaker, 30 milliliters of concentrated hydrochloric acids and 100 gram deionized waters are heated to 90 ℃ with this solution, make methylacryoyloxyethyl-benzyl-alkyl dimethyl ammonium chloride intercalator.In addition, 45 gram polynites are dispersed in the solvent deionized water of 90 ℃ of 500 grams, stir.The solution that will contain methylacryoyloxyethyl-benzyl-alkyl dimethyl ammonium chloride intercalator then joins in the suspended dispersed liquid of this polynite, and vigorous stirring 1 hour.After overanxious white precipitate placed 1000 milliliters beaker, add 700 gram hot water, stirred 1 hour, and filtration.This process repeats more than three times, to remove wherein residual ammonium salt.Final product filtration and cooling drying is standby.Be to mix 15 minutes on 600 rev/mins the high-speed mixer then with the organo montmorillonite that makes 30 grams and the 0.5 dispersant liq paraffin that restrains, thereby make the polynite that can form stable and uniform colloidal solution with vinylbenzene at 70 ℃, rotating speed.The above-mentioned polynite that obtains 3 grams and 100 gram vinylbenzene are made it to mix with magnetic stirrer in large beaker, add 0.5g initiator benzoyl peroxide, restir is even, place polymerization reactor, under the parallel direct current electric field action of 200 millivolts, 80 ℃ of following constant temperature polymerizations 40 hours, obtain polynite/pipe/polyhenylethylene nano functional gradient composite materials, polystyrene and polynite have formed intercalation type nano composite material in this matrix material, and because effect of electric field, polynite and polystyrene present Gradient distribution, this material is compared with the polynite polystyrene that contains same ratio has better barrier and thermostability, its barrier has improved 1.2 times, and heat decomposition temperature has raise 8 ℃.
Embodiment 2
Add 110 gram dimethyl stearyl ammonia chlorides in 500 milliliters beaker, 35 milliliters of concentrated hydrochloric acids and 200 gram deionized waters are heated to 80 ℃ with this solution, make dimethyl stearyl ammonium chloride intercalator.In addition, 25 gram polynites are dispersed in the solvent deionized water of 80 ℃ of 400 grams, stir.The solution that will contain dimethyl stearyl ammonium chloride intercalator then joins in the dispersion liquid of this polynite, and vigorous stirring 1 hour.After overanxious white precipitate placed 500 milliliters beaker, add 400 gram hot water, stirred 1 hour, and filtration.This process repeats more than three times, to remove wherein residual ammonium salt.Final product filtration and cooling drying is standby.Be to mix 20 minutes on 800 rev/mins the high-speed mixer then with the organo montmorillonite that makes 15 grams and the 0.2 dispersion agent vulcabond that restrains, thereby make the polynite that can form stable and uniform colloidal solution with vinylbenzene at 75 ℃, rotating speed.The above-mentioned polynite that obtains 5 grams and 100 gram vinylbenzene are made it to mix with magnetic stirrer in large beaker, add 0.4g initiator azo-bis-isobutyl cyanide, restir is even, place polymerization reactor, under 8 volts of parallel alternating-electric field effects, in 65 ℃ of following constant temperature polymerizations 25 hours, obtain polynite/pipe/polyhenylethylene nano functional gradient composite materials, polystyrene and polynite have formed intercalation type nano composite material in this matrix material, and because effect of electric field, polynite and polystyrene present Gradient distribution, this material is compared with the polynite polystyrene that contains same ratio has better barrier and thermostability, its barrier has improved 1 times, and heat decomposition temperature has raise 5 ℃.
Embodiment 3
In 500 milliliters beaker, add 30 gram hexadecyl-phenyl-azo pyridine ammonia chloride and 45 hexadecyl trimethyl ammonium bromide, 40 milliliters of concentrated hydrochloric acids and 320 gram deionized waters, this solution is heated to 100 ℃, makes the mixing intercalator of hexadecyl-phenyl-azo pyridine ammonium chloride and cetyl trimethylammonium bromide.In addition, 28 gram polynites are dispersed in the solvent deionized water of 105 ℃ of 350 grams, stir.The solution that will contain above-mentioned mixing intercalator then joins in the dispersion liquid of this polynite, and vigorous stirring 3.5 hours.After overanxious white precipitate placed 500 milliliters beaker, add 360 gram hot water, stirred 2 hours, and filtration.This process repeats more than three times, to remove wherein residual ammonium salt.Final product filtration and cooling drying is standby.Be to mix 15 minutes on 2400 rev/mins the high-speed mixer then with the dispersion agent ethylene waxes of the organo montmorillonite that makes 20 grams and 0.2 gram and 0.1 ethyl acetate that restrains, thereby make the polynite that can form stable and uniform colloidal solution with vinylbenzene at 90 ℃, rotating speed.The above-mentioned polynite that obtains 30 grams and 100 gram vinylbenzene are made it to mix with magnetic stirrer in large beaker, add 0.2g initiator azo-bis-isobutyl cyanide (AIBN) and 0.4 gram dicumyl peroxide (DCP), restir is even, place polymerization reactor, under 90 volts of parallel direct current electric field actions, in 90 ℃ of following constant temperature polymerase 17s 2 hours, obtain polynite/pipe/polyhenylethylene nano functional gradient composite materials, polystyrene and polynite have formed intercalation type nano composite material in this matrix material, and because effect of electric field, polynite and polystyrene present Gradient distribution, this material is compared with the polynite polystyrene that contains same ratio has better barrier and thermostability, its barrier has improved 1.5 times, and heat decomposition temperature has raise 7 ℃.
Embodiment 4
Add 90 gram vinyl benzyl-dimethyl dodecyl bromination amine in 1000 milliliters beaker, 45 milliliters of concentrated hydrochloric acids and 800 gram deionized waters are heated to 95 ℃ with this solution, make vinyl benzyl-dimethyl dodecyl bromination ammonium intercalator.In addition, 36 gram polynites are dispersed in the solvent deionized water of 55 ℃ of 400 grams, stir.The solution that will contain above-mentioned mixing intercalator then joins in the dispersion liquid of this polynite, and vigorous stirring 6 hours.After overanxious white precipitate placed 1000 milliliters beaker, add 600 gram hot water, stirred 3 hours, and filtration.This process repeats more than three times, to remove wherein residual ammonium salt.Final product filtration and cooling drying is standby.Be to mix 30 minutes on 3000 rev/mins the high-speed mixer then with the organo montmorillonite that makes 30 grams and 0.5 titanate coupling agent that restrains, thereby make the polynite that can form stable and uniform colloidal solution with vinylbenzene at 160 ℃, rotating speed.The above-mentioned polynite that obtains 30 grams and 100 gram vinylbenzene are made it to mix with magnetic stirrer in large beaker, add 0.8 gram initiator dicumyl peroxide (DCP), restir is even, place polymerization reactor, under 70 volts of parallel alternating-electric field effects, in 100 ℃ of following constant temperature polymerase 17s 2 hours, obtain polynite/pipe/polyhenylethylene nano functional gradient composite materials, polystyrene and polynite have formed intercalation type nano composite material in this matrix material, and because effect of electric field, polynite and polystyrene present Gradient distribution, this material is compared with the polynite polystyrene that contains same ratio has better barrier and thermostability, its barrier has improved 1.3 times, and heat decomposition temperature has raise 9 ℃.
Embodiment 5
Add 96 gram 3,5-dimethylphenyl octadecyl chlorination amine in 1000 milliliters beaker, 38 milliliters of concentrated hydrochloric acids and 700 gram deionized waters are heated to 105 ℃ with this solution, make 3,5-dimethylphenyl octadecyl ammonium chloride intercalator.In addition, 60 gram polynites are dispersed in the solvent deionized water of 70 ℃ of 500 grams, stir.The solution that will contain above-mentioned mixing intercalator then joins in the dispersion liquid of this polynite, and vigorous stirring 5 hours.After overanxious white precipitate placed 1000 milliliters beaker, add 650 gram hot water, stirred 2 hours, and filtration.This process repeats more than three times, to remove wherein residual ammonium salt.Final product filtration and cooling drying is standby.Be to mix 50 minutes on 1800 rev/mins the high-speed mixer then with the organo montmorillonite that makes 45 grams and 5 titanate coupling agents that restrain, thereby make the polynite that can form stable and uniform colloidal solution with vinylbenzene at 130 ℃, rotating speed.The above-mentioned polynite that obtains 15 grams and 100 gram vinylbenzene are made it to mix with magnetic stirrer in large beaker, add 0.75 gram initiator benzoyl peroxide, restir is even, place polymerization reactor, under 45 volts of parallel alternating-electric field effects, in 85 ℃ of following constant temperature polymerizations 48 hours, obtain polynite/pipe/polyhenylethylene nano functional gradient composite materials, polystyrene and polynite have formed intercalation type nano composite material in this matrix material, and because effect of electric field, polynite and polystyrene present Gradient distribution, this material is compared with the polynite polystyrene that contains same ratio has better barrier and thermostability, its barrier has improved 1.2 times, and heat decomposition temperature has raise 6 ℃.
Claims (7)
1, the preparation method of a kind of polynite/pipe/polyhenylethylene nano functional gradient composite materials is characterized in that carrying out as follows:
1) adopting base exchange method that organic intercalation agent is carried out in the inorganic nano polynite modifies, with nano imvite powder and solvent by weight 1: 1～500 on high-speed mixer high-speed stirring, rotating speed is 500-4500 rev/min, makes to form stable montmorillonite suspension liquid; In addition organic intercalation agent is mixed by weight 1: 1～100 with solvent, stirring makes it abundant dissolving, then this solution is joined in the suspension of polynite by the weight ratio with montmorillonite suspension liquid 1: 1～300, under 20-300 ℃ of temperature vigorous stirring 0.5-80 hour, after the filtration throw out is washed with hot solvent, the hot solvent consumption is equivalent to 2-50 times of weight of precipitate, stir 0.5-10 hour after-filtration, washing process repeats 2-5 all over to remove wherein remaining organism, with final product in 60 ℃ of following vacuum-dryings;
2) be to mix 5-60 minute on 500-6000 rev/min the high-speed mixer by weight with the dispersion agent of organo montmorillonite 80-99.9 part of obtaining in the step 1 and 0.1-20 part, thereby make the polynite that can form stable and uniform colloidal solution with vinylbenzene at 30-200 ℃, rotating speed;
3) in polymerization equipment, be that nano imvite material in the step 2 of 0.05%-40% and the weight percent styrene monomer that is 60%-99.95% is at room temperature even with magnetic stirrer with weight percent, add 0.5 ‰-15% the initiator be equivalent to styrene monomer weight again, under 0.001～100 voltaism field action, in 40-120 ℃ of following isothermal polymerization 4-100 hour, make nano imvite/pipe/polyhenylethylene nano functional gradient composite materials.
2, the preparation method of polynite as claimed in claim 1/pipe/polyhenylethylene nano functional gradient composite materials is characterized in that described inorganic nano polynite is of a size of nano level at least on the one dimension direction, and the disperse phase yardstick is the 1-100 nanometer.
3, the preparation method of polynite as claimed in claim 1/pipe/polyhenylethylene nano functional gradient composite materials is characterized in that described solvent is toluene, dimethylbenzene, perhydronaphthalene, whiteruss, kerosene, water, ethanol, methyl alcohol, acetone, ethylene dichloride or sherwood oil.
4, the preparation method of polynite as claimed in claim 1/pipe/polyhenylethylene nano functional gradient composite materials, it is characterized in that described organic intercalation agent is the hexadecyl brometo de amonio, the n-cetyltrimethyl ammonium, dimethyl benzene ethyl dodecyl chlorination ammonium, two octadecyl bromination ammoniums, octadecyl bromination ammonium, cetyl trimethylammonium bromide, methylacryoyloxyethyl-benzyl-alkyl dimethyl ammonium chloride, hexadecyl-phenyl-azo pyridine ammonium chloride, vinyl benzyl-dimethyl dodecyl chlorination ammonium, vinyl benzyl-dimethyl cetyl chloride ammonium, methylacryoyloxyethyl-benzyl-dimethyl brometo de amonio, the 3,5-dimethylphenyl octadecyl ammonium chloride, dimethyl stearyl ammonium chloride or vinyl benzyl-dimethyl dodecyl bromination ammonium, or the mixture of their compositions.
5, the preparation method of polynite as claimed in claim 1/pipe/polyhenylethylene nano functional gradient composite materials, it is characterized in that described dispersion agent agent is whiteruss, Resins, epoxy, silane coupling agent, titanate coupling agent, silicone oil, vulcabond, glycerine, ethylene glycol, ethylene waxes, ethyl acetate or methyl methacrylate, or the mixture of their compositions.
6, the preparation method of polynite as claimed in claim 1/pipe/polyhenylethylene nano functional gradient composite materials, it is characterized in that described initiator is azo-bis-isobutyl cyanide (AIBN), dicumyl peroxide (DCP), benzoyl peroxide (BPO), t-butyl peroxide (TBP), or the mixture of their compositions.
7, the preparation method of polynite as claimed in claim 1/pipe/polyhenylethylene nano functional gradient composite materials is characterized in that described electric field is a parallel electric field, is alternating-electric field or DC electric field.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100577703C (en) * | 2005-12-22 | 2010-01-06 | 固特异轮胎和橡胶公司 | Water-based process for the preparation of polymer-clay nanocomposites |
| CN104744842A (en) * | 2015-03-24 | 2015-07-01 | 合肥会通新材料有限公司 | Polystyrene composite material reinforced by in situ-polymerization of montmorillonite intercalation and preparation method of polystyrene composite material |
| CN106924804A (en) * | 2017-02-17 | 2017-07-07 | 江汉大学 | Nanometer hydroxyapatite/polycaprolactone function-graded material prepared using high voltage electric field induction and preparation method thereof |
| CN107523057A (en) * | 2017-09-22 | 2017-12-29 | 南京肯特复合材料股份有限公司 | Corrosion-resistant end plane sealing strip PPS resin composite and preparation method thereof |
| CN107603047A (en) * | 2017-10-31 | 2018-01-19 | 江汉大学 | The preparation method of gradient function composite is blended in polymer |
| CN116240006A (en) * | 2021-12-07 | 2023-06-09 | 天津大港油田滨港集团博弘石油化工有限公司 | Modified nano thick oil viscosity reducer and preparation method thereof |
-
2004
- 2004-03-18 CN CN 200410017015 patent/CN1257221C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100577703C (en) * | 2005-12-22 | 2010-01-06 | 固特异轮胎和橡胶公司 | Water-based process for the preparation of polymer-clay nanocomposites |
| CN104744842A (en) * | 2015-03-24 | 2015-07-01 | 合肥会通新材料有限公司 | Polystyrene composite material reinforced by in situ-polymerization of montmorillonite intercalation and preparation method of polystyrene composite material |
| CN106924804A (en) * | 2017-02-17 | 2017-07-07 | 江汉大学 | Nanometer hydroxyapatite/polycaprolactone function-graded material prepared using high voltage electric field induction and preparation method thereof |
| CN106924804B (en) * | 2017-02-17 | 2020-08-14 | 江汉大学 | Nano-hydroxyapatite/polycaprolactone gradient functional material prepared by high-voltage electric field induction and preparation method thereof |
| CN107523057A (en) * | 2017-09-22 | 2017-12-29 | 南京肯特复合材料股份有限公司 | Corrosion-resistant end plane sealing strip PPS resin composite and preparation method thereof |
| CN107603047A (en) * | 2017-10-31 | 2018-01-19 | 江汉大学 | The preparation method of gradient function composite is blended in polymer |
| CN116240006A (en) * | 2021-12-07 | 2023-06-09 | 天津大港油田滨港集团博弘石油化工有限公司 | Modified nano thick oil viscosity reducer and preparation method thereof |
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| CN1257221C (en) | 2006-05-24 |
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