CN103059179A - Preparation method of carbon-nanotube-modified polystyrene composite material - Google Patents
Preparation method of carbon-nanotube-modified polystyrene composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a carbon-nanotube-modified polystyrene composite material. The carbon-nanotube-modified polystyrene composite material is mainly prepared from the following components in parts by mass: 100 parts of styrene, 5-20 parts of carbon nanotube, 0.05-0.2 part of initiator, 60-80 parts of concentrated sulfuric acid, 180-240 parts of concentrated nitric acid, 100-200 parts of deionized water, 0.1-0.5 part of potassium persulfate, 3-6 parts of sodium lauryl sulfate and 100-200 parts of 10% sodium hydroxide solution. The preparation method is simple and easy to operate; and the prepared composite material has the advantages of favorable carbon nanotube dispersion properties and excellent mechanical properties.
Description
Technical field
The present invention relates to a kind of preparation method of modified polystyrene composite material, particularly a kind of preparation method of carbon nano-tube modification poly styrene composite material.
Background technology
Carbon nanotube is the most typical in nano material, and is the material of excellent performance.Carbon nanotube can be regarded the C of elongation as
60After Japanese scientist Iijima in 1991 at first finds carbon nanotube, caused extensive concern both domestic and external.The various methods that prepare carbon nanotube are invented in succession.Carbon nanotube has the excellent performances such as mechanics, optics, electricity and Chu Qing, has broad application prospects.After carbon nanotube and polymer were compound, mechanical property and electric property all were improved, and can be used as high-strength material and antistatic material etc.; Carbon nanotube is modified by the physics and chemistry method, can produce excellent physics, chemistry and biological property; In addition, carbon nanotube also is widely used in military field.
Generally speaking, there are many defectives in the carbon nanotube of production in enormous quantities, and dispersing property is also poor, and particularly the defective of carbon nano tube surface structure tends to damage the performances such as its electricity, optics and mechanics.These factors have reduced the high-performance of carbon nanotube as nano material, have affected carbon nanotubes application.In order to improve the surface tissue of carbon nanotube, generally adopt the method for finishing improve carbon nanotube dispersing property and and other materials between consistency.For this reason, researcher both domestic and external has carried out the research of various surface modification methods to carbon nanotube.
Polystyrene is a kind of commercialization polymkeric substance that is widely used, but also because of the large use range that has limited it of himself fragility, usually needs to add rubber elastomer to its toughening modifying the preparation high-impact polystyrene.But method improves in the human nature among using, and tends to make its strength degradation.The at present research of Carbon Nanotubes/Polystyrene Nanocomposites mainly concentrates on two aspects: the one, with carbon nanotube as packing material, adopt the methods such as solution, melt blending and in-situ polymerization to prepare Carbon Nanotubes/Polystyrene Nanocomposites, to improve mechanics, electricity and the thermal property of matrix material; The 2nd, carbon nanotube as main body, is modified carbon nanotube with polystyrene, make it in organic solvent, to obtain good solubility.Very active about the research of Carbon Nanotubes/Polystyrene Nanocomposites in recent years, in the conduction that improves matrix material! The aspects such as mechanical property have obtained good progress.
From present Research both domestic and external, carbon nanotube is not yet being given play to desirable effect aspect the mechanical property that improves matrix material.Will be with carbon nano-tube filled matrix material really as lightweight, high-intensity materials'use, much remains to be done, especially the scattering problem of carbon nanotube in polymkeric substance.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, a kind of good dispersion property is provided, have the preparation method of the modified polystyrene composite material of excellent mechanical property.
In order to realize above goal of the invention, the present invention by the following technical solutions: a kind of preparation method of carbon nano-tube modification poly styrene composite material, in may further comprise the steps:
(1) prepares raw material by following weight proportion: vinylbenzene 100; Carbon nanotube 5～20; Initiator 0.05～0.2; The vitriol oil 60～80; Concentrated nitric acid 180～240; Deionized water 100～200; Potassium Persulphate 0.1～0.5; Sodium lauryl sulphate 3～6; 10% sodium hydroxide solution 10～20;
(2) carbon nanotube is added in the mixed solution of the vitriol oil and concentrated nitric acid, supersound process 30min, extremely neutral with deionized water wash, dry 24h in 80 ℃ of baking ovens;
(3) vinylbenzene, carbon nanotube, Potassium Persulphate, sodium lauryl sulphate are mixed, add 10% sodium hydroxide solution and regulate pH value to 9, supersound process 30min, 80 ℃ of constant temperature, add initiator for reaction 24h, till reaction end centrifugation adds the methyl alcohol inclusion-free to the upper strata stillness of night, 50 ℃ of oven drying 24h of product.
Described carbon nanotube is multi-walled carbon nano-tubes, and the external diameter scope is 10～20nm, and length is 5～15 μ m.
Described initiator is Diisopropyl azodicarboxylate or benzoyl peroxide.
The main preparation methods of carbon current nanotube has three kinds: graphite acr method, laser evaporation method and chemical Vapor deposition process (CVD method).But the carbon nano tube surface of usually preparing contains many impurity, such as impurity such as non-crystalline state agraphitic carbon, graphite granule, granules of catalyst, and the carbon nanotube shape that has is irregular, these have all reduced the effective surface area of carbon nanotube, even carbon nanotube is reunited mutually, affected the dispersiveness of carbon nanotube.These factors have reduced the high-performance of carbon nanotube as nano material, have affected carbon nanotubes application.Strong van der Waals interaction is arranged between the carbon nanotube, it is twined mutually, form pencil and the membrane structure of arrangement disorder, and be mingled with some nanoparticles.Organic covalent linkage modification mainly is group or the side chain that the method by chemical graft makes carbon nanotube have functionalization, the purpose that makes it reach dissolving and disperse.By strongly acidic solution carbon nanotube is carried out purifying and finishing, can play purification to the carbon pipe, carbon nanotube can be disperseed in polymkeric substance well.
For improving bonding strength and the dispersion effect of filler in matrix of Nano filling and polymer interface, in-situ polymerization is the effective way of a preparation polymer based nanocomposites.The method is to utilize the surface functional group of carbon nanotube to participate in polymerization, or utilizes initiator to open the towering key of carbon nanotube, thus the excellent compatibility of acquisition and polymkeric substance.Multi-walled carbon nano-tubes is through the strong acid oxide treatment, and the surface has active function groups.The adding of carbon nanotube does not make induction period in polymerization prolong, but system viscosity is increased, and the autoacceleration phenomenon occurs ahead of time.
Carbon nano-tube modification poly styrene composite material preparation method of the present invention is simple, easy handling, and the matrix material carbon nanotube dispersed of preparation is functional, has the mechanical property excellence.
Embodiment
The present invention is further illustrated below by embodiment.
Embodiment one:
Prepare raw material by following weight proportion: vinylbenzene 100; Carbon nanotube 5; Diisopropyl azodicarboxylate 0.05; The vitriol oil 60; Concentrated nitric acid 180; Deionized water 100; Potassium Persulphate 0.5; Sodium lauryl sulphate 6; 10% sodium hydroxide solution 10;
Carbon nanotube is added in the mixed solution of the vitriol oil and concentrated nitric acid, supersound process 30min, extremely neutral with deionized water wash, dry 24h in 80 ℃ of baking ovens;
Vinylbenzene, carbon nanotube, Potassium Persulphate, sodium lauryl sulphate are mixed, add 10% sodium hydroxide solution and regulate pH value to 9, supersound process 30min, 80 ℃ of constant temperature, add Diisopropyl azodicarboxylate reaction 24h, till reaction end centrifugation adds the methyl alcohol inclusion-free to the upper strata stillness of night, 50 ℃ of oven drying 24h of product.
Embodiment two:
Prepare raw material by following weight proportion: vinylbenzene 100; Carbon nanotube 10; BP 0.1; The vitriol oil 70; Concentrated nitric acid 210; Deionized water 120; Potassium Persulphate 0.2; Sodium lauryl sulphate 4; 10% sodium hydroxide solution 12;
Carbon nanotube is added in the mixed solution of the vitriol oil and concentrated nitric acid, supersound process 30min, extremely neutral with deionized water wash, dry 24h in 80 ℃ of baking ovens;
Vinylbenzene, carbon nanotube, Potassium Persulphate, sodium lauryl sulphate are mixed, add 10% sodium hydroxide solution and regulate pH value to 9, supersound process 30min, 80 ℃ of constant temperature, add BP reaction 24h, till reaction end centrifugation adds the methyl alcohol inclusion-free to the upper strata stillness of night, 50 ℃ of oven drying 24h of product.
Embodiment three:
Prepare raw material by following weight proportion: vinylbenzene 100; Carbon nanotube 12; BP 0.12; The vitriol oil 80; Concentrated nitric acid 240; Deionized water 200; Potassium Persulphate 0.5; Sodium lauryl sulphate 5; 10% sodium hydroxide solution 15;
Carbon nanotube is added in the mixed solution of the vitriol oil and concentrated nitric acid, supersound process 30min, extremely neutral with deionized water wash, dry 24h in 80 ℃ of baking ovens;
Vinylbenzene, carbon nanotube, Potassium Persulphate, sodium lauryl sulphate are mixed, add 10% sodium hydroxide solution and regulate pH value to 9, supersound process 30min, 80 ℃ of constant temperature, add BP reaction 24h, till reaction end centrifugation adds the methyl alcohol inclusion-free to the upper strata stillness of night, 50 ℃ of oven drying 24h of product.
Embodiment four:
Prepare raw material by following weight proportion: vinylbenzene 100; Carbon nanotube 20; Diisopropyl azodicarboxylate 0.2; The vitriol oil 65; Concentrated nitric acid 195; Deionized water 160; Potassium Persulphate 0.3; Sodium lauryl sulphate 4; 10% sodium hydroxide solution 16;
Carbon nanotube is added in the mixed solution of the vitriol oil and concentrated nitric acid, supersound process 30min, extremely neutral with deionized water wash, dry 24h in 80 ℃ of baking ovens;
Vinylbenzene, carbon nanotube, Potassium Persulphate, sodium lauryl sulphate are mixed, add 10% sodium hydroxide solution and regulate pH value to 9, supersound process 30min, 80 ℃ of constant temperature, add Diisopropyl azodicarboxylate reaction 24h, till reaction end centrifugation adds the methyl alcohol inclusion-free to the upper strata stillness of night, 50 ℃ of oven drying 24h of product.
Embodiment five:
Prepare raw material by following weight proportion: vinylbenzene 100; Carbon nanotube 8; Diisopropyl azodicarboxylate 0.1; The vitriol oil 60; Concentrated nitric acid 180; Deionized water 150; Potassium Persulphate 0.3; Sodium lauryl sulphate 6; 10% sodium hydroxide solution 20;
Carbon nanotube is added in the mixed solution of the vitriol oil and concentrated nitric acid, supersound process 30min, extremely neutral with deionized water wash, dry 24h in 80 ℃ of baking ovens;
Vinylbenzene, carbon nanotube, Potassium Persulphate, sodium lauryl sulphate are mixed, add 10% sodium hydroxide solution and regulate pH value to 9, supersound process 30min, 80 ℃ of constant temperature, add Diisopropyl azodicarboxylate reaction 24h, till reaction end centrifugation adds the methyl alcohol inclusion-free to the upper strata stillness of night, 50 ℃ of oven drying 24h of product.
Performance test:
(1) carbon nanotube dispersed: observe at Hltaehi-800 projection electron microscope (TEM), the aqueous solution of the carbon nanotube after the oxide treatment that takes a morsel (or matrix material) drops on the copper mesh that scribbles carbon film, the dry rear dispersiveness that is used for observing carbon nanotube.
(2) mechanical property: test shock strength according to GB1040-93 test tensile property, GB/T1043-93.
Test result: can find out that from electromicroscopic photograph carbon nanotube is dispersed in the polymeric matrix more uniformly, and agglomeration does not occur.The tensile strength of matrix material is at 25.8～45.4MPa, and shock strength is at 13.8～18.7kJ/m
2, the tensile property of illustrative material is greatly improved, and resistance to impact shock is more suitable, and mechanical property has larger improvement.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (3)
1. the preparation method of a carbon nano-tube modification poly styrene composite material is characterized in that may further comprise the steps:
(1) prepares raw material by following weight proportion: vinylbenzene 100; Carbon nanotube 5～20; Initiator 0.05～0.2; The vitriol oil 60～80; Concentrated nitric acid 180～240; Deionized water 100～200; Potassium Persulphate 0.1～0.5; Sodium lauryl sulphate 3～6; 10% sodium hydroxide solution 10～20;
(2) carbon nanotube is added in the mixed solution of the vitriol oil and concentrated nitric acid, supersound process 30min, extremely neutral with deionized water wash, dry 24h in 80 ℃ of baking ovens;
(3) vinylbenzene, carbon nanotube, Potassium Persulphate, sodium lauryl sulphate are mixed, add 10% sodium hydroxide solution and regulate pH value to 9, supersound process 30min, 80 ℃ of constant temperature, add initiator for reaction 24h, till reaction end centrifugation adds the methyl alcohol inclusion-free to the upper strata stillness of night, 50 ℃ of oven drying 24h of product.
2. the preparation method of carbon nano-tube modification poly styrene composite material according to claim 1, it is characterized in that: described carbon nanotube is multi-walled carbon nano-tubes, and the external diameter scope is 10～20nm, and length is 5～15 μ m.
3. the preparation method of carbon nano-tube modification poly styrene composite material according to claim 1, it is characterized in that: described initiator is Diisopropyl azodicarboxylate or benzoyl peroxide.
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Cited By (4)
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| CN105061648A (en) * | 2015-07-17 | 2015-11-18 | 北京化工大学 | Preparation method of polystyrene ultrafine powder by use of acryloyl chloride-phenethylene copolymer azide modified carbon nano tube as antistatic agent |
| CN105440467A (en) * | 2014-08-12 | 2016-03-30 | 中国石油化工股份有限公司 | Carbon nanotube-polystyrene microsphere and preparation method thereof and application |
| CN109610046A (en) * | 2018-11-12 | 2019-04-12 | 深圳烯湾科技有限公司 | A kind of method and modified carbon nano-tube using Polystyrene carbon nanotube |
| CN116574360A (en) * | 2023-07-12 | 2023-08-11 | 广州声博士声学技术有限公司 | Vibration and noise reduction material for carbon nano tube and preparation method thereof |
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| CN1410455A (en) * | 2002-03-14 | 2003-04-16 | 四川大学 | Preparation method of polymer/carbon nano pipe composite emulsion and its in situ emulsion polymerization |
| CN1556124A (en) * | 2003-12-30 | 2004-12-22 | 上海交通大学 | Polysulfonated styrene grafted water soluble carbon nano pipe and its preparation method |
| CN101624470A (en) * | 2009-07-14 | 2010-01-13 | 蔡芳昌 | High-conductivity composition and preparation method thereof and preparation method of molding part |
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Patent Citations (3)
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| CN1410455A (en) * | 2002-03-14 | 2003-04-16 | 四川大学 | Preparation method of polymer/carbon nano pipe composite emulsion and its in situ emulsion polymerization |
| CN1556124A (en) * | 2003-12-30 | 2004-12-22 | 上海交通大学 | Polysulfonated styrene grafted water soluble carbon nano pipe and its preparation method |
| CN101624470A (en) * | 2009-07-14 | 2010-01-13 | 蔡芳昌 | High-conductivity composition and preparation method thereof and preparation method of molding part |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105440467A (en) * | 2014-08-12 | 2016-03-30 | 中国石油化工股份有限公司 | Carbon nanotube-polystyrene microsphere and preparation method thereof and application |
| CN105440467B (en) * | 2014-08-12 | 2018-06-15 | 中国石油化工股份有限公司 | A kind of carbon nanotube-polystyrene microsphere and preparation method thereof, application |
| CN105061648A (en) * | 2015-07-17 | 2015-11-18 | 北京化工大学 | Preparation method of polystyrene ultrafine powder by use of acryloyl chloride-phenethylene copolymer azide modified carbon nano tube as antistatic agent |
| CN105061648B (en) * | 2015-07-17 | 2018-05-25 | 北京化工大学 | It is a kind of using modified carbon nano-tube as the preparation method of the polystyrene ultrafine powder of antistatic agent |
| CN109610046A (en) * | 2018-11-12 | 2019-04-12 | 深圳烯湾科技有限公司 | A kind of method and modified carbon nano-tube using Polystyrene carbon nanotube |
| CN116574360A (en) * | 2023-07-12 | 2023-08-11 | 广州声博士声学技术有限公司 | Vibration and noise reduction material for carbon nano tube and preparation method thereof |
| CN116574360B (en) * | 2023-07-12 | 2023-09-19 | 广州声博士声学技术有限公司 | Vibration and noise reduction material for carbon nano tube and preparation method thereof |
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Application publication date: 20130424 |