CN101214722A - Method for preparing designable layered polymer base conductive composite material - Google Patents
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- CN101214722A CN101214722A CNA200710051024XA CN200710051024A CN101214722A CN 101214722 A CN101214722 A CN 101214722A CN A200710051024X A CNA200710051024X A CN A200710051024XA CN 200710051024 A CN200710051024 A CN 200710051024A CN 101214722 A CN101214722 A CN 101214722A
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Abstract
The invention provides a microlayer coextrusion device to prepare layered polymer-based conducting composite material with insulating layers and conducting layers, which are interlaced. The insulating layer granules and the conducting layer granules are fed into two extruders of the microlayer coextrusion device for fusion and plastification. Two streams of fusant are superposed into two layers at the position of a convergence unit. After the fusant is cut and superposed by n separation and superposition units, the composite material of 2<n+1> layers is got. The conductibility of the material has anisotropy. The proportion of the number of the layers to the thickness of the conducting layers and the insulating layers is determined by the number of the separation and superposition units and the speed ratio of the extruders. Accordingly, the percolation value and the resistivity of the conducting material are designable. Compared with the traditional method of preparation, the polymer conduction composite material prepared by the invention has the characteristics of low percolation value, low resistivity, and high breaking extensibility. The equipment provided by the invention is simple and available. The required raw materials are sold in the market without synthetizing other chemicals. The equipment is operated simply; the manufacturing cost is low; the efficiency is high.
Description
One, technical field
The present invention relates to polymer processing field, in particular, the present invention relates to the preparation of polymer base conductive composite material.
Two, background technology
Polymer base conductive composite material is conductive materials to be filled in the polymeric matrix with processing technology in some way and a kind of functional composite material of forming, it not only can satisfy the needs of people to conductive material, and shape, chemical stability in light weight owing to it, that easily be processed into various complexity reach electrical conductivity characteristics such as can regulate well and are widely used in a big way, and cause that academia and industrial quarters study the very big interest of its conductive structure and performance, promoted the modern material the reach of science.Polymer base conductive composite material can be widely used as antistatic material, conductive material, resistive element material (ptc material) and electromagnetic shielding material etc.Conductive filler commonly used is divided into carbon, metal and metal oxide three major types, and wherein carbon class conductive filler is mainly carbon black, graphite, carbon fiber and CNT.
Usually, the percolation threshold of polymer base conductive composite material is higher.Higher conductive materials addition not only causes the toughness of composite to descend significantly, and causes the machine-shaping difficulty, and production cost increases.Therefore, the electric conductivity that improves material under percolation threshold that reduces material under the requirement of satisfying electric conductivity or the condition at fixing conductive materials content becomes the target of research and production worker pursuit.Studies show that in a large number, the electric conductivity of polymer base conductive composite material depends primarily on the conductive channel or the network of conductive materials relevant formation with long-range in polymeric matrix, and the formation of conductive network and improve with the aggregated structure and the distribution of carbon black in polymer of the lax behavior of polymer macromolecule chain, polymer closely related in the system.
In real world applications, a kind of method that can effectively reduce percolation threshold is that matrix resin adopts heterogeneous system, the most generally three-phase system (containing conductive materials).Conductive materials is added in two kinds of incompatible polymer matrixes, by suitable technology controlling and process make the conductive materials precedence partition incompatible polymer blend one mutually in or two-phase at the interface, the proportioning of regulating incompatible polymer makes the conductive materials place become continuous phase or common continuous phase mutually, realize conductive materials in a continuous phase or exceeding on the continuous interfacial blend this continuous phase exceeding in another polymer and ooze (promptly two exceeding oozes), thereby the reduction percolation threshold.Such as (Selective Localizationof Carbon Black in Immiscible Polymer Blends:A Useful Tool To Design ElectricalConductive Composites Macromolecules such as Gubbels; 1994; 27 (7); 1972-74.) the conductive black particle is filled into polyethylene phase in polyethylene/polystyrene co-continuous system selectively, the excess effusion value of prepared conducing composite material is reduced to 3wt%.Li Zhongmings etc. (can form the preparation method of the composite of original position conduction fento network: Chinese patent, CN1528816,2004) by drying-masterbatch preparation-melt blending extrude-processing step such as hot-stretch-quenching-granulation and condition prepared In-situ Composite, conductive filler be present in dystectic fiber mutually in, these fibers can form conductive network again mutually in the goods of back machine-shaping, therefore the conductive filler amount that adds is few, greatly reduces the conduction excess effusion value of composite.
Obviously in said method, realize twoly exceeding the precondition of oozing and being to use the bi-component polymeric matrix, and conductive materials place polymer phase must be present in another phase with the form of continuous phase.And because the distribution in the conductive materials two-phase is wayward and calculating, the structural form of two-phase is subject to the influence of various factors such as proportioning, ratio of viscosities, surface tension ratio and processing technology of component, thereby from thermodynamics, the consideration of rheology angle, be difficult to obtain to repeat and controllable ideal form structure, be difficult to prepare and have the composite that can design electric conductivity by traditional blend complex method.
Three, summary of the invention
The objective of the invention is provides a kind of new method for preparing polymer base conductive composite material at the present situation for preparing polymer base conductive composite material, the very difficult acquisition of conducing composite material for preparing with the conducing composite material preparation method who solves prior art can repeat and controllable ideal form structure, and electric conductivity is difficult to have technical problems such as designability.
The method for preparing designable layered polymer base conductive composite material disclosed by the invention, be that conductive layer material and insulating barrier material are dropped into respectively in the two extruders of layering co-extrusion device, behind the fusion plastification, make two strands of melts superimposed in convergence device, through the cutting of the folded unit of n branch and superimposed after, promptly make 2 from exporting the mould outflow
(n+1))Layer is by conductive layer and the alternatively distributed polymer base conductive composite material of insulating barrier.The conductive layer of polymer base conductive composite material is recently adjusted than leading to the rotating speed that changed two extruders with thickness of insulating layer.。
In technique scheme, described conductive layer material is served as reasons and is extruded the pellet of producing through extruder as the filler of conductive materials with as the mixed with polymers of matrix.The weight content of conductive materials in the conductive layer material generally is controlled in the scope of 1-30%.Conductive materials can be a kind of in carbon black, graphite, carbon fiber, CNT, metal and the burning, or two or more.Matrix polymer also can be a kind of in polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyamide, polymethyl methacrylate, PETG, synthetic rubber and the polyurethane, or two or more.
In technique scheme, described insulating barrier material can be and is selected from a kind of straight polymer in polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyamide, polymethyl methacrylate, PETG, synthetic rubber and the polyurethane, or for being selected from the pellet that two kinds polymer is produced through blend that is no less than in them.
In technique scheme, when the conductive layer matrix polymer is incompatible with the insulating barrier polymer, when preparation conductive layer material pellet or insulating barrier material pellet, add the compatilizer that polymer is merged mutually.Compatilizer can be maleic anhydride grafted polyethylene, maleic anhydride inoculated polypropylene, SBS etc.The particular type of compatilizer is determined according to polymer property.
In technique scheme, before the preparation layered polymer base conductive composite material, will prepare the raw material drying of layered polymer base conductive composite material to moisture content＜0.02%.
In technique scheme, the two extruders of preparation layered polymer base conductive composite material is put connection by convergence device and the branch closed assembly that contains the folded unit of n branch.
The method for preparing designable layered polymer base conductive composite material disclosed by the invention, be characterized in utilizing layering co-extrusion device to prepare conductive layer and the alternatively distributed laminar composite of insulating barrier, the material of conductive layer and insulating barrier is extruded by two extruders respectively, enter convergence device through two connectors, after the convergence device exit is superimposed, enter several and divide folded unit, after dividing the folded unit multiplication number of plies, composite product pulls out the layering unit through cooling device under the draw-gear effect at last.Conductive layer and insulating barrier are continuous phase extruding on the direction.Conductive layer is the common infill system of polymer and conductive materials, and insulating barrier is pure polymer.The polymer of conductive layer and insulating barrier can be with a kind of polymer.Therefore, two the exceeding of using this method to can be implemented in the single polymer matrix oozes.The number of plies of stratiform conducing composite material is n by the number control that divides folded unit if divide the number of folded unit, and number of plies N is 2 so
(n+1)The bed thickness of conductive layer and insulating barrier is than can recently controlling by the rotating speed of regulating two extruders.Like this, the structure of stratiform conducing composite material is programmable, thereby obtains controllable percolation threshold and resistivity.
Experimental result shows that the polymer base conductive composite material that adopts method of the present invention to prepare is compared with the polymer base conductive composite material that conventional method prepares, and excess effusion value reduces, and room temperature resistivity reduces.Conductive materials is littler more even in the dispersion size of polymeric matrix, and Du Te layer structure makes elongation at break increase substantially in addition.
The present invention has following advantage:
1, equipment involved in the present invention is simple and easy to, and only needs the logical extruder of two Daeporis is connect by convergence device, and adds the folded unit of some branches at mouth mould place; Needed raw material is commercially available, need not synthesize other chemicals.This method has simple to operation, and production cost is low, characteristics such as efficient height.
2, the polymer base conductive composite material by the present invention's preparation has layer structure, and conductive layer and insulating barrier are alternately arranged, and conductivity has anisotropy.
3, number that can be by change dividing folded unit and the number of plies that the extruder rotating speed is recently controlled polymer base conductive composite material and the thickness rate of conductive layer and insulating barrier, thus can regulate and control its excess effusion value and resistivity effectively.
4, through the prepared polymer base conductive composite material of method provided by the invention, its elongation at break increases substantially.
5,, can in the single polymer matrix, realize pair exceeding and ooze by the polymer base conductive composite material of the inventive method preparation.
The present invention also has more otherwise advantages.
Four, description of drawings
Fig. 1 is the structural representation of layering co-extrusion device involved in the present invention.In the drawings, A, B: extruder, C: convergence device D: divide folded unit E: outlet mould
Fig. 2 is the structural representation of the polymer base conductive composite material of the present invention's preparation.In the drawings, F: insulating barrier, G: conductive layer.
Five, the specific embodiment
By the following examples the present invention is further described specifically.In following each embodiment, the consumption of each component is weight consumption.Be necessary to be pointed out that at this following examples only are used for that the present invention is described further; can not be interpreted as limiting the scope of the invention; this art skilled person makes some nonessential improvement and adjustment according to the invention described above content to the present invention, still belongs to protection scope of the present invention.
The good effect that the present invention produces can describe with embodiment.
Embodiment 1
Raw material is polypropylene and carbon black, and insulating barrier and conductive layer are respectively virgin pp and carbon black filled polypropylene.At first prepare common carbon black filled polypropylene, content of carbon black is 11%: after polypropylene and carbon black drying, and melting mixing granulation in double screw extruder.Conductive layer and insulating barrier pellet drop into respectively in the two extruders of layering co-extrusion device, the extruder rotating ratio is 1: 1, each section of extruder temperature is controlled between 170-200 ℃, the temperature of convergence device, the folded unit of branch and outlet mould is 200 ℃, use 2 branches to fold the unit, conducing composite material goods melt flows out from the outlet mould under the traction of draw-gear, after the cooling device cooling, promptly prepares 8 layers stratiform polypropylene-base conducing composite material.The resistivity of this material is 5.91 * 10
3Ω cm, PTC intensity is 3.38, elongation at break is 416%.As a comparison, the resistivity and the elongation at break of traditional polypropylene based conductive composite material of identical content of carbon black are respectively 2.16 * 10
4Ω cm and 50%.
Embodiment 2
Raw material is polyethylene and carbon black, and insulating barrier and conductive layer are respectively pure polyethylene and carbon black filled polyethylene.At first prepare common carbon black filled polyethylene, content of carbon black is 11%: after polyethylene and carbon black drying, and melting mixing granulation in double screw extruder.Conductive layer and insulating barrier pellet drop into respectively in the two extruders of microbedding co-extrusion device, the extruder rotating ratio is 2: 1, each section of extruder temperature is controlled between 170-200 ℃, the temperature of convergence device, the folded unit of branch and outlet mould is 200 ℃, use 1 branch to fold the unit, prepare 4 layers stratiform polyvinyl conducing composite material.The resistivity of this material is 5.02 * 10
3Ω cm, PTC intensity is 3.26, elongation at break is 316%.As a comparison, the resistivity and the elongation at break of the conventional polyethylene based conductive composite material of identical content of carbon black are respectively 4.67 * 10
4Ω cm and 89%.
Embodiment 3
Raw material is polypropylene and carbon black, and insulating barrier and conductive layer are respectively virgin pp and carbon black filled polypropylene.At first prepare common carbon black filled polypropylene, content of carbon black is respectively 2,4,6,8,10,12,14,18,22,30%: after polypropylene and carbon black drying, and melting mixing granulation in double screw extruder.Conductive layer and insulating barrier pellet drop into respectively in the two extruders of microbedding co-extrusion device, the extruder rotating ratio is 1: 1, each section of extruder temperature is controlled between 170-200 ℃, the temperature of convergence device, the folded unit of branch and outlet mould is 200 ℃, use 1 branch to fold the unit, prepare 4 layers stratiform polypropylene-base conducing composite material.The excess effusion value of this material is approximately 5.0wt%.As a comparison, the excess effusion value of traditional polypropylene based conductive composite material is approximately 7.0wt%.
Embodiment 4
Raw material is polystyrene, carbon black and CNT, and insulating barrier and conductive layer are respectively pure polystyrene and carbon black, carbon nano-tube filled polystyrene.At first prepare common carbon black filled polystyrene, carbon black and content of carbon nanotubes are respectively 14.35 and 0.55%: after polypropylene, carbon black and CNT drying, and melting mixing granulation in double screw extruder.Conductive layer and insulating barrier pellet drop into respectively in the two extruders of microbedding co-extrusion device, the extruder rotating ratio is 1: 2, each section of extruder temperature is controlled between 170-200 ℃, the temperature of convergence device, the folded unit of branch and outlet mould is 200 ℃, use 2 branches to fold the unit, prepare 8 layers stratiform polypropylene-base conducing composite material.The resistivity of this material is 3.9 * 10
2Ω cm.As a comparison, when conductive materials filling content was identical, the carbon black of conventional method preparation, the resistivity of carbon nano-tube filled polystyrene were 7.84 * 10
5Ω cm.
Embodiment 5
Raw material is polypropylene, carbon black and CNT, and insulating barrier and conductive layer are respectively virgin pp and carbon black, carbon nano-tube filled polypropylene.At first prepare common carbon black filled polypropylene, carbon black and content of carbon nanotubes are respectively 12.35 and 0.65%: after polypropylene, carbon black and CNT drying, and melting mixing granulation in double screw extruder.Conductive layer and insulating barrier pellet drop into respectively in the two extruders of microbedding co-extrusion device, the extruder rotating ratio is 1: 1, each section of extruder temperature is controlled between 170-200 ℃, the temperature of convergence device, the folded unit of branch and outlet mould is 200 ℃, use 3 branches to fold the unit, prepare 16 layers stratiform polypropylene-base conducing composite material.The resistivity of this material is 7.0 * 10
2Ω cm, elongation at break are 680%.As a comparison, when conductive materials filling content was identical, carbon black, the carbon nano-tube filled polyacrylic resistivity of conventional method preparation were 2.40 * 10
6Ω cm, elongation at break are 35%.
Embodiment 6
Raw material is polypropylene, nylon 6, maleic anhydride inoculated polypropylene (as the compatilizer of polypropylene and nylon) and carbon black, and insulating barrier and conductive layer are respectively polypropylene and (add and carbon black filled nylon 6.At first prepare common carbon black filled nylon 6, content of carbon black is 14%: after nylon 6 and carbon black drying, and melting mixing granulation in double screw extruder.Conductive layer and insulating barrier pellet drop into respectively in the two extruders of microbedding co-extrusion device, the extruder rotating ratio is 1: 1, each section of extruder temperature is controlled between 230～250 ℃, the temperature of convergence device, the folded unit of branch and outlet mould is 250 ℃, use 7 branches to fold the unit, prepare 256 layers stratiform polypropylene-base conducing composite material.The resistivity of this material is 2.16 * 10
3Ω cm.
Claims (10)
1. method for preparing designable layered polymer base conductive composite material, it is characterized in that conductive layer material and insulating barrier material drop into respectively in the two extruders of layering co-extrusion device (A, B), behind the fusion plastification, two strands of melts are superimposed in convergence device (C), through the cutting of the folded unit (D) of n branch and superimposed after, obtain 2 from exporting mould (E) outflow
(n+1))Layer is by conductive layer and the alternatively distributed polymer base conductive composite material of insulating barrier.
2. according to the described method for preparing designable layered polymer base conductive composite material of claim 1, it is characterized in that the conductive layer and the thickness ratio of insulating barrier pass through the rotating ratio adjustment of two extruders.
3. according to the described method for preparing designable layered polymer base conductive composite material of claim 1, it is characterized in that the conductive layer material is served as reasons to extrude the pellet of producing through extruder as the filler of conductive materials with as the mixed with polymers of matrix.
4. according to the described method for preparing designable layered polymer base conductive composite material of claim 3, it is characterized in that the weight content of conductive materials in the conductive layer material is 1-30%.
5. according to the described method for preparing designable layered polymer base conductive composite material of claim 4, it is characterized in that conductive materials is at least a in carbon black, graphite, carbon fiber, CNT, metal and the burning.
6. according to the described method for preparing designable layered polymer base conductive composite material of claim 4, it is characterized in that matrix polymer is at least a in polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyamide, polymethyl methacrylate, PETG, synthetic rubber and the polyurethane.
7. according to the described method for preparing designable layered polymer base conductive composite material of each claim in the claim 1 to 6, it is characterized in that the insulating barrier material for being selected from a kind of straight polymer in polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyamide, polymethyl methacrylate, PETG, synthetic rubber and the polyurethane, or for being selected from the pellet that two kinds polymer is produced through blend that is no less than in them.
8. according to the described method for preparing designable layered polymer base conductive composite material of claim 7; it is characterized in that when the conductive layer matrix polymer is incompatible with the insulating barrier polymer, at preparation conductive layer material particles or/and add the compatilizer that polymer is merged mutually during the insulating barrier material particles.
9. according to the described method for preparing designable layered polymer base conductive composite material of claim 7, it is characterized in that before the preparation layered polymer base conductive composite material, will preparing the raw material drying of layered polymer base conductive composite material to moisture content＜0.02%.
10. according to the described method for preparing designable layered polymer base conductive composite material of claim 7, the two extruders (A, B) that it is characterized in that preparing layered polymer base conductive composite material is put connection by convergence device (C) and the branch closed assembly that contains the folded unit (D) of n branch.
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| CN106344497B (en) * | 2016-09-05 | 2021-06-04 | 四川大学 | Method for preparing polymer multilayer hydrogel drug sustained-release material |
| CN106848081A (en) * | 2017-03-08 | 2017-06-13 | 武汉华星光电技术有限公司 | The preparation method of flexible AMOLED display screens and conducting resinl film layer |
| CN106848081B (en) * | 2017-03-08 | 2018-11-09 | 武汉华星光电技术有限公司 | The production method of flexible AMOLED display screens and conducting resinl film layer |
| CN109904705A (en) * | 2017-12-07 | 2019-06-18 | 泰科电子(上海)有限公司 | The manufacturing method of conductive terminal blank item and the manufacturing method of conductive terminal |
| CN108659245A (en) * | 2018-05-17 | 2018-10-16 | 中国人民解放军国防科技大学 | Shielding reinforced periodic structure |
| CN108659245B (en) * | 2018-05-17 | 2020-07-31 | 中国人民解放军国防科技大学 | Shielding reinforced periodic structure |
| CN108855621A (en) * | 2018-06-07 | 2018-11-23 | 汉王科技股份有限公司 | Processing method, electrostatic precipitation piece and the precipitator of electrostatic precipitation piece |
| CN113799286A (en) * | 2020-06-12 | 2021-12-17 | 四川大学 | Preparation method of polymer blend with controllable dispersed phase size and dimension |
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