CN106589866A - PCL conductive shapable material and preparation method thereof - Google Patents
PCL conductive shapable material and preparation method thereof Download PDFInfo
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- CN106589866A CN106589866A CN201611022088.2A CN201611022088A CN106589866A CN 106589866 A CN106589866 A CN 106589866A CN 201611022088 A CN201611022088 A CN 201611022088A CN 106589866 A CN106589866 A CN 106589866A
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- pcl
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- plasticizer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/43—Compounds containing sulfur bound to nitrogen
- C08K5/435—Sulfonamides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a PCL conductive shapable material, and a preparation method and an application thereof, and belongs to the field of functional polymer materials. The PCL conductive shapable material is composed of the following substances by the mass percentage: 49%-98.4% of PCL, 1%-30% of a plasticizer, 0.5%-20% of carbon nanotubes, and 0.1%-1% of an antioxidant. After the components are mixed, the PCL conductive shapable material is obtained by melting the mixture with a twin-screw or single-screw extruder or an internal mixer. The PCL is modified by the carbon nanotubes, and with addition of N-N-butyl sulfonamide, the PCL is plasticized and the carbon nanotubes are subjected to surface treatment, so good dispersion of the carbon nanotubes is achieved while the softening temperature of the composite material is reduced, and good conductivity and shapable effect are obtained. The prepared conductive shapable functional material has the advantages of small volume resistance, low softening temperature and the like, and has good application prospects in the fields of hot compress medical apparatus and instruments, medical insulation pads, electric blankets and the like.
Description
Technical field
The invention belongs to technical field of polymer materials, more particularly to a kind of PCL conduction Plastic implants and its preparation side
Method, and in particular to a kind of carbon nano-tube modification, the PCL conductions of N- butyl sulfonamide plasticising, shaping functional material and its preparation
Method.The material have resistance little and at low temperature shaping the features such as.
Background technology
CNT is found for 1991, as a kind of new monodimension nanometer material, with lightweight, mechanics, electricity
It is excellent with chemical property to wait many merits, become one of study hotspot of material science.In recent years, with carbon nanometer
The production domesticization of pipe and its reduction of cost, the performance study to CNT is progressively goed deep into, and is applied to constantly expansion.Using carbon
Pipe size is little for nanometer, big surface area and the features such as excellent electric conductivity, can be with the excellent composite of processability, such as macromolecule
CNT is added to significantly improve the property such as conductivity, intensity, elasticity, toughness and durability of original polymer in material
Matter, obtains the advanced composite material (ACM) such as good mechanical performance, good conductivity, corrosion-resistant, shielding radio wave.
The characteristics of having compared with big L/D ratio using CNT, can prepare the carbon nano-tube modification composite of high intensity.
Such as CNT is dispersed in into polyethylene (PE), polypropylene (PP), nylon (PA), polyaryl thioether sulfone and polylactic acid (PLA) material
In material, CNT heat-conductive composite material can be prepared, mainly using microelectronics, office appliance, auto industry and Aero-Space etc.
Field.
There is excellent heat conductivility using CNT, temperature sensitive water-setting is prepared by CNT and shitosan etc. are compound
Glue, has potential application prospect in medicine and hygiene fieldses such as tumor thermal therapeutical.
There is excellent electric conductivity using CNT, antistatic or conducing composite material can be prepared.In CNT
The P of carbon atom electronically forms large-scale delocalized pi-bond, and conjugation significantly, shows excellent electric conductivity, and electrical conductivity is up to copper
10,000 times.Macromolecular material is modified using CNT, in the case of adding proportion relatively low (≤10%), can be prepared
With the little conducing composite material of volume resistance.Such as CNT is added in polyethylene with polysulfones ether material, can be made
Get everything ready the polymer composite having conductivity.Compared with common conductive white carbon black, with adding proportion it is little, conductive effect is good,
The features such as mechanical property conservation rate is high, in the fields such as industrial heat preservation, household electrical appliance, medical apparatus and instruments, petrochemical industry, electronic apparatus tool
Have wide practical use.
However, the fusing point of polyethylene is higher more than 110 DEG C, polysulfones ether softening temperature is higher than 200 DEG C, at 50～60 DEG C
Cannot moulding or deformation.Consider safety problem, the medical apparatus and instruments and medical supplies for hot compression therapy are needed using below 36V directly
Stream power supply heating, in order to reach good application and raising hot compression therapy effect, it is desirable to the shaping at a temperature of 50～60 DEG C
Functional material, has not yet to see all reports.
The content of the invention
The primary and foremost purpose of the present invention is to overcome shortcoming present in above-mentioned prior art with deficiency, there is provided a kind of PCL leads
Electric Plastic implant.The present invention is with PCL as main material, and it is right to realize while carrying out plasticising to PCL using N- butyl sulfonamides
CNT is surface-treated, and is heat stabilizer from phenolic antioxidant 1010, a kind of volume resistance is obtained little, at low temperature
The PCL conduction composite functional materials of shaping, have extensive in fields such as hot compress medical apparatus and instruments, medical heat keeper and electric blankets
Application prospect.
Another object of the present invention is to provide the preparation method of the PCL conductions Plastic implant.
The purpose of the present invention is achieved through the following technical solutions：
A kind of PCL conductions Plastic implant, by following material composition by mass percentage：49%～98.4%
PCL, 1%～30% plasticizer, 0.5%～20% CNT, 0.1%～1% antioxidant.
The PCL preferred molecular weights are 30000～200000 polycaprolactone, can meet the mechanical property of composite
Require.
The CNT refers to the single wall or multi-walled carbon nano-tubes of a diameter of 2～20nm.
The plasticizer is N-N- butyl sulfonamides.
The antioxidant for plastic processing antioxidant, preferably phenolic antioxidant.
The phenolic antioxidant is preferably four [β-(3,5- di-tert-butyl-hydroxy phenyls) propanoic acid] pentaerythritol esters
Or/and β-positive octadecanol ester (1076) of (3,5- di-tert-butyl-hydroxy phenyls) propanoic acid (1010).
The PCL conductions Plastic implant can be entered using Single screw extrusion technique, banburying process or twin screw extrusion process
It is prepared by row.
The preparation method of the PCL conductions Plastic implant, comprises the steps：By 49%～98.4%PCL, 1%～
After 30% plasticizer, 0.5%～20% CNT, 0.1%～1% antioxidant mix homogeneously, using single screw extrusion machine or
Double screw extruder melting mixing, extruding pelletization, temperature is 100～180 DEG C, and engine speed is 10～400rpm, obtains PCL and leads
Electric Plastic implant；The percentage ratio is mass percent.
Preferably, the preparation method of the PCL conductions Plastic implant, comprises the steps：By 49%～98.4%
After PCL, 1%～30% plasticizer, 0.5%～20% CNT, 0.1%～1% antioxidant mix homogeneously, using banbury
Melting mixing, then using single screw extrusion machine or double screw extruder pelletize, obtains PCL conduction Plastic implants；Banburying temperature
It is 3～10min to spend for 110～150 DEG C, time, and extrusion temperature is 120～160 DEG C, and engine speed is 50～400rpm；It is described
Percentage ratio is mass percent.
Described PCL conduction Plastic implants can apply to hot compress medical apparatus and instruments, medical heat keeper and electric blanket field.
The present invention has the following advantages and effect relative to prior art：
(1) present invention adopts carbon nano-tube modification PCL, with electrical efficiency is high, addition is little and mechanical property conservation rate
High the advantages of；
(2) present invention adopts N- butyl sulfonamide plasticising PCL/ carbon nano tube compound materials, the addition of plasticizer to reduce
The softening temperature of PCL, can free moulding at 50～60 DEG C；
(3) N- butyl sulfonamides have surface treatment effect to CNT, can improve CNT in PCL matrixes
Dispersion effect, obtains good electric conductivity.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
In following embodiment, the number-average molecular weight of described PCL-1, PCL-2, PCL-3 is respectively 50000,80000 Hes
100000；N- butyl sulfonamides (NBBS) plasticizer is purchased from Zhejiang Wei Pulun companies；CNT CNTS-5 (average caliber 5nm)
Shenzhen Sanshun Zhongke New Material Co., Ltd. is purchased from CNTS-10 (average caliber 10nm)；Other raw materials and reagent etc., such as nothing
Specified otherwise, is the raw material and reagent that can be obtained from commercial sources such as conventional markets.
Embodiment 1
Accurately weigh 94.4 parts of PCL-1,5 parts of N- butyl sulfonamides, 0.5 part of CNT CNTS-5,0.1 part of antioxidant
1010, said components are pre-mixed uniformly, using single screw extrusion machine melting mixing, extruding pelletization, obtain PCL conductions plastic
Shape material；The thermal treatment zone of single screw extrusion machine is set as successively from the temperature of feed opening to head：130℃、150℃、150℃、
150 DEG C, 150 DEG C, 150 DEG C, rotating speed 300rpm.
Embodiment 2
Accurately weigh conductive compound, the 15 parts of N- butyl sulfonamides of 79.8 parts of PCL-2,5 parts of CNT CNTS-5,0.1 part
Antioxidant 1076,0.1 part of antioxidant 1010, are then pre-mixed said components uniformly, mixed using double screw extruder melting
Refining, extruding pelletization, obtain PCL conduction Plastic implants；The double screw extruder thermal treatment zone from the temperature of feed opening to head successively
It is set as：100 DEG C, 100 DEG C, 120 DEG C, 120 DEG C, 120 DEG C, 120 DEG C, rotating speed 200rpm.
Embodiment 3
Accurately weigh conductive compound, the 20 parts of N- butyl sulfonamides of 69.8 parts of PCL-3,10 parts of CNT CNTS-10,0.2
Part antioxidant 1076.Then said components are pre-mixed uniformly, using banbury melting mixing；Single screw extrusion pelletize, obtains
To PCL conduction Plastic implants；Mixing temperature：120 DEG C, rotating speed 50rpm, mixing time 5 minutes；The single screw extrusion machine thermal treatment zone
It is set as successively from the temperature of feed opening to head：130 DEG C, 150 DEG C, 150 DEG C, 170 DEG C, 170 DEG C, 170 DEG C, rotating speed
400rpm。
Embodiment 4
Accurately weigh 54.9 parts of PCL-2,30 parts of N- butyl sulfonamides, 15 parts of CNT CNTS-10,0.1 part of antioxidant
1010.Then said components are pre-mixed uniformly, are melted under conditions of 140 DEG C of temperature, rotating speed 30rpm using banbury
Melt mixing, banburying discharges after 8 minutes；Then double-screw extruding pelletizing is adopted, PCL conduction Plastic implants are obtained；Single screw rod is squeezed
Go out the machine thermal treatment zone to be set as successively from the temperature of feed opening to head：130 DEG C, 150 DEG C, 160 DEG C, 170 DEG C, 170 DEG C, 170 DEG C,
Rotating speed 50rpm.
Embodiment 5
Accurately weigh 49 parts of PCL-2,30 parts of N- butyl sulfonamides, 20 parts of CNT CNTS-5,1 part of antioxidant 1076.
Then said components are pre-mixed uniformly, mixing, extruding pelletization is melted using double screw extruder, obtain PCL conduction shapings
Material；The double screw extruder thermal treatment zone is set as successively from the temperature of feed opening to head：130℃、150℃、160℃、170
DEG C, 170 DEG C, 170 DEG C, rotating speed 250rpm.
Reference examples 1
Accurately weigh 89 parts of PCL-1,10 parts of conductive black XC72,1 part of antioxidant 1010.Preparation method is with embodiment 3.
Reference examples 2
Accurately weigh 69.8 parts of PCL-2,10 parts of conductive black XC72,30 parts of N- butyl sulfonamides, 0.2 part of antioxidant
1010.Preparation method is with embodiment 3.
Reference examples 3
Accurately weigh 49.8 parts of PCL-3,20 parts of conductive black XC72,30 parts of N- butyl sulfonamides, 0.2 part of antioxidant
1010.Preparation method is with embodiment 3.
Reference examples 4
Accurately weigh 39.8 parts of PCL-2,30 parts of conductive black XC72,30 parts of N- butyl sulfonamides, 0.2 part of antioxidant
1010.Preparation method is with embodiment 3.
Embodiment effect
The conductive compound plastification materials of PCL that embodiment 1～5 and reference examples 1～4 are prepared carry out performance test, survey
Method for testing is as follows, and test result is shown in Table 1.
Melt index is tested according to GB 3682-2000,150 DEG C of temperature, load 2.16Kg.
Tensile strength and elongation at break press GB/T 1040.3-2006 tests, and rate of extension is 200mm/min.
Surface resistivity is carried out according to GB/T 1410-2006.
Specific insulation is carried out according to GB/T 15662-1995.
Softening temperature is carried out according to A50 methods described in GB/T 1633-2000.
The performance test results of each embodiment of table 1
In embodiment, add 5% CNT, the sheet resistance and volume resistance of material are remarkably decreased, reach and partly lead
The conductivity level of body；Its Vicat softening point between 45～50 DEG C, with good low temperature shaping ability.And comparative example
In, the level of quasiconductor is can be only achieved during conductive black addition 20%, the carbon of addition 5% in its specific insulation and embodiment
Nanotube is on level terms, but the melt index of material is greatly lowered, and tensile strength and elongation at break are poor.
The performance test results of each reference examples of table 2
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention not by above-described embodiment
Limit, other any spirit without departing from the present invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of PCL conduction Plastic implant, it is characterised in that by following material composition by mass percentage：49%～
98.4% PCL, 1%～30% plasticizer, 0.5%～20% CNT, 0.1%～1% antioxidant.
2. PCL according to claim 1 conduction Plastic implant, it is characterised in that it is 30000 that the PCL is molecular weight
～200000 polycaprolactone.
3. PCL according to claim 1 conduction Plastic implant, it is characterised in that the CNT refers to a diameter of 2
The single wall or multi-walled carbon nano-tubes of～20nm.
4. PCL according to claim 1 conduction Plastic implant, it is characterised in that the plasticizer is N-N- butyl sulphurs
Amide.
5. PCL according to claim 1 conduction Plastic implant, it is characterised in that the antioxidant is phenolic antioxidant.
6. PCL according to claim 5 conduction Plastic implant, it is characterised in that the phenolic antioxidant be four [β-
(3,5- di-tert-butyl-hydroxy phenyls) propanoic acid] pentaerythritol ester or/and β-(3,5- di-tert-butyl-hydroxy phenyls) propanoic acid
Positive octadecanol ester.
7. the preparation method of the conductive Plastic implants of PCL described in any one of claim 1-3, it is characterised in that including as follows
Step：49%～98.4%PCL, 1%～30% plasticizer, 0.5%～20% CNT, 0.1%～1% antioxidant are mixed
After closing uniformly, using single screw extrusion machine or double screw extruder melting mixing, extruding pelletization, temperature is 100～180 DEG C, main
Machine rotating speed is 10～400rpm, obtains PCL conduction Plastic implants；The percentage ratio is mass percent.
8. the preparation method of the conductive Plastic implants of PCL described in any one of claim 1-3, it is characterised in that including as follows
Step：49%～98.4%PCL, 1%～30% plasticizer, 0.5%～20% CNT, 0.1%～1% antioxidant are mixed
After closing uniformly, using banbury melting mixing, then using single screw extrusion machine or double screw extruder pelletize, obtain PCL and lead
Electric Plastic implant；Mixing temperature is 110～150 DEG C, the time is 3～10min, and extrusion temperature is 120～160 DEG C, and main frame turns
Speed is 50～400rpm；The percentage ratio is mass percent.
9. the PCL conduction Plastic implants described in claim 1 are applied to hot compress medical apparatus and instruments, medical heat keeper and electric blanket neck
Domain.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109862638A (en) * | 2018-12-17 | 2019-06-07 | 广州医科大学 | A kind of temp auto-controlled exothermic material and preparation method thereof |
| CN115554455A (en) * | 2022-10-18 | 2023-01-03 | 中科兰丁(天津)医疗科学技术有限公司 | Material capable of being softened by electrifying and having temperature control function, and preparation method and application thereof |
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| CN103534298A (en) * | 2011-02-28 | 2014-01-22 | 奥菲特工业公司 | Sheet-like carbon nanotube-polymer composite material |
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| CN103534298A (en) * | 2011-02-28 | 2014-01-22 | 奥菲特工业公司 | Sheet-like carbon nanotube-polymer composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109862638A (en) * | 2018-12-17 | 2019-06-07 | 广州医科大学 | A kind of temp auto-controlled exothermic material and preparation method thereof |
| CN115554455A (en) * | 2022-10-18 | 2023-01-03 | 中科兰丁(天津)医疗科学技术有限公司 | Material capable of being softened by electrifying and having temperature control function, and preparation method and application thereof |
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Effective date of registration: 20220712 Address after: 413000 first floor, building D6, standardization plant, East Industrial Park, Yiyang high tech Zone, Yiyang City, Hunan Province Patentee after: Hunan Bosheng New Material Technology Co.,Ltd. Address before: No. 195, Dongfeng West Road, Yuexiu District, Guangzhou, Guangdong 510180 Patentee before: GUANGZHOU MEDICAL University |