CN104877232A - Beta-type polypropylene conductive composite material and preparation method thereof - Google Patents
Beta-type polypropylene conductive composite material and preparation method thereof Download PDFInfo
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- CN104877232A CN104877232A CN201510242088.2A CN201510242088A CN104877232A CN 104877232 A CN104877232 A CN 104877232A CN 201510242088 A CN201510242088 A CN 201510242088A CN 104877232 A CN104877232 A CN 104877232A
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2201/001—Conductive additives
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- C08L2205/00—Polymer mixtures characterised by other features
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- C08L2205/242—Beta spherulite nucleating agents
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Abstract
The invention relates to the technical field of high molecular materials and particularly discloses a beta-type polypropylene conductive composite material and a preparation method thereof. The beta-type polypropylene conductive composite material contains a modified carbonized bacterial cellulose nanomaterial. As the modified carbonized bacterial cellulose nanomaterial is taken as conductive filler, the defect that expensive conductive filler such as graphene micro-sheets, carbon nanotubes and the like used for preparing the conductive composite material in the prior art is overcome, so that the preparation cost of the conductive composite material is greatly lowered. The beta-type polypropylene conductive composite material has good conductive and mechanical properties.
Description
Technical field
The present invention relates to technical field of polymer materials, be specifically related to a kind of β type polypropylene conductive matrix material and preparation method thereof.
Background technology
Conducing composite material has and prevents electrostatic interaction, at electronics, electrically, petrochemical complex, machinery, photograph, the field widespread use such as munitions industry.Usually be all add conductive filler material to reach the effect improving electroconductibility, using many is metal species powder filler and carbon system weighting material, as graphene microchip, carbon nanotube etc.But there is a problem is exactly, owing to being difficult to contact with each other formation conductive network between conductive filler, need to add the many conductive fillers of comparision contents, conducing composite material just can be made to conduct electricity, and so the mechanical property of conducing composite material can reduce.In addition the filler such as graphene microchip, carbon nanotube is expensive, causes conducing composite material cost higher.In the use of nowadays polypropylene (PP), compare the shock resistance focusing on goods, i.e. the toughness of material, common polypropylene normally alpha-crystal form, property is crisp, and shock resistance is more weak.And beta crystal effectively can improve the toughness of material, but stretch, flexural strength is slightly weak.Therefore, research one there is good mechanical properties, cost low and have superior electrical conductivity can polypropylene conductive matrix material there are good market outlook.
Bacteria cellulose (BC) is the nano material of a kind of close friend, compared with plant cellulose, not containing the association such as xylogen and hemicellulose product, there is the biocompatibility of high-crystallinity, high-polymerization degree, superfine network structure, high tensile strength and excellence simultaneously, be subject to people in the application in the fields such as medical material, food, chemical industry and pay close attention to widely.As the material of a kind of novel environmental friendliness, excellent performance, the application of bacteria cellulose in matrix material is also developed gradually, mainly concentrates on the following aspects at present: (1) utilizes the mechanical property of bacteria cellulose excellence for strengthening macromolecular material; (2) utilize the fento of bacteria cellulose simultaneously
Size is less than characteristic and the high strength of 1/10th of visible wavelength, the transparent material that preparation strengthens; (3) utilize the hyperfine structure of bacteria cellulose, original position prepares hybrid inorganic-organic materials.There is no the report of bacteria cellulose for the preparation of polypropylene conductive matrix material in prior art.
Summary of the invention
Technical problem to be solved by this invention is, provides the β type polypropylene conductive matrix material that a kind of conductivity is excellent, mechanical property is good.
Above-mentioned technical problem to be solved by this invention is achieved by the following technical programs:
A kind of β type polypropylene conductive matrix material, containing modified carbonize bacteria cellulose nano material.
Preferably, described β type polypropylene conductive matrix material, containing weight percent be 1 ~ 20% modified carbonize bacteria cellulose nano material and weight percent be the homo-polypropylene of 80 ~ 99%.
Further preferably, described β type polypropylene conductive matrix material, is characterized in that, containing weight percent be 1 ~ 10% modified carbonize bacteria cellulose nano material and weight percent be the homo-polypropylene of 90 ~ 99%.
Most preferably, described β type polypropylene conductive matrix material, containing weight percent be 1 ~ 5% modified carbonize bacteria cellulose nano material and weight percent be the homo-polypropylene of 95 ~ 99%.
Preferably, described modified carbonize bacteria cellulose nano material prepares by the following method:
S01. bacteria cellulose is placed in distilled water to soak, then by extruding, obtains bacteria cellulose film;
S02. bacteria cellulose film is put into the calcium acetate aqueous solution and soak 1 ~ 5h, the bacteria cellulose film BCa of the calcium acetate solution that is absorbed;
S03. bacteria cellulose film BCa is placed in dehydrated alcohol and soaks 1 ~ 3h, separate out the surface being adsorbed on bacteria cellulose film BCa to calcium acetate, obtain bacteria cellulose film BCb;
S04. bacteria cellulose film BCb is processed 1 ~ 5h under 800 ~ 1000 DEG C of oxygen free conditions, obtain CBCb mixture;
S05. ethanolic soln CBCb mixture being placed in pimelic acid soaks 1 ~ 3h, and heating volatilization ethanol, obtains modified carbonize bacteria cellulose nano material.
Bacteria cellulose film is placed in calcium acetate solution by the present invention, then in dehydrated alcohol, soak the surface making calcium acetate precipitation to bacteria cellulose film, then under high temperature anaerobic condition, calcium acetate is oxidized to calcium oxide, bacteria cellulose carbonization, form new denatured conductive network structure, with pimelic acid solution, this conductive network structure is processed again, obtain the carbonization bacteria cellulose nano material that load has β nucleation properties-correcting agent.Described carbonization bacteria cellulose nano material has exclusive spongy nanostructure, prepares polypropylene conductive matrix material and can build good conductive network, improve the conductivity of polypropylene conductive matrix material greatly with it; In addition, in carbonization bacteria cellulose nano material of the present invention, load has β nucleation properties-correcting agent, be used for being added in polypropylene conductive matrix material, polypropylene alpha-crystal form originally can be made to become beta crystal, greatly improve the toughness of polypropylene composite material, and there is very high tensile strength and flexural strength.
Preferably, the concentration of the calcium acetate aqueous solution described in S02. is 0.1 ~ 0.2 mol/L; S02. the soak time described in is 4h.
Preferably, the soak time described in S03. is 2h,
Preferably, the bacteria cellulose film BCb described in S04. processes 4h under 900 DEG C of oxygen free conditions.
Preferably, the concentration of the ethanolic soln of the pimelic acid described in S05. is 0.08 ~ 0.4 g/L; S05. the soak time described in is 2h.
The preparation method of above-mentioned β type polypropylene conductive matrix material, is characterized in that, comprise following steps:
S11. modified carbonize bacteria cellulose nano material is dissolved in dehydrated alcohol, obtains modified carbonize bacteria cellulose nanomaterial solution, for subsequent use;
S12. homo-polypropylene is put into the machine of mixing, then add the solution configured in S11., stir, after absolute ethanol volatilizes, obtain raw material;
S13. the raw material prepared by S12. is undertaken extruding pelletizing by melt extruding means, obtains β type polypropylene conductive matrix material.
Beneficial effect: it take bacteria cellulose as the conductive filler material of novelty prepared by raw material that (1) β of the present invention type polypropylene conductive matrix material employs a kind of, this conductive filler material cost is low, overcome the shortcoming that prior art prepares in conducing composite material the conductive filler material using the costliness such as graphene microchip, carbon nanotube, greatly reduce the preparation cost of conducing composite material; (2) β type polypropylene conductive matrix material of the present invention of the present invention, modified carbonize bacteria cellulose nano material wherein can form efficient conductive network, greatly improves electrical efficiency; (3) in modified carbonize bacteria cellulose nano material of the present invention because load has β nucleation properties-correcting agent, prepare on β type polypropylene conductive matrix material containing a large amount of β crystal, the resistance to impact shock of the β type polypropylene conductive matrix material prepared is strengthened greatly, also overcomes the shortcoming that in prior art, polypropylene material resistance to impact shock is weak; (4) the β type polypropylene conductive matrix material described in, along with the increase of modified carbonize bacteria cellulose nano material, its shock strength, tensile strength and flexural strength all increase, and overcome conducing composite material in prior art makes material impact intensity, tensile strength and flexural strength reduce technology prejudice along with adding of conductive filler material.
Embodiment
Explain the present invention further below in conjunction with specific embodiment, but embodiment does not limit in any form to the present invention.
The bacteria cellulose used in following examples and homo-polypropylene all can commercially obtain; The molecular weight of the homo-polypropylene used is 10W.
Embodiment 1
The preparation of modified carbonize bacteria cellulose nano material:
S1. bacteria cellulose (BC) is placed in distilled water to soak, then by extruding, obtains bacteria cellulose film (BC film);
S2. calcium acetate aqueous solution bacteria cellulose film (BC film) being put into 0.13 mol/L soaks 4h, the bacteria cellulose film BCa of the calcium acetate solution that is absorbed;
S3. bacteria cellulose film BCa is placed in dehydrated alcohol and soaks 2h, separate out the surface being adsorbed on bacteria cellulose film BCa to calcium acetate, obtain bacteria cellulose film BCb;
S4. bacteria cellulose film BCb is processed 4h under 900 DEG C of oxygen free conditions, obtain CBCb mixture;
S5. CBCb mixture being placed in concentration is that the ethanolic soln of 0.4 g/L pimelic acid soaks 2h, and heating volatilization ethanol, obtains modified carbonize bacteria cellulose nano material.
The preparation of β type polypropylene conductive matrix material:
Above-mentioned 10g modified carbonize bacteria cellulose nano material being added in appropriate dehydrated alcohol, by stirring, obtaining the homodisperse ethanolic soln of modified carbonize bacteria cellulose nano material, for subsequent use; Again 990g powder homo-polypropylene is put into homogenizer and then add modified carbonize bacteria cellulose nano material ethanolic soln, then stirrer is started, both are stirred, the modified carbonize bacteria cellulose nano material be scattered in ethanol sticks to the surface of homo-polypropylene, after treating ethanol volatilization, obtain the raw material mixed; Last raw material is undertaken extruding pelletizing by melt extruding means, obtains β type polypropylene conductive matrix material.
Embodiment 2
The preparation of β type polypropylene conductive matrix material:
Above-mentioned 20g modified carbonize bacteria cellulose nano material (preparing with reference to embodiment 1) being added in appropriate dehydrated alcohol, by stirring, obtaining the homodisperse ethanolic soln of modified carbonize bacteria cellulose nano material, for subsequent use; Again 980g powder homo-polypropylene is put into homogenizer and then add modified carbonize bacteria cellulose nano material ethanolic soln, then stirrer is started, both are stirred, the modified carbonize bacteria cellulose nano material be scattered in ethanol sticks to the surface of homo-polypropylene, after treating ethanol volatilization, obtain the raw material mixed; Last raw material is undertaken extruding pelletizing by melt extruding means, obtains β type polypropylene conductive matrix material.
Embodiment 3
The preparation of β type polypropylene conductive matrix material:
Above-mentioned 30g modified carbonize bacteria cellulose nano material (preparing with reference to embodiment 1) being added in appropriate dehydrated alcohol, by stirring, obtaining the homodisperse ethanolic soln of modified carbonize bacteria cellulose nano material, for subsequent use; Again 970g powder homo-polypropylene is put into homogenizer and then add modified carbonize bacteria cellulose nano material ethanolic soln, then stirrer is started, both are stirred, the modified carbonize bacteria cellulose nano material be scattered in ethanol sticks to the surface of homo-polypropylene, after treating ethanol volatilization, obtain the raw material mixed; Last raw material is undertaken extruding pelletizing by melt extruding means, obtains β type polypropylene conductive matrix material.
Embodiment 4
The preparation of β type polypropylene conductive matrix material:
Above-mentioned 50g modified carbonize bacteria cellulose nano material (preparing with reference to embodiment 1) being added in appropriate dehydrated alcohol, by stirring, obtaining the homodisperse ethanolic soln of modified carbonize bacteria cellulose nano material, for subsequent use; Again 950g powder homo-polypropylene is put into homogenizer and then add modified carbonize bacteria cellulose nano material ethanolic soln, then stirrer is started, both are stirred, the modified carbonize bacteria cellulose nano material be scattered in ethanol sticks to the surface of homo-polypropylene, after treating ethanol volatilization, obtain the raw material mixed; Last raw material is undertaken extruding pelletizing by melt extruding means, obtains β type polypropylene conductive matrix material.
Embodiment 5
The preparation of β type polypropylene conductive matrix material:
Above-mentioned 100g modified carbonize bacteria cellulose nano material (preparing with reference to embodiment 1) being added in appropriate dehydrated alcohol, by stirring, obtaining the homodisperse ethanolic soln of modified carbonize bacteria cellulose nano material, for subsequent use; Again 900g powder homo-polypropylene is put into homogenizer and then add modified carbonize bacteria cellulose nano material ethanolic soln, then stirrer is started, both are stirred, the modified carbonize bacteria cellulose nano material be scattered in ethanol sticks to the surface of homo-polypropylene, after treating ethanol volatilization, obtain the raw material mixed; Last raw material is undertaken extruding pelletizing by melt extruding means, obtains β type polypropylene conductive matrix material.
Embodiment 6
Carry out stretching according to ASTM standard method, the test of bending and impact property.Method is as follows: in the matrix material that each is not of the same race, gets 5 samples and has carried out different Mechanics Performance Testings.Tensile strength presses ASTMD-638 standard testing, and draw speed is 50mm min
-1, probe temperature is 23 DEG C; Bending property presses ASTMD-790 standard testing, and test rate is 2mm min
-1, probe temperature is 23 DEG C; Izod notched impact presses ASTMD-256 test, and probe temperature is 23 DEG C, and pendulum energy grade is 5.5J.
The testing method of volume specific resistance: adopt EST121 type numeral ultra-high resistance, micro current instrument, according to GB/T1410-2006 test, sample diameter 82mm, thick 2mm, each sample surveys five groups, gets its mean value.
As can be seen from the data of table 1, add in homo-polypropylene modified carbonize bacteria cellulose that the present invention prepares nano-material modified after the β type polypropylene conductive matrix material that obtains, there is very excellent conductivity, illustrate that modified carbonize bacteria cellulose nano material of the present invention joins in polypropylene and can form efficient conductive network in polypropylene, greatly improve electrical efficiency.And along with the increase volume specific resistance decline highly significant of modified carbonize bacteria cellulose, when in β type polypropylene conductive matrix material, the content of modified carbonize bacteria cellulose reaches 5% and 10%, its volume specific resistance is respectively 1.0*10^3 and 5*10^2, and conductivity is very good.
In addition, because load has β nucleation properties-correcting agent in modified carbonize bacteria cellulose nano material of the present invention, prepare on β type polypropylene conductive matrix material containing a large amount of β crystal, the resistance to impact shock of the β type polypropylene conductive matrix material prepared is strengthened greatly, also overcomes the shortcoming that in prior art, polypropylene material resistance to impact shock is weak.It also has good tensile strength and flexural strength, suitable with homo-polypropylene.Along with the increase of modified carbonize bacteria cellulose nano material, the shock strength of β type polypropylene conductive matrix material, tensile strength and flexural strength all increase, and overcome conducing composite material in prior art makes material impact intensity, tensile strength and flexural strength reduce technology prejudice along with adding of conductive filler material.
β type polypropylene conductive matrix material of the present invention, the modified carbonize bacteria cellulose nano material employed is as conductive filler material, and production cost is low, overcomes in prior art the conductive filler material using graphene microchip, carbon nanotube etc. expensive.Greatly can reduce the preparation cost of conducing composite material.
Claims (10)
1. a β type polypropylene conductive matrix material, is characterized in that, containing modified carbonize bacteria cellulose nano material.
2. β type polypropylene conductive matrix material according to claim 1, is characterized in that, containing weight percent be 1 ~ 20% modified carbonize bacteria cellulose nano material and weight percent be the homo-polypropylene of 80 ~ 99%.
3. β type polypropylene conductive matrix material according to claim 1, is characterized in that, containing weight percent be 1 ~ 10% modified carbonize bacteria cellulose nano material and weight percent be the homo-polypropylene of 90 ~ 99%.
4. β type polypropylene conductive matrix material according to claim 1, is characterized in that, containing weight percent be 1 ~ 5% modified carbonize bacteria cellulose nano material and weight percent be the homo-polypropylene of 95 ~ 99%.
5. the β type polypropylene conductive matrix material according to any one of claim 1 ~ 4, is characterized in that, described modified carbonize bacteria cellulose nano material prepares by the following method:
S01. bacteria cellulose is placed in distilled water to soak, then by extruding, obtains bacteria cellulose film;
S02. bacteria cellulose film is put into the calcium acetate aqueous solution and soak 1 ~ 5h, the bacteria cellulose film BCa of the calcium acetate solution that is absorbed;
S03. bacteria cellulose film BCa is placed in dehydrated alcohol and soaks 1 ~ 3h, separate out the surface being adsorbed on bacteria cellulose film BCa to calcium acetate, obtain bacteria cellulose film BCb;
S04. bacteria cellulose film BCb is processed 1 ~ 5h under 800 ~ 1000 DEG C of oxygen free conditions, obtain CBCb mixture;
S05. ethanolic soln CBCb mixture being placed in pimelic acid soaks 1 ~ 3h, and heating volatilization ethanol, obtains modified carbonize bacteria cellulose nano material.
6. β type polypropylene conductive matrix material according to claim 5, is characterized in that, the concentration of the calcium acetate aqueous solution described in S02. is 0.1 ~ 0.2 mol/L; S02. the soak time described in is 4h.
7. β type polypropylene conductive matrix material according to claim 5, it is characterized in that, the soak time described in S03. is 2h.
8. β type polypropylene conductive matrix material according to claim 5, it is characterized in that, the bacteria cellulose film BCb described in S04. processes 4h under 900 DEG C of oxygen free conditions.
9. β type polypropylene conductive matrix material according to claim 5, is characterized in that, the concentration of the ethanolic soln of the pimelic acid described in S05. is 0.08 ~ 0.4 g/L; S05. the soak time described in is 2h.
10. the preparation method of the β type polypropylene conductive matrix material described in any one of claim 1 ~ 4, is characterized in that, comprise following steps:
S11. modified carbonize bacteria cellulose nano material is dissolved in dehydrated alcohol, obtains modified carbonize bacteria cellulose nanomaterial solution, for subsequent use;
S12. homo-polypropylene is put into the machine of mixing, then add the solution configured in S11., stir, after absolute ethanol volatilizes, obtain raw material;
S13. the raw material prepared by S12. is undertaken extruding pelletizing by melt extruding means, obtains β type polypropylene conductive matrix material.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110021701A1 (en) * | 2006-08-16 | 2011-01-27 | Imperial Innovations Limited | Material comprising microbially synthesized cellulose associated with a support like a polymer and/or fibre |
| CN104532407A (en) * | 2014-12-24 | 2015-04-22 | 暨南大学 | Carbon nanofibers based on carbonized bacterial cellulose as well as composition and application of carbon nanofibers |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110021701A1 (en) * | 2006-08-16 | 2011-01-27 | Imperial Innovations Limited | Material comprising microbially synthesized cellulose associated with a support like a polymer and/or fibre |
| CN104532407A (en) * | 2014-12-24 | 2015-04-22 | 暨南大学 | Carbon nanofibers based on carbonized bacterial cellulose as well as composition and application of carbon nanofibers |
Non-Patent Citations (4)
| Title |
|---|
| FENG JING JIANG ET AL: "Bacterial cellulose nanofibrous membrane as thermal stable separator for lithium-ion batteries", 《JOURNAL OF POWER SOURCES》 * |
| 吴慧等: ""碳化细菌纤维素/石墨烯(CBC/CCG)复合材料的制备及电化学性能研究"", 《功能材料》 * |
| 张秀菊等: ""细菌纤维素纳米复合材料的研究进展"", 《合成纤维》 * |
| 汪丽粉等: ""细菌纤维素性质及应用的研究进展"", 《微生物学通报》 * |
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