CN104877232B - A kind of β type polypropylene conductive composite material and preparation method - Google Patents
A kind of β type polypropylene conductive composite material and preparation method Download PDFInfo
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- CN104877232B CN104877232B CN201510242088.2A CN201510242088A CN104877232B CN 104877232 B CN104877232 B CN 104877232B CN 201510242088 A CN201510242088 A CN 201510242088A CN 104877232 B CN104877232 B CN 104877232B
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- bacteria cellulose
- composite material
- type polypropylene
- conductive composite
- polypropylene conductive
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- 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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- 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
- C08K9/04—Ingredients treated with organic substances
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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
- 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
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
- C08L2205/242—Beta spherulite nucleating agents
Abstract
The present invention relates to technical field of polymer materials, specifically disclose a kind of β type polypropylene conductive composite material and preparation method.The β type polypropylene conductive composite material contains modified carbonization bacteria cellulose nano material.Since it is using modified carbonization bacteria cellulose nano material as conductive filler, the shortcomings that overcoming in prior art preparation conducing composite material using the expensive conductive filler such as graphene microchip, carbon nanotube, the preparation cost of conducing composite material is substantially reduced.The β type polypropylene conductive composite material has good conductive property and mechanical property.
Description
Technical field
The present invention relates to technical field of polymer materials, and in particular to a kind of β type polypropylene conductive composite material and its system
Preparation Method.
Background technique
Conducing composite material is with electrostatic interaction is prevented, in electronics, electrical, petrochemical industry, machinery, photograph, munitions industry
Equal fields are widely applied.Usually all be addition conductive filler come achieve the effect that improve electric conductivity, using it is more be metal
Class powder filler and carbon system filler, such as graphene microchip, carbon nanotube.But have a problem that and be exactly, due to leading
It is difficult to contact with each other to form conductive network between electric filler, needs to add the conductive filler more than comparision contents, could to lead
Composite is conductive, and so the mechanical property of conducing composite material can reduce.Furthermore graphene microchip, carbon nanotube etc.
Filler is expensive, leads to conducing composite material higher cost.Nowadays polypropylene (PP) in use, comparing focuses on the anti-of product
Impact property, the i.e. toughness of material, common polypropylene are usually alpha-crystal form, and property is crisp, and shock resistance is weaker.And beta crystal can
Be effectively improved the toughness of material, but stretch, bending strength it is slightly weak.Therefore, study it is a kind of there are good mechanical properties, it is at low cost and
Polypropylene conductive composite material with superior electrical conductivity energy has good market prospects.
Bacteria cellulose (BC) is the nano material of close friend a kind of, compared with plant cellulose, is free of lignin and half fiber
The associations product such as element is tieed up, while there is high-crystallinity, high polymerization degree, hyperfine network structure, high tensile strength and excellent
Different biocompatibility, the application in fields such as medical material, food, chemical industry are widely paid close attention to by people.As a kind of new
Environmental-friendly, the material that has excellent performance of type, application of the bacteria cellulose in terms of composite material is also gradually developed, main at present
Concentrate on the following aspects: (1) mechanical property for utilizing bacteria cellulose excellent is for enhancing high molecular material；(2) same
The fento of Shi Liyong bacteria cellulose
Size is less than 1/10th characteristic and high intensity of visible wavelength, prepares the transparent material of enhancing；(3) it utilizes
The hyperfine structure of bacteria cellulose, is prepared in situ hybrid inorganic-organic materials.It there is no in the prior art and use bacteria cellulose
In the report for preparing polypropylene conductive composite material.
Summary of the invention
The β type polypropylene that the technical problem to be solved by the invention is to provide a kind of electric conductivities is excellent, mechanical property is good
Conducing composite material.
Above-mentioned technical problem to be solved by this invention is achieved by the following technical programs:
A kind of β type polypropylene conductive composite material contains modified carbonization bacteria cellulose nano material.
Preferably, the β type polypropylene conductive composite material, the modified carbonization for being 1 ~ 20% containing weight percent are thin
The homopolypropylene that fungin nano material and weight percent are 80 ~ 99%.
It is further preferred that the β type polypropylene conductive composite material, which is characterized in that containing weight percent be 1
The homopolypropylene that ~ 10% modified carbonization bacteria cellulose nano material and weight percent is 90 ~ 99%.
Most preferably, the β type polypropylene conductive composite material, the modified carbonization for being 1 ~ 5% containing weight percent are thin
The homopolypropylene that fungin nano material and weight percent are 95 ~ 99%.
Preferably, the modified carbonization bacteria cellulose nano material is prepared via a method which to obtain:
S01. bacteria cellulose is placed in distilled water and is impregnated, then by squeezing, obtain bacteria cellulose film；
S02. bacteria cellulose film is put into 1 ~ 5h of immersion, the bacterium for the calcium acetate solution that is absorbed in calcium acetate aqueous solution
Cellulose membrane BCa；
S03. bacteria cellulose film BCa is placed in 1 ~ 3h of immersion in dehydrated alcohol, until calcium acetate precipitation is adsorbed on bacterium fibre
The surface for tieing up plain film BCa, obtains bacteria cellulose film BCb；
S04., bacteria cellulose film BCb is handled to 1 ~ 5h under 800 ~ 1000 DEG C of oxygen free conditions, obtains CBCb compound；
S05. CBCb compound is placed in 1 ~ 3h of immersion in the ethanol solution of pimelic acid, heating volatilization ethyl alcohol obtains carbon modified
Change bacteria cellulose nano material.
Bacteria cellulose film is placed in calcium acetate solution by the present invention, and then impregnating in dehydrated alcohol is precipitated calcium acetate
To the surface of bacteria cellulose film, calcium acetate is then oxidized to calcium oxide, bacteria cellulose carbonization under the conditions of high temperature anaerobic,
Form new denatured conductive network structure, then the conductive network structure handled with pimelic acid solution, obtain load have β at
The carbonization bacteria cellulose nano material of core modifying agent.The carbonization bacteria cellulose nano material has exclusive spongy receive
Rice structure, good conductive network can be constructed by preparing polypropylene conductive composite material with it, greatly improved polypropylene and led
The electric conductivity of composite；In addition, the present invention is carbonized, load has β to be nucleated modifying agent in bacteria cellulose nano material, uses
It is added in polypropylene conductive composite material, the polypropylene alpha-crystal form of script can be made to become beta crystal, greatly improves polypropylene
The toughness of composite material, and there is very high tensile strength and bending strength.
Preferably, the concentration of calcium acetate aqueous solution described in S02. is 0.1 ~ 0.2 mol/L；S02. the immersion described in
Time is 4h.
Preferably, soaking time described in S03. is 2h,
Preferably, bacteria cellulose film BCb described in S04. handles 4h under 900 DEG C of oxygen free conditions.
Preferably, the concentration of the ethanol solution of pimelic acid described in S05. is 0.08 ~ 0.4 g/L；S05. the leaching described in
The bubble time is 2h.
The preparation method of above-mentioned β type polypropylene conductive composite material, which is characterized in that comprise the following steps:
S11. modified carbonization bacteria cellulose nano material is dissolved in dehydrated alcohol, carbonization bacteria cellulose must be modified and received
Rice material solution, it is spare；
S12. homopolypropylene is put into the machine of mixing, the solution configured in S11. is then added, stirs evenly, to anhydrous second
After alcohol volatilization, raw material is obtained；
S13. raw material S12. being prepared carries out extrusion pelletizing by melting extrusion means, obtains β type polypropylene and leads
Composite.
The utility model has the advantages that (1) β type polypropylene conductive composite material of the present invention has used one kind using bacteria cellulose as raw material system
Standby novel conductive filler, the conductive filler is at low cost, overcomes and uses graphite in prior art preparation conducing composite material
The shortcomings that conductive filler of the valuableness such as alkene microplate, carbon nanotube, substantially reduce the preparation cost of conducing composite material；(2) this hair
The bright β type polypropylene conductive composite material of the present invention, modified carbonization bacteria cellulose nano material therein can form height
The conductive network of effect, greatly improves electrical efficiency；(3) since load has in the modified carbonization bacteria cellulose nano material of the present invention
β is nucleated modifying agent, is prepared on β type polypropylene conductive composite material containing a large amount of β crystal, so that the β type being prepared
The impact strength of polypropylene conductive composite material greatly enhances, and also overcomes polypropylene material impact strength in the prior art
Weak disadvantage；(4) the β type polypropylene conductive composite material described in, with the increase of modified carbonization bacteria cellulose nano material,
Its impact strength, tensile strength and bending strength all increase, overcome in the prior art conducing composite material with conductive filler
Addition and the technology prejudice that reduces material impact intensity, tensile strength and bending strength.
Specific embodiment
The present invention is explained further below in conjunction with specific embodiment, but embodiment does not do any type of limit to the present invention
It is fixed.
Bacteria cellulose used in the following embodiment and homopolypropylene is commercially available obtains；It is used
The molecular weight of homopolypropylene is 10W.
Embodiment 1
The preparation of modified carbonization bacteria cellulose nano material:
S1. bacteria cellulose (BC) is placed in distilled water and is impregnated, then by squeezing, obtain bacteria cellulose film (BC
Film)；
S2. bacteria cellulose film (BC film) is put into the calcium acetate aqueous solution of 0.13 mol/L and impregnates 4h, be absorbed
The bacteria cellulose film BCa of calcium acetate solution；
S3. bacteria cellulose film BCa is placed in dehydrated alcohol and impregnates 2h, until calcium acetate precipitation is adsorbed on bacteria cellulose
The surface of film BCa obtains bacteria cellulose film BCb；
S4. bacteria cellulose film BCb is handled into 4h under 900 DEG C of oxygen free conditions, obtains CBCb compound；
S5. CBCb compound is placed in the ethanol solution that concentration is 0.4 g/L pimelic acid and impregnates 2h, heating volatilization second
Alcohol must be modified carbonization bacteria cellulose nano material.
The preparation of β type polypropylene conductive composite material:
The modified carbonization bacteria cellulose nano material of above-mentioned 10g is added in suitable dehydrated alcohol, by stirring, is obtained
The ethanol solution evenly dispersed to modified carbonization bacteria cellulose nano material, it is spare；990g powder homopolypropylene is put again
Enter and modified carbonization bacteria cellulose nano material ethanol solution is then added in high-speed mixer, then starts blender, by two
Person stirs evenly, and the modified carbonization bacteria cellulose nano material being scattered in ethyl alcohol is adhered to the surface of homopolypropylene, to
After ethyl alcohol volatilization, uniformly mixed raw material is obtained；Last raw material carries out extrusion pelletizing by melting extrusion means, obtains β type
Polypropylene conductive composite material.
Embodiment 2
The preparation of β type polypropylene conductive composite material:
Modified carbonization bacteria cellulose nano material (being prepared referring to embodiment 1) of above-mentioned 20g is added into suitable
In dehydrated alcohol, by stirring, the evenly dispersed ethanol solution of modified carbonization bacteria cellulose nano material is obtained, it is spare；Again
It is molten that 980g powder homopolypropylene is put into high-speed mixer the modified carbonization bacteria cellulose nano material ethyl alcohol of then addition
Then liquid starts blender, the two is stirred evenly, the modified carbonization bacteria cellulose nano material adherency being scattered in ethyl alcohol
Uniformly mixed raw material is obtained after ethyl alcohol volatilization on the surface of homopolypropylene；Last raw material passes through melting extrusion means
Extrusion pelletizing is carried out, β type polypropylene conductive composite material is obtained.
Embodiment 3
The preparation of β type polypropylene conductive composite material:
Modified carbonization bacteria cellulose nano material (being prepared referring to embodiment 1) of above-mentioned 30g is added into suitable
In dehydrated alcohol, by stirring, the evenly dispersed ethanol solution of modified carbonization bacteria cellulose nano material is obtained, it is spare；Again
It is molten that 970g powder homopolypropylene is put into high-speed mixer the modified carbonization bacteria cellulose nano material ethyl alcohol of then addition
Then liquid starts blender, the two is stirred evenly, the modified carbonization bacteria cellulose nano material adherency being scattered in ethyl alcohol
Uniformly mixed raw material is obtained after ethyl alcohol volatilization on the surface of homopolypropylene；Last raw material passes through melting extrusion means
Extrusion pelletizing is carried out, β type polypropylene conductive composite material is obtained.
Embodiment 4
The preparation of β type polypropylene conductive composite material:
Modified carbonization bacteria cellulose nano material (being prepared referring to embodiment 1) of above-mentioned 50g is added into suitable
In dehydrated alcohol, by stirring, the evenly dispersed ethanol solution of modified carbonization bacteria cellulose nano material is obtained, it is spare；Again
It is molten that 950g powder homopolypropylene is put into high-speed mixer the modified carbonization bacteria cellulose nano material ethyl alcohol of then addition
Then liquid starts blender, the two is stirred evenly, the modified carbonization bacteria cellulose nano material adherency being scattered in ethyl alcohol
Uniformly mixed raw material is obtained after ethyl alcohol volatilization on the surface of homopolypropylene；Last raw material passes through melting extrusion means
Extrusion pelletizing is carried out, β type polypropylene conductive composite material is obtained.
Embodiment 5
The preparation of β type polypropylene conductive composite material:
Modified carbonization bacteria cellulose nano material (being prepared referring to embodiment 1) of above-mentioned 100g is added into suitable
In dehydrated alcohol, by stirring, the evenly dispersed ethanol solution of modified carbonization bacteria cellulose nano material is obtained, it is spare；Again
It is molten that 900g powder homopolypropylene is put into high-speed mixer the modified carbonization bacteria cellulose nano material ethyl alcohol of then addition
Then liquid starts blender, the two is stirred evenly, the modified carbonization bacteria cellulose nano material adherency being scattered in ethyl alcohol
Uniformly mixed raw material is obtained after ethyl alcohol volatilization on the surface of homopolypropylene；Last raw material passes through melting extrusion means
Extrusion pelletizing is carried out, β type polypropylene conductive composite material is obtained.
Embodiment 6
It stretched, be bent and the test of impact property according to ASTM standard method.Method is as follows: for each difference
In the composite material of kind, 5 samples is taken to carry out different Mechanics Performance Testings.Tensile strength presses ASTMD-638 standard testing,
Tensile speed is 50mm min-1, test temperature is 23 DEG C；Bending property presses ASTMD-790 standard testing, test rate 2mm
min-1, test temperature is 23 DEG C；Izod notched impact is tested by ASTMD-256, and test temperature is 23 DEG C, pendulum energy grade
For 5.5J.
The test method of volume resistivity: using EST121 type number ultra-high resistance, micro current instrument, according to GB/
T1410-2006 test, sample diameter 82mm, thick 2mm, each sample survey five groups, take its average value.
The modified carbonization bacterial fibers that the present invention is prepared are added in homopolypropylene it can be seen from the data of table 1
The β type polypropylene conductive composite material obtained after element is nano-material modified has very excellent electric conductivity, illustrates the present invention
Modified carbonization bacteria cellulose nano material is added in polypropylene can form efficient conductive network in polypropylene, significantly
Improve electrical efficiency.And as the increase volume resistivity of modified carbonization bacteria cellulose declines highly significant, when β type polypropylene
When the content of modified carbonization bacteria cellulose reaches 5% and 10% in conducing composite material, volume resistivity is respectively 1.0*10^
3 and 5*10^2, electric conductivity are very good.
In addition, being prepared in the modified carbonization bacteria cellulose nano material of the present invention since load has β to be nucleated modifying agent
Contain a large amount of β crystal on β type polypropylene conductive composite material, so that the β type polypropylene conductive composite material being prepared
Impact strength greatly enhances, and also overcomes the disadvantage that polypropylene material impact strength is weak in the prior art.It also has good
Good tensile strength and bending strength is suitable with homopolypropylene.With the increase of modified carbonization bacteria cellulose nano material,
Impact strength, tensile strength and the bending strength of β type polypropylene conductive composite material all increase, and overcome conductive in the prior art
The technology prejudice that composite material reduces material impact intensity, tensile strength and bending strength with the addition of conductive filler.
β type polypropylene conductive composite material of the present invention, the modified carbonization bacteria cellulose nano material used is as leading
Electric filler, production cost is low, overcomes conductive filler expensive using graphene microchip, carbon nanotube etc. in the prior art.It can
To substantially reduce the preparation cost of conducing composite material.
Claims (7)
1. a kind of β type polypropylene conductive composite material, which is characterized in that
Containing weight percent be 1~10% modified carbonization bacteria cellulose nano material and weight percent be 90~99%
Homopolypropylene；
The modified carbonization bacteria cellulose nano material is prepared via a method which to obtain:
S01. bacteria cellulose is placed in distilled water and is impregnated, then by squeezing, obtain bacteria cellulose film；
S02. bacteria cellulose film is put into 1~5h of immersion in calcium acetate aqueous solution, the bacterium for the calcium acetate solution that is absorbed is fine
Tie up plain film BCa；The concentration of the calcium acetate aqueous solution is 0.1~0.2mol/L；
S03. bacteria cellulose film BCa is placed in 1~3h of immersion in dehydrated alcohol, until calcium acetate precipitation is adsorbed on bacteria cellulose
The surface of film BCa obtains bacteria cellulose film BCb；
S04., bacteria cellulose film BCb is handled to 1~5h under 800~1000 DEG C of oxygen free conditions, obtains CBCb compound；
S05. CBCb compound is placed in 1~3h of immersion in the ethanol solution of pimelic acid, it is thin must to be modified carbonization for heating volatilization ethyl alcohol
Fungin nano material.
2. β type polypropylene conductive composite material according to claim 1, which is characterized in that containing weight percent be 1~
The homopolypropylene that 5% modified carbonization bacteria cellulose nano material and weight percent is 95~99%.
3. β type polypropylene conductive composite material according to claim 1, which is characterized in that when immersion described in S02.
Between be 4h.
4. β type polypropylene conductive composite material according to claim 1, which is characterized in that soaking time described in S03.
For 2h.
5. β type polypropylene conductive composite material according to claim 1, which is characterized in that bacterial fibers described in S04.
Plain film BCb handles 4h under 900 DEG C of oxygen free conditions.
6. β type polypropylene conductive composite material according to claim 1, which is characterized in that pimelic acid described in S05.
The concentration of ethanol solution is 0.08~0.4g/L；S05. the soaking time described in is 2h.
7. the preparation method of the described in any item β type polypropylene conductive composite materials of claim 1~6, which is characterized in that include
Following steps:
S11. modified carbonization bacteria cellulose nano material is dissolved in dehydrated alcohol, carbonization bacteria cellulose nanometer material must be modified
Expect solution, it is spare；
S12. homopolypropylene is put into the machine of mixing, the solution configured in S11. is then added, stirs evenly, is waved to dehydrated alcohol
After hair, raw material is obtained；
S13. raw material S12. being prepared carries out extrusion pelletizing by melting extrusion means, and it is multiple to obtain β type polypropylene conductive
Condensation material.
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| CN201510242088.2A CN104877232B (en) | 2015-05-13 | 2015-05-13 | A kind of β type polypropylene conductive composite material and preparation method |
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| CN104877232B true CN104877232B (en) | 2019-05-14 |
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| GB0616290D0 (en) * | 2006-08-16 | 2006-09-27 | Imp Innovations Ltd | Material |
| CN104532407B (en) * | 2014-12-24 | 2016-07-20 | 暨南大学 | A kind of carbon nano-fiber based on carbonization Bacterial cellulose and compositions thereof and application |
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