CN104893102A - Polypropylene resin-based nano composite material and preparation method thereof - Google Patents
Polypropylene resin-based nano composite material and preparation method thereof Download PDFInfo
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention relates to a polypropylene resin material and a preparation method thereof, and specifically relates to a polypropylene resin-based nano composite material and a preparation method thereof. The nano composite material is prepared from a graphene oxide-silicon dioxide hybrid material serving as a filler and polypropylene resin serving as a matrix, wherein the graphene oxide is obtained from natural graphite powder by oxidation with a strong oxidant and powerful ultrasonic dispersion; and in the process of preparing the graphene oxide by oxidizing the natural graphite powder, a large amount of polar oxygen-containing functional groups are introduced to the surface of the graphene oxide, and diphenyl methane diisocyanate acting as a middle bridge effectively links the graphene oxide with silicon dioxide to form the hybrid material. According to the polypropylene resin-based nano composite material and the preparation method thereof, the preparation process is simple, the net content of the filler in the product can be controlled to 0.25-2%, and the obtained composite material has relatively high mechanical property and thermal property.
Description
Technical field
The present invention relates to polyacrylic resin material and preparation method thereof, be specially acrylic resin based nano composite material and preparation method thereof.
Background technology
Polypropylene (PP) is a kind of widely used thermoplastic resin, its have cheap, be easy to the premium propertiess such as machine-shaping.But the low-temperature impact toughness of PP is poor, heat-resistant stability is not enough and shaping time shrinking percentage comparatively large, which has limited the application of PP in some field.In order to widen the Application Areas of PP, improve the added value of PP, the main direction of studying that modification is current PP is implemented to it.Wherein, melt blending possesses skills simply, is suitable for large-scale industrial production and becomes the major technique mode of PP modification.But traditional filler and the consistency of PP is poor, interface bond strength is low, causes the dispersing uniformity of filler poor, need to improve addition and could obtain the good matrix material of performance.Current, Graphene and derivative thereof and PP compound can be given full play to the excellent mechanics of Graphene, calorifics, electricity and other functional performances, for preparation high-performance PP based nano composite material provides new thinking.But because the nanometer size effect of Graphene and derivative thereof and high specific surface energy cause it very easily to reunite in PP matrix, not only can not give full play to the excellent properties of Graphene, also can reduce the performance of matrix resin.Therefore, explore and improve the dispersion of Graphene in PP matrix, the interface cohesion improving itself and PP has important engineering significance.
Summary of the invention
For above-mentioned technical problem, the object of the present invention is to provide a kind of polymer based nanocomposites with excellent mechanical property and resistance toheat, while improving nano composite material performance, widening its range of application, reduce the production cost of matrix material.
In order to achieve the above object, technical scheme of the present invention is:
Acrylic resin based nano composite material, with graphene oxide-silicon dioxide hybrid materials be filler, acrylic resin makes for matrix, according to parts by weight, filler 0.25 ~ 2 part, matrix 99.75 ~ 98 parts;
After graphene oxide-silicon dioxide hybrid materials mixes with acrylic resin particle, on mixing roll, melt blending prepares acrylic resin based nano composite material; Melt blending temperature is 200 ~ 230 DEG C, and the blended time is 5 ~ 20min, and the rotating speed of rotor is 10 ~ 50r/min.
Wherein, graphene oxide-silicon dioxide hybrid materials, is obtained by following methods:
(1) silicon-dioxide is in 105 DEG C of dry 12h;
(2) graphene oxide is scattered in solvent dimethylformamide, obtains finely dispersed graphene oxide solution through ultrasonic; Every 2g graphene oxide 100mL solvent dimethylformamide;
(3) silicon-dioxide, diphenylmethanediisocyanate join in graphene oxide solution, and the total amount ratio of silicon-dioxide, diphenylmethanediisocyanate, graphene oxide is 1: 2: 1; At room temperature ultrasonic disperse 1h;
(4) react 24h at said mixture 80 DEG C, after filtration and remove unnecessary diphenylmethanediisocyanate with dimethyl formamide washing leaching cake, filter cake after drying, grinding, mistake 200 mesh sieves, after obtain graphene oxide-silicon dioxide hybrid materials.
Wherein, graphene oxide, is obtained by following methods:
(1) in the beaker of drying, add the vitriol oil, be cooled to 0 ~ 4 DEG C with ice-water bath, under high degree of agitation, add natural graphite powder and NaNO
3mixture.Natural graphite powder and NaNO
3mass ratio be 2: 1;
(2) and then slowly KMnO is added
4, natural graphite powder and KMnO
4mass ratio be 1: 3, temperature controls between 0 ~ 20 DEG C, and after stirring reaction 5min, temperature rises to 35 ± 3 DEG C, and constant temperature stirs after 30min, and heating temperatures 98 ± 2 DEG C, adds 150mL under vigorous stirring
goionized water, every gram of natural graphite powder adds deionization 30mL, keeps 15min;
(4) add deionized water again and carry out pyrohydrolysis, every gram of natural graphite powder adds deionized water 60mL, then adds H
2o
2neutralize unreacted strong oxidizer, every gram of natural graphite powder adds H
2o
260mL, while hot suction filtration be that 5% hydrochloric acid and deionized water fully wash by mass concentration, in 90 DEG C of vacuum drying ovens, dry 24h, obtains graphite oxide;
(5) graphite oxide obtains graphene oxide through powerful supersound process again.
Acrylic resin based nano composite material provided by the invention and preparation method thereof, the filler adopted is graphene oxide-silicon dioxide hybrid materials, graphene oxide is obtained through strong oxidizer oxidation and powerful ultrasonic disperse by natural graphite powder, prepare in the process of graphene oxide in natural graphite powder oxidation, a large amount of polarity oxygen-containing functional groups is introduced, as hydroxyl, carboxyl and epoxy group(ing) etc. on the surface of graphene oxide, simultaneously, silica sphere is also containing great amount of hydroxy group, these oxy radicals can with diphenylmethanediisocyanate generation chemical reaction or hydrogen bond action, diphenylmethanediisocyanate serves as middle bridge and effectively gets up to form hybrid material by graphene oxide and silicon-dioxide link, because graphene oxide is two-dimentional sheet layer material, and silicon-dioxide is zero dimension particulate material, can intercept each other after the two hydridization, utilize graphene oxide-silicon dioxide hybrid materials as the properties-correcting agent of polymkeric substance, give full play to the mutual blocking effect of graphene oxide-silicon dioxide hybrid materials to suppress reunion each other, and significantly collaborative activeness and quietness effect is produced to PP matrix, thus promote its dispersiveness in the base.
Acrylic resin based nano composite material provided by the invention and preparation method thereof, preparation process is simple, and in product, the net content of filler can be controlled in 0.25 ~ 2%, and the matrix material of acquisition has higher mechanical property and thermal characteristics.
Accompanying drawing explanation
Fig. 1 heterogeneity acrylic resin based nano composite material tensile strength test results;
Fig. 2 heterogeneity acrylic resin based nano composite material Young's modulus test result;
Fig. 3 heterogeneity acrylic resin based nano composite material shock strength test result;
Fig. 4 acrylic resin based nano composite material DSC temperature lowering curve;
Fig. 5 acrylic resin based nano composite material DSC heating curve;
Fig. 6 acrylic resin based nano composite material and SiO
2infrared spectrogram;
The X-ray diffracting spectrum of Fig. 7 graphene oxide-silicon dioxide hybrid materials;
The X-ray diffracting spectrum of the acrylic resin based nano composite material of the different filler content of Fig. 8;
Fig. 9 content 0.5wt.%SiO
2acrylic resin based nano composite material stereoscan photograph;
Figure 10 content 0.5wt.% (SiO
2-GO) acrylic resin based nano composite material stereoscan photograph;
Figure 11 content 2wt.%SiO
2acrylic resin based nano composite material stereoscan photograph;
Figure 12 content 2wt.%SiO
2acrylic resin based nano composite material stereoscan photograph;
Figure 13 content 2wt.% (SiO
2-GO) acrylic resin based nano composite material stereoscan photograph;
Figure 14 content 2wt.% (SiO
2-GO) acrylic resin based nano composite material stereoscan photograph.
Embodiment
The invention is further illustrated by the following examples.
For ease of contrast, pure PP and separately employing silicon-dioxide are that the matrix material of filler adopts the melt blending condition preparation identical with the present invention.
Embodiment 1
The preparation of graphite oxide: the vitriol oil adding 115mL98% in the beaker of drying, is cooled to less than 4 DEG C with ice-water bath, adds 5gNGP and 2.5gNaNO under high degree of agitation
3mixture, and then slowly add 15gKMnO
4, and the temperature of reaction system is controlled below 20 DEG C, after continuing stirring reaction 5min, system temperature is risen to 35 ± 3 DEG C, constant temperature adds 230mL deionized water after stirring 30min under vigorous stirring.Above-mentioned system is proceeded to the oil bath pan of heating, system temperature of reaction is at about 98 DEG C, and keep 15min, the deionized water then adding 355mL heat carries out pyrohydrolysis, adds 30mLH
2o
2neutralize unreacted strong oxidizer, suction filtration also fully washs with 5% hydrochloric acid and deionized water while hot, and in 90 DEG C of vacuum drying ovens, dry 24h, obtains graphite oxide.Graphite oxide obtains graphene oxide through powerful supersound process again.
Graphene-silicon dioxide hybrid materials preparation: the moisture that 2g silicon-dioxide dry 12h at 105 DEG C is gone out in its surface adsorption air; 2g graphite oxide is scattered in 100mLDMF solvent simultaneously, obtains finely dispersed graphene oxide solution through brute force is ultrasonic; Subsequently by 2gSiO
2, 4gMDI adds in above-mentioned graphene oxide solution, at room temperature after ultrasonic disperse 1h, again above-mentioned system is reacted 24h at 80 DEG C, system also removes unnecessary MDI with DMF washing leaching cake after filtration, filter cake after drying, grind, obtain Graphene-silicon dioxide hybrid materials after 200 orders that sieve, hybrid material is preserved stand-by in moisture eliminator.
The preparation of acrylic resin based nano composite material: after 0.1g Graphene-silicon dioxide hybrid materials and 39.9gPP being mixed, mixture to be joined in melting mixing machine mixing 15min at 200 DEG C, rotor speed is 50r/min.In acrylic resin based nano composite material, the mass content of filler is 0.25%.
The acrylic resin based nano composite material of gained adopts vulcanizing press compressing tablet.Sample preparation is become dumbbell-shaped specimen, is of a size of 62.5 × 3.25 × 0.7mm
3, do Elongation test, sample preparation become rectangular parallelepiped, be of a size of 10 × 1.5mm
2, do Impact Test.Wherein draw speed is 10mm/min, and shock pendulum is 7.5J.Stretch and Impact Test result as shown in table 1.Can find out, compared with pure PP, adopt the tensile strength of the acrylic resin based nano composite material of Graphene-silicon dioxide hybrid materials gained and shock strength all to improve, improve 3.19% and 22.33% respectively.And be that the matrix material of filler gained is high than adopting separately silicon-dioxide under same amount.
Embodiment 2
Preparation, the Graphene-silicon dioxide hybrid materials of graphite oxide are prepared with embodiment 1.In preparation process, by 0.2g Graphene-silicon dioxide hybrid materials and 39.8gPP through with the melt blending of embodiment 1 identical process after, obtain the acrylic resin based nano composite material that packing quality content is 0.5%.
Acrylic resin based nano composite material test sample preparation and test condition with embodiment 1, stretch and Impact Test result as shown in table 1.Can find out, compared with pure PP, adopt the tensile strength of the acrylic resin based nano composite material of Graphene-silicon dioxide hybrid materials gained and shock strength to improve 15.71% and 27.67% respectively.And be that the matrix material of filler gained is high than adopting separately silicon-dioxide under same amount.
Thermal performance test result is as shown in table 2.Can find out, compared with pure PP, adopt the thermal characteristics of the nano composite material of Graphene-silicon dioxide hybrid materials gained all to improve, peak crystallization and melting peak temperature improve 3 DEG C and 1.5 DEG C respectively.And be that the matrix material of filler gained is high than adopting separately silicon-dioxide under same amount.
Embodiment 3
Preparation, the Graphene-silicon dioxide hybrid materials of graphite oxide are prepared with embodiment 1.In preparation process, by 0.4g Graphene-silicon dioxide hybrid materials and 39.6gPP through with the melt blending of embodiment 1 identical process after, obtain the acrylic resin based nano composite material that packing quality content is 1%.Acrylic resin based nano composite material test sample preparation and test condition with embodiment 1, stretch and Impact Test result as shown in table 1.Can find out, compared with pure PP, adopt the tensile strength of the nano composite material of Graphene-silicon dioxide hybrid materials gained and shock strength to improve 18.59% and 40.33% respectively.And be that the matrix material of filler gained is high than adopting separately silicon-dioxide under same amount.
Embodiment 4
Preparation, the Graphene-silicon dioxide hybrid materials of graphite oxide are prepared with embodiment 1.In preparation process, by 0.8g Graphene-silicon dioxide hybrid materials and 39.2gPP through with the melt blending of embodiment 1 identical process after, obtain the acrylic resin based nano composite material that packing quality content is 2%.Acrylic resin based nano composite material test sample preparation and test condition with embodiment 1, stretch and Impact Test result as shown in table 1.Can find out, compared with pure PP, adopt the tensile strength of the nano composite material of Graphene-silicon dioxide hybrid materials gained and shock strength to improve 21.37% and 51% respectively.And be that the matrix material of filler gained is high than adopting separately silicon-dioxide under same amount.
Thermal performance test result is as shown in table 2.Can find out, compared with pure PP, adopt the thermal characteristics of the acrylic resin based nano composite material of graphene oxide-silicon dioxide hybrid materials gained all to improve, peak crystallization and melting peak temperature improve 5.6 DEG C and 3.8 DEG C respectively.And be that the matrix material of filler gained is high than adopting separately silicon-dioxide under same amount.
The composition of table 1 Polypropylene Nanocomposites and mechanical experimental results
The composition of table 2 Polypropylene Nanocomposites and thermal property
Every test of the acrylic resin based nano composite material in the present invention is as Fig. 1 to Figure 13.
Claims (3)
1. acrylic resin based nano composite material, is characterized in that: with graphene oxide-silicon dioxide hybrid materials be filler, acrylic resin makes for matrix, according to parts by weight, filler 0.25 ~ 2 part, matrix 99.75 ~ 98 parts;
After graphene oxide-silicon dioxide hybrid materials mixes with acrylic resin particle, on mixing roll, melt blending prepares acrylic resin based nano composite material; Melt blending temperature is 200 ~ 230 DEG C, and the blended time is 5 ~ 20min, and the rotating speed of rotor is 10 ~ 50r/min.
2. acrylic resin based nano composite material according to claim 1, is characterized in that: described graphene oxide-silicon dioxide hybrid materials, is obtained by following methods:
(1) silicon-dioxide is in 105 DEG C of dry 12h;
(2) graphene oxide is scattered in solvent dimethylformamide, obtains finely dispersed graphene oxide solution through ultrasonic; Every 2g graphene oxide 100mL solvent dimethylformamide;
(3) silicon-dioxide, diphenylmethanediisocyanate join in graphene oxide solution, and the total amount of silicon-dioxide, diphenylmethanediisocyanate, graphene oxide is than being 1:2:1; At room temperature ultrasonic disperse 1h;
(4) react 24h at said mixture 80 DEG C, after filtration and remove unnecessary diphenylmethanediisocyanate with dimethyl formamide washing leaching cake, filter cake after drying, grinding, mistake 200 mesh sieves, after obtain graphene oxide-silicon dioxide hybrid materials.
3. acrylic resin based nano composite material according to claim 2, is characterized in that: described graphene oxide, is obtained by following methods:
(1) in the beaker of drying, add the vitriol oil, be cooled to 0 ~ 4 DEG C with ice-water bath, under high degree of agitation, add natural graphite powder and NaNO
3mixture.Natural graphite powder and NaNO
3mass ratio be 2:1;
(2) and then slowly KMnO is added
4, natural graphite powder and KMnO
4mass ratio be 1:3, temperature controls between 0 ~ 20 DEG C, after stirring reaction 5min, temperature rises to 35 ± 3 DEG C, after constant temperature stirs 30min, and heating temperatures 98 ± 2 DEG C, add 150mL deionized water under vigorous stirring, every gram of natural graphite powder adds deionization 30mL, keeps 15min;
(4) add deionized water again and carry out pyrohydrolysis, every gram of natural graphite powder adds deionized water 60mL, then adds H
2o
2neutralize unreacted strong oxidizer, every gram of natural graphite powder adds H
2o
260mL, while hot suction filtration be that 5% hydrochloric acid and deionized water fully wash by mass concentration, in 90 DEG C of vacuum drying ovens, dry 24h, obtains graphite oxide;
(5) graphite oxide obtains graphene oxide through powerful supersound process again.
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| CN105585789A (en) * | 2015-12-22 | 2016-05-18 | 西华大学 | Polystyrene-resin-based composite material and preparation method thereof |
| CN105778472A (en) * | 2016-04-19 | 2016-07-20 | 滁州环球聚氨酯科技有限公司 | High strength heat resistant modified polyurethane composite material |
| CN106221179A (en) * | 2016-07-25 | 2016-12-14 | 西华大学 | Graphene silicon dioxide hybrid materials and the method preparing polyurethane-base nano composite material |
| CN109456522A (en) * | 2018-09-26 | 2019-03-12 | 上海敏孑图文设计事务所（有限合伙） | A kind of semirigid plastic row button and its preparation process |
| CN114590002A (en) * | 2022-03-03 | 2022-06-07 | 中塑新材料科技（杭州）有限公司 | High-sealing strong heat-resistant composite film |
| CN115926381A (en) * | 2023-02-01 | 2023-04-07 | 江苏耀鸿电子有限公司 | Silicon dioxide filled epoxy resin copper-clad plate and preparation method thereof |
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| CN114590002A (en) * | 2022-03-03 | 2022-06-07 | 中塑新材料科技（杭州）有限公司 | High-sealing strong heat-resistant composite film |
| CN115926381A (en) * | 2023-02-01 | 2023-04-07 | 江苏耀鸿电子有限公司 | Silicon dioxide filled epoxy resin copper-clad plate and preparation method thereof |
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