CN113773583A - Graphene modified composite material and preparation method thereof - Google Patents

Graphene modified composite material and preparation method thereof Download PDF

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CN113773583A
CN113773583A CN202111041642.2A CN202111041642A CN113773583A CN 113773583 A CN113773583 A CN 113773583A CN 202111041642 A CN202111041642 A CN 202111041642A CN 113773583 A CN113773583 A CN 113773583A
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graphene
composite material
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李娟�
胡志坚
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Shenzhen Huasheng Super Material System Engineering Co ltd
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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
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • 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
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
    • 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
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • 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
    • C08K5/16—Nitrogen-containing compounds
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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
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds

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Abstract

The invention relates to the technical field of graphene, and discloses a graphene modified composite material which comprises the following components in parts by weight: 2-2.5 parts of modified graphene, 60-65 parts of co-polypropylene resin, 35-40 parts of dimethylformamide, 10-12 parts of phthalic acid ester, 2-3 parts of alkyl diethanolamide, 1-2 parts of diethylenetriamine and 1-2 parts of stearate. The modified graphene/ABS alloy material disclosed by the invention consists of modified graphene, co-polypropylene resin, dimethylformamide, phthalate, alkyl diethanolamide, diethylenetriamine and stearate, has higher tensile strength, tensile modulus, breaking strength and impact strength, further has higher bearing capacity and elastic deformation stress, is not easy to damage under the action of external force impact, has stronger bending deformation resistance within an elastic limit, and has the characteristics of higher abrasion resistance, good relaxation resistance and smaller deformation.

Description

Graphene modified composite material and preparation method thereof
Technical Field
The invention relates to the technical field of graphene, in particular to a graphene modified composite material and a preparation method thereof.
Background
Graphene is the thinnest and highest-strength material in the natural world at present, the breaking strength of the graphene is 200 times higher than that of the best steel, and meanwhile the graphene has good elasticity, and the stretching amplitude can reach 20% of the size of the graphene. However, graphene is difficult to be used as a single raw material to produce a certain product, and is mainly compounded with other material systems by utilizing the outstanding characteristics of graphene, so that a novel composite material with excellent performance is obtained.
Chinese patent discloses a graphene modified composite material and a preparation method thereof (publication No. CN113150490A), the graphene modified composite material prepared by the patent technology has good dimensional stability, toughness and antibacterial property, but the bearing capacity and elastic deformation stress are not good, and the phenomenon of damage is easy to occur under the action of external force impact.
Disclosure of Invention
The invention aims to provide a graphene modified composite material and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the graphene modified composite material comprises the following components in parts by weight: 2-2.5 parts of modified graphene, 60-65 parts of co-polypropylene resin, 35-40 parts of dimethylformamide, 10-12 parts of phthalic acid ester, 2-3 parts of alkyl diethanolamide, 1-2 parts of diethylenetriamine and 1-2 parts of stearate.
The preparation method of the graphene modified composite material comprises the following steps:
s1, adding 2-2.5 parts of modified graphene into 35-40 parts of dimethylformamide solvent, and dispersing at high speed for 1 hour to completely dissolve the graphene in the dimethylformamide;
s2, adding 60-65 parts of co-polypropylene resin and 10-12 parts of phthalic acid ester, continuously dispersing at a high speed, heating at 60-65 ℃ for 2 hours, then heating to 85-90 ℃, and continuously ultrasonically stirring for 2 hours;
and S2, sequentially adding 2-3 parts of alkyl diethanolamide, 1-2 parts of diethylenetriamine and 1-2 parts of stearate, performing vacuum degassing, placing the mixture into a mold, curing at the temperature of 60 +/-2 ℃ for more than 3 hours, demolding, and cutting to obtain the graphene modified composite material.
As a still further scheme of the invention: the modified graphene comprises the following components in parts by weight: 25-30 parts of graphite powder, 500-550 parts of concentrated sulfuric acid, 10-12 parts of sodium nitrate, 60-65 parts of potassium permanganate, 120-130 parts of hydrogen peroxide and 0.5-0.8 part of silane coupling agent.
As a still further scheme of the invention: the preparation method of the modified graphene comprises the following steps:
s11, placing the reaction kettle in ice water mixed liquid, adding 500-550 parts of 98% concentrated sulfuric acid, adding 25-30 parts of graphite powder, and stirring;
s12, after the graphite powder and concentrated sulfuric acid are fully mixed, adding 10-12 parts of sodium nitrate and 60-65 parts of potassium permanganate, and fully reacting;
s13, heating to 95-100 ℃, continuously adding distilled water, reacting for 1 hour, adding 120-130 parts of hydrogen peroxide, and uniformly mixing to obtain a mixed solution;
s14, filtering the mixed solution obtained in the step S13 to obtain a filter cake, washing the filter cake with hydrochloric acid until no sulfate ions exist in the filter cake, adjusting the pH value of the solution to 4.5-5, adding 0.5-0.8 part of silane coupling agent, uniformly stirring, heating, filtering and drying to obtain the modified graphene.
As a still further scheme of the invention: the reaction conditions in the step S12 are as follows: the temperature is controlled to be 3-4 ℃, the reaction is carried out for 2 hours, then the temperature is increased to 33-38 ℃, and the reaction is carried out for 30 min.
As a still further scheme of the invention: the heating, filtering and drying conditions in the step S14 are as follows: heating at 60-65 ℃ for 2h, washing with acetone to remove unreacted silane coupling agent, filtering, washing with ethanol to neutrality, and drying.
As a still further scheme of the invention: the stearate can be one or more of calcium stearate, zinc stearate and barium stearate.
Compared with the prior art, the invention has the beneficial effects that:
the modified graphene/ABS alloy material disclosed by the invention consists of modified graphene, co-polypropylene resin, dimethylformamide, phthalate, alkyl diethanolamide, diethylenetriamine and stearate, has higher tensile strength, tensile modulus, breaking strength and impact strength, further has higher bearing capacity and elastic deformation stress, is not easy to damage under the action of external force impact, has stronger bending deformation resistance within an elastic limit, and has the characteristics of higher abrasion resistance, good relaxation resistance and smaller deformation.
Detailed Description
In the embodiment of the invention, the graphene modified composite material comprises the following components in parts by weight: 2-2.5 parts of modified graphene, 60-65 parts of co-polypropylene resin, 35-40 parts of dimethylformamide, 10-12 parts of phthalic acid ester, 2-3 parts of alkyl diethanolamide, 1-2 parts of diethylenetriamine and 1-2 parts of stearate.
The preparation method of the graphene modified composite material comprises the following steps:
s1, adding 2-2.5 parts of modified graphene into 35-40 parts of dimethylformamide solvent, and dispersing at high speed for 1 hour to completely dissolve the graphene in the dimethylformamide;
s2, adding 60-65 parts of co-polypropylene resin and 10-12 parts of phthalic acid ester, continuously dispersing at a high speed, heating at 60-65 ℃ for 2 hours, then heating to 85-90 ℃, and continuously ultrasonically stirring for 2 hours;
and S2, sequentially adding 2-3 parts of alkyl diethanolamide, 1-2 parts of diethylenetriamine and 1-2 parts of stearate, performing vacuum degassing, placing the mixture into a mold, curing at the temperature of 60 +/-2 ℃ for more than 3 hours, demolding, and cutting to obtain the graphene modified composite material.
Preferably, the modified graphene comprises the following components in parts by weight: 25-30 parts of graphite powder, 500-550 parts of concentrated sulfuric acid, 10-12 parts of sodium nitrate, 60-65 parts of potassium permanganate, 120-130 parts of hydrogen peroxide and 0.5-0.8 part of silane coupling agent.
Preferably, the preparation method of the modified graphene comprises the following steps:
s11, placing the reaction kettle in ice water mixed liquid, adding 500-550 parts of 98% concentrated sulfuric acid, adding 25-30 parts of graphite powder, and stirring;
s12, after the graphite powder and concentrated sulfuric acid are fully mixed, adding 10-12 parts of sodium nitrate and 60-65 parts of potassium permanganate, and fully reacting;
s13, heating to 95-100 ℃, continuously adding distilled water, reacting for 1 hour, adding 120-130 parts of hydrogen peroxide, and uniformly mixing to obtain a mixed solution;
s14, filtering the mixed solution obtained in the step S13 to obtain a filter cake, washing the filter cake with hydrochloric acid until no sulfate ions exist in the filter cake, adjusting the pH value of the solution to 4.5-5, adding 0.5-0.8 part of silane coupling agent, uniformly stirring, heating, filtering and drying to obtain the modified graphene.
Preferably, the reaction conditions in the step S12 are as follows: the temperature is controlled to be 3-4 ℃, the reaction is carried out for 2 hours, then the temperature is increased to 33-38 ℃, and the reaction is carried out for 30 min.
Preferably, the conditions of heating, filtering and drying in the step S14 are as follows: heating at 60-65 ℃ for 2h, washing with acetone to remove unreacted silane coupling agent, filtering, washing with ethanol to neutrality, and drying.
Preferably, the stearate can be one or more of calcium stearate, zinc stearate and barium stearate.
To better illustrate the technical effect of the present invention, it is illustrated by the following tests:
selecting the graphene modified composite material prepared by the invention as an embodiment;
selecting a graphene modified composite material (publication number: CN108864541A, day: 2018-11-23) prepared from a graphene modified composite material disclosed by Chinese patent as a first comparative example;
selecting a graphene modified composite material disclosed in Chinese patent and a preparation method thereof (publication number: CN113150490A, Japanese 2021-07-23) as a second comparative example;
the graphene-modified composite materials of examples, comparative examples one and comparative examples two were processed to 200 × 10 × 2mm, respectively3The strip-shaped structure of (1);
the strip-shaped structures of the first embodiment, the first comparative example and the second comparative example are respectively subjected to a tensile property test, an impact property test, a bending property test and a friction and wear property test.
The impact strengths (unit: KJ/m) of the graphene-modified composite materials of examples, comparative examples I and comparative examples II were obtained by an impact property test2) (ii) a The bending strength (unit: MPa) and the bending modulus (unit: GPa) of the graphene modified composite materials of the examples, the comparative examples I and the comparative examples II are obtained through a bending performance test; the breaking strength (unit: kN), tensile strength (unit: MPa) and tensile modulus (unit: GPa) of the graphene-modified composite materials of examples, comparative examples first and second were obtained by tensile property test tests, and the results were recorded in table 1 below.
Table 1: table for strength property analysis of examples, comparative examples first and second
Figure BDA0003249517340000051
The analysis of table 1 can result in:
the results of the tensile property test show that: the tensile strength and the tensile modulus in the embodiment are both obviously greater than those in the first comparative example and the second comparative example, so that the graphene modified composite material prepared by the invention has higher tensile strength and tensile modulus, and further has higher bearing capacity and elastic deformation stress;
through the impact performance test, the following results can be obtained: the fracture strength and the impact strength in the embodiment are obviously higher than those in the first comparative example and the second comparative example, so that the graphene modified composite material prepared by the invention has higher fracture strength and impact strength, and further has better impact toughness, and is not easy to damage under the action of external force impact;
the bending performance test proves that: the bending strength and the bending modulus in the embodiment are both obviously higher than those in the comparative example I and the comparative example II, so that the graphene modified composite material prepared by the invention has higher bending strength and bending modulus, and further has stronger external force resistance and stronger bending deformation resistance within the elastic limit.
Secondly, the friction wear performance test, the creep performance test, the stress relaxation test and the dynamic mechanical analysis test are respectively carried out on the long strip structures of the embodiment, the comparative example I and the comparative example II
Wherein, the friction and wear performance test detects the surface wear amount after 5min at the rotating speed of 480r/min and the pressure of 0.98 MPa; the creep performance test and the stress relaxation test are carried out under the conditions that the strain is 0.5 percent, the temperature is 150 ℃, the time is 2 hours, and the single cantilever mode is adopted; the dynamic mechanical analysis is carried out at a heating rate of 3K/min in an air atmosphere in a single cantilever mode.
The abrasion loss (unit: g) of the graphene modified composite materials of the examples, the comparative example I and the comparative example II is obtained through a frictional abrasion performance test; equilibrium values (unit: MPa) of relaxation moduli of the graphene-modified composite materials of examples, comparative examples one and comparative examples two were obtained by a stress relaxation test; the deformation rates (unit:%) of the graphene modified composite materials of the examples, the comparative example I and the comparative example II are obtained through a creep property test; the storage modulus change rates (unit: MPa/. degree. C.) of the graphene modified composite materials of examples, comparative examples I and comparative examples II were obtained by a dynamic mechanical analysis test
Table 2: deformation performance analysis tables of examples, comparative examples first and comparative examples second
Figure BDA0003249517340000061
The analysis of table 2 can result in: the results of the friction and wear performance test tests show that: the abrasion loss in the embodiment is obviously smaller than that in the comparative example I and the comparative example II, so that the graphene modified composite material prepared by the method has higher abrasion resistance;
the stress relaxation test and the creep performance test show that: the balance value and the deformation rate of the relaxation modulus in the embodiment are both obviously smaller than those of the first comparative example and the second comparative example, so that the graphene modified composite material prepared by the method has the characteristics of good relaxation resistance and small deformation;
the results of the dynamic mechanical analysis test show that: the change rate of the storage modulus in the embodiment is obviously smaller than that of the storage modulus in the comparative example I and the comparative example II, so that the graphene modified composite material prepared by the method has smaller rebound change rate.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.

Claims (7)

1. The graphene modified composite material is characterized by comprising the following components in parts by weight: 2-2.5 parts of modified graphene, 60-65 parts of co-polypropylene resin, 35-40 parts of dimethylformamide, 10-12 parts of phthalic acid ester, 2-3 parts of alkyl diethanolamide, 1-2 parts of diethylenetriamine and 1-2 parts of stearate.
2. The preparation method for realizing the graphene modified composite material of claim 1 is characterized by comprising the following steps:
s1, adding 2-2.5 parts of modified graphene into 35-40 parts of dimethylformamide solvent, and dispersing at high speed for 1 hour to completely dissolve the graphene in the dimethylformamide;
s2, adding 60-65 parts of co-polypropylene resin and 10-12 parts of phthalic acid ester, continuously dispersing at a high speed, heating at 60-65 ℃ for 2 hours, then heating to 85-90 ℃, and continuously ultrasonically stirring for 2 hours;
and S2, sequentially adding 2-3 parts of alkyl diethanolamide, 1-2 parts of diethylenetriamine and 1-2 parts of stearate, performing vacuum degassing, placing the mixture into a mold, curing at the temperature of 60 +/-2 ℃ for more than 3 hours, demolding, and cutting to obtain the graphene modified composite material.
3. The graphene-modified composite material according to claim 1, wherein the modified graphene comprises the following components in parts by weight: 25-30 parts of graphite powder, 500-550 parts of concentrated sulfuric acid, 10-12 parts of sodium nitrate, 60-65 parts of potassium permanganate, 120-130 parts of hydrogen peroxide and 0.5-0.8 part of silane coupling agent.
4. The graphene-modified composite material according to claim 3, wherein the preparation method of the modified graphene comprises the following steps:
s11, placing the reaction kettle in ice water mixed liquid, adding 500-550 parts of 98% concentrated sulfuric acid, adding 25-30 parts of graphite powder, and stirring;
s12, after the graphite powder and concentrated sulfuric acid are fully mixed, adding 10-12 parts of sodium nitrate and 60-65 parts of potassium permanganate, and fully reacting;
s13, heating to 95-100 ℃, continuously adding distilled water, reacting for 1 hour, adding 120-130 parts of hydrogen peroxide, and uniformly mixing to obtain a mixed solution;
s14, filtering the mixed solution obtained in the step S13 to obtain a filter cake, washing the filter cake with hydrochloric acid until no sulfate ions exist in the filter cake, adjusting the pH value of the solution to 4.5-5, adding 0.5-0.8 part of silane coupling agent, uniformly stirring, heating, filtering and drying to obtain the modified graphene.
5. The graphene-modified composite material according to claim 4, wherein the reaction conditions in the S12 step are as follows: the temperature is controlled to be 3-4 ℃, the reaction is carried out for 2 hours, then the temperature is increased to 33-38 ℃, and the reaction is carried out for 30 min.
6. The graphene-modified composite material according to claim 4, wherein the heating, filtering and drying conditions in the S14 step are as follows: heating at 60-65 ℃ for 2h, washing with acetone to remove unreacted silane coupling agent, filtering, washing with ethanol to neutrality, and drying.
7. The graphene-modified composite material according to claim 1, wherein the stearate is one or more selected from calcium stearate, zinc stearate, and barium stearate.
CN202111041642.2A 2021-09-07 2021-09-07 Graphene modified composite material and preparation method thereof Withdrawn CN113773583A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11767416B1 (en) * 2022-04-07 2023-09-26 Zhongshan Huayang Plastic Dyestuffs Co., Ltd. Graphene composite plastic and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11767416B1 (en) * 2022-04-07 2023-09-26 Zhongshan Huayang Plastic Dyestuffs Co., Ltd. Graphene composite plastic and preparation method thereof

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