CN111925473B - Graphene oxide-based composite material modified resin material with strong mechanical property - Google Patents
Graphene oxide-based composite material modified resin material with strong mechanical property Download PDFInfo
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Abstract
The invention discloses a graphene oxide-based composite material modified resin material with enhanced mechanical properties, which is obtained by in-situ doping of a graphene oxide-based composite material in a suspension polymerization synthesis process, wherein the graphene oxide-based composite material is one or more of graphene oxide and magnesium aluminum hydrotalcite-graphene composite material, the graphene oxide is used as an additive, and the high-dispersion graphene oxide-polyacrylic acid resin is prepared by in-situ suspension polymerization, so that the graphene oxide-polyacrylic acid resin has significantly enhanced mechanical properties, and the sphericity rate after grinding is increased from 43.8% to 91.8% and increased by 109.6%. Furthermore, the magnesium-aluminum hydrotalcite-graphene oxide composite additive is prepared by a coprecipitation method, so that the dispersion of graphene oxide is promoted, the addition amount of the graphene oxide is reduced, and the sphericity rate after grinding is still 88.6%. The graphene oxide-based composite material modified resin material with enhanced mechanical properties provided by the invention can reduce resin damage loss and secondary pollution caused by resin loss in practical application.
Description
Technical Field
The invention relates to the technical field of gelatin, in particular to a graphene oxide-based composite material modified resin material with strong mechanical property.
Background
Polyacrylic resin is a porous polymer resin material which is prepared by taking acrylic substances as monomers (such as methyl acrylate, methyl methacrylate and the like) and carrying out initiation crosslinking with a multifunctional crosslinking agent in the presence of a pore-forming agent, a dispersing agent and the like without functional grouping, and occupies a great proportion in the research and production fields of the current water-absorbent resin. The water-absorbing resin occupies a great proportion in the current research and production fields of water-absorbing resin. At present, a floating polymerization method is generally adopted, and a suspension system phase is divided into an oil phase and a water phase, wherein the oil phase mainly comprises a monomer, an initiator, a cross-linking agent and a pore-making agent, and the water phase mainly comprises water and a dispersing agent.
The polyacrylic resin can be exchanged with polyvalent metal ions, so that the adsorbent for removing heavy metal ions poisoned by industrial wastewater can be effectively removed, the transition metal and noble ion adsorbent can be recovered, the transition metal and noble ions can be recovered, the number of times of recycling is large, and the polyacrylic resin has important industrial application values for heavy metal recovery and water treatment and important industrial application values for treatment.
The polyacrylic resin has the defects of weak mechanical strength, easy breakage in the using process, easy resin loss and secondary pollution, so that the method for improving the mechanical property of the polyacrylic resin is important for industrial application. In recent years, carbon nanomaterials as a modifying additive are incorporated into a polymer matrix to obtain a polymer matrix composite having excellent properties, and based on this, we provide a graphene oxide-based composite modified resin material having strong mechanical properties.
Disclosure of Invention
The invention aims to provide a graphene oxide-based composite material modified resin material with strong mechanical property, which aims to solve the defects that polyacrylic resin in the background art is weak in mechanical strength, easy to break in use and use, easy to break in use, and cause resin loss and secondary pollution, so that a method for improving the mechanical property of the polyacrylic resin is important for industrial application. In recent years, carbon nanomaterials have been incorporated as modifying additives into polymer matrices to obtain polymer-based composites having excellent properties, and for this purpose, we propose a graphene oxide-based composite modified resin material having strong mechanical properties.
In order to achieve the purpose, the invention provides the following technical scheme: the graphene oxide-based composite material modified resin material with strong mechanical property is characterized in that the graphene oxide-based composite material is doped into polypropylene resin in situ to obtain a novel modified resin material with remarkably improved mechanical property, the sphericity rate after grinding is improved from 43.76% to more than 88.62%, wherein the modified material is any one or more of graphene oxide and magnesium aluminum hydrotalcite-graphene composite material.
Preferably, the modified material is graphene oxide, and the mass fraction is 0.2 wt% -0.7 wt%.
Preferably, the modified material is a magnesium aluminum hydrotalcite-graphene composite material, the mass fraction is 0.1 wt% -5 wt%, and graphene oxide accounts for 1 wt% -10 wt% of the magnesium aluminum hydrotalcite-graphene composite material.
Preferably, the resin is prepared by adopting a suspension polymerization mode, firstly, methyl acrylate, divinylbenzene, benzoyl peroxide accounting for 1 percent of the total monomer and a certain proportion of modified materials are put into a 500ml three-neck flask according to the crosslinking degree of 8 percent, and are stirred and mixed uniformly at room temperature; adding 1 wt% of gelatin into deionized water, stirring, heating to 75 ℃, keeping for 0.5h, adding a dispersing agent after no yellow particles, continuously stirring until the mixture is a uniform solution, stopping heating, dissolving 15 wt% of added sodium chloride by using residual temperature, and cooling the prepared water phase solution to room temperature; after the stirring of the oil phase is stopped, adding a water phase with the weight 4 times of the total weight of the oil phase, standing for several minutes to uniformly mix the oil phase and the water phase, then stirring at the rotating speed of 300-400rpm, heating to 45 ℃, keeping the temperature for 30min, heating to 62 ℃, keeping the temperature for 60min, raising the reaction temperature to 72 ℃ in a manner of raising the temperature by 2 ℃ every 60min, and then keeping the temperature overnight; the solid product after reaction is washed with deionized water and filtered 6-8 times to remove unreacted monomers.
The invention provides a graphene oxide-based composite material modified resin material with strong mechanical property, which has the following beneficial effects:
the modified polyacrylic resin is synthesized by a novel inorganic material in-situ doped suspension polymerization method, the inorganic material is one or more of graphene oxide and magnesium aluminum hydrotalcite-graphene oxide composite materials, so that the purpose of improving the mechanical property of the resin is achieved, and the magnesium aluminum hydrotalcite-graphene oxide composite modified material effectively reduces the occurrence of the phenomenon of internal fracture of the composite material caused by agglomeration of added materials due to the introduction of a hydrotalcite structure, greatly reduces the addition amount of carbon nano tubes, and greatly reduces the cost of the material; the interaction between the hydrotalcite and the carbon nano tube further improves the mechanical property of the material, and the sphericity of the ground hydrotalcite is improved from 43.76% to 91.78%.
Drawings
FIG. 1 shows the mechanical properties (sphericity after grinding) of a typical resin sample
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
wherein the modified material is graphene oxide.
Putting monomer methyl acrylate into a 500ml three-neck flask A, sequentially adding a cross-linking agent divinylbenzene (with the cross-linking degree of 8%), an initiator benzoyl peroxide (accounting for 1 percent of the total amount of the monomers) and a modified material (accounting for 0.1 percent of the total amount of the monomers), and stirring and mixing uniformly at room temperature to obtain an oil phase;
adding gelatin with the mass fraction of 1 wt% into deionized water, placing the mixture into a 500ml three-neck flask B, stirring and heating to 80 ℃, keeping stirring until the mixture is uniform (30 minutes), stopping heating, dissolving the mixture by using sodium chloride (with the amount of 15 wt%) added at the rest temperature, and cooling the prepared water phase solution to room temperature to obtain a water phase;
after the stirring of the oil phase is stopped, adding the water phase with 4 times of the total mass of the oil phase into the oil phase, standing for a few minutes to mix the oil phase and the water phase, then stirring at the rotating speed of 400rpm of 300-. Washing the reacted solid product with deionized water, filtering for 6-8 times to remove unreacted monomers, naturally drying in air, putting into a 60 ℃ oven, and drying to obtain the sample of example 1: magnesium aluminum hydrotalcite-polyacrylic resin composite material (0.1 GO-PMA).
Example 2:
wherein the modified material is graphene oxide.
Putting monomer methyl acrylate into a 500ml three-neck flask A, sequentially adding a cross-linking agent divinylbenzene (with the cross-linking degree of 8%), an initiator benzoyl peroxide (accounting for 1 percent of the total amount of the monomers) and a modified material (accounting for 0.3 percent of the total amount of the monomers), and stirring and mixing uniformly at room temperature to obtain an oil phase;
adding gelatin with the mass fraction of 1 wt% into deionized water, placing the mixture into a 500ml three-neck flask B, stirring and heating to 80 ℃, keeping stirring until the mixture is uniform (30 minutes), stopping heating, dissolving the mixture by using sodium chloride (with the amount of 15 wt%) added at the rest temperature, and cooling the prepared water phase solution to room temperature to obtain a water phase;
after the stirring of the oil phase is stopped, adding the water phase with 4 times of the total mass of the oil phase into the oil phase, standing for a few minutes to mix the oil phase and the water phase, then stirring at the rotating speed of 400rpm of 300-. Washing the reacted solid product with deionized water, filtering for 6-8 times to remove unreacted monomers, naturally drying in air, putting into a 60 ℃ oven, and drying to obtain the sample of the embodiment 2: magnesium aluminum hydrotalcite-polyacrylic resin composite material (0.3 GO-PMA).
Example 3:
wherein the modified material is graphene oxide.
Putting monomer methyl acrylate into a 500ml three-neck flask A, sequentially adding a cross-linking agent divinylbenzene (with the cross-linking degree of 8%), an initiator benzoyl peroxide (accounting for 1 percent of the total amount of the monomers) and a modified material (accounting for 1 percent of the total amount of the monomers), and stirring and mixing uniformly at room temperature to obtain an oil phase;
adding gelatin with the mass fraction of 1 wt% into deionized water, placing the mixture into a 500ml three-neck flask B, stirring and heating to 80 ℃, keeping stirring until the mixture is uniform (30 minutes), stopping heating, dissolving the mixture by using sodium chloride (with the amount of 15 wt%) added at the rest temperature, and cooling the prepared water phase solution to room temperature to obtain a water phase;
after the stirring of the oil phase is stopped, adding the water phase with 4 times of the total mass of the oil phase into the oil phase, standing for a few minutes to mix the oil phase and the water phase, then stirring at the rotating speed of 400rpm of 300-. Washing the reacted solid product with deionized water, filtering for 6-8 times to remove unreacted monomers, naturally drying in air, putting into a 60 ℃ oven, and drying to obtain the sample of the embodiment 3: magnesium aluminum hydrotalcite-polyacrylic resin composite material (1 GO-PMA).
Example 4:
wherein the modified material is a composite material of magnesium-aluminum hydrotalcite and graphene oxide (the mass of the graphene oxide accounts for 1% of that of the composite material).
Preparing a magnesium-aluminum hydrotalcite and graphene oxide composite material (MgAl-LDH @1GO) by a precipitation method;
step 1: dissolving a proper amount of magnesium nitrate and aluminum nitrate in deionized water to form a metal ion solution A;
step 2: then adding a proper amount of boron nitride into the solution A, and mixing the boron nitride with the solution A by using ultrasonic waves to ensure uniform mixing so that the boron nitride is uniformly dispersed in the metal ion solution;
and step 3: weighing a proper amount of sodium hydroxide and anhydrous sodium carbonate to prepare a sodium hydroxide-sodium carbonate mixed solution B;
and 4, step 4: dropwise adding the solution B into the solution A under the condition of strong stirring until the pH value of a reaction system is 10.0;
and 5: aging the obtained suspension for 24h under the condition of water bath at 60 ℃;
step 6: filtering and washing the aged suspension, and drying in an oven at 60 ℃ overnight to obtain magnesium-aluminum hydrotalcite @ boron nitride (MgAl-LDH @1GO for short);
preparing the magnesium aluminum hydrotalcite @ boron nitride-polyacrylic resin composite material by a suspension polymerization method;
putting monomer methyl acrylate into a 500ml three-neck flask A, sequentially adding a cross-linking agent divinylbenzene (with the cross-linking degree of 8%), an initiator benzoyl peroxide (accounting for 1 percent of the total amount of the monomers) and a modified material (accounting for 1 percent of the total amount of the monomers), and stirring and mixing uniformly at room temperature to obtain an oil phase;
adding gelatin with the mass fraction of 1 wt% into deionized water, placing the mixture into a 500ml three-neck flask B, stirring and heating to 80 ℃, keeping stirring until the mixture is uniform (30 minutes), stopping heating, dissolving the mixture by using sodium chloride (with the amount of 15 wt%) added at the rest temperature, and cooling the prepared water phase solution to room temperature to obtain a water phase;
after the stirring of the oil phase is stopped, adding the water phase with 4 times of the total mass of the oil phase into the oil phase, standing for a few minutes to mix the oil phase and the water phase, then stirring at the rotating speed of 400rpm of 300-. Washing the reacted solid product with deionized water, filtering for 6-8 times to remove unreacted monomers, naturally drying in air, putting into a 60 ℃ oven, and drying to obtain the sample of the embodiment 4: magnesium aluminum hydrotalcite @ boron nitride-polyacrylic resin composite material (Mg/Al-LDHs @1GO-PMA for short).
Example 5:
wherein the modified material is a composite material of magnesium-aluminum hydrotalcite and graphene oxide (the mass of the graphene oxide accounts for 3% of the composite material).
Preparing a magnesium-aluminum hydrotalcite and graphene oxide composite material (MgAl-LDH @3GO) by a precipitation method;
step 1: dissolving a proper amount of magnesium nitrate and aluminum nitrate in deionized water to form a metal ion solution A;
step 2: then adding a proper amount of boron nitride into the solution A, and mixing the boron nitride with the solution A by using ultrasonic waves to ensure uniform mixing so that the boron nitride is uniformly dispersed in the metal ion solution;
and step 3: weighing a proper amount of sodium hydroxide and anhydrous sodium carbonate to prepare a sodium hydroxide-sodium carbonate mixed solution B;
and 4, step 4: dropwise adding the solution B into the solution A under the condition of strong stirring until the pH value of a reaction system is 10.0;
and 5: aging the obtained suspension for 24h under the condition of water bath at 60 ℃;
step 6: filtering and washing the aged suspension, and drying in an oven at 60 ℃ overnight to obtain magnesium-aluminum hydrotalcite @ boron nitride (MgAl-LDH @3 GO);
preparing the magnesium aluminum hydrotalcite @ boron nitride-polyacrylic resin composite material by a suspension polymerization method;
putting monomer methyl acrylate into a 500ml three-neck flask A, sequentially adding a cross-linking agent divinylbenzene (with the cross-linking degree of 8%), an initiator benzoyl peroxide (accounting for 1 percent of the total amount of the monomers) and a modified material (accounting for 1 percent of the total amount of the monomers), and stirring and mixing uniformly at room temperature to obtain an oil phase;
adding gelatin with the mass fraction of 1 wt% into deionized water, placing the mixture into a 500ml three-neck flask B, stirring and heating to 80 ℃, keeping stirring until the mixture is uniform (30 minutes), stopping heating, dissolving the mixture by using sodium chloride (with the amount of 15 wt%) added at the rest temperature, and cooling the prepared water phase solution to room temperature to obtain a water phase;
after the stirring of the oil phase is stopped, adding the water phase with 4 times of the total mass of the oil phase into the oil phase, standing for a few minutes to mix the oil phase and the water phase, then stirring at the rotating speed of 400rpm of 300-. Washing the reacted solid product with deionized water, filtering for 6-8 times to remove unreacted monomers, naturally drying in air, putting into a 60 ℃ oven, and drying to obtain the sample of example 5: magnesium aluminum hydrotalcite @ boron nitride-polyacrylic resin composite material (Mg/Al-LDHs @3GO-PMA for short).
Example 6:
wherein the modified material is a composite material of magnesium-aluminum hydrotalcite and graphene oxide (the mass of the graphene oxide accounts for 4% of that of the composite material).
Preparing a magnesium-aluminum hydrotalcite and graphene oxide composite material (MgAl-LDH @4GO) by a precipitation method;
step 1: dissolving a proper amount of magnesium nitrate and aluminum nitrate in deionized water to form a metal ion solution A;
step 2: then adding a proper amount of boron nitride into the solution A, and mixing the boron nitride with the solution A by using ultrasonic waves to ensure uniform mixing so that the boron nitride is uniformly dispersed in the metal ion solution;
and step 3: weighing a proper amount of sodium hydroxide and anhydrous sodium carbonate to prepare a sodium hydroxide-sodium carbonate mixed solution B;
and 4, step 4: dropwise adding the solution B into the solution A under the condition of strong stirring until the pH value of a reaction system is 10.0;
and 5: aging the obtained suspension for 24h under the condition of water bath at 60 ℃;
step 6: filtering and washing the aged suspension, and drying in an oven at 60 ℃ overnight to obtain magnesium-aluminum hydrotalcite @ boron nitride (MgAl-LDH @4 GO);
preparing the magnesium aluminum hydrotalcite @ boron nitride-polyacrylic resin composite material by a suspension polymerization method;
putting monomer methyl acrylate into a 500ml three-neck flask A, sequentially adding a cross-linking agent divinylbenzene (with the cross-linking degree of 8%), an initiator benzoyl peroxide (accounting for 1 percent of the total amount of the monomers) and a modified material (accounting for 1 percent of the total amount of the monomers), and stirring and mixing uniformly at room temperature to obtain an oil phase;
adding gelatin with the mass fraction of 1 wt% into deionized water, placing the mixture into a 500ml three-neck flask B, stirring and heating to 80 ℃, keeping stirring until the mixture is uniform (30 minutes), stopping heating, dissolving the mixture by using sodium chloride (with the amount of 15 wt%) added at the rest temperature, and cooling the prepared water phase solution to room temperature to obtain a water phase;
after the stirring of the oil phase is stopped, adding the water phase with 4 times of the total mass of the oil phase into the oil phase, standing for a few minutes to mix the oil phase and the water phase, then stirring at the rotating speed of 400rpm of 300-. Washing the reacted solid product with deionized water, filtering for 6-8 times to remove unreacted monomers, naturally drying in air, putting into a 60 ℃ oven, and drying to obtain the sample of the embodiment 4: magnesium aluminum hydrotalcite @ boron nitride-polyacrylic resin composite material (Mg/Al-LDHs @4GO-PMA for short).
Example 7:
and (3) measuring the sphericity after grinding:
selecting the modified polyacrylic resin prepared in examples 1-4 and the polyacrylic resin without the modified material as experimental samples, measuring 50ml of the resin sample (no bubbles are ensured in the resin layer, and the reading is carried out after the resin layer is knocked down) by using a 100ml measuring cylinder, and keeping 5ml of water above the resin layer; using 145ml deionized water to transfer the resin into a roller, putting 10 ceramic balls, and screwing a roller cover; and (3) loading the roller on a ball mill, and performing roller milling for 30min +/-4 s. Taking down the roller, opening the cover, transferring all the resin in the roller to a test screen cloth by using deionized water, throwing away free water, spreading, drying at 60 ℃ (about 2-3 h) or air-drying at room temperature until the particles can roll freely; the sample is arranged in enamel dish upper left corner, raises enamel dish and inclines to place on one side, makes the ball roll down in slight vibrations and the particle static can, if the difficult situation of separating of ball granule and particle appears, can stir a small part resin gently with the brush, so operate to the sample separation and finish. In the separated sample, the residual particles of the round spherical particles and the residual round spherical particles in the particles are less than 50 particles. Weigh and record the mass of the balls and nibs as m1And m2。
The sphericity a after grinding is calculated according to formula (1):
in the formula: a-ball percentage after grinding%
m1Mass of the spherical particles, g
m2-mass of broken particles, g.
The calculated results of the ground sphericity are shown in the following table:
TABLE 1 mechanical Properties (sphericity after grinding) of 7 resin samples in total for comparative example and example
It can be seen from the table that the milled sphericity of the comparative example 1 (unmodified polyacrylic resin, PMA) is 43.76%, the milled sphericity can be improved by adding the Graphene Oxide (GO) and the magnesium aluminum hydrotalcite-graphene oxide composite material, and the milled sphericity of the graphene oxide with 0.3 wt% is obviously improved, which reaches 91.78% and is improved by 109.6%. The magnesium-aluminum hydrotalcite and the graphene oxide are compounded and then used for modifying polyacrylic resin, so that the addition amount of the graphene oxide is reduced to 0.03%, and the sphericity rate after grinding can still reach 88.62%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations may be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. A graphene oxide-based composite material modified resin material with strong mechanical property is characterized in that graphene oxide is doped in situ in a process of synthesizing polypropylene resin by a suspension polymerization method, a novel modified resin material with remarkably improved mechanical property can be obtained, and the sphericity rate after grinding is improved from 43.76% to 91.78%; the mass fraction of the graphene oxide is 0.3 wt%;
putting a monomer methyl acrylate into a 500mL three-neck flask A, sequentially adding a cross-linking agent divinylbenzene, an initiator benzoyl peroxide and graphene oxide, and stirring and mixing uniformly at room temperature to obtain an oil phase; the crosslinking degree of the divinylbenzene is 8 percent; the benzoyl peroxide accounts for 1% of the total monomer amount; the graphene oxide accounts for 0.3 wt% of the total amount of the monomers;
adding gelatin with the mass fraction of 1 wt% into deionized water, placing the mixture into a 500mL three-neck flask B, stirring and heating to 80 ℃, keeping stirring for 30 minutes until the mixture is uniform and is dissolved for 30 minutes, stopping heating, adding 15 wt% of sodium chloride into the rest temperature for dissolving, and cooling the prepared water phase solution to room temperature to obtain a water phase;
and after the stirring of the oil phase is stopped, adding the water phase of which the mass is 4 times of the total mass of the oil phase into the oil phase, standing for several minutes to mix the oil phase and the water phase, then stirring at the rotating speed of 400rpm of 300-. Washing the reacted solid product with deionized water, filtering for 6-8 times to remove unreacted monomer, naturally drying in air, and oven drying at 60 deg.C.
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