CN107603131B - Low-energy-consumption large-scale preparation method of graphene filling master batch - Google Patents
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Abstract
The invention provides a method for preparing a graphene filling master batch in a large scale with low energy consumption, which comprises the steps of adsorbing graphene by porous resin microspheres with good compatibility with matrix resin, dissolving a foaming agent H in an organic solvent, removing the organic solvent through atomization, depositing the foaming agent H on the surfaces of the porous resin microspheres for packaging and coating, separating by a centrifuge, and crushing to obtain the functional master batch. The technical defects that a screw extruder is used, the process is complicated, the equipment cost is high, and the energy consumption is high are overcome, extrusion equipment is not needed for preparing the master batch, the equipment cost and the energy consumption are reduced, and the large-scale production is facilitated; furthermore, the graphene dispersion effect is improved by utilizing the good compatibility of the porous resin microspheres and the matrix resin, and when the master batch is used, graphene is uniformly and slowly released into the resin along with the decomposition of the foaming agent, so that the graphene dispersion effect is improved, and the porous resin microspheres are prevented from being agglomerated again when the resin matrix is fused.
Description
Technical Field
The invention relates to the field of material processing, in particular to a method for preparing a graphene filling master batch in a low-energy-consumption and large-scale manner.
Background
In 2004, graphene materials were successfully prepared, and thus, a hot tide of research on new wave carbon materials is initiated. Graphene is a planar carbon nanomaterial consisting of a layer of carbon atoms, the thinnest two-dimensional material currently known, with a thickness of only 0.335nm, consisting of a hexagonal lattice. Carbon atoms in the graphene are connected by sigma bonds, so that the graphene is endowed with extremely excellent mechanical properties and structural rigidity. Moreover, in graphene, each carbon atom has an unbound p electron, and the p electrons can move freely in the crystal and move at 1/300 with the speed as high as the speed of light, so that the graphene is endowed with good conductivity. Optically, graphene is almost completely transparent, absorbing only 2.3% of light. Graphene has peculiar mechanical, optical and electrical properties, and thus is considered to have a wide industrial application prospect in reinforcing, electrically and thermally conductive fillers as a polymer matrix.
The conventional method for preparing various master batches at present comprises the steps of firstly kneading and mixing the components in a high-speed kneading machine or a mixing machine, then discharging, and then extruding and granulating in a double-screw extruder to obtain the master batch.
Chinese patent publication No. 106564175a discloses a graphene conductive masterbatch and a preparation method thereof, which comprises the steps of using a strong shearing screw extruder with shearing teeth to uniformly mix graphite raw materials with hot melt materials, stripping graphite into graphene by using the strong shearing action of the shearing teeth, uniformly dispersing the graphene along the rotation direction of a screw rod to obtain uniformly dispersed graphene melts, and finally obtaining the graphene conductive masterbatch by extrusion granulation.
Chinese patent publication No. 105694102 a uses a screw extruder as a continuous reactor, and graphite powder is dispersed and fixed by a three-dimensional porous inorganic substance while being peeled off, and further a heat conducting network is formed by continuous polymerization, so as to prepare a composite graphene microchip heat dissipation master batch. The heat dissipation device is widely applied to heat dissipation of high-load rubber tires, heat dissipation of rubber pads, heat dissipation of electronic component joints, heat dissipation of LEDs and the like, and has wide market prospect.
Chinese patent publication No. 107200947a discloses a graphene nanoplatelets conductive masterbatch and a preparation method thereof, which comprises mixing graphite powder with metallic tin, melting tin at high temperature, stripping graphite into graphene nanoplatelets by stirring, crushing and shearing, and rapidly cooling the graphene nanoplatelets with glass beads to make graphene stably and uniformly dispersed in the metallic tin and coated on the glass beads, further forming graphene particles stabilized by tin by grinding, dispersing in a high molecular material, and preparing by a screw extruder. The graphene microchip conductive master batch has good dispersibility, and is suitable for the conductivity of various conductive plastics, electronic plastics and photovoltaic plastics.
The method needs a screw extruder, so that the process is complicated, the equipment cost is high, and the energy consumption is high. If the masterbatch particles are prepared by a method without using a screw extruder, the production cost is greatly reduced. Meanwhile, graphene can generate self-aggregation to destroy the uniformity and compactness of dispersion of the graphene, so that the mechanical properties and the like of the composite material are reduced. Therefore, a preparation method for preparing the graphene filling master batch with good graphene dispersibility, low energy consumption and large scale is needed to be developed.
Disclosure of Invention
Aiming at the technical defects of complex process, poor dispersion effect and high energy consumption of the graphene master batch prepared by using a screw extruder in the prior art, the invention provides the preparation method of the graphene filling master batch with good graphene dispersibility and low energy consumption in a large scale.
In order to solve the problems, the invention adopts the following technical scheme:
a method for preparing a graphene filling master batch in a low-energy-consumption and large-scale mode comprises the following steps:
(1) taking 3-15 parts by weight of graphene powder, 30-65 parts by weight of porous resin microspheres, 20-25 parts by weight of foaming agent H, 40-100 parts by weight of organic solvent and 1-2 parts by weight of graphene dispersing agent as raw materials;
(2) dividing the foaming agent H into two parts, and compounding the graphene powder, the graphene dispersing agent and the first part of foaming agent H with the porous resin microspheres at the rotation speed of 160-430rpm, and stirring for 20-50 minutes to uniformly load graphene on the porous resin microspheres, thereby obtaining the composite porous resin microspheres;
(3) adding the composite porous resin microspheres into the organic solvent, adding a second foaming agent H, uniformly stirring, removing the organic solvent through an atomization process, depositing the foaming agent H on the surfaces of the porous resin microspheres to encapsulate and coat the porous resin microspheres, separating through a centrifuge, and crushing to obtain the graphene filling master batch.
Preferably, the graphene powder is one or a combination of more than two of single-layer graphene, double-layer graphene, multi-layer graphene, graphene oxide and nitrogen-doped graphene.
Preferably, the porous resin microspheres are one or a combination of two of phenolic resin microspheres and polystyrene microspheres, the particle size of the porous microspheres is 10-200 μm, and the pore diameter is 50-800 nm.
Preferably, the organic solvent is any one or a combination of more than two of methanol, ethanol, isopropanol, acetone and diethyl ether.
Preferably, the graphene dispersant is any one or a combination of more than two of polyvinyl alcohol, pyrrolidone, cellulose, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide, tween-80 and triton-100.
Preferably, the weight ratio of the first part of foaming agent H to the second part of foaming agent H is 1: 1-2.
Preferably, the atomization process adopts a spraying device, the air flow speed is controlled to be 10-60m/s, and the centrifugal speed of the centrifugal machine is 2000-.
Preferably, the step of crushing to obtain the graphene filling master batch is to crush by ball milling with a ball mill, and the rotation speed of the ball mill is controlled to be 360-800rpm, so that the graphene filling master batch is obtained by crushing.
The double-screw extruder used in the existing scheme is complex in process, high in equipment cost and high in energy consumption. Meanwhile, graphene can generate self-aggregation to destroy the uniformity and compactness of dispersion of the graphene, so that the mechanical properties and the like of the composite material are reduced. In view of the above, a method for preparing a graphene filling master batch in a large scale with low energy consumption is provided, wherein porous resin microspheres with good compatibility with matrix resin are used for adsorbing graphene, then a foaming agent H is dissolved in an organic solvent, the organic solvent is removed through atomization, the foaming agent H is deposited on the surfaces of the porous resin microspheres for packaging and coating, and the functional master batch is obtained through separation by a centrifuge and then crushing. When the master batch is used, graphene is uniformly and slowly released into the resin along with the decomposition of the foaming agent; the method for preparing the master batch does not need extrusion equipment, reduces equipment cost and energy consumption, and is beneficial to large-scale production; furthermore, the porous resin microspheres have good compatibility with matrix resin, so that the graphene dispersion effect is improved, and the porous resin microspheres are prevented from reuniting when the resin matrix is fused by the foaming agent for encapsulation.
Compared with the prior art, the internal mixer for preparing the graphene through stretching stripping and the method for preparing the graphene have the outstanding characteristics and excellent effects that:
1. the invention provides a preparation method for preparing a graphene filling master batch with good graphene dispersibility, low energy consumption and large scale.
2. The invention provides a preparation method for preparing a graphene filling master batch with good graphene dispersibility, low energy consumption and large scale.
3. The foaming agent H is divided into two parts to be mixed with the porous resin microspheres, so that the porous resin microspheres can be more effectively packaged and coated.
4. The master batch has stable performance, is easy to store and convenient to use, thereby promoting the application of the graphene filling material in the field of resin.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Taking 3 parts by weight of single-layer graphene powder, 65 parts by weight of porous phenolic resin microspheres with the particle size of 200 mu m and the pore diameter of 50nm, 25 parts by weight of foaming agent H, 50 parts by weight of acetone and 2 parts by weight of polyvinyl alcohol as raw materials;
(2) dividing the foaming agent H into two parts, wherein the weight ratio of the first part of foaming agent H to the second part of foaming agent H is 1:1, compounding the graphene powder, the graphene dispersing agent, the first part of foaming agent H and the porous resin microspheres at the rotation speed of 430rpm, and stirring for 20 minutes to enable the porous resin microspheres to uniformly load graphene, so as to obtain composite porous resin microspheres;
(3) adding the composite porous resin microspheres into the organic solvent, then adding a second foaming agent H, stirring uniformly at a stirring speed of 120rpm, removing the organic solvent by atomization, controlling the air flow rate at 60m/s by using a spraying device, separating by using a centrifuge at a centrifugal speed of 2000rpm, depositing the foaming agent H on the surfaces of the porous resin microspheres to encapsulate and coat the porous resin microspheres, grinding by using a ball mill at a rotating speed of 360rpm, and grinding to obtain the graphene filling master batch.
Example 2
(1) Taking 15 parts by weight of double-layer graphene and multi-layer graphene combined powder, 50 parts by weight of polystyrene microspheres with the particle size of 200 mu m and the pore diameter of 800nm, 20 parts by weight of foaming agent H, 100 parts by weight of methanol and ethanol mixed solution and 1 part by weight of a mixture of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and hexadecyl trimethyl ammonium bromide as raw materials;
(2) dividing the foaming agent H into two parts, wherein the weight ratio of the first part of foaming agent H to the second part of foaming agent H is 1: 2, compounding the graphene powder, the graphene dispersing agent, the first part of foaming agent H and the porous resin microspheres at the rotation speed of 430rpm, and stirring for 20 minutes to enable the porous resin microspheres to uniformly load graphene, so as to obtain composite porous resin microspheres;
(3) adding the composite porous resin microspheres into the organic solvent, then adding a second foaming agent H, stirring uniformly at a stirring speed of 30rpm, removing the organic solvent by atomization, controlling the air flow rate at 10m/s by using a spraying device, separating by using a centrifuge, depositing the foaming agent H on the surfaces of the porous resin microspheres to encapsulate and coat the porous resin microspheres, grinding by using a ball mill, controlling the rotation speed of the ball mill at 360rpm, and grinding to obtain the graphene filling master batch.
Example 3
(1) Taking 5 parts by weight of mixed graphene powder of graphene oxide and nitrogen-doped graphene, 35 parts by weight of porous phenolic resin microspheres with the particle size of 150 microns and the pore diameter of 700nm, 23 parts by weight of foaming agent H, 85 parts by weight of ethanol and isopropanol mixture and 2 parts by weight of polyvinyl alcohol as raw materials;
(2) dividing the foaming agent H into two parts, wherein the weight ratio of the first part of foaming agent H to the second part of foaming agent H is 1:1, compounding the graphene powder, the graphene dispersing agent, the first part of foaming agent H and the porous resin microspheres at the rotation speed of 180rpm, and stirring for 30 minutes to enable the porous resin microspheres to uniformly load graphene, so as to obtain composite porous resin microspheres;
(3) adding the composite porous resin microspheres into the organic solvent, then adding a second foaming agent H, stirring uniformly at a stirring speed of 100rpm, removing the organic solvent by atomization, controlling the air flow rate at 30m/s by using a spraying device, separating by using a centrifuge at a centrifugal speed of 6000rpm, depositing the foaming agent H on the surfaces of the porous resin microspheres to encapsulate and coat the porous resin microspheres, grinding by using a ball mill at a rotation speed of 400rpm, and grinding to obtain the graphene filling master batch.
Example 4
(1) Taking 6 parts by weight of double-layer graphene, multi-layer graphene and graphene oxide mixed graphene powder, 35 parts by weight of porous microspheres with the particle size of 180 mu m and the pore diameter of 200nm, 22 parts by weight of foaming agent H, 50 parts by weight of organic solvent methanol and 2 parts by weight of Tween-80 as raw materials;
(2) dividing the foaming agent H into two parts, wherein the weight ratio of the first part of foaming agent H to the second part of foaming agent H is 1:1, compounding the graphene powder, the graphene dispersing agent, the first part of foaming agent H and the porous resin microspheres at the rotating speed of 300rpm, and stirring for 25 minutes to enable the porous resin microspheres to uniformly load graphene, so as to obtain composite porous resin microspheres;
(3) adding the composite porous resin microspheres into the organic solvent, then adding a second foaming agent H, stirring uniformly at a stirring speed of 110rpm, removing the organic solvent by atomization, controlling the air flow speed at 50m/s by using a spraying device, separating by using a centrifuge, wherein the centrifugal speed of the centrifuge is 3500rpm, depositing the foaming agent H on the surfaces of the porous resin microspheres to package and coat the porous resin microspheres, grinding by using a ball mill, controlling the rotation speed of the ball mill at 550rpm, and grinding to obtain the graphene filling master batch.
Example 5
(1) Taking 10 parts by weight of graphene powder, 30 parts by weight of porous resin microspheres, wherein the porous resin microspheres are a mixture of porous microspheres with the particle size of 180 micrometers and the pore diameter of 230nm, 24 parts by weight of foaming agent H, 45 parts by weight of organic solvent isopropanol, and 1.5 parts by weight of sodium dodecyl sulfate and triton-100 as raw materials;
(2) dividing the foaming agent H into two parts, wherein the weight ratio of a first part of foaming agent H to a second part of foaming agent H is 1:1.5, compounding the graphene powder, the graphene dispersing agent, the first part of foaming agent H and the porous resin microspheres at the rotation speed of 350rpm, stirring for 45 minutes, and uniformly loading graphene on the porous resin microspheres to obtain composite porous resin microspheres;
(3) adding the composite porous resin microspheres into the organic solvent, then adding a second foaming agent H, stirring uniformly at a stirring speed of 500rpm, removing the organic solvent by atomization, controlling the air flow speed at 45m/s by using a spraying device, separating by using a centrifuge, depositing the foaming agent H on the surfaces of the porous resin microspheres to encapsulate and coat the porous resin microspheres, and crushing by using a ball mill at a rotation speed of 650rpm to obtain the graphene filling master batch.
Comparative example 1
(1) Taking 10 parts by weight of graphene powder, 30 parts by weight of porous resin microspheres, wherein the porous resin microspheres are a mixture of porous microspheres with the particle size of 180 mu m and the pore diameter of 230nm, 45 parts by weight of organic solvent isopropanol, and 1.5 parts by weight of sodium dodecyl sulfate and triton-100 as raw materials;
(2) compounding graphene powder, the graphene dispersing agent and the porous resin microspheres, and stirring for 45 minutes at the rotating speed of 350rpm to uniformly load graphene on the porous resin microspheres to obtain composite porous resin microspheres;
(3) adding the composite porous resin microspheres into the organic solvent, uniformly stirring at a stirring speed of 500rpm, then removing the organic solvent through atomization, adopting a spraying device, controlling the air flow rate at 45m/s, separating by using a centrifuge, controlling the centrifugal speed of the centrifuge at 7200rpm, ball-milling by using a ball mill, controlling the rotation speed of the ball mill at 650rpm, and crushing to obtain the graphene filling master batch.
The graphene filling master batches prepared in examples 1 to 5 and comparative example 1 were added to PP8303 in a mass ratio of 5%, dispersed by a screw extruder, and calendered to obtain a sheet, and the dispersibility of the graphene filling master batch was measured by testing the properties of the sheet, as shown in table 1 below.
Table 1:
| DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION | Sheet thickness (mm) | Sheet tensile Strength (MPa) | Sheet elongation at Break (%) |
| Example 1 | 1.5 | 48 | 350 |
| Example 2 | 1.5 | 51 | 399 |
| Example 3 | 1.8 | 44 | 400 |
| Example 4 | 1,8 | 47 | 385 |
| Example 5 | 1.5 | 49 | 392 |
| Comparative example 1 | 1.5 | 27 | 215 |
Through application analysis of the master batch, the foaming agent H is divided into two parts and mixed with the porous resin microspheres in a dividing manner, so that the porous resin microspheres can be more effectively encapsulated and coated, when the master batch is used, graphene is uniformly and slowly released into resin along with decomposition of the foaming agent, the graphene dispersion effect is improved, the strength and flexibility of the obtained plastic product are obviously enhanced, and the graphene cannot be effectively dispersed due to lack of dispersion promotion of the foaming agent in comparative example 1, which is not encapsulated by the foaming agent under the same condition, so that the reinforcement is not obvious.
Furthermore, the foaming agent is adopted to encapsulate the porous resin microspheres loaded with graphene, and then the porous resin microspheres are crushed to prepare the master batch, so that the technical defects of complex process and high energy consumption of a screw extruder are overcome.
Claims (6)
1. The method for preparing the graphene filling master batch in a large scale with low energy consumption is characterized by comprising the following steps of:
(1) taking 3-15 parts by weight of graphene powder, 30-65 parts by weight of porous resin microspheres, 20-25 parts by weight of foaming agent H, 40-100 parts by weight of organic solvent and 1-2 parts by weight of graphene dispersing agent as raw materials;
(2) dividing the foaming agent H into two parts, and compounding the graphene powder, the graphene dispersing agent and the first part of foaming agent H with the porous resin microspheres at the rotation speed of 160-430rpm, and stirring for 20-50 minutes to uniformly load graphene on the porous resin microspheres, thereby obtaining the composite porous resin microspheres;
(3) adding the composite porous resin microspheres into the organic solvent, adding a second foaming agent H, uniformly stirring, removing the organic solvent through an atomization process, depositing the foaming agent H on the surfaces of the porous resin microspheres to package and coat the porous resin microspheres, separating through a centrifuge, and crushing to obtain a graphene filling master batch;
the weight ratio of the first part of foaming agent H to the second part of foaming agent H is 1: 1-2;
the porous resin microspheres are one or two of porous phenolic resin microspheres and polystyrene microspheres, the particle diameter of the porous microspheres is 10-200 mu m, and the pore diameter is 50-800 nm.
2. The method for preparing the graphene filling master batch in a large scale with low energy consumption according to claim 1, wherein the graphene powder is one or a combination of more than two of single-layer graphene, double-layer graphene, multi-layer graphene, graphene oxide and nitrogen-doped graphene.
3. The method for preparing the graphene filling masterbatch in a large scale with low energy consumption according to claim 1, wherein the organic solvent is any one or a combination of more than two of methanol, ethanol, isopropanol, acetone and diethyl ether.
4. The method for low-energy-consumption large-scale preparation of the graphene filling masterbatch according to claim 1, wherein the graphene dispersing agent is any one or a combination of more than two of polyvinyl alcohol, polyethylene, pyrrolidone, cellulose, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide, tween-80 and triton-100.
5. The method for preparing the graphene filling masterbatch with low energy consumption and large scale according to claim 1, wherein a spraying device is adopted in the atomization process, the air flow rate is controlled to be 10-60m/s, and the centrifugal speed of the centrifuge is 2000-8000 rpm.
6. The method for preparing the graphene filling master batch in a large scale with low energy consumption according to claim 1, wherein the step of crushing to obtain the graphene filling master batch is specifically to crush by ball milling with a ball mill, and the rotation speed of the ball mill is controlled to be 360-800rpm, so that the graphene filling master batch is obtained by crushing.
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| CN109111822A (en) * | 2018-07-19 | 2019-01-01 | 佛山腾鲤新能源科技有限公司 | A kind of conductive corrosion-resistant coating |
| CN109796682B (en) * | 2018-12-18 | 2021-08-17 | 武汉金牛经济发展有限公司 | Toughened heat-resistant PPR pipe and preparation method thereof |
| CN110144083A (en) * | 2019-05-14 | 2019-08-20 | 合肥市丽红塑胶材料有限公司 | A kind of impact-resistant modified PP material and preparation method thereof |
| CN110105666A (en) * | 2019-05-21 | 2019-08-09 | 合肥市丽红塑胶材料有限公司 | A kind of nucleating agent master batch and preparation method thereof for toughening modifying PP resin |
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| CN101864098A (en) * | 2010-06-03 | 2010-10-20 | 四川大学 | Preparation method of polymer/graphene composite material through in situ reduction |
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Effective date of registration: 20220914 Address after: No. 1, Plastic Packaging Industrial Park, Economic Development Zone, Weishan County, Jining City, Shandong Province, 277600 Patentee after: Jining Sanhe Plastic Products Co.,Ltd. Address before: 610091, Sichuan, Chengdu province Qingyang dragon industrial port, East Sea 4 Patentee before: CHENDU NEW KELI CHEMICAL SCIENCE Co.,Ltd. CHINA |