CN110627059B - Dispersible graphite powder and preparation method thereof - Google Patents
Dispersible graphite powder and preparation method thereof Download PDFInfo
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- CN110627059B CN110627059B CN201910970384.2A CN201910970384A CN110627059B CN 110627059 B CN110627059 B CN 110627059B CN 201910970384 A CN201910970384 A CN 201910970384A CN 110627059 B CN110627059 B CN 110627059B
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Abstract
The invention provides dispersible graphite powder, which is a composite body which is formed by adhering weight powder and a gelling agent by adopting a macromolecular dispersion adhesive and is sintered and takes graphite as a core, wherein the molar ratio of crystalline flake graphite, the macromolecular dispersion adhesive, the weight powder and the gelling agent in the raw materials is 1: 0.01-0.2: 0.2-1: 0.0010-0.0015, wherein the counterweight powder is a mixed powder formed by mixing fumed alumina, superfine metal silicon powder, fumed silica and silicone resin powder; the macromolecular dispersion binder is copolymer powder polymerized by polymerization monomers; the gelatinizing agent is PVA powder. The graphite powder has good hydrophilicity, can be uniformly dispersed in slurry, improves the integral toughness of the refractory material, does not introduce other harmful impurities into the preparation ring joint, and eliminates the influence on the high-temperature mechanical property of the material due to the introduction of other impurities.
Description
Technical Field
The invention provides graphite powder and a preparation method thereof, in particular relates to dispersible graphite powder used in refractory materials, and belongs to the technical field of composite materials.
Background
The flake graphite is widely used in high-grade refractory materials and coatings in metallurgy industry. Such as magnesia carbon brick, crucible, etc. A fire material stabilizer in the military industry, a desulfurization accelerator in the smelting industry, a pencil lead in the light industry, a carbon brush in the electrical industry, an electrode in the battery industry, a catalyst in the fertilizer industry and the like. The scale graphite can be further processed to produce graphite emulsion used for lubricants, release agents, wire drawing agents, conductive coatings and the like. The expanded graphite can also be used as raw material of flexible graphite products, such as flexible graphite sealing elements, flexible graphite composite products and the like.
In the prior refractory material prepared by taking crystalline flake graphite as a raw material, graphite is often directly added into the preparation link of the refractory material or is added into the production link after other modification treatment, and the following defects generally exist: 1. graphite has poor hydrophilicity, is easy to float to the surface of the slurry in the process of preparing the slurry, and has poor dispersion performance. 2. Some of the substances used in modifying graphite to enhance its dispersion properties can adversely affect the high temperature mechanical properties of the overall refractory.
Disclosure of Invention
The invention solves the defects in the prior art and provides the dispersible graphite powder and the preparation method thereof, the graphite powder has good hydrophilicity, can be uniformly dispersed in slurry, improves the integral toughness of the refractory material, does not introduce other harmful impurities in a preparation ring, and eliminates the influence on the high-temperature mechanical property of the material caused by introducing other impurities.
The technical scheme adopted for realizing the above purpose of the invention is as follows:
a dispersible graphite powder is a composite body which is formed by adopting a macromolecular dispersion adhesive to adhere balance weight powder and a gelling agent and takes graphite as a core through sintering, wherein the molar ratio of crystalline flake graphite, the macromolecular dispersion adhesive, the balance weight powder and the gelling agent in raw materials is 1: 0.01-0.2: 0.2-1: 0.0010 to 0.0015, wherein the weight powder is formed by mixing fumed alumina, superfine metal silicon powder, fumed silica and silicone resin powder, and the density of the weight powder is 2.8 to 4.0g/cm3The mixed powder of (1); the macromolecular dispersion binder is copolymer powder polymerized by polymerization monomers, and the average molecular weight of the macromolecular dispersion binder is 50000-300000; the gelatinizing agent is PVA powder.
The crystalline flake graphite is crystalline flake graphite with the carbon content higher than 90% and the grain size larger than 3000 meshes.
The macromolecular dispersion binder is a copolymer powder material which adopts acrylic acid, isopentenol polyglycol ether, acrylamide, maleic acid, monobutyl maleate, styrene and polyether amine as monomers, wherein the molecular weight of the polyether amine is 230.
The mass ratio of the fumed alumina, the superfine metal silicon powder, the fumed silica and the silicon resin powder in the balance weight powder is 0.02-0.06: 100: 0.02-0.06: 70-150.
The specific surface area of the gas-phase alumina is 150-260 m2A powder of fumed alumina per gram.
The fumed silica has a specific surface area of 200-220 m2Gas per gA fumed silica powder.
The superfine metal silicon powder is metal silicon powder with D50 ═ 5 mu m and silicon content of more than 99%.
The silicone resin powder is MQ silicone resin powder with the MQ ratio of 0.6-0.8: 1 and the particle size of 3000 meshes.
The gelatinizing agent is one or a mixture of more than two of three PVA powders with the grain sizes of 3000 meshes, 1500 meshes and 6000 meshes.
The invention also provides a preparation method of the dispersible graphite powder, which comprises the following steps: (1) respectively weighing fumed alumina, superfine metal silicon powder, fumed silica and silicon resin powder, and fully mixing the raw materials in a mixer to prepare balance weight powder;
(2) weighing the flake graphite, the macromolecular dispersion binder, the weight powder and the gelling agent according to the proportion, and continuously and fully mixing the materials uniformly;
(3) and feeding the uniformly mixed raw materials into an air pipe and blowing the raw materials into a laser sintering device, forming the raw materials in a sintering area, and then feeding the raw materials into a cyclone separator for separation and screening to obtain the dispersible graphite.
Compared with the prior art, the dispersible graphite powder provided by the invention can form uniformly distributed graphite colloid in refractory materials and ceramic slurry, and simultaneously endows graphite with good hydrophilicity, so that the graphite is not easy to float to the surface, thereby improving the overall toughness of the material. Besides the introduction of graphite, the invention does not introduce other harmful impurities into the high-temperature sintered material, thereby eliminating the influence on the high-temperature mechanical property of the material caused by the introduction of other impurities.
In conclusion, the beneficial effects of the invention are as follows: 1. good hydrophilicity is not easy to float to the surface, and the toughness of the whole material is improved. 2. The toughness of the whole material is improved. 3. Other harmful impurities are not introduced into the material sintered at high temperature, so that the influence on the high-temperature mechanical property of the material caused by introducing other impurities is eliminated.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the scope of the present invention is not limited to the examples.
Example 1
The dispersible graphite powder provided in the present example is prepared by the following method: mixing fumed alumina, superfine metal silicon powder, fumed silica and 3000-mesh silicon resin powder according to the weight ratio of 0.02: 100: 0.04: 90 for 45min in a double-cone mixer, adding the crystalline flake graphite, the macromolecular dispersion binder and the gelling agent after uniformly mixing, and then mixing for more than 1.5h, wherein the molar ratio of the crystalline flake graphite to the macromolecular dispersion binder to the weight-balancing powder to the gelling agent is 1: 0.01-0.2: 0.2-1: 0.0015. after being uniformly mixed, the mixture is conveyed into an air pipe by a conveying screw according to the conveying capacity of 30kg/h and is blown into a laser sintering device, and the mixture enters a cyclone separator for separation and screening after being formed in a sintering area to obtain the dispersible graphite.
In this embodiment, the flake graphite is flake graphite having a carbon content higher than 90% and a particle size larger than 3000 mesh. The macromolecular dispersion binder is a copolymer powder material which adopts acrylic acid, isopentenol polyglycol ether, acrylamide, maleic acid, monobutyl maleate, styrene and polyether amine as monomers, wherein the molecular weight of the polyether amine is 230, and the average molecular weight of the copolymer is 250000. The specific surface area of the gas-phase alumina is 150-260 m2A powder of fumed alumina per gram. The fumed silica has a specific surface area of 200-220 m2Fumed silica powder per gram. The superfine metal silicon powder is metal silicon powder with D50 ═ 5 mu m and silicon content of more than 99%. The silicone resin powder is MQ silicone resin powder with the MQ ratio of 0.6:1 and the particle size of 3000 meshes. The gelatinizing agent is PVA powder with the grain size of 3000 meshes.
Example 2
The dispersible graphite powder provided in the present example is prepared by the following method: mixing fumed alumina, superfine metal silicon powder, fumed silica and 3000-mesh silicon resin powder according to the weight ratio of 0.06: 100: 0.04: 110 for 45min in a double-cone mixer, adding the crystalline flake graphite, the macromolecular dispersion binder and the gelling agent after uniformly mixing, and mixing for more than 1.5h again, wherein the molar ratio of the crystalline flake graphite to the macromolecular dispersion binder to the weight-balancing powder to the gelling agent is 1: 0.01-0.2: 0.2-1: 0.0015. after being uniformly mixed, the mixture is conveyed into an air pipe by a conveying screw according to the conveying capacity of 30kg/h and is blown into a laser sintering device, and the mixture enters a cyclone separator for separation and screening after being formed in a sintering area to obtain the dispersible graphite.
In this embodiment, the flake graphite is flake graphite having a carbon content higher than 90% and a particle size larger than 3000 mesh. The macromolecular dispersion binder is a copolymer powder material which adopts acrylic acid, isopentenol polyglycol ether, acrylamide, maleic acid, monobutyl maleate, styrene and polyether amine as monomers, wherein the molecular weight of the polyether amine is 230, and the average molecular weight of the copolymer is 150000. The specific surface area of the gas-phase alumina is 150-260 m2A powder of fumed alumina per gram. The fumed silica has a specific surface area of 200-220 m2Fumed silica powder per gram. The superfine metal silicon powder is metal silicon powder with D50 ═ 5 mu m and silicon content of more than 99%. The silicone resin powder is MQ silicone resin powder with the MQ ratio of 0.7:1 and the particle size of 3000 meshes. The gelatinizing agent is PVA powder with the grain size of 6000 meshes.
Example 3
The dispersible graphite powder provided in the present example is prepared by the following method: mixing fumed alumina, superfine metal silicon powder, fumed silica and 3000-mesh silicon resin powder according to the weight ratio of 0.04: 100: 0.02: 130 for 45min in a double-cone mixer, adding the crystalline flake graphite, the macromolecular dispersion binder and the gelling agent after uniformly mixing, and then mixing for more than 1.5h, wherein the molar ratio of the crystalline flake graphite to the macromolecular dispersion binder to the weight-balancing powder to the gelling agent is 1: 0.01-0.2: 0.2-1: 0.0015. after being uniformly mixed, the mixture is conveyed into an air pipe by a conveying screw according to the conveying capacity of 30kg/h and is blown into a laser sintering device, and the mixture enters a cyclone separator for separation and screening after being formed in a sintering area to obtain the dispersible graphite.
In this embodiment, the flake graphite is flake graphite having a carbon content higher than 90% and a particle size larger than 3000 mesh. The macromolecular dispersion binder is prepared from acrylic acid, isopentenol polyglycol ether, acrylamide, maleic acid, monobutyl maleate and styreneThe molecular weight of the polyether amine is 230, and the average molecular weight of the copolymer is 100000. The specific surface area of the gas-phase alumina is 150-260 m2A powder of fumed alumina per gram. The fumed silica has a specific surface area of 200-220 m2Fumed silica powder per gram. The superfine metal silicon powder is metal silicon powder with D50 ═ 5 mu m and silicon content of more than 99%. The silicone resin powder is MQ silicone resin powder with the MQ ratio of 0.8:1 and the particle size of 3000 meshes. The gelatinizing agent is mixed PVA powder with the grain size of 3000 meshes and 1500 meshes.
The dispersible graphite powder prepared in the three embodiments is used for preparing a refractory material, and the performance of the prepared refractory material is detected, and the specific experimental results are as follows:
from the experimental results, the refractory material prepared by using the dispersible graphite powder prepared by the method as the additive has the advantages of good high-temperature bending resistance, excellent erosion resistance, long service life at high temperature, good toughness and high-temperature mechanical property.
Claims (8)
1. A dispersible graphite powder is a composite body which is formed by adopting a macromolecular dispersion binder to adhere balance weight powder and a gelling agent and takes graphite as a core through sintering, wherein the molar ratio of crystalline flake graphite, the macromolecular dispersion binder, the balance weight powder and the gelling agent in raw materials is 1: 0.01-0.2: 0.2-1: 0.0010 to 0.0015;
the counterweight powder is formed by mixing fumed alumina, superfine metal silicon powder, fumed silica and silicon resin powder, and the density of the counterweight powder is 2.8-4.0 g/cm3The mass ratio of the four mixed powders is 0.02-0.06: 100: 0.02-0.06: 70-150 parts by weight;
the macromolecular dispersion binder is copolymer powder polymerized by polymerization monomers, the average molecular weight of the macromolecular dispersion binder is 50000-300000, and the macromolecular dispersion binder is a copolymer powder material taking acrylic acid, prenol polyglycol ether, acrylamide, maleic acid, monobutyl maleate, styrene and polyether amine as monomers, wherein the molecular weight of the polyether amine is 230;
the gelatinizing agent is PVA powder.
2. A dispersible graphite powder according to claim 1, characterized in that: the crystalline flake graphite is crystalline flake graphite with the carbon content higher than 90% and the grain size larger than 3000 meshes.
3. A dispersible graphite powder according to claim 1, characterized in that: the specific surface area of the gas-phase alumina is 150-260 m2A powder of fumed alumina per gram.
4. A dispersible graphite powder according to claim 1, characterized in that: the fumed silica has a specific surface area of 200-220 m2Fumed silica powder per gram.
5. A dispersible graphite powder according to claim 1, characterized in that: the superfine metal silicon powder is metal silicon powder with D50=5 μm and silicon content of more than 99%.
6. A dispersible graphite powder according to claim 1, characterized in that: the silicone resin powder is MQ silicone resin powder with the MQ ratio of 0.6-0.8: 1 and the particle size of 3000 meshes.
7. A dispersible graphite powder according to claim 1, characterized in that: the gelatinizing agent is one or a mixture of more than two of three PVA powders with the grain sizes of 3000 meshes, 1500 meshes and 6000 meshes.
8. A process for preparing a dispersible graphite powder according to any one of claims 1 to 7, characterized by comprising the steps of: (1) respectively weighing fumed alumina, superfine metal silicon powder, fumed silica and silicon resin powder, and fully mixing the raw materials in a mixer to prepare balance weight powder;
(2) weighing the flake graphite, the macromolecular dispersion binder, the weight powder and the gelling agent according to the proportion, and continuously and fully mixing the materials uniformly;
(3) and feeding the uniformly mixed raw materials into an air pipe and blowing the raw materials into a laser sintering device, forming the raw materials in a sintering area, and then feeding the raw materials into a cyclone separator for separation and screening to obtain the dispersible graphite.
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