CN114956829B - Silicon nitride combined silicon carbide brick for dry quenching chute and preparation method thereof - Google Patents
Silicon nitride combined silicon carbide brick for dry quenching chute and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silicon nitride combined silicon carbide brick for a coke dry quenching chute and a preparation method thereof, belonging to the technical field of preparation of silicon carbide bricks, wherein the silicon carbide brick comprises the following raw materials in percentage by weight: 10-20% of polysilicon waste slurry reclaimed material, 10-20% of metallic silicon, 1-5% of reinforcing agent, 0.1-0.6% of catalyst, 0.1-0.5% of sintering aid, 3-4% of bonding agent, 0.4-2% of adding agent and the balance of silicon carbide, and the preparation method comprises the following steps: s1-1, preparing materials; s1-2, mixing materials; s1-3, molding; s1-4, sintering; the waste polysilicon slurry is treated and recovered in green, and is fully deironized to obtain a high-purity mixture of metal silicon and silicon carbide, and the mixture is used as a raw material for preparing the silicon nitride-bonded silicon carbide brick, so that the production cost of the product is reduced, and the problem of environmental pollution caused by roughly treating the waste polysilicon is avoided.
Description
Technical Field
The invention relates to the technical field of preparation of silicon carbide bricks, in particular to a silicon nitride combined silicon carbide brick for a coke dry quenching chute and a preparation method thereof.
Background
The dry quenching furnace is energy-saving and environment-friendly equipment which encourages development and popularization in recent countries, compared with the traditional wet quenching, the dry quenching process has the advantages of greatly reducing environmental pollution, fully utilizing red Jiao Xianre, improving coke quality and the like, and the produced coke can effectively improve the benefit of a blast furnace when being used on the blast furnace. However, the running life of the dry quenching furnace in China is generally low, and the energy efficiency of the dry quenching furnace is seriously influenced by small repair in one year, middle repair in three years and major repair in five years. The chute area is the most critical and most damaged part in the dry quenching furnace, and the service condition of the refractory material of the part directly influences the service life of the whole dry quenching system.
In recent years, the silicon nitride-silicon carbide combined brick is used in a dry quenching chute area due to higher strength, wear resistance and thermal shock resistance, and the service life is prolonged to about 6 years, but the production cost is higher, and the silicon nitride-silicon carbide combined brick is difficult to popularize and apply in a large range. And because the size of the refractory bricks adopted in the dry quenching chute area is larger and thicker, and the shape is complex, in order to ensure the sufficient nitriding reaction, the nitriding reaction time at high temperature needs to be prolonged, and simultaneously, higher requirements are put on the performance of the nitriding kiln.
Under the influence of international policy, raw material prices of silicon carbide and metallic silicon are greatly increased, and supply is difficult to ensure. The waste polysilicon slurry is mainly composed of silicon carbide and metal silicon, responds to the national circulation economic policy, takes the reasonable utilization of resource recovery and changes waste into valuable, carries out green treatment and recovery on polysilicon waste, takes the mixture of silicon carbide and metal silicon after the recovery of the polysilicon waste as a raw material for producing silicon nitride combined silicon carbide bricks, reduces the manufacturing cost of the raw material, and has positive significance for environmental protection.
Disclosure of Invention
In order to solve the technical problems, the invention provides a silicon nitride combined silicon carbide brick for a dry quenching chute and a preparation method thereof.
The technical scheme of the invention is as follows: the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following raw materials in percentage by weight: 10-20% of polysilicon waste slurry reclaimed materials, 10-20% of metallic silicon, 1-5% of reinforcing agents, 0.1-0.6% of catalysts, 0.1-0.5% of sintering aids, 3-4% of binding agents, 0.4-2% of adding agents and the balance of silicon carbide;
the granularity of the silicon carbide is 1-3mm, 0.1-1mm and 240 meshes, the granularity of the polysilicon waste slurry recovery material is 15 mu m, the granularity of the metal silicon is 240 meshes and 325 meshes, the granularity of the reinforcing agent is 325 meshes, and the proportion of different granularities of the silicon carbide is as follows: 45-60% of 1-3mm, 18-28% of 0.1-1mm and 12-38% of < 0.1 mm.
The preparation method of the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following steps of:
s1-1, preparing materials:
proportioning the raw materials according to the weight percentage, mixing the proportioned polysilicon waste slurry recovery material, the additive, the catalyst and the sintering aid in a ball mill for 1-2 hours to obtain mixed powder, and mixing metal silicon with 240 meshes and 325 meshes according to the weight ratio of 1:1, mixing to obtain metal silicon fine powder, and then blending the ball-milled mixed powder, the well-proportioned 240-mesh silicon carbide fine powder and the metal silicon fine powder in a Raymond mill to obtain mixed fine powder, so as to ensure the distribution uniformity of various raw materials;
s1-2, mixing:
adding the proportioned silicon carbide with the granularity of 1-3mm and 0.1-1mm into a stirrer, stirring for 1-2min, adding the binding agent, stirring for 3-5min, adding the mixed fine powder obtained in the step S1, and stirring for 30-35min;
s1-3, molding:
according to the size of the brick of the silicon nitride combined silicon carbide brick, selecting a 630t-1000t friction press for press molding to obtain a press molded brick blank;
s1-4, sintering:
drying the pressed green bricks in a drying kiln for 24-48h, wherein the drying temperature of the drying kiln is 100-120 ℃, and then transferring the green bricks into a nitriding furnace for heat preservation for 6-10h, and the temperature of the nitriding furnace is 1400-1430 ℃ to obtain the silicon nitride combined silicon carbide bricks.
The preparation method of the polysilicon waste slurry recovery material comprises the following steps:
s2-1: adding dilute hydrochloric acid into the waste polysilicon slurry, wherein the concentration of the dilute hydrochloric acid is 4mol/L, and the weight ratio of the waste polysilicon slurry to the dilute hydrochloric acid is 88:3, fully stirring to obtain waste slurry, so that the waste slurry has good fluidity;
s2-2: heating the waste slurry obtained in the step S1 to 30-90 ℃ to obtain heated slurry;
s3-2: pumping the heated slurry obtained in the step S2 into a filter for solid-liquid separation to obtain a solid mixture A;
s3-4: and (3) performing superconducting magnetic separation on the solid mixture A obtained in the step (S3) to obtain a high-purity reclaimed material.
The reinforcing agent is alumina micropowder or a mixture of the alumina micropowder and yttrium oxide micropowder, so that the strength of the silicon carbide brick is enhanced.
The catalyst is nickel oxide micropowder, and the preparation method of the nickel oxide micropowder comprises the following steps:
s3-1: preparing a nickel nitrate hexahydrate solution with the concentration of 30mol/L, heating the nickel nitrate hexahydrate solution, simultaneously adding an ethylenediamine solution with the concentration of 25mol/L in the heating process, and fully stirring, wherein the volume ratio of the nickel nitrate hexahydrate solution to the ethylenediamine solution is 1:1, heating to 70-80 ℃, stirring for 10-20min, and cooling to room temperature to obtain a mixed solution B;
s3-2: magnetically stirring the mixed solution B in a special magnetic stirrer at the stirring speed of 60-80r/min, and adding a sodium hydroxide solution with the concentration of 33mol/L in the stirring process to obtain a precipitate C;
s3-3: filtering and washing the precipitate C to obtain a solid D;
s3-4: drying the solid D in a drying furnace for 8-12h at 75-85 ℃ to obtain nickel oxide micropowder after drying.
The sintering aid is nano silicon nitride, and the sintered silicon carbide brick has high strength and good quality.
The rotating speed of the Raymond mill in the step S1-1 is 140-180r/min, the blending time is 10-15min, the blending effect is good, and the efficiency is high.
The addition agent is prepared from tungsten oxide and aluminum powder according to the mass ratio of 1:1, the granularity of the tungsten oxide and the aluminum powder is 40-50 mu m, and the strength of the silicon carbide brick is enhanced.
The bonding agent in the step S1-2 is phenolic resin, the viscosity at 25 ℃ is 13000-14000mpa.s, the solid content is 85-90, the curing temperature is 180 ℃, the polymerization degree is 5-8, and the molecular mass is 10000-20000, so that the bonding agent has good use effect and meets the process requirements.
The magnetic field intensity of the superconducting magnetic separation in the step S3-4 is 4.5-6.5T, the flow velocity of the solid mixture A in the superconducting magnetic separation equipment is 8-14cm/S, and the magnetic separation efficiency is high.
The beneficial effects of the invention are as follows:
(1) The waste polysilicon slurry is treated and recovered in green, and is fully deironized to obtain a high-purity mixture of metal silicon and silicon carbide, and the mixture is used as a raw material for preparing the silicon nitride-bonded silicon carbide brick, so that the production cost of the product is reduced, and the problem of environmental pollution caused by roughly treating the waste polysilicon is avoided.
(2) Proper amount of alumina micropowder is added, and the alumina micropowder can react with silicon oxynitride and silicate glass phase in a substrate at high temperature to generate sialon phase, so that the sialon has the characteristics of high melting point, high steam oxidation resistance, high alkali corrosion resistance and the like, and the substrate bonding strength of a silicon nitride-bonded silicon carbide product is improved, and the wear resistance of the product is further improved.
(3) By adding a proper amount of yttrium oxide micro powder, the silicon nitride whisker generated by in-situ reaction can be in a long rod shape and interweaved around silicon carbide particles, and the compressive strength, the flexural strength and the thermal shock stability of the silicon nitride combined silicon carbide product can be obviously improved.
(4) The nickel oxide micropowder is used as a catalyst, so that the nitriding of metal silicon and the growth of silicon nitride whiskers can be promoted, the high-temperature flexural strength, oxidation resistance and erosion resistance of the material are improved, the sintering time required by combining silicon nitride with silicon carbide bricks can be shortened, and the manufacturing cost is reduced.
(5) The nano silicon nitride is adopted as the sintering aid, and has the characteristics of high surface energy, high activity, small particles and the like, so that the deposition probability of the new silicon nitride on the nano silicon nitride is accelerated, the nitriding rate of silicon powder is remarkably improved, the silicon nitride content of the silicon nitride combined silicon carbide product is improved, and the mechanical property and the uniformity of the tissue structure of the material are improved.
(6) Adopting a two-step premixing fine powder process, and ensuring the uniformity of distribution of the reinforcing agent, the catalyst and the sintering aid in the matrix; by controlling the mixing time, the matrix uniformly wraps the aggregate, so that the uniformity of the organization structure of the silicon nitride-combined silicon carbide product is ensured, and the performance of three additives is facilitated. The structural strength of the product can be improved by adopting a high-tonnage press for molding.
Drawings
FIG. 1 is a flow chart of the preparation of the silicon carbide brick of the present invention.
Detailed Description
Example 1:
the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following raw materials in percentage by weight: 18% of polysilicon waste slurry recovery material, 15.8% of metallic silicon, 1% of reinforcing agent, 0.1% of catalyst, 0.1% of sintering aid, 3% of bonding agent, 2% of adding agent and the balance of silicon carbide;
the granularity of the silicon carbide is 1-3mm, 0.1-1mm and 240 meshes, the granularity of the polysilicon waste slurry recovery material is 15 mu m, the granularity of the metal silicon is 240 meshes and 325 meshes, the granularity of the reinforcing agent is 325 meshes, and the proportion of different granularities of the silicon carbide is as follows: 45% of 1-3mm, 18% of 0.1-1mm and 37% of less than 0.1 mm.
The preparation method of the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following steps of:
s1-1, preparing materials:
proportioning the raw materials according to the weight percentage, mixing the proportioned polysilicon waste slurry recovery material, the additive, the catalyst and the sintering aid in a ball mill for 1h to obtain mixed powder, and mixing metal silicon with 240 meshes and 325 meshes according to the weight ratio of 1:1, mixing to obtain metal silicon fine powder, and then blending the ball-milled mixed powder, the well-proportioned 240-mesh silicon carbide fine powder and the metal silicon fine powder in a Raymond mill to obtain mixed fine powder, so as to ensure the distribution uniformity of various raw materials;
s1-2, mixing:
adding the proportioned silicon carbide with the granularity of 1-3mm and 0.1-1mm into a stirrer, stirring for 1min, adding the binding agent, stirring for 3min, adding the mixed fine powder obtained in the step S1, and stirring for 30min;
s1-3, molding:
according to the brick size of the silicon nitride combined silicon carbide brick, selecting a 630t friction press for press molding to obtain a press molded brick blank;
s1-4, sintering:
drying the pressed green bricks in a drying kiln for 24 hours, wherein the drying temperature of the drying kiln is 100 ℃, then transferring the green bricks into a nitriding furnace for heat preservation for 6 hours, and the temperature of the nitriding furnace is 1400 ℃ to obtain the silicon nitride combined silicon carbide bricks.
The preparation method of the polysilicon waste slurry recovery material comprises the following steps:
s2-1: adding dilute hydrochloric acid into the waste polysilicon slurry, wherein the concentration of the dilute hydrochloric acid is 4mol/L, and the weight ratio of the waste polysilicon slurry to the dilute hydrochloric acid is 88:3, fully stirring to obtain waste slurry, so that the waste slurry has good fluidity;
s2-2: heating the waste slurry obtained in the step S1 to 30 ℃ to obtain heated slurry;
s3-2: pumping the heated slurry obtained in the step S2 into a filter for solid-liquid separation to obtain a solid mixture A;
s3-4: and (3) performing superconducting magnetic separation on the solid mixture A obtained in the step (S3) to obtain a high-purity reclaimed material.
The reinforcing agent is alumina micropowder or a mixture of the alumina micropowder and yttrium oxide micropowder, so that the strength of the silicon carbide brick is enhanced.
The catalyst is nickel oxide micropowder, and the preparation method of the nickel oxide micropowder comprises the following steps:
s3-1: preparing a nickel nitrate hexahydrate solution with the concentration of 30mol/L, heating the nickel nitrate hexahydrate solution, simultaneously adding an ethylenediamine solution with the concentration of 25mol/L in the heating process, and fully stirring, wherein the volume ratio of the nickel nitrate hexahydrate solution to the ethylenediamine solution is 1:1, heating to 70 ℃, stirring for 10min, and cooling to room temperature to obtain a mixed solution B;
s3-2: magnetically stirring the mixed solution B in a special magnetic stirrer at the stirring speed of 60r/min, and adding a sodium hydroxide solution with the concentration of 33mol/L in the stirring process to obtain a precipitate C;
s3-3: filtering and washing the precipitate C to obtain a solid D;
s3-4: and drying the solid D in a drying furnace for 8 hours at the drying temperature of 75 ℃ to obtain the nickel oxide micro powder after the drying is completed.
The sintering aid is nano silicon nitride, and the sintered silicon carbide brick has high strength and good quality.
The rotating speed of the Raymond mill in the step S1-1 is 140r/min, the blending time is 10min, and the blending effect is good and the efficiency is high.
The addition agent is prepared from tungsten oxide and aluminum powder according to the mass ratio of 1:1, the granularity of the tungsten oxide and the aluminum powder is 40-50 mu m, and the strength of the silicon carbide brick is enhanced.
The bonding agent in the step S1-2 is phenolic resin, the viscosity is 13000mpa.s at 25 ℃, the solid content is 85, the curing temperature is 180 ℃, the polymerization degree is 5, the molecular mass is 10000, and the bonding agent has good use effect and meets the process requirements.
The magnetic field intensity of the superconducting magnetic separation in the step S3-4 is 4.5T, the flow velocity of the solid mixture A in the superconducting magnetic separation equipment is 8cm/S, and the magnetic separation efficiency is high.
The performance indexes of the silicon nitride combined silicon carbide product are as follows: the apparent porosity is 14.9 percent, and the volume density is 2.71g/cm 3 The normal temperature compressive strength is 223MPa, and the high temperature flexural strength (1200 ℃ C. Multiplied by 0.5 h) is 61MPa; the thermal shock stability (1100 ℃ C., water cooling) is 53 times; abrasion resistance of 2.09cm 3 。
Example 2:
the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following raw materials in percentage by weight: 14% of polysilicon waste slurry recovery material, 10% of metallic silicon, 4.3% of reinforcing agent, 0.4% of catalyst, 0.3% of sintering aid, 3.5% of bonding agent, 0.5% of adding agent and the balance of silicon carbide;
the granularity of the silicon carbide is 1-3mm, 0.1-1mm and 240 meshes, the granularity of the polysilicon waste slurry recovery material is 15 mu m, the granularity of the metal silicon is 240 meshes and 325 meshes, the granularity of the reinforcing agent is 325 meshes, and the proportion of different granularities of the silicon carbide is as follows: 1-3mm50%, 0.1-1mm20%, less than 0.1mm30%.
The preparation method of the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following steps of:
s1-1, preparing materials:
proportioning the raw materials according to the weight percentage, mixing the proportioned polysilicon waste slurry recovery material, the additive, the catalyst and the sintering aid in a ball mill for 1.5 hours to obtain mixed powder, and mixing metal silicon with 240 meshes and 325 meshes according to the weight ratio of 1:1, mixing to obtain metal silicon fine powder, and then blending the ball-milled mixed powder, the well-proportioned 240-mesh silicon carbide fine powder and the metal silicon fine powder in a Raymond mill to obtain mixed fine powder, so as to ensure the distribution uniformity of various raw materials;
s1-2, mixing:
adding the proportioned silicon carbide with the granularity of 1-3mm and 0.1-1mm into a stirrer, stirring for 1.5min, adding the binding agent, stirring for 4min, adding the mixed fine powder obtained in the step S1, and stirring for 32min;
s1-3, molding:
according to the brick size of the silicon nitride combined silicon carbide brick, selecting an 800t friction press for press molding to obtain a press molded brick blank;
s1-4, sintering:
drying the pressed green bricks in a drying kiln for 40 hours, wherein the drying temperature of the drying kiln is 110 ℃, then transferring the green bricks into a nitriding furnace for heat preservation for 8 hours, and the temperature of the nitriding furnace is 1420 ℃, thus obtaining the silicon nitride combined silicon carbide bricks.
The preparation method of the polysilicon waste slurry recovery material comprises the following steps:
s2-1: adding dilute hydrochloric acid into the waste polysilicon slurry, wherein the concentration of the dilute hydrochloric acid is 4mol/L, and the weight ratio of the waste polysilicon slurry to the dilute hydrochloric acid is 88:3, fully stirring to obtain waste slurry, so that the waste slurry has good fluidity;
s2-2: heating the waste slurry obtained in the step S1 to 50 ℃ to obtain heated slurry;
s3-2: pumping the heated slurry obtained in the step S2 into a filter for solid-liquid separation to obtain a solid mixture A;
s3-4: and (3) performing superconducting magnetic separation on the solid mixture A obtained in the step (S3) to obtain a high-purity reclaimed material.
The reinforcing agent is alumina micropowder or a mixture of the alumina micropowder and yttrium oxide micropowder, so that the strength of the silicon carbide brick is enhanced.
The catalyst is nickel oxide micropowder, and the preparation method of the nickel oxide micropowder comprises the following steps:
s3-1: preparing a nickel nitrate hexahydrate solution with the concentration of 30mol/L, heating the nickel nitrate hexahydrate solution, simultaneously adding an ethylenediamine solution with the concentration of 25mol/L in the heating process, and fully stirring, wherein the volume ratio of the nickel nitrate hexahydrate solution to the ethylenediamine solution is 1:1, heating to 75 ℃, stirring for 15min, and cooling to room temperature to obtain a mixed solution B;
s3-2: magnetically stirring the mixed solution B in a special magnetic stirrer at the stirring speed of 70r/min, and adding a sodium hydroxide solution with the concentration of 33mol/L in the stirring process to obtain a precipitate C;
s3-3: filtering and washing the precipitate C to obtain a solid D;
s3-4: and drying the solid D in a drying furnace for 10 hours at the drying temperature of 80 ℃ to obtain the nickel oxide micro powder after the drying is completed.
The sintering aid is nano silicon nitride, and the sintered silicon carbide brick has high strength and good quality.
The rotating speed of the Raymond mill in the step S1-1 is 150r/min, the blending time is 14min, and the blending effect and the efficiency are good.
The addition agent is prepared from tungsten oxide and aluminum powder according to the mass ratio of 1:1, the granularity of the tungsten oxide and the aluminum powder is 45 mu m, and the strength of the silicon carbide brick is enhanced.
The bonding agent in the step S1-2 is phenolic resin, the viscosity is 13200mpa.s at 25 ℃, the solid content is 88, the curing temperature is 180 ℃, the polymerization degree is 6, the molecular mass is 15000, and the bonding agent has good use effect and meets the process requirement.
The magnetic field intensity of the superconducting magnetic separation in the step S3-4 is 5.5T, the flow velocity of the solid mixture A in the superconducting magnetic separation equipment is 10cm/S, and the magnetic separation efficiency is high.
The performance indexes of the silicon nitride combined silicon carbide product are as follows: the apparent porosity is 14.97%, and the volume density is 2.72g/cm 3 Normal temperature pressure resistanceThe degree is 236MPa, and the high-temperature flexural strength (1200 ℃ C. Multiplied by 0.5 h) is 64MPa; the thermal shock stability (1100 ℃ C., water cooling) is 55 times; abrasion resistance of 2.07cm 3 。
Example 3:
the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following raw materials in percentage by weight: 10% of polysilicon waste slurry recovery material, 10% of metallic silicon, 1% of reinforcing agent, 0.1% of catalyst, 0.1% of sintering aid, 3% of bonding agent, 0.8% of adding agent and the balance of silicon carbide;
the granularity of the silicon carbide is 1-3mm, 0.1-1mm and 240 meshes, the granularity of the polysilicon waste slurry recovery material is 15 mu m, the granularity of the metal silicon is 240 meshes and 325 meshes, the granularity of the reinforcing agent is 325 meshes, and the proportion of different granularities of the silicon carbide is as follows: 60% of 1-3mm, 18% of 0.1-1mm and 22% of less than 0.1 mm.
The preparation method of the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following steps of:
s1-1, preparing materials:
proportioning the raw materials according to the weight percentage, mixing the proportioned polysilicon waste slurry recovery material, the additive, the catalyst and the sintering aid in a ball mill for 2 hours to obtain mixed powder, and mixing metal silicon with 240 meshes and 325 meshes according to the weight ratio of 1:1, mixing to obtain metal silicon fine powder, and then blending the ball-milled mixed powder, the well-proportioned 240-mesh silicon carbide fine powder and the metal silicon fine powder in a Raymond mill to obtain mixed fine powder, so as to ensure the distribution uniformity of various raw materials;
s1-2, mixing:
adding the proportioned silicon carbide with the granularity of 1-3mm and 0.1-1mm into a stirrer, stirring for 1-2min, adding the binding agent, stirring for 5min, adding the mixed fine powder obtained in the step S1, and stirring for 35min;
s1-3, molding:
selecting a 1000t friction press for press molding according to the brick size of the silicon nitride combined silicon carbide brick to obtain a press molded brick blank;
s1-4, sintering:
drying the pressed green bricks in a drying kiln for 48 hours, wherein the drying temperature of the drying kiln is 120 ℃, and then transferring the green bricks into a nitriding furnace for heat preservation for 10 hours, and the temperature of the nitriding furnace is 1430 ℃ to obtain the silicon nitride combined silicon carbide bricks.
The preparation method of the polysilicon waste slurry recovery material comprises the following steps:
s2-1: adding dilute hydrochloric acid into the waste polysilicon slurry, wherein the concentration of the dilute hydrochloric acid is 4mol/L, and the weight ratio of the waste polysilicon slurry to the dilute hydrochloric acid is 88:3, fully stirring to obtain waste slurry, so that the waste slurry has good fluidity;
s2-2: heating the waste slurry obtained in the step S1 to 90 ℃ to obtain heated slurry;
s3-2: pumping the heated slurry obtained in the step S2 into a filter for solid-liquid separation to obtain a solid mixture A;
s3-4: and (3) performing superconducting magnetic separation on the solid mixture A obtained in the step (S3) to obtain a high-purity reclaimed material.
The reinforcing agent is alumina micropowder or a mixture of the alumina micropowder and yttrium oxide micropowder, so that the strength of the silicon carbide brick is enhanced.
The catalyst is nickel oxide micropowder, and the preparation method of the nickel oxide micropowder comprises the following steps:
s3-1: preparing a nickel nitrate hexahydrate solution with the concentration of 30mol/L, heating the nickel nitrate hexahydrate solution, simultaneously adding an ethylenediamine solution with the concentration of 25mol/L in the heating process, and fully stirring, wherein the volume ratio of the nickel nitrate hexahydrate solution to the ethylenediamine solution is 1:1, heating to 80 ℃, stirring for 20min, and cooling to room temperature to obtain a mixed solution B;
s3-2: magnetically stirring the mixed solution B in a special magnetic stirrer at the stirring speed of 80r/min, and adding a sodium hydroxide solution with the concentration of 33mol/L in the stirring process to obtain a precipitate C;
s3-3: filtering and washing the precipitate C to obtain a solid D;
s3-4: drying the solid D in a drying furnace for 8-12h at 85 ℃ to obtain nickel oxide micropowder after drying.
The sintering aid is nano silicon nitride, and the sintered silicon carbide brick has high strength and good quality.
The rotating speed of the Raymond mill in the step S1-1 is 180r/min, the blending time is 15min, and the blending effect and the efficiency are good.
The addition agent is prepared from tungsten oxide and aluminum powder according to the mass ratio of 1:1, the granularity of the tungsten oxide and the aluminum powder is 50 mu m, and the strength of the silicon carbide brick is enhanced.
The bonding agent in the step S1-2 is phenolic resin, the viscosity is 14000mpa.s at 25 ℃, the solid content is 90, the curing temperature is 180 ℃, the polymerization degree is 8, the molecular mass is 20000, the bonding agent has good use effect, and the process requirement is met.
The magnetic field intensity of the superconducting magnetic separation in the step S3-4 is 6.5T, the flow velocity of the solid mixture A in the superconducting magnetic separation equipment is 14cm/S, and the magnetic separation efficiency is high.
The performance indexes of the silicon nitride combined silicon carbide product are as follows: the apparent porosity is 14.93 percent, and the volume density is 2.74g/cm 3 The normal temperature compressive strength is 255MPa, and the high temperature flexural strength (1200 ℃ C. Multiplied by 0.5 h) is 65MPa; the thermal shock stability (1100 ℃ C., water cooling) is 60 times; abrasion resistance of 2.0cm 3 。
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (3)
1. The silicon nitride combined silicon carbide brick for the dry quenching chute is characterized by comprising the following raw materials in percentage by weight: 10-20% of polysilicon waste slurry reclaimed materials, 10-20% of metallic silicon, 1-5% of reinforcing agents, 0.1-0.6% of catalysts, 0.1-0.5% of sintering aids, 3-4% of binding agents, 0.4-2% of adding agents and the balance of silicon carbide;
the granularity of the silicon carbide is 1-3mm, 0.1-1mm and 240 meshes, the granularity of the polysilicon waste slurry recovery material is 15 mu m, the granularity of the metal silicon is 240 meshes and 325 meshes, the granularity of the reinforcing agent is 325 meshes, and the proportion of different granularities of the silicon carbide is as follows: 45-60% of 1-3mm, 18-28% of 0.1-1mm and 12-38% of < 0.1 mm;
the preparation method of the silicon nitride combined silicon carbide brick for the dry quenching chute comprises the following steps:
s1-1, preparing materials:
proportioning the raw materials according to the weight percentage, mixing the proportioned polysilicon waste slurry recovery material, the additive, the catalyst and the sintering aid in a ball mill for 1-2 hours to obtain mixed powder, and mixing metal silicon with 240 meshes and 325 meshes according to the weight ratio of 1:1, mixing to obtain metal silicon fine powder, and then blending the ball-milled mixed powder with the mixed 240-mesh silicon carbide fine powder and the metal silicon fine powder in a Raymond mill to obtain mixed fine powder;
s1-2, mixing:
adding the proportioned silicon carbide with the granularity of 1-3mm and 0.1-1mm into a stirrer, stirring for 1-2min, adding the binding agent, stirring for 3-5min, adding the mixed fine powder obtained in the step S1, and stirring for 30-35min;
s1-3, molding:
according to the size of the brick of the silicon nitride combined silicon carbide brick, selecting a 630t-1000t friction press for press molding to obtain a press molded brick blank;
s1-4, sintering:
drying the pressed green bricks in a drying kiln for 24-48h, wherein the drying temperature of the drying kiln is 100-120 ℃, and then transferring the green bricks into a nitriding furnace for heat preservation for 6-10h, and the temperature of the nitriding furnace is 1400-1430 ℃ to obtain silicon nitride combined silicon carbide bricks;
the preparation method of the polysilicon waste slurry recovery material comprises the following steps:
s2-1: adding dilute hydrochloric acid into the waste polysilicon slurry, wherein the concentration of the dilute hydrochloric acid is 4mol/L, and the weight ratio of the waste polysilicon slurry to the dilute hydrochloric acid is 88:3, fully stirring to obtain waste slurry, so that the slurry has good fluidity;
s2-2: heating the waste slurry obtained in the step S1 to 30-90 ℃ to obtain heated slurry;
s3-2: pumping the heated slurry obtained in the step S2 into a filter for solid-liquid separation to obtain a solid mixture A;
s3-4: performing superconducting magnetic separation on the solid mixture A obtained in the step S3 to obtain a high-purity reclaimed material;
the reinforcing agent is alumina micropowder or a mixture of alumina micropowder and yttrium oxide micropowder;
the catalyst is nickel oxide micropowder, and the preparation method of the nickel oxide micropowder comprises the following steps:
s3-1: preparing a nickel nitrate hexahydrate solution with the concentration of 30mol/L, heating the nickel nitrate hexahydrate solution, simultaneously adding an ethylenediamine solution with the concentration of 25mol/L in the heating process, and fully stirring, wherein the volume ratio of the nickel nitrate hexahydrate solution to the ethylenediamine solution is 1:1, heating to 70-80 ℃, stirring for 10-20min, and cooling to room temperature to obtain a mixed solution B;
s3-2: magnetically stirring the mixed solution B in a special magnetic stirrer at the stirring speed of 60-80r/min, and adding a sodium hydroxide solution with the concentration of 33mol/L in the stirring process to obtain a precipitate C;
s3-3: filtering and washing the precipitate C to obtain a solid D;
s3-4: drying the solid D in a drying furnace for 8-12h at 75-85 ℃ to obtain nickel oxide micro powder after drying;
the sintering aid is nano silicon nitride;
the rotating speed of the Raymond mill in the step S1-1 is 140-180r/min, and the blending time is 10-15min;
the addition agent is prepared from tungsten oxide and aluminum powder according to the mass ratio of 1:1, wherein the granularity of the tungsten oxide and the aluminum powder is 40-50 mu m.
2. A silicon nitride bonded silicon carbide brick for a dry quenching chute as claimed in claim 1 wherein the bonding agent in step S1-2 is a phenolic resin.
3. The silicon nitride-bonded silicon carbide brick for a dry quenching chute according to claim 1, wherein the magnetic field strength of the superconducting magnetic separation in the step S3-4 is 4.5-6.5T, and the flow rate of the solid mixture a in the superconducting magnetic separation equipment is 8-14cm/S.
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