CN110372399A

CN110372399A - A kind of preparation method of the low magnesia carbon brick of resistance to compression for building

Info

Publication number: CN110372399A
Application number: CN201910505791.6A
Authority: CN
Inventors: 苏成康
Original assignee: Individual
Current assignee: Individual
Priority date: 2019-06-12
Filing date: 2019-06-12
Publication date: 2019-10-25

Abstract

The invention discloses a kind of preparation methods of the low magnesia carbon brick of resistance to compression for building, belong to building material technical field.The present invention crushes rice hull cellulose, and sieving obtains pretreatment rice hull cellulose；Rice hull cellulose will be pre-processed, biogas slurry, nutrient solution, water mixed fermentation is subsequently added into ferric chloride solution and sodium fluoride, it is stirred, ammonium hydroxide is then added dropwise and adjusts pH to 5.6~5.8, filters, freezes, crushes, the sieve of 220 mesh is crossed, it is dry, it heats up step by step, carbonizes, obtain modified rice hull cellulose；According to parts by weight, by 80~100 parts of electric-melting magnesium slags, 10~20 parts of modified rice hull celluloses, 10~20 parts of pre-dispersed graphene oxides, 8~10 parts of low-melting alloys, 10~20 parts of thermosetting resins, 1~2 part of curing agent, 0.1~0.2 part of fluxing agent mixing, injection molding, compression moulding, baking-curing, discharging is to get the low magnesia carbon brick of resistance to compression for building.The low magnesia carbon brick of resistance to compression for building provided by the invention has excellent mechanical property.

Description

A kind of preparation method of the low magnesia carbon brick of resistance to compression for building

Technical field

The invention discloses a kind of preparation methods of the low magnesia carbon brick of resistance to compression for building, belong to building material technical field.

Background technique

With the development of steel and iron industry, the smelting ratio of ultra-low-carbon steel is continuously increased.To solve traditional magnesia carbon brick thermal losses Carburetting problem big and to molten steel, low carbon magnesia carbon brick are increasingly becoming the hot spot of people's research.But with the reduction of carbon content, material High-temperature behavior also decline, wherein impacted most notably material thermal shock resistance and resistance to slag reduce.It is well known that magnesium carbon After carbon content reduces in brick, the thermal conductivity of brick can be made to decline, elasticity modulus increases, so that brick thermal shock resistance be made to be deteriorated；In addition, After carbon content reduces, the wetability of slag and molten steel and material can also enhanced, the permeability of material anti-slag and molten steel is deteriorated.

Due to graphite and clinker is nonwetting and graphite has good thermal conductivity, makes magnesia carbon brick that there is excellent anti-slag to invade Erosion and thermal shock resistance energy and be widely used in STEELMAKING PRODUCTION.Magnesia carbon brick has excellent resistance to slag corrosion, comparatively ideal Thermal shock resistance, heat conductivity and dense structure's property, the steelmaking converter that is widely used, electric furnace and ladle refining furnace and ladle slag On line.Additive is added in magnesia carbon brick can effectively prevent oxidation of coal, and be conducive to improve the applied at elevated temperature of refractory material Performance.The effect of additive is divided into two aspects: being on the one hand from thermodynamics, i.e., at the working temperature, additive Or the affinity of the product and oxygen of additive and carbon reaction is bigger than the affinity of carbon and oxygen, prior to being oxidized, to rise To the effect of protection carbon；It on the other hand is additive and O from the viewpoint of dynamics₂, CO or C reaction generate chemical combination The microstructure that object can change material such as increases consistency, blocks stomata, hinders O₂And diffusion of reaction product etc..

Currently, there are two main classes: metal or alloy fine powder for common magnesia carbon brick additive；Nonmetallic fine powder.The gold of addition Belonging to fine powder mainly has Al, Si, Mg, Ca etc., and wherein Al, Si are most commonly seen.During heat treatment, Al and Si can be sent out in the material The carbon content of raw reaction but traditional magnesia carbon brick generally all between 10%~20%, finds exist during long-term practical application Following problem: 1. since high heat conductance increases thermal losses, therefore tapping temperature is improved, brings energy consumption to increase, while increasing resistance to A series of problems, such as erosion of fiery material；2. smelting high quality clean steel such as in VOD as the furnace lining material of special refining furnace And when ultra-low-carbon steel, carburetting problem can be caused；3. a large amount of valuable graphite resources of consumption；4. with clean steel, mild steel is smelted With the increase of ultra-low-carbon steel kind ratio, the problem of magnesia carbon brick is contaminated molten steel molten steel recarburization, becomes increasingly severe, Therefore its carbon content must be reduced to reduce the pollution to molten steel.In view of the above circumstances, in recent years, refined steel ladles low-carbon amount, property Attention of the exploitation of low carbon magnesia carbon brick that can be excellent by social related industry, becomes the new development focus of magnesia-carbon refractory material. The low magnesia carbon brick traditional at present problem bad there is also mechanical property, therefore also need to study it.

Summary of the invention

The present invention solves the technical problem of: for the bad problem of the low magnesia carbon brick mechanical property of tradition, provide A kind of preparation method of the low magnesia carbon brick of resistance to compression for building.

In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:

(1) rice hull cellulose is crushed, crosses the sieve of 80 mesh, obtains pretreatment rice hull cellulose；

(2) according to parts by weight, by 10~20 parts of pretreatment rice hull celluloses, 1~2 part of biogas slurry, 1~2 portion of nutrient solution, 20~30 parts Water mixed fermentation is subsequently added into the ferric chloride solution and pretreatment rice hull cellulose matter of 0.2~0.3 times of rice hull cellulose quality of pretreatment The sodium fluoride of 0.02~0.03 times of amount, is stirred, and ammonium hydroxide is then added dropwise and adjusts pH to 5.6~5.8, filters, freezes, crushes, The sieve of 220 mesh is crossed, it is dry, it heats up step by step, carbonizes, obtain modified rice hull cellulose；

(3) according to parts by weight, by 80~100 parts of electric-melting magnesium slags, 10~20 parts of modified rice hull celluloses, 10~20 parts of pre-dispersed oxygen Graphite alkene, 8~10 parts of low-melting alloys, 10~20 parts of thermosetting resins, 1~2 part of curing agent, 0.1~0.2 part of fluxing agent are mixed It closes, injection molding, compression moulding, baking-curing, discharges to get the low magnesia carbon brick of resistance to compression for building.

Step (2) described nutrient solution is made of the raw material of following parts by weight: 2~3 parts of glucose, 1~2 part of glycerol, and 1 ~2 parts of polyethylene glycol, 20~30 parts of water.

The preparation process of step (3) the pre-dispersed graphene oxide are as follows: in mass ratio by graphene oxide and gelatin solution 1:20~1:30 mixing is then added dropwise ammonium hydroxide and adjusts pH to 8.3~8.6, and mixing ultrasound filters, and washing obtains pre-dispersed oxidation stone Black alkene.

Step (3) low-melting alloy is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51% (ω), tin account for 30%(ω), lead accounts for 8%(ω), indium accounts for 11%(ω).

Step (3) thermosetting resin is appointing in phenolic resin 2123, phenolic resin 2127 or phenolic resin 2130 It anticipates one kind.

Step (3) curing agent is hexa, any one in butyl acrylate or methyl methacrylate Kind.

Step (3) described fluxing agent is made of the raw material of following parts by weight: 40~50 parts of boraxs, 10~15 parts of oxidations Boron, 8~10 parts of sodium carbonate.

The modified carbon fiber aeroge of pretreatment rice hull cellulose quality 8~15% can also be added in step (2) described water； The preparation process of the modified carbon fiber aeroge are as follows:

(1) according to parts by weight, successively take 8~10 parts of isoelectric points be 6.0~6.5 gelatin, 1~3 part of sodium metaperiodate, 100~ 150 parts of deionized waters after gelatin and water are first mixed 6~8h of swelling, add sodium metaperiodate, and heating stirring reaction obtains modification Gelatin dispersion liquid；

(2) according to parts by weight, 4~6 parts of short fibres of carbon fiber, 100~150 parts of modified gelatin dispersion liquids, ultrasonic disperse are successively taken Afterwards, heating stirring is reacted, then through vacuum freeze drying, obtains modified carbon fiber aeroge；The short fine selection length of the carbon fiber is 6 ~12mm, the short fibre of carbon fiber that diameter is 6~8 μm.

The beneficial effects of the present invention are:

(1) present invention is by adding modified rice hull cellulose, firstly, during the fermentation, being decomposed using the enzyme that microorganism generates pre- Part organic matter in rice hull cellulose is handled, so that interfibrous bond strength reduces, is conducive to fiber in subsequent processes It is discrete, meanwhile, the hole that part organic matter leaves after being etched proposes the permeance property pre-processed inside rice hull cellulose It rises, then, by addition ferric chloride solution, iron ion is introduced into system, since the permeance property of rice hull cellulose gets a promotion, So iron ion good can penetrate into system, then adjust pH by the way that ammonium hydroxide is added dropwise so that the iron in rice hull cellulose from Son precipitating, and once have sediment Crystallization, it can be adsorbed and fix by the pore structure of rice hull cellulose, avoid sediment crystal Further grow up and reunite, so that its size is maintained at nanoscale；Then, by freezing, so that rice hull cellulose iuntercellular is formed Ice crystal is then passed through ball milling, under the action of the friction of the nanoprecipitation object nucleus of ice crystal and hard, so that fiber hydrolization Cheng Wei Nanoscale fibrous crystal palpus；

(2) technical solution of the present invention utilizes during high temperature carbonization, as the temperature of system is gradually increasing, in rice hull cellulose Ferric hydroxide precipitate dehydration generates nano iron oxide, meanwhile, rice hull cellulose charing occurs, but rice hull cellulose surface horny The obstruction of silica silicrete, so that fibrous crystal beard and hair gives birth to helix-coil, as system temperature continues to increase, the charcoal in system The iron oxide in system is enabled to be reduced into nano simple substance iron, under the catalytic action of elemental iron powder and sodium fluoride, fibrous crystal Charcoal qualitative response in the silica and system on palpus surface, generates silicon carbide skeleton, makes carbonaceous skeleton and surface silica dioxide shape At chemical bonding, so that the mechanical property of modified rice hull cellulose gets a promotion, when adding modified rice hull cellulose, due to helical form Structure good lubricating action is played in system in mixing process so that each component in system uniformly divides It dissipates, enables brick body uniform stressed, so that the mechanical property of system gets a promotion, it is spiral helicine after brick body molding Modified rice hull cellulose can form good mechanical snap with matrix, meanwhile, there are hard silicon carbide skeletons on surface, thus So that the further promotion of the mechanical property of system.

Specific embodiment

According to parts by weight, successively take 8~10 parts of isoelectric points be 6.0~6.5 gelatin, 1~3 part of sodium metaperiodate, 100~ 150 parts of deionized waters after gelatin and water are first mixed 6~8h of swelling, add sodium metaperiodate, and heating stirring reaction obtains modification Gelatin dispersion liquid；According to parts by weight, 4~6 parts of short fibres of carbon fiber, 100~150 parts of modified gelatin dispersion liquids, ultrasound are successively taken After dispersion, heating stirring reaction, then through vacuum freeze drying, obtain modified carbon fiber aeroge；Short fine select of the carbon fiber is grown Degree is 6~12mm, the short fibre of carbon fiber that diameter is 6~8 μm；According to parts by weight, by 2~3 parts of glucose, 1~2 part of glycerol, 1 ~2 parts of polyethylene glycol, 20~30 parts of water are placed in No. 1 beaker, and No. 1 beaker is placed in digital display and is tested the speed constant temperature blender with magnetic force In, it is 30~35 DEG C in temperature, under the conditions of revolving speed is 300~500r/min, heating stirring mixes 40~60min, obtains nutrient solution； Gelatin and water 1:50~1:100 in mass ratio are placed in No. 2 beakers, stir 10~20min with glass bar, stand swelling 3~ No. 2 beakers are then placed in digital display and tested the speed in constant temperature blender with magnetic force by 5h, are 80~85 DEG C in temperature, and revolving speed is 300~ Under the conditions of 500r/min, heating stirring dissolves 40~60min to get gelatin solution；In mass ratio by graphene oxide and gelatin solution 1:20~1:30 is placed in No. 3 beakers, and the ammonium hydroxide that mass fraction is 20~30% is then added dropwise into No. 3 beakers and adjusts pH to 8.3 ~8.6, then No. 3 beakers are placed in ultrasonic disperse instrument, under the conditions of supersonic frequency is 55~75kHz, mixing ultrasound 40~ After 60min, dispersion liquid is obtained, then filters dispersion liquid, obtain filter cake, is then obtained pre- Washing of Filter Cake 5~8 times with deionized water Disperse graphene oxide；Rice hull cellulose is placed in pulverizer and is crushed, the sieve of 80 mesh is crossed, obtains pretreatment rice hull cellulose；By weight Number meter, by 10~20 parts of pretreatment rice hull celluloses, 1~2 part of biogas slurry, 1~2 portion of nutrient solution, 20~30 parts of water are placed in fermentation cauldron In, and be added pretreatment rice hull cellulose quality 8~15% carbon fiber aeroge, in temperature be 30~35 DEG C, revolving speed be 100~ Under the conditions of 200r/min, mixed fermentation 3~5 days, 0.2~0.3 times of rice hull cellulose quality of pretreatment is then added into fermentation cauldron The sodium fluoride of 0.02~0.03 times of rice hull cellulose quality of ferric chloride solution and pretreatment that mass fraction is 10~20%, in revolving speed Under the conditions of 200~300r/min, it is stirred 40~60min, it is 20~30% that mass fraction is then added dropwise into fermentation cauldron Ammonium hydroxide adjusts pH to 5.6~5.8, obtains fermentation mixed liquor, then filters fermentation mixed liquor, filter residue is then placed in liquid by filter residue It is freezed in nitrogen, obtains frozen block, then frozen block is placed in pulverizer and is crushed, crossed the sieve of 220 mesh, crushed material is obtained, then by powder Particle is placed in baking oven, dry to constant weight under the conditions of temperature is 105~110 DEG C, obtains xeraphium particle, then by drying and crushing Material is placed in retort, and nitrogen is filled with into furnace with the rate of 60~90mL/min, then with the heating speed of 8~10 DEG C/min Rate in-furnace temperature rises to 1400~1600 DEG C, under the conditions of temperature is 1400~1600 DEG C, carbonizes 2~3h, it is fine to obtain modified rice husk Dimension；According to parts by weight, by 80~100 parts of electric-melting magnesium slags, 10~20 parts of modified rice hull celluloses, 10~20 parts of pre-dispersed oxidation stones Black alkene, 8~10 parts of low-melting alloys, 10~20 parts of thermosetting resins, 1~2 part of curing agent, 0.1~0.2 part of fluxing agent are placed in and stir It mixes in machine, under the conditions of revolving speed is 100~200r/min, is stirred 40~60min, obtains mixed slurry, sprayed to die surface Methyl-silicone oil is spilt, then injects mixed slurry in mold, under the conditions of pressure is 200~300MPa, after compression moulding, Yu Wen Under the conditions of degree is 230~260 DEG C, heat preservation solidification 12~for 24 hours, it demoulds, discharging, cooled to room temperature is to get resistance to compression for building Low magnesia carbon brick.The low-melting alloy is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for 30%(ω), lead accounts for 8%(ω), indium accounts for 11%(ω).The thermosetting resin is phenolic resin 2123, phenolic resin 2127 or phenol Any one in urea formaldehyde 2130.The curing agent is hexa, in butyl acrylate or methyl methacrylate Any one.The fluxing agent is made of the raw material of following parts by weight: 40~50 parts of boraxs, 10~15 parts of boron oxides, and 8 ~10 parts of sodium carbonate.

Example 1

According to parts by weight, successively taking 10 parts of isoelectric points is 6.5 gelatin, and 3 parts of sodium metaperiodates, 150 parts of deionized waters first will be bright After glue and water mixing are swollen 8h, sodium metaperiodate is added, heating stirring reaction obtains modified gelatin dispersion liquid；According to parts by weight, Successively take 6 parts of short fibres of carbon fiber, 150 parts of modified gelatin dispersion liquids, after ultrasonic disperse, heating stirring reaction, then through vacuum refrigeration It is dry, obtain modified carbon fiber aeroge；The short fine selection length of the carbon fiber is 6mm, the short fibre of carbon fiber that diameter is 6 μm；It presses Parts by weight meter, by 3 parts of glucose, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of water are placed in No. 1 beaker, and No. 1 beaker is set Test the speed in constant temperature blender with magnetic force in digital display, in temperature be 35 DEG C, under the conditions of revolving speed is 500r/min, heating stirring mixing 60min obtains nutrient solution；Gelatin and water 1:100 in mass ratio are placed in No. 2 beakers, 20min is stirred with glass bar, stands molten No. 2 beakers are then placed in digital display and tested the speed in constant temperature blender with magnetic force by swollen 5h, are 85 DEG C in temperature, revolving speed is 500r/min item Under part, heating stirring dissolves 60min to get gelatin solution；Graphene oxide and gelatin solution 1:30 in mass ratio are placed in No. 3 beakers In, the ammonium hydroxide that mass fraction is 30% is then added dropwise into No. 3 beakers and adjusts pH to 8.6, then No. 3 beakers are placed in ultrasonic disperse In instrument, under the conditions of supersonic frequency is 75kHz, after mixing ultrasound 60min, dispersion liquid is obtained, then filters dispersion liquid, must be filtered Cake then obtains pre-dispersed graphene oxide for Washing of Filter Cake 8 times with deionized water；Rice hull cellulose is placed in pulverizer and is crushed, The sieve for crossing 80 mesh obtains pretreatment rice hull cellulose；According to parts by weight, by 20 parts of pretreatment rice hull celluloses, 2 parts of biogas slurries, 2 parts of nutrition Liquid, 30 parts of water are placed in fermentation cauldron, and be added pretreatment rice hull cellulose quality 15% carbon fiber aeroge, in temperature be 35 DEG C, Under the conditions of revolving speed is 200r/min, mixed fermentation 5 days, pretreatment 0.3 times of matter of rice hull cellulose quality is then added into fermentation cauldron Measure 0.03 times of rice hull cellulose quality of the sodium fluoride of ferric chloride solution and pretreatment that score is 20%, in revolving speed be 300r/min item Under part, it is stirred 60min, the ammonium hydroxide that mass fraction is 30% is then added dropwise into fermentation cauldron and adjusts pH to 5.8, must ferment mixed Liquid is closed, is then filtered fermentation mixed liquor, filter residue is then placed in liquid nitrogen and freezes by filter residue, frozen block is obtained, then by frozen block Be placed in pulverizer and crush, cross 220 mesh sieve, obtain crushed material, then crushed material be placed in baking oven, in temperature be 110 DEG C of items It is dry to constant weight under part, obtain xeraphium particle, then xeraphium particle is placed in retort, and with the rate of 90mL/min to It is filled with nitrogen in furnace, then rises to 1600 DEG C with the heating rate in-furnace temperature of 10 DEG C/min, under the conditions of temperature is 1600 DEG C, 3h is carbonized, modified rice hull cellulose is obtained；According to parts by weight, by 100 parts of electric-melting magnesium slags, 20 parts of modified rice hull celluloses, 20 parts are divided in advance Scattered graphene oxide, 10 parts of low-melting alloys, 20 parts of thermosetting resins, 2 parts of curing agent, 0.2 part of fluxing agent are placed in blender, Under the conditions of revolving speed is 200r/min, it is stirred 60min, obtains mixed slurry, spray methyl-silicone oil to die surface, then will Mixed slurry injects in mold, and under the conditions of pressure is 300MPa, after compression moulding, under the conditions of temperature is 260 DEG C, heat preservation is solid Change for 24 hours, demould, discharging, cooled to room temperature is to get the low magnesia carbon brick of resistance to compression for building.The low-melting alloy is the conjunction of bismuth tin Gold, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for 30%(ω), lead accounts for 8%(ω), indium accounts for 11%(ω). The thermosetting resin is phenolic resin 2123.The curing agent is hexa.The fluxing agent is by following weight The raw material of number forms: 50 parts of boraxs, 15 parts of boron oxides, 10 parts of sodium carbonate.

Example 2

According to parts by weight, by 3 parts of glucose, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of water are placed in No. 1 beaker, and by No. 1 Beaker is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 500r/min, heating stirring is mixed 60min is closed, nutrient solution is obtained；Gelatin and water 1:100 in mass ratio are placed in No. 2 beakers, 20min is stirred with glass bar, stands Be swollen 5h, No. 2 beakers be then placed in digital display and are tested the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, revolving speed 500r/min Under the conditions of, heating stirring dissolves 60min to get gelatin solution；Graphene oxide and gelatin solution 1:30 in mass ratio are placed in No. 3 burnings In cup, the ammonium hydroxide that mass fraction is 30% is then added dropwise into No. 3 beakers and adjusts pH to 8.6, then No. 3 beakers are placed in ultrasound point It dissipates in instrument, under the conditions of supersonic frequency is 75kHz, after mixing ultrasound 60min, obtains dispersion liquid, then filter dispersion liquid, must filter Cake then obtains pre-dispersed graphene oxide for Washing of Filter Cake 8 times with deionized water；According to parts by weight, by 100 parts of electric-melting magnesiums Slag, 20 parts of rice hull celluloses, 20 parts of pre-dispersed graphene oxides, 10 parts of low-melting alloys, 20 parts of thermosetting resins, 2 parts of curing agent, 0.2 part of fluxing agent is placed in blender, under the conditions of revolving speed is 200r/min, is stirred 60min, is obtained mixed slurry, Xiang Mo Have surface and spray methyl-silicone oil, then injects mixed slurry in mold, under the conditions of pressure is 300MPa, after compression moulding, Under the conditions of temperature is 260 DEG C, heat preservation solidification for 24 hours, is demoulded, and discharging, cooled to room temperature is to get the low magnesium carbon of resistance to compression for building Brick.The low-melting alloy is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for 30% (ω), lead account for 8%(ω), indium accounts for 11%(ω).The thermosetting resin is phenolic resin 2123.The curing agent is hexa-methylene Tetramine.The fluxing agent is made of the raw material of following parts by weight: 50 parts of boraxs, 15 parts of boron oxides, 10 parts of sodium carbonate.

Example 3

According to parts by weight, by 3 parts of glucose, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of water are placed in No. 1 beaker, and by No. 1 Beaker is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 500r/min, heating stirring is mixed 60min is closed, nutrient solution is obtained；Gelatin and water 1:100 in mass ratio are placed in No. 2 beakers, 20min is stirred with glass bar, stands Be swollen 5h, No. 2 beakers be then placed in digital display and are tested the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, revolving speed 500r/min Under the conditions of, heating stirring dissolves 60min to get gelatin solution；Rice hull cellulose is placed in pulverizer and is crushed, the sieve of 80 mesh is crossed, obtains Pre-process rice hull cellulose；According to parts by weight, by 20 parts of pretreatment rice hull celluloses, 2 parts of biogas slurries, 2 portions of nutrient solutions, 30 parts of water are placed in In fermentation cauldron, it is 35 DEG C in temperature, under the conditions of revolving speed is 200r/min, mixed fermentation 5 days, pre- place is then added into fermentation cauldron Manage the fluorination of 0.03 times of rice hull cellulose quality of the ferric chloride solution that 0.3 times of mass fraction of rice hull cellulose quality is 20% and pretreatment Sodium is stirred 60min under the conditions of revolving speed is 300r/min, and the ammonium hydroxide that mass fraction is 30% is then added dropwise into fermentation cauldron PH to 5.8 is adjusted, fermentation mixed liquor is obtained, then filters fermentation mixed liquor, filter residue is then placed in liquid nitrogen and freezes by filter residue, Frozen block is obtained, then frozen block is placed in pulverizer and is crushed, the sieve of 220 mesh is crossed, obtains crushed material, crushed material is then placed in baking It is dry to obtain xeraphium particle, then xeraphium particle is placed in retort to constant weight under the conditions of temperature is 110 DEG C in case, And nitrogen is filled with into furnace with the rate of 90mL/min, 1600 DEG C then are risen to the heating rate in-furnace temperature of 10 DEG C/min, Under the conditions of temperature is 1600 DEG C, 3h is carbonized, modified rice hull cellulose is obtained；According to parts by weight, by 100 parts of electric-melting magnesium slags, 20 parts Modified rice hull cellulose, 20 parts of graphene oxides, 10 parts of low-melting alloys, 20 parts of thermosetting resins, 2 parts of curing agent, 0.2 part fluxing Agent is placed in blender, under the conditions of revolving speed is 200r/min, is stirred 60min, is obtained mixed slurry, sprays to die surface Methyl-silicone oil, then by mixed slurry inject mold in, in pressure be 300MPa under the conditions of, after compression moulding, in temperature be 260 Under the conditions of DEG C, heat preservation solidification for 24 hours, is demoulded, and discharging, cooled to room temperature is to get the low magnesia carbon brick of resistance to compression for building.The eutectic Point alloy is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for 30%(ω), lead accounts for 8% (ω), indium account for 11%(ω).The thermosetting resin is phenolic resin 2123.The curing agent is hexa.It is described to help Flux is made of the raw material of following parts by weight: 50 parts of boraxs, 15 parts of boron oxides, 10 parts of sodium carbonate.

Example 4

According to parts by weight, by 3 parts of glucose, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of water are placed in No. 1 beaker, and by No. 1 Beaker is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 500r/min, heating stirring is mixed 60min is closed, nutrient solution is obtained；Gelatin and water 1:100 in mass ratio are placed in No. 2 beakers, 20min is stirred with glass bar, stands Be swollen 5h, No. 2 beakers be then placed in digital display and are tested the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, revolving speed 500r/min Under the conditions of, heating stirring dissolves 60min to get gelatin solution；Graphene oxide and gelatin solution 1:30 in mass ratio are placed in No. 3 burnings In cup, the ammonium hydroxide that mass fraction is 30% is then added dropwise into No. 3 beakers and adjusts pH to 8.6, then No. 3 beakers are placed in ultrasound point It dissipates in instrument, under the conditions of supersonic frequency is 75kHz, after mixing ultrasound 60min, obtains dispersion liquid, then filter dispersion liquid, must filter Cake then obtains pre-dispersed graphene oxide for Washing of Filter Cake 8 times with deionized water；Rice hull cellulose is placed in pulverizer and is crushed, The sieve for crossing 80 mesh obtains pretreatment rice hull cellulose；According to parts by weight, by 20 parts of pretreatment rice hull celluloses, 2 parts of biogas slurries, 2 parts of nutrition Liquid, 30 parts of water are placed in fermentation cauldron, in temperature be 35 DEG C, revolving speed be 200r/min under the conditions of, mixed fermentation 5 days, then to hair The ferric chloride solution and pretreatment rice hull cellulose matter that pretreatment 0.3 times of mass fraction of rice hull cellulose quality is 20% are added in ferment kettle The sodium fluoride of 0.03 times of amount is stirred 60min, quality is then added dropwise into fermentation cauldron under the conditions of revolving speed is 300r/min The ammonium hydroxide that score is 30% adjusts pH to 5.8, obtains fermentation mixed liquor, and will then ferment mixed liquor filtering, filter residue, then by filter residue It is placed in liquid nitrogen and freezes, obtain frozen block, then frozen block is placed in pulverizer and is crushed, cross the sieve of 220 mesh, obtain crushed material, connect Crushed material is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain xeraphium particle, then by drying and crushing Material is placed in retort, and nitrogen is filled with into furnace with the rate of 90mL/min, then in the heating rate furnace of 10 DEG C/min Temperature rises to 1600 DEG C, under the conditions of temperature is 1600 DEG C, carbonizes 3h, obtains modified rice hull cellulose；According to parts by weight, by 100 Part electric-melting magnesium slag, 20 parts of modified rice hull celluloses, 20 parts of pre-dispersed graphene oxides, 20 parts of thermosetting resins, 2 parts of curing agent, 0.2 Part fluxing agent is placed in blender, under the conditions of revolving speed is 200r/min, is stirred 60min, is obtained mixed slurry, to mold table Methyl-silicone oil is sprayed in face, then injects mixed slurry in mold, under the conditions of pressure is 300MPa, after compression moulding, and Yu Wen Under the conditions of degree is 260 DEG C, heat preservation solidification for 24 hours, is demoulded, and discharging, cooled to room temperature is to get the low magnesia carbon brick of resistance to compression for building. The thermosetting resin is phenolic resin 2123.The curing agent is hexa.The fluxing agent is by following weight The raw material of number forms: 50 parts of boraxs, 15 parts of boron oxides, 10 parts of sodium carbonate.

Comparative example: the low magnesia carbon brick of Nanjing Materials Co., Ltd production.

The low magnesia carbon brick of 1 to 4 gained of example and comparative example product are subjected to performance detection, the specific detection method is as follows:

Its mechanical property is detected according to GB/T22589, specific detection method is as shown in table 1:

Table 1: performance detection table

Detection content	Example 1	Example 2	Example 3	Example 4	Comparative example
						Compression strength/MPa	118	80	76	82	57
Flexural strength/MPa	14.6	10.7	11.2	11.6	8.2

By 1 testing result of table it is found that the low magnesia carbon brick of present invention gained resistance to compression for building has excellent mechanical property.

Claims

1. a kind of preparation method of the low magnesia carbon brick of resistance to compression for building, it is characterised in that specific preparation process is as follows:

2. the preparation method of the low magnesia carbon brick of a kind of resistance to compression for building according to claim 1, it is characterised in that: step (2) institute Nutrient solution is stated to be made of the raw material of following parts by weight: 2~3 parts of glucose, 1~2 part of glycerol, 1~2 part of polyethylene glycol, 20 ~30 parts of water.

3. the preparation method of the low magnesia carbon brick of a kind of resistance to compression for building according to claim 1, it is characterised in that: step (3) institute State the preparation process of pre-dispersed graphene oxide are as follows: graphene oxide is mixed with gelatin solution 1:20~1:30 in mass ratio, is connect Dropwise addition ammonium hydroxide adjust pH to 8.3~8.6, mixing ultrasound, filter, washing, obtain pre-dispersed graphene oxide.

4. the preparation method of the low magnesia carbon brick of a kind of resistance to compression for building according to claim 1, it is characterised in that: step (3) institute Stating low-melting alloy is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for 30%(ω), lead Account for 8%(ω), indium accounts for 11%(ω).

5. the preparation method of the low magnesia carbon brick of a kind of resistance to compression for building according to claim 1, it is characterised in that: step (3) institute Stating thermosetting resin is any one in phenolic resin 2123, phenolic resin 2127 or phenolic resin 2130.

6. the preparation method of the low magnesia carbon brick of a kind of resistance to compression for building according to claim 1, it is characterised in that: step (3) institute Stating curing agent is hexa, any one in butyl acrylate or methyl methacrylate.

7. the preparation method of the low magnesia carbon brick of a kind of resistance to compression for building according to claim 1, it is characterised in that: step (3) institute It states fluxing agent to be made of the raw material of following parts by weight: 40~50 parts of boraxs, 10~15 parts of boron oxides, 8~10 parts of sodium carbonate.

8. the preparation method of the low magnesia carbon brick of a kind of resistance to compression for building according to claim 1, it is characterised in that: step (2) institute State the modified carbon fiber aeroge that pretreatment rice hull cellulose quality 8~15% can also be added in water；The modified carbon fiber airsetting The preparation process of glue are as follows: