CN106673631A - Preparation method of quartz silica bricks with high thermal conductivity and cracking resistance - Google Patents

Preparation method of quartz silica bricks with high thermal conductivity and cracking resistance Download PDF

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CN106673631A
CN106673631A CN201611265217.0A CN201611265217A CN106673631A CN 106673631 A CN106673631 A CN 106673631A CN 201611265217 A CN201611265217 A CN 201611265217A CN 106673631 A CN106673631 A CN 106673631A
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silica brick
silica bricks
silica
beaker
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雷笑天
王维
孙冬
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Abstract

The invention discloses a preparation method of quartz silica bricks with high thermal conductivity and cracking resistance, and belongs to the technical field of silica bricks. The preparation method provided by the invention comprises the following steps: crushing and sieving quartzite and graphene first; heating for reaction with a calcium hydroxide solution and micro silicon powder to obtain suspension; ball-milling aluminum oxide, iron oxide and the like, and then stirring together with the suspension, a silane coupling agent and the like to obtain a mixture; crushing and sieving coconut shells, acid-hydrolyzing with hydrochloric acid to obtain microcrystalline cellulose; finally, pressing and forming the microcrystalline cellulose together with the mixture, sintering and discharging from a kiln to obtain the quartz silica bricks with high thermal conductivity and cracking resistance. The preparation method provided by the invention solves a problem of loose structure of the silica bricks caused by volume expansion, contributes to forming of brick bodies and stabilizing of the crystal form transformation of silica rock, reduces cracks or cracking of a finished product, and increases the density of silica bricks; the silica bricks prepared in the invention have uniform distribution of pores inside the silica bricks, have a compact structure, greatly increases thermal conductivity of the silica bricks, and have good application prospect.

Description

A kind of preparation method of the resistance to quartzy silica brick that bursts apart of high heat conduction
Technical field
The invention discloses a kind of preparation method of the resistance to quartzy silica brick that bursts apart of high heat conduction, belongs to silica brick preparing technical field.
Background technology
The design direction of advanced coke oven is efficient, long-lived, energy-conservation and environmental protection, and the properties of silica brick directly affect coke oven The advance of technology.For a long time, the fire resistances such as intensity, thermal shock, the loading softening of silica brick are paid close attention to people more, it is most in the hope of coke oven The possible long-life.But with energy-conservation and the increasingly severization of environmental requirement, enterprise requirements coke oven saves coal in process of coking Gas is consumed, while reducing the discharge of nitrogen oxides and oxycarbide.The combustor and carbonizing chamber of coke oven is removed and is subjected to 1300 DEG C for a long time Also subject to top masonry and the dead weight of equipment outside high temperature action above, charging car and ram dynamic load operationally, Pressure produced by expanding during coal coking, with the rubbing action of coke etc. during coke pushing, therefore it is required that silica brick need to have high intensity, Intensity is higher, and wearability is better, the life-span is higher.
Due to the silica brick characteristic such as there is refractoriness under load point height, high volume good stability, life-time service not to shrink, Also it is widely applied in lightweight refracrory system and studies.At present both at home and abroad the method for manufacture light silicious brick is a lot, wherein extensively General application is that foam method and machine press flammable method.
However, in existing silica brick manufacturing technology, there is a problem of that silica brick internal structure performance is relatively uneven, silica brick system Make in kneading operation, the addition of traditional mineralizer-lime cream is added in edge runner-wet mill, rapidly by part Silicon stone by pipeline Grain and fine powder parcel, it is impossible to be evenly distributed on well in pug, this causes the skewness of calcium oxide in adobe.In sintering During cause at the same temperature silicon dioxide crystal conversion is uneven between granule and substrate, some local conversions are too fast, have Local conversion it is again excessively slow, the swelling stress produced due to crystal conversion inside such brick body is very uneven, it is easy to make Into gross blow hole, the generation of even crackle, yield rate is so not only affected, have an effect on the stability of silica brick quality.So only leading to The mechanical agitation methods for crossing physics are wanted to make the distribution of mineralizer homogenization have limitation, can so affect the equal of silica brick internal structure Even property, so as to silica brick performance can be affected.Additionally, existing silica brick is due to its traditional mineralizer remineralization efficacy and the limitation of addition form Property, moisture distribution during base is not uniform enough to make silica brick semi-finished product, and pug moisture is also higher.Silica brick after burning till, arrange by moisture Except the gas cell distribution for staying is also very uneven, pore cluster concentration of local situation is projected, and this has all severely impacted silica brick and has led The raising of heating rate.
The content of the invention
Present invention mainly solves technical problem：Relatively uneven for existing silica brick internal structure performance, brick body is easy There is gross blow hole and seminess, and due to mineralizer remineralization efficacy in silica brick and the limitation of addition form, cause silica brick to be led The undesirable defect of heating rate, there is provided a kind of Graphene strengthens silica brick heat conductivity, is coordinated with metal-oxide and calcium hydroxide and does ore deposit Agent improves the transformation degree of quartz, and silicon carbide whisker is formed in sintering process by Microcrystalline Cellulose and inorganic silicon increases close The method of solidity, reduction crackle to prepare the resistance to quartzy silica brick that bursts apart of high heat conduction, the present invention first crushes quartzite and Graphene Obtain suspension with aqua calcises, silicon powder reacting by heating after sieving, subsequently by after the ball millings such as aluminium oxide, ferrum oxide with it is suspended Liquid, silane coupler etc. stir to obtain compound, then hydrochloric acidolysiss are used after Exocarpium cocois (Cocos nucifera L) is pulverized and sieved, and obtain Microcrystalline Cellulose, finally By the compressing rear sintering kiln discharge of itself and compound, you can obtain the resistance to quartzy silica brick that bursts apart of high heat conduction, the present invention solves silica brick Because of the loosely organized problem that volumetric expansion causes, contribute to the transformation of crystal of brick body molding and stable Silicon stone, reduce finished product Crackle or cracking, increased the consistency of silica brick, and the obtained silica brick internal void of the present invention is evenly distributed, and structure system is close, makes Silica brick thermal conductivity obtains larger raising, with preferable application prospect.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Weigh 2~3kg quartzites and 25~30g Graphenes are added in pulverizer and crush, cross 80~100 mesh sieves, collected Sieve thing, weighs 600~700g sievings and is added in beaker, add 1~2L mass fractions for 1% aqua calcises and 8~ 12g silicon powders, after stirring 2~3min of mixing, beaker are moved in water-bath, control temperature at 70~80 DEG C, stirring reaction 2~ After 3h, stop heating, obtain suspension；
（2）15~20g aluminium oxidies, 30~40g ferrum oxides, 8~12g cerium oxide and 5~8g manganese oxide are weighed respectively, are added to ball In grinding machine after 30~40min of ball milling, cross 120~150 mesh sieves, obtain mixed-powder, take 10~12g mixed-powders be added to it is above-mentioned In suspension, 0.3~0.5g silane resin acceptor kh-550s, 0.5~0.8g carboxymethyl celluloses and 6~8g alginic acid are added Sodium, after stirring 15~20min of mixing, obtains compound, standby；
（3）Weigh 400~500g Exocarpium cocois (Cocos nucifera L) and be added in pulverizer and crush, cross 80~100 mesh sieves, collect sieving, take 100~ 200g sievings are added to and fill in the beaker that 400~500mL mass fractions are 10% hydrochloric acid, and beaker is placed in water-bath, control Temperature processed soaks 4~5h of acidolysis at 40~50 DEG C, treats to be filtered after the completion of acidolysis, collects filter cake, and is 75% second with mass fraction Alcoholic solution is cleaned 3~5 times, obtains Microcrystalline Cellulose；
（4）Above-mentioned Microcrystalline Cellulose is added to into step（2）In standby compound, after 5~10min of stirring, move into molding and shake It is compressing in dynamic forming machine, adobe is obtained, adobe is moved in hyperthermia tunnel Kiln, tunnel cave temperature is set as 1100~1200 DEG C, heating rate is 180~200 DEG C/h, after reaching design temperature, 3~4h of heat preservation sintering, then it is warming up to 1400~1500 DEG C, Continue to sinter after 23~25h, be cooled to 25~35 DEG C, control rate of temperature fall for 120~150 DEG C/h, kiln discharge, you can obtain height and lead The resistance to quartzy silica brick that bursts apart of heat.
The present invention application process be：Carry out live bracing wire positioning with horizontal line pole first, and count by weight, take 50 ~60 parts of cement, 20~30 parts of sand, 20~30 parts of water stirring mixes to obtain mud, subsequently bursts apart high heat conduction obtained in the present invention is resistance to Quartzy one layer of mud of silica brick surface layer uniform application, then at positioning build the silica brick for spreading mud by laying bricks or stones by the way of stacking is piled up Stamp charging coke oven body of heater, after the completion for the treatment of that body of heater is built by laying bricks or stones, in body of heater facade plastering construction is carried out, and is finally carried out after the completion of plastering often Warm body of heater is conserved 5~7 days.After testing, the obtained resistance to quartzy silica brick internal void that bursts apart of high heat conduction of the present invention is evenly distributed, Compact structure, brick body density is 2.16~2.28g/cm3, apparent porosity is 15.8~17.2%, with higher heat conductivility, Up to 2.42~2.75W/mK, more traditional silica brick improves 25~30% to thermal conductivity, while silica brick intensity of the present invention is high, silica brick Yield rate up to more than 96.5%, brick body compressive resistance up to 65~73MPa, and silica brick refractoriness under load of the present invention up to 1700~ 1800 DEG C, up to 10~12 years, more traditional silica brick extended 4~8 years to silica brick service life.
The invention has the beneficial effects as follows：
（1）The obtained resistance to quartzy silica brick internal void that bursts apart of high heat conduction of the invention is evenly distributed, and aperture ratio tradition silica brick is little, silica brick Structure is more uniform, and is not likely to produce crackle, can effectively provide silica brick yield rate and silica brick quality stability；
（2）The resistance to quartzy silica brick that bursts apart of high heat conduction of the invention obtained has high-termal conductivity, can keep silica brick other comprehensive Optimalities Can, moreover it is possible to while meeting coke oven's long campaign, energy-conservation and the needs for efficiently producing, have broad application prospects.
Specific embodiment
2~3kg quartzites are weighed first and 25~30g Graphenes are added in pulverizer and crush, cross 80~100 mesh sieves, Sieving is collected, 600~700g sievings is weighed and is added in beaker, it is that 1% calcium hydroxide is molten to add 1~2L mass fractions Liquid and 8~12g silicon powders, after stirring 2~3min of mixing, beaker are moved in water-bath, and control temperature is stirred at 70~80 DEG C After 2~3h of reaction, stop heating, obtain suspension；Subsequently weigh respectively 15~20g aluminium oxidies, 30~40g ferrum oxides, 8~ 12g cerium oxide and 5~8g manganese oxide, are added in ball mill after 30~40min of ball milling, cross 120~150 mesh sieves, are mixed Powder, takes 10~12g mixed-powders and is added in above-mentioned suspension, add 0.3~0.5g silane resin acceptor kh-550s, 0.5 ~0.8g carboxymethyl celluloses and 6g sodium alginates, after stirring 15~20min of mixing, obtain compound, standby；400 are weighed again ~500g Exocarpium cocois (Cocos nucifera L) is added in pulverizer and crushes, and crosses 80~100 mesh sieves, collects sieving, takes the addition of 100~200g sievings To filling in the beaker that 400~500mL mass fractions are 10% hydrochloric acid, beaker is placed in water-bath, control temperature is 40~50 DEG C, 4~5h of acidolysis is soaked, treat to be filtered after the completion of acidolysis, filter cake is collected, and clean 3~5 for 75% ethanol solution with mass fraction It is secondary, obtain Microcrystalline Cellulose；Finally above-mentioned Microcrystalline Cellulose is added in above-mentioned standby compound, 5~10min is stirred Afterwards, it is compressing in immigration molding vibrating forming machine, adobe is obtained, adobe is moved in hyperthermia tunnel Kiln, set tunnel kiln temperature Spend for 1100~1200 DEG C, heating rate is 180~200 DEG C/h, after reaching design temperature, 3~4h of heat preservation sintering, then be warming up to 1400~1500 DEG C, continue to sinter after 23~25h, be cooled to 25~35 DEG C, it is 120~150 DEG C/h to control rate of temperature fall, is gone out Kiln, you can obtain the resistance to quartzy silica brick that bursts apart of high heat conduction.
Example 1
2kg quartzites are weighed first and 25g Graphenes are added in pulverizer and crush, cross 80 mesh sieves, collect sieving, weigh 600g sievings are added in beaker, add 1L mass fractions for 1% aqua calcises and 8g silicon powders, stirring mixing After 2min, beaker is moved in water-bath, control temperature after stirring reaction 2h, stops heating at 70 DEG C, obtains suspension；With Weigh 15g aluminium oxidies, 30g ferrum oxides, 8g cerium oxide and 5g manganese oxide respectively afterwards, be added in ball mill after ball milling 30min, mistake 120 mesh sieves, obtain mixed-powder, take 10g mixed-powders and are added in above-mentioned suspension, add 0.3g silane coupler KH- 550th, 0.5g carboxymethyl celluloses and 7g sodium alginates, after stirring mixing 15min, obtain compound, standby；400g coconut palms are weighed again Sub- shell is added in pulverizer and crushes, and crosses 80 mesh sieves, collects sieving, takes 100g sievings and is added to and fills 400mL mass point During number is for the beaker of 10% hydrochloric acid, beaker is placed in water-bath, control temperature soaks acidolysis 4h, after the completion for the treatment of acidolysis at 40 DEG C Filter, collect filter cake, and cleaned 3 times for 75% ethanol solution with mass fraction, obtain Microcrystalline Cellulose；Finally by above-mentioned crystallite Cellulose is added in above-mentioned standby compound, compressing in immigration molding vibrating forming machine after stirring 5min, obtains brick Base, adobe is moved in hyperthermia tunnel Kiln, sets tunnel cave temperature as 1100 DEG C, and heating rate is 180 DEG C/h, reaches setting temperature After degree, heat preservation sintering 3h, then be warming up to 1400 DEG C continues to sinter after 23h, is cooled to 25 DEG C, control rate of temperature fall be 120 DEG C/ H, kiln discharge, you can obtain the resistance to quartzy silica brick that bursts apart of high heat conduction.
This example operation is easy, when using, carries out live bracing wire positioning with horizontal line pole first, and counts by weight, 50 parts of cement are taken, 20 parts of sand, 20 parts of water stirrings mix to obtain mud, subsequently in the resistance to quartzy silica brick that bursts apart of high heat conduction obtained in the present invention One layer of mud of surface layer uniform application, then build the silica brick for spreading mud by laying bricks or stones tampering type Jiao at positioning by the way of stacking is piled up Furnace body, after the completion for the treatment of that body of heater is built by laying bricks or stones, in body of heater facade plastering construction is carried out, and room temperature body of heater is finally carried out after the completion of plastering and is supported Shield 5 days.After testing, the obtained resistance to quartzy silica brick internal void that bursts apart of high heat conduction of the present invention is evenly distributed, compact structure, brick Body density is 2.16g/cm3, apparent porosity is 15.8%, and with higher heat conductivility, thermal conductivity reaches 2.42W/mK, relatively passes System silica brick improves 25%, while silica brick intensity of the present invention is high, up to 96.7%, brick body compressive resistance reaches 65MPa to the yield rate of silica brick, And silica brick refractoriness under load of the present invention, up to 1700 DEG C, up to 10 years, more traditional silica brick extended 4 years to silica brick service life.
Example 2
2kg quartzites are weighed first and 28g Graphenes are added in pulverizer and crush, cross 90 mesh sieves, collect sieving, weigh 650g sievings are added in beaker, add 1L mass fractions for 1% aqua calcises and 10g silicon powders, stirring mixing After 2min, beaker is moved in water-bath, control temperature after stirring reaction 2h, stops heating at 75 DEG C, obtains suspension；With Weigh 18g aluminium oxidies, 35g ferrum oxides, 10g cerium oxide and 7 manganese oxide respectively afterwards, be added in ball mill after ball milling 35min, mistake 135 mesh sieves, obtain mixed-powder, take 11g mixed-powders and are added in above-mentioned suspension, add 0.4g silane coupler KH- 550th, 0.7g carboxymethyl celluloses and 8g sodium alginates, after stirring mixing 18min, obtain compound, standby；450g coconut palms are weighed again Sub- shell is added in pulverizer and crushes, and crosses 90 mesh sieves, collects sieving, takes 150g sievings and is added to and fills 4500mL mass point During number is for the beaker of 10% hydrochloric acid, beaker is placed in water-bath, control temperature soaks acidolysis 4h, after the completion for the treatment of acidolysis at 45 DEG C Filter, collect filter cake, and cleaned 4 times for 75% ethanol solution with mass fraction, obtain Microcrystalline Cellulose；Finally by above-mentioned crystallite Cellulose is added in above-mentioned standby compound, compressing in immigration molding vibrating forming machine after stirring 8min, obtains brick Base, adobe is moved in hyperthermia tunnel Kiln, sets tunnel cave temperature as 1150 DEG C, and heating rate is 190 DEG C/h, reaches setting temperature After degree, heat preservation sintering 3h, then be warming up to 1450 DEG C continues to sinter after 24h, is cooled to 30 DEG C, control rate of temperature fall be 135 DEG C/ H, kiln discharge, you can obtain the resistance to quartzy silica brick that bursts apart of high heat conduction.
This example operation is easy, when using, carries out live bracing wire positioning with horizontal line pole first, and counts by weight, 55 parts of cement are taken, 25 parts of sand, 25 parts of water stirrings mix to obtain mud, subsequently in the resistance to quartzy silica brick that bursts apart of high heat conduction obtained in the present invention One layer of mud of surface layer uniform application, then build the silica brick for spreading mud by laying bricks or stones tampering type Jiao at positioning by the way of stacking is piled up Furnace body, after the completion for the treatment of that body of heater is built by laying bricks or stones, in body of heater facade plastering construction is carried out, and room temperature body of heater is finally carried out after the completion of plastering and is supported Shield 6 days.After testing, the obtained resistance to quartzy silica brick internal void that bursts apart of high heat conduction of the present invention is evenly distributed, compact structure, brick Body density is 2.22g/cm3, apparent porosity is 16.5%, and with higher heat conductivility, thermal conductivity reaches 2.588W/mK, relatively passes System silica brick improves 28%, while silica brick intensity of the present invention is high, up to 97.2%, brick body compressive resistance reaches 69MPa to the yield rate of silica brick, And silica brick refractoriness under load of the present invention, up to 1750 DEG C, up to 11 years, more traditional silica brick extended 6 years to silica brick service life.
Example 3
3kg quartzites are weighed first and 30g Graphenes are added in pulverizer and crush, cross 100 mesh sieves, collect sieving, weigh 700g sievings are added in beaker, add 2L mass fractions for 1% aqua calcises and 12g silicon powders, stirring mixing After 3min, beaker is moved in water-bath, control temperature after stirring reaction 3h, stops heating at 80 DEG C, obtains suspension；With Weigh 20g aluminium oxidies, 40g ferrum oxides, 12g cerium oxide and 8g manganese oxide respectively afterwards, be added in ball mill after ball milling 40min, 150 mesh sieves are crossed, mixed-powder is obtained, 12g mixed-powders is taken and is added in above-mentioned suspension, add 0.5g silane couplers KH-550 and 0.8g carboxymethyl celluloses, after stirring mixing 20min, obtain compound, standby；The addition of 500g Exocarpium cocois (Cocos nucifera L) is weighed again Crush in pulverizer, cross 100 mesh sieves, collect sieving, take 200g sievings and be added to and fill 500mL mass fractions for 10% In the beaker of hydrochloric acid, beaker is placed in water-bath, control temperature soaks acidolysis 5h at 50 DEG C, treats to be filtered after the completion of acidolysis, received Collection filter cake, and cleaned 5 times for 75% ethanol solution with mass fraction, obtain Microcrystalline Cellulose；Finally above-mentioned Microcrystalline Cellulose is added Enter in above-mentioned standby compound, it is compressing in immigration molding vibrating forming machine after stirring 10min, adobe is obtained, by brick Base is moved in hyperthermia tunnel Kiln, sets tunnel cave temperature as 1200 DEG C, and heating rate is 200 DEG C/h, after reaching design temperature, is protected Temperature sintering 4h, then be warming up to 1500 DEG C, continues to sinter after 25h, is cooled to 35 DEG C, and it is 150 DEG C/h control rate of temperature fall, kiln discharge, The resistance to quartzy silica brick that bursts apart of high heat conduction is obtained.
This example operation is easy, when using, carries out live bracing wire positioning with horizontal line pole first, and counts by weight, 60 parts of cement are taken, 30 parts of sand, 30 parts of water stirrings mix to obtain mud, subsequently in the resistance to quartzy silica brick that bursts apart of high heat conduction obtained in the present invention One layer of mud of surface layer uniform application, then build the silica brick for spreading mud by laying bricks or stones tampering type Jiao at positioning by the way of stacking is piled up Furnace body, after the completion for the treatment of that body of heater is built by laying bricks or stones, in body of heater facade plastering construction is carried out, and room temperature body of heater is finally carried out after the completion of plastering and is supported Shield 7 days.After testing, the obtained resistance to quartzy silica brick internal void that bursts apart of high heat conduction of the present invention is evenly distributed, compact structure, brick Body density is 2.28g/cm3, apparent porosity is 17.2%, and with higher heat conductivility, thermal conductivity reaches 2.75W/mK, relatively passes System silica brick improves 30%, while silica brick intensity of the present invention is high, up to 97.5%, brick body compressive resistance reaches 73MPa to the yield rate of silica brick, And silica brick refractoriness under load of the present invention, up to 1800 DEG C, up to 12 years, more traditional silica brick extended 8 years to silica brick service life.

Claims (1)

1. the preparation method of the resistance to quartzy silica brick that bursts apart of a kind of high heat conduction, it is characterised in that concrete preparation process is：
（1）Weigh 2~3kg quartzites and 25~30g Graphenes are added in pulverizer and crush, cross 80~100 mesh sieves, collected Sieve thing, weighs 600~700g sievings and is added in beaker, add 1~2L mass fractions for 1% aqua calcises and 8~ 12g silicon powders, after stirring 2~3min of mixing, beaker are moved in water-bath, control temperature at 70~80 DEG C, stirring reaction 2~ After 3h, stop heating, obtain suspension；
（2）15~20g aluminium oxidies, 30~40g ferrum oxides, 8~12g cerium oxide and 5~8g manganese oxide are weighed respectively, are added to ball In grinding machine after 30~40min of ball milling, cross 120~150 mesh sieves, obtain mixed-powder, take 10~12g mixed-powders be added to it is above-mentioned In suspension, 0.3~0.5g silane resin acceptor kh-550s, 0.5~0.8g carboxymethyl celluloses and 6~8g alginic acid are added Sodium, after stirring 15~20min of mixing, obtains compound, standby；
（3）Weigh 400~500g Exocarpium cocois (Cocos nucifera L) and be added in pulverizer and crush, cross 80~100 mesh sieves, collect sieving, take 100~ 200g sievings are added to and fill in the beaker that 400~500mL mass fractions are 10% hydrochloric acid, and beaker is placed in water-bath, control Temperature processed soaks 4~5h of acidolysis at 40~50 DEG C, treats to be filtered after the completion of acidolysis, collects filter cake, and is 75% second with mass fraction Alcoholic solution is cleaned 3~5 times, obtains Microcrystalline Cellulose；
（4）Above-mentioned Microcrystalline Cellulose is added to into step（2）In standby compound, after 5~10min of stirring, move into molding and shake It is compressing in dynamic forming machine, adobe is obtained, adobe is moved in hyperthermia tunnel Kiln, tunnel cave temperature is set as 1100~1200 DEG C, heating rate is 180~200 DEG C/h, after reaching design temperature, 3~4h of heat preservation sintering, then it is warming up to 1400~1500 DEG C, Continue to sinter after 23~25h, be cooled to 25~35 DEG C, control rate of temperature fall for 120~150 DEG C/h, kiln discharge, you can obtain height and lead The resistance to quartzy silica brick that bursts apart of heat.
CN201611265217.0A 2016-12-30 2016-12-30 Preparation method of quartz silica bricks with high thermal conductivity and cracking resistance Pending CN106673631A (en)

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CN105504609A (en) * 2015-12-28 2016-04-20 常州亚环环保科技有限公司 Method for preparing silicon carbide whisker and polytetrafluoroethylene composite friction materials through sea sedge slag

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CN102531648A (en) * 2011-12-26 2012-07-04 北京航空航天大学 Calcium oxide-based ceramic core for casting titanium alloy and manufacturing method thereof
CN103060890A (en) * 2013-01-22 2013-04-24 华南理工大学 Method for synthesizing nano silicon carbide crystal whiskers
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Application publication date: 20170517