CN101723693B - Method for improving mechanical performance and thermal shock resistance of compact heavy refractory product - Google Patents
Method for improving mechanical performance and thermal shock resistance of compact heavy refractory product Download PDFInfo
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- CN101723693B CN101723693B CN 200910263025 CN200910263025A CN101723693B CN 101723693 B CN101723693 B CN 101723693B CN 200910263025 CN200910263025 CN 200910263025 CN 200910263025 A CN200910263025 A CN 200910263025A CN 101723693 B CN101723693 B CN 101723693B
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Abstract
The invention relates to a method for improving the mechanical performance and the thermal shock resistance of a compact heavy refractory product, which is characterized by comprising the following steps of: immerging the produced compact heavy refractory product into a phosphate solution which is formed by adding phosphorous acid with the concentration not less than 85wt% into active magnesium oxide and/or active aluminum oxide with the phosphorous acid weight of 3-5wt% for reaction, wherein the previous and subsequent weighing change is larger than 5-8 percent; taking out the mixture, drying and carrying out medium temperature processing at the temperature of 600-800 DEG C, thereby not only improving the mechanical performance of the refractory product, for example, the density is improved by 3-6 percent, the intensity is improved by about 20-40 percent, the high temperature folding strength at the temperature of 1,100 DEG C is respectively improved to 28 (porzite-silicon carbide) from the original about 23 and improved to 25 (porzite) from the original about 18, and the porosity is also reduced; but also improving the toughness of the compact heavy refractory product, for example, the porosity is reduced, the thermal shock resistance is improved, the times of water cooling at the temperature of 1,100 DEG C are respectively increased to 70 times (porzite-silicon carbide) from the original about 50 times and increased to 14 times (porzite) from the original 3 times, and wearing resistance tests are decreased to 5.4 percent from the original 6.3 percent (a weighing method), so that the service life of a dry coke quenching furnace can be prolonged by 1-2 times.
Description
Technical field
The present invention relates to a kind of raising compact heavy refractory product mechanical property and heat-shock resistance method, relate in particular to coke dry quenching furnace and use compact heavy refractory product.
Background technology
Dry quenched coke oven chute district supporting beam (being commonly called as bracket), because of long-time running in the frequent severe environment that cold and heat succeed each other, temperature variation is big; Its upper pressure load-bearing big (about 190 tons); Simultaneously receive air-flow and dust to wash away, clash into again, and the coke extruding, special because it protrudes from big-wall; Bear from each side resistance and pressure greatlyyer, cause easy damage.Prior art is used AL usually
2O
3>=35%, the mullite silicon carbide compact heavy refractory brick of SiC>=30%, for example Chinese patent CN1854106 dry coke quenching is used mullite silicon carbide refractory material; Adopt the 3-15wt% Pure Silicon Metal; 35-65wt% sintering and/or electrofused mullite, 25-45wt% silit, 3-5% α-Al
2O
3Micro mist, the 4-10% clay is formed.Chinese patent CN1927767 high thermal shock abrasive brick for dry quenched coke oven chute pillar; Is base stock with silit 62～80% with silicon nitride 17～35%; Add 0.1～0.8% rare earth lanthanide oxide, be equipped with 0.4～3% mineral binder bond, form through mixing, compacting, sintering.Cooling section washes away because of receiving coke, requires wear resistance to get well, and uses the compact heavy mullite brick usually.Yet above-mentioned compact heavy refractory product (is used for the hot operation layer; Direct contact thermal-flame) intensity, anti-folding, antiscour, heat-shock resistance still can not satisfy the requirement of coke dry quenching furnace fully, and the material quality is unstable, and work-ing life is shorter relatively; Be about 1 year general work-ing life; Had a strong impact on the work-ing life of coke dry quenching furnace, increased the frequency of maintenance of coke dry quenching furnace, become national coal tar industry coke dry quenching furnace and had a common issue with.Improve above-mentioned position refractory product work-ing life, must improve 1100 ℃ of high temperature break resistant intensities of refractory product; Anti-scouring capability under 1100 ℃ of high temperature; Compressive strength; And thermal shock resistance four big technical indicators.In the above-mentioned four big indexs; All void content, the density with refractory product has much relations; Former three requires to have higher density and lower void content; The latter requires low density and higher void content again, and the former three and the latter are inverse relation, and refractory product is difficult to obtain simultaneously to improve usually.The applicant is repeatedly analyzing the back discovery; Above-mentioned reason mainly is that compact heavy refractory brick adopts friction press compression moulding; Because friction press pressure is inhomogeneous; Add all factors such as eutectic that contain in the mixing uniformity coefficient of raw material, material purity, low-temperature binder, the raw material; Can cause the refractory product moulding to fire inevitable existence the in the internal structure of back in the production process unavoidably, cause the refractory product inner quality unstable, degradation like small crackle, small fusion hole, hole not of uniform size or the like scar defective.
Though prior art is employed in neutrality, acid refractory product, through adding phosphoric acid and phosphagel phosphaljel, make aluminium formation phosphagel phosphaljel in phosphoric acid and the refractory product, improve refractory product mechanical strength method.For example:
Chinese patent CN101544504 phosphate-bonded aluminum silicon carbide brick; In bauxite chamotte, add 4～10% phosphate binders, produce apparent porosity less than 15%, cold crushing strength begins temperature greater than 1600 ℃, fine aluminum silicon carbide brick that oxidation-resistance is strong greater than 130MPa, loading softening.
Chinese patent CN1052841 highiy refractory brick includes fire-retardant high aluminium powder, fireclay in its material component, be added with the vitriol oil, phosphoric acid, oxalic acid and fire and form.Can anti-high temperature more than 1580 ℃, can make the high-temperature flame-proof structured material.
Chinese patent CN1041149 phosphate-combined high-aluminium kiln-lining brick adds 35～55wt% phosphoric acid solution in the kaolin raw material, by weight 1: 0.8～1.0 mixed, drop into the back extrusion forming, and under 600 ℃ of temperature, constant temperature was finished product after 8 hours.The load softening point temperature is in 1500～1700 ℃ of scopes, and the stable number of times of heat-resisting shake reaches 50～100 times.
Above-mentionedly add phosphoric acid solution in the blending process in refractory product early stage; Its effect is to make MOX generation phosphoric acid salt (aluminum oxide in the refractory raw material, silicon oxide, Natural manganese dioxide and phosphatase reaction generate phosphoric acid salt) in phosphoric acid and the refractory materials; Strengthen the gumminess of refractory raw material particle and fine powder, improve the mechanical property of refractory brick.But in blending process, add phosphoric acid solution, still can not eliminate the structural defect that brings when making refractory product, therefore comprehensive can not being overally improved.
Chinese patent CN1557779 refractory materials or metal founding dip treating technology, are put into steeper with refractory materials or metal casting product and are sealed the first step, take out inner air with vacuum pump, and vacuum kept 5-180 minute; Second step, open the liquid flowing valve of the pipeline that is connected with said steeper, with aluminium dihydrogen phosphate liquid or Lutafei F type resin liquid (English name: Rutaphen F-Type Resins) be input in the steeper; The 3rd step, open blow-off valve and make in the steeper and to close blow-off valve after reaching balance with outside pressure; The 4th step, open air compressor machine and in steeper, pressurizes, pressurize is 0.2-5 hour when treating that pressure reaches 0.05-2Mpa; The 5th goes on foot, slowly opens said liquid flowing valve discharges liquid in the steeper; After liquid in the container to be impregnated is discharged fully; Close feed liquor valve and air compressor machine; Open blow-off valve and make pressure and extraneous balance in the steeper, unlatching steeper lid takes out refractory materials or the metal founding oven dry gets final product.The refractory materials or the metal founding that adopt above-mentioned impregnation technology to handle improve 2-5 doubly work-ing life.Yet its solution is the low excessively defective of bringing of light-weight refractory extrudate density; Through filling up the Lu Tafen resin in the dipping pore; Porosity drops to below 3% from 13%, makes the slit of internal injury obtain bonding, and hot environment has been cut off production medium osmosis chance; Can keep the refractory materials Chemical Composition to remain unchanged for a long period of time, thereby improve work-ing life.This method is not only flooded the modified technique complicacy; And the aluminium dihydrogen phosphate of dipping belongs to metaphosphoric acid, can not complete reaction generate phosphoric acid salt with aluminum oxide in the refractory materials, silicon-dioxide, Natural manganese dioxide, in high temperature, uses for a long time and separates out easily; Same Lu Tafen resin; In high temperature, use for a long time to burn easily and lose, finally cause filling and lost efficacy, so can only be used for the modification of non-direct contact pyritous light-weight refractory goods; Not ideal enough for direct contact pyritous compact heavy refractory product modified effect, secondly enlightenment can not improve heat-shock resistance.
Chinese patent CN101475402 uses phosphoric acid to improve the light-weight refractory brick mechanical property method, and it is that time of immersion is 2～5 hours in 25～85% the phosphoric acid solution that light fire brick is immersed in mass concentration; Taking-up refractory brick is put into 450～600 ℃ of High Temperature Furnaces Heating Apparatuss and is heat-treated, and is incubated 1～3 hour, cools to the light fire brick that room temperature obtains modification then with the furnace.Aluminum oxide, silicon-dioxide, Natural manganese dioxide can not complete reaction generate phosphoric acid salt in same impregnation of phosphoric acid and the refractory materials; In high temperature, use for a long time and separate out easily; So can only be used for noncontact pyritous light-weight refractory goods; Not ideal enough for direct contact pyritous compact heavy refractory product modified effect, secondly modification has just improved ultimate compression strength, and enlightenment can not improve heat-shock resistance.
Above-mentioned deficiency still has is worth improved place.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned prior art, provides a kind of and can improve mechanical property, can improve thermal shock resistance again, contacts raising compact heavy refractory product mechanical property and heat-shock resistance method that high-temperature behavior can not reduce for a long time.
The object of the invention realizes that main the improvement is the compact heavy refractory product that just makes, and impregnated in the activated magnesia and/or the activated alumina that are added phosphoric acid weight 3～5wt% by the phosphoric acid of concentration >=85wt%; The aqueous phosphate solution that complete reaction forms fully adsorbs, and makes aluminum oxide, silicon-dioxide, Natural manganese dioxide reaction in submerged phosphoric acid salt and the refractory product generate crystalloid phosphoric acid salt through 600-800 ℃ of baking again and resides in the defective such as crackle, repair the tiny crack isostructuralism defective of manufacturing processed existence; Through plugging the gap, strengthen refractory product density, reduce void content; Enhanced toughness; Improve over-all properties, and resident owing to having formed crystalloid phosphoric acid salt, and long term high temperature uses and can not separate out; Guaranteed that the modification performance does not reduce because of use; Have long work-ing life, overcome the deficiency of prior art, realize the object of the invention.Specifically; The present invention improves compact heavy refractory product mechanical property and heat-shock resistance method, comprises that batching, batch mixing, pressure forming, sintering process compact heavy refractory product, it is characterized in that the compact heavy refractory product that makes is immersed; The activated magnesia and/or the activated alumina that add phosphoric acid weight 3～5wt% by the phosphoric acid of concentration >=85wt%; The aqueous phosphate solution that reaction forms, the front and back of weighing change greater than+5%～+ 8% taking-up dry, the warm processing in 600～800 ℃.
Among the present invention
It is low excessively to dispose phosphatic phosphoric acid concentration, can be prone to form Vanadium Pentoxide in FLAKES because of washiness, and baking parses easy the branch, and is ineffective.For example find in the test that phosphoric acid concentration is lower than 85wt%, find in the bake process that adularescent liquid flows out; The concentration height then flows out few, so phosphoric acid concentration should be high as far as possible.
Dipping is more excellent to soak into gained refractory product performance fully, because compact heavy refractory product density is high relatively, time of immersion is short, causes surface impregnation easily, and interior in-core soaks into, and causes the ectonexine dipping inhomogeneous, influences overall performance and improves.Can judge that not increase weight basically, for example weightening finish+5%～+ 8% is a judgement criteria through weight change before and after the dipping.
600～800 ℃ middle temperature is handled; Mainly be aluminum oxide, silicon-dioxide, Natural manganese dioxide in submerged phosphoric acid salt and the refractory product is further reacted generate stable crystalloid phosphoric acid salt resident; Prevent not form stable crystalloid phosphoric acid salt and use in high temperature for a long time and separate out that (dipping only plays interim filling like this; Can not be resident for a long time, disappear along with long term high temperature uses progressively).Test finds that storing temperature is lower than 600 ℃, then is difficult for being completed into stable crystalloid phosphoric acid salt, and the immersion thing gets damp easily to run off in storage and reduces; Temperature is too high, for example then there is no need greater than 800 ℃, can increase energy consumption.
Compact heavy refractory product among the present invention is in particular mullite silicon carbide brick and mullite brick that the coke dry quenching furnace working lining uses.
Said interval range among the present invention for testing definite preferred values, is not the accurate end value on the mathematical meaning, and suitably departing from not is cannot.
The present invention improves compact heavy refractory product mechanical property and heat-shock resistance method, and with respect to prior art, because the phosphoric acid salt dipping of generation has been reacted in employing, the temperature baking makes reactive metal oxide generation phosphagel phosphaljel (AlPO in phosphoric acid salt and the refractory product in adding
4), phosphoric acid silicon (SiP
2O
7), crystalloid phosphoric acid salt such as trimagnesium phosphate is resident; Phosphagel phosphaljel composition for example; Improve 3-4%, filled and repaired the inner inevitable all kinds of defectives (like microtexture property defectives such as pore, small solution cavity, fine cracks) that produce of compact heavy refractory product production process, strengthened hole wall structure intensity; And can not separate out the minimizing of running off owing to become the use of crystalloid phosphoric acid salt long term high temperature, not reducing immersion amount.Because the Natural manganese dioxide in the aqueous phosphate solution belongs to basic metal, in the coke dry quenching furnace use, stop the erosion of coke in addition, be equivalent to wear dress, thereby protected the refractory product internal structure.Not only improved the refractory product mechanical property, for example density improves 3-6%, and intensity improves about 20-40%; 1100 ℃ of high temperature break resistant intensities by original about 23, are brought up to 28 (mullite-carborundums) respectively; With original about 18 bring up to 25 (mullites), also reduced void content; And improved compact heavy refractory product toughness; Void content is reduced, thereby has improved thermal shock resistance, 1100 ℃ of water-cooleds; Bring up to (mullite-carborundum) 70 times by 50 times respectively; With bring up to (mullite) 14 times 3 times, cut resistance test drops to 5.4% (weighting method) by original 6.3%, can make coke dry quenching furnace prolong 1～2 times work-ing life.The inventive method modified technique is simple; Be easy to regulate and control; Cost is low, economical and practical, become economical and practical prolongation compact heavy refractory product for example the effective ways in coke dry quenching furnace refractory brick work-ing life (prolong coke dry quenching furnace work-ing life, reduce the coke dry quenching furnace frequency of maintenance; Practice thrift maintenance cost, improve production capacity).After adopting the inventive method dipping, the brick color and luster is deepened to some extent, and human eye can contrast and distinguish, this can become whether adopt one of the inventive method dipping recognition methods; Secondly, through the comparison and detection performance index, also can judge as detecting.The inventive method is used for eliminating the structural defect that the compact heavy refractory product moulding produces, and can be used for the compact heavy refractory product of various materials, improves their mechanical properties and resistance to shock.
Below in conjunction with two exemplary embodiments, the present invention is further understood in exemplary illustration and help, but the embodiment detail only is for the present invention is described; Do not represent the present invention to conceive whole technical schemes down; Therefore should not be construed as the qualification to the total technical scheme of the present invention, some are In the view of the technician, and the unsubstantiality that does not depart from the present invention's design increases and/or change; For example simple the change or replacement of technical characterictic to have same or similar technique effect all belongs to protection domain of the present invention.
Description of drawings
Fig. 1 is with the impregnated mullite of trimagnesium phosphate-SiC brick section photo.
The untreated mullite of Fig. 2-SiC brick section photo.
Section photo after the impregnated mullite of Fig. 3 trimagnesium phosphate-SiC brick thermal shock test.
Section photo after the untreated mullite of Fig. 4-SiC brick thermal shock test.
Embodiment
Embodiment: 30wt% silit, the 65wt% mullite, 5wt% clay wedding agent, particle diameter is: the 5-3mm coarse particles of 45wt%; The 1-0mm small-particle of 20wt%, the following fine powder of 35wt%200 order mixes each material and adds about water 4wt%; Mix with the forced action type mixing roll, brick, drying are pressed in discharging; Put into stove and be warming up to 1450 ℃ of high temperature sinterings 48 hours, be incubated 24 hours, cooling obtains the coke dry quenching furnace bracket with mullite silicon carbide compact heavy refractory brick (apparent porosity is 15%～25%).
The coke dry quenching furnace cooling section is used mullite brick, 70wt% mullite, 20wt% andaluzite; 5wt% Alpha-alumina ultrafine powder (≤1 micron), 5wt% clay wedding agent, size grading is the same; Batch mixing adds water and mixes the pressure brick; Put into stove and be warming up to 1420 ℃ of high temperature sinterings 48 hours, be incubated 24 hours, cool off cooling section with mullite firebrick (apparent porosity is 15%～25%).
Use concentration to be 85wt% phosphoric acid; The activated magnesia that adds phosphoric acid weight 5wt%, reaction forms trimagnesium phosphate solution, and aforementioned two kinds of bricks are immersed in respectively in the trimagnesium phosphate solution that is disposed; Change before and after weighing greater than+6wt% (weightening finish 6wt%) takes out dry; Till the no phosphoric acid salt trickling in refractory brick surface, put into kiln and handled naturally cooling 3 hours 650 ℃ of temperature.Performance sees Table 1, and comparing result sees Table 2.
To those skilled in the art, under this patent design and specific embodiment enlightenment, some distortion that can directly derive or associate from this patent disclosure and general knowledge; Those of ordinary skills will recognize also can adopt additive method; Or use substituting of known technology in the prior art always, and the mutual various combination between characteristic, other compact heavy refractory products for example adopted; Also have similar effect through dip treating, can be directly with primary magnesium phosphate [Mg (H
2PO
4)
2] solution, perhaps add activated alumina again in the phosphoric acid again and flood, or the like unsubstantiality change, can be employed equally, can both realize and basic identical function of the foregoing description and effect, launch for example no longer one by one to describe in detail, all belong to this patent protection domain.
Table 1 dipping back compact heavy mullite-SiC refractory brick physical and chemical index
Table 2 dip treating and the not brick measured performance comparison of dip treating
Can know by table 2,, strengthen four big technical indicators greatly, improve thermal shock resistance simultaneously with trimagnesium phosphate solution impregnation compact heavy mullite-SiC brick and mullite brick.
The explanation of accompanying drawing photo
Fig. 1 and Fig. 2 relatively are significantly improved through the brick compactness extent after the dip treating.
Fig. 3 and Fig. 4 are relatively; Dip treating and the mullite of dip treating-SiC brick not →; Carry out the test of 1100 ℃-water-cooled thermal shock resistance simultaneously; Only have fine crack to occur after the brick thermal shock test that Fig. 3 dip treating is crossed 16 times, Fig. 4 bigger transverse crack do not occur after the dip treating brick thermal shock test of crossing 9 times, shows that the thermal shock resistance of dip treating brick obviously is better than the not brick of dip treating.
Claims (3)
1. improve compact heavy refractory product mechanical property and heat-shock resistance method; Comprise that batching, batch mixing, pressure forming, sintering process compact heavy refractory product; It is characterized in that the compact heavy refractory product that makes is immersed, add activated magnesia and/or the activated alumina of phosphoric acid weight 3～5wt%, the aqueous phosphate solution that reaction forms by the phosphoric acid of concentration >=85wt%; Change+5%～+ 8% before and after weighing and take out drying, through 600～800 ℃ of processing.
2. according to claim 1 said raising compact heavy refractory product mechanical property and heat-shock resistance method, it is characterized in that said compact heavy refractory product uses mullite silicon carbide brick and mullite brick for the coke dry quenching furnace working lining.
3. according to claim 2 said raising compact heavy refractory product mechanical property and heat-shock resistance method, it is characterized in that mullite silicon carbide brick and mullite brick apparent porosity are 15%～25%.
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| CN 200910263025 CN101723693B (en) | 2009-12-15 | 2009-12-15 | Method for improving mechanical performance and thermal shock resistance of compact heavy refractory product |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229500A (en) * | 2010-07-27 | 2011-11-02 | 广州市石基耐火材料厂 | Preparation method for compact zirconite overflow brick with high breaking-resistance and low expansion |
| CN103130516B (en) * | 2011-12-02 | 2014-12-03 | 河南省新密市青屏耐火材料有限责任公司 | Mullite carborundum brick used for dry quenching stove |
| CN102765955B (en) * | 2012-08-14 | 2014-11-05 | 湖南仁海科技材料发展有限公司 | Fireproof material and preparation method thereof |
| CN112279660A (en) * | 2020-11-02 | 2021-01-29 | 阳泉市千诚耐火材料销售有限公司 | Production method of furnace brick for light-burned activating furnace |
| CN116283234A (en) * | 2023-03-29 | 2023-06-23 | 安徽精公检测检验中心有限公司 | Environment-friendly fireproof magnesia brick for cement kiln and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134676A (en) * | 2006-08-30 | 2008-03-05 | 宝山钢铁股份有限公司 | Fire resistive material for coke oven door |
| CN101269983A (en) * | 2008-04-23 | 2008-09-24 | 宜兴市丁山耐火器材有限公司 | Stress buffering type fire resistive material for dry coke quenching equipment and method for manufacturing same |
| CN101386545A (en) * | 2008-10-23 | 2009-03-18 | 武汉理工大学 | Method for improving light-weight refractory brick mechanical property |
| CN101475402A (en) * | 2009-01-19 | 2009-07-08 | 武汉理工大学 | Method for improving light-weight refractory brick mechanical property by using phosphoric acid |
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2009
- 2009-12-15 CN CN 200910263025 patent/CN101723693B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134676A (en) * | 2006-08-30 | 2008-03-05 | 宝山钢铁股份有限公司 | Fire resistive material for coke oven door |
| CN101269983A (en) * | 2008-04-23 | 2008-09-24 | 宜兴市丁山耐火器材有限公司 | Stress buffering type fire resistive material for dry coke quenching equipment and method for manufacturing same |
| CN101386545A (en) * | 2008-10-23 | 2009-03-18 | 武汉理工大学 | Method for improving light-weight refractory brick mechanical property |
| CN101475402A (en) * | 2009-01-19 | 2009-07-08 | 武汉理工大学 | Method for improving light-weight refractory brick mechanical property by using phosphoric acid |
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