CN105859305A - Method for preparing hydration-resistant and thermal-shock-resistant calcium oxide crucible by dry process - Google Patents

Method for preparing hydration-resistant and thermal-shock-resistant calcium oxide crucible by dry process Download PDF

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CN105859305A
CN105859305A CN201610182706.3A CN201610182706A CN105859305A CN 105859305 A CN105859305 A CN 105859305A CN 201610182706 A CN201610182706 A CN 201610182706A CN 105859305 A CN105859305 A CN 105859305A
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张峰
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Xian Shiyou University
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Abstract

The invention discloses a method for preparing a hydration-resistant and thermal-shock-resistant calcium oxide crucible by a dry process. The method comprises the following steps: purifying quicklime lumps, and crushing and fining the quicklime lumps with calcium oxide purity higher than 96%; mixing the quicklime fines with additives so as to form a mixture, and then, pressing the mixture into brick-shaped products; carrying out first-time temperature-controlled sintering on the brick-shaped products; crushing the sintered material obtained after first-time sintering, carrying out screening, then, carrying out proportioning proportionally, and carrying out uniform mixing so as to form clinker; loading the clinker obtained through carrying out uniform mixing in the step (4) to a crucible die, carrying out compaction on a vibrating platform, and carrying out pressing by a cold isostatic press; and putting a calcium oxide crucible green body in an electric furnace, carrying out second-time temperature-controlled sintering according to a secondary temperature-control curve, thereby obtaining a calcium oxide crucible product. The calcium oxide crucible prepared by using the method has the advantages that the hydration resistance is higher, the thermal-shock resistance is better, the sintering is denser, and the strength of the crucible is good.

Description

A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock
[technical field]
The present invention relates to high melt oxide refractories technical field, be specifically related to the dry method oxygen of a kind of hydration-resisting, anti-thermal shock Change calcium crucible preparation method.
[background technology]
At present the demand of ultra-clean metal and alloy increases day by day, needs in a large number in vacuum contact field electrically, mechanical performance excellence Chromiumcopper, copper-tungsten, need titanium alloy, memorial alloy in the field such as space flight, medical science, crucible die industry, oil Pipeline needs ultra clean steel, special steel.
For meeting the demand in above-mentioned field, metal and the purity of alloy, performance during materials processing, need to be improved, a lot of in the case of all use Purification smelted by vaccum sensitive stove, and the crucible used mostly is graphite crucible (graphite boat) or magnesia crucible, in smelting process It is very easy to penetrate into substantial amounts of carbon or oxygen supplement, affects purity and electric property, the mechanical property of material.Lime crucible at metal or The excellent performance of de-O, N, S, P etc. in alloy smelting, is especially suitable for substituting graphite crucible or magnesia crucible.But calcium oxide earthenware The easy aquation of crucible, thermal shock resistance is the best, and Reusability easily ftractures, and affects production efficiency.
[summary of the invention]
For technical problem present in above-mentioned prior art, the present invention is on the basis of prior art, it is provided that a kind of hydration-resisting, anti- The dry oxidation calcium crucible preparation method of thermal shock, lime crucible prepared by the present invention has stronger hydration-resisting, thermal shock resistance, And can solve the problem that in lime crucible, calcium oxide purity is low, and introduce impurity easily to the metal or alloy of melting, lime crucible is easy to crack Technical problem.
The present invention is mainly achieved through the following technical solutions the purpose that foregoing invention is created.
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, quick lime block purifies, and by broken for the calcium oxide purity quick lime block more than 96% and refinement, obtains quick lime Fines;
Step 2, is mixed to form compound by quick lime fines and additive, then compound is pressed into brick shape goods;
Brick shape goods are piled up in temp. Control electric stove neatly, are carried out first sintering by step 3, have sintered rear natural cooling and have obtained Sintering feed;
Step 4, carries out the sintering feed after first sintering crushing, sieving, and is then the sintering feed of below 4mm by granularity Mix homogeneously, forms grog;
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold Tool puts into cold isostatic press compacting, obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time and sinters, has sintered rear natural cooling, obtained oxygen Change calcium crucible.
Quick lime fines granularity in described step one is less than 2mm.
Using forcing press to suppress in described step 2, the ram pressures value of forcing press is 10~20MPa, uses forcing press twice Compressed mixture obtains brick shape goods, and the weight of brick shape goods is 2~2.5kg.
Additive in described step 2 includes the following components by compound oeverall quality percentage mix:
Described first sintering comprises the following steps:
By the intensification of 1~2.5 hour, ambient temperature is risen to 300 DEG C, and is incubated 0.5~2 hour;
Afterwards by the intensification of 1~3 hour, ambient temperature is risen to 1000 DEG C from 300 DEG C, and is incubated 0.5~2 hour;
Afterwards by the intensification of 1~2 hour, ambient temperature is risen to 1380 DEG C from 1000 DEG C, and is incubated 0.5~4 hour.
Described first sintering may also include states following steps: by the intensification of 2 hours, ambient temperature risen to from 1380 DEG C 1680 DEG C, and it is incubated 2~3 hours.
Sintering feed in described step 4 makes a distinction according to following mass percent proportioning mix homogeneously with surmising of sintering feed:
Described isostatic cool pressing compressing head is suppressed with the pressure of 160-200MPa, and pressurize 60-180s.
Described second time sintering comprises the following steps:
By the intensification of 1~3 hour, ambient temperature is risen to 300 DEG C, and is incubated 0.5~2 hour;
Afterwards by the intensification of 1~3 hour, ambient temperature is risen to 1000 DEG C from 300 DEG C, and is incubated 0.5~2.5 hour;
Afterwards by the intensification of 1~1.5 hour, ambient temperature is risen to 1380 DEG C from 1000 DEG C, and is incubated 0.5~4 hour.
Described second time sintering may also include states following steps: by the intensification of 1~2 hour, ambient temperature risen to from 1380 DEG C 1680 DEG C, and it is incubated 2~4 hours.
Compared with prior art, the present invention at least have the advantages that the present invention select quick lime fines that purity is higher and The additive that the composition such as calcium fluoride, boric acid is constituted makes compound, then final molding after twice compacting, twice temperature control sintering, The lime crucible consistency manufactured by the present invention is higher, and specific area is less, so hydration-resisting ability is higher, simple evacuation is packed After can keep 1 month not aquation.The compound additive using the composition such as calcium fluoride, zirconium dioxide to constitute can expand receipts at high temperature Contracting effect, can produce a large amount of atomic hair check inside crucible, adds the hot buffer capacity of crucible, and therefore thermal shock resistance is more preferably, Reuse often, averagely can use 20 stoves.
Further, owing to the present invention uses two-step sintering, additive package during first sintering, it is possible to make distribution of additives Being more uniformly distributed, sinter finer and close, crucible intensity is more preferable.
Further, the present invention uses the additive of Multiple components, reduces sintering temperature, thus reduces cost of manufacture, saves The energy.
[detailed description of the invention]
Below in conjunction with detailed description of the invention, the present invention is further explained.
Embodiment 1:
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, carries out crushing, refining by the calcium oxide purity quick lime block more than 96%, obtains the granularity life less than 2mm Calx fines;
Step 2, mixs homogeneously above-mentioned quick lime fines with additive and obtains the compound of 2kg, and wherein quick lime fines accounts for mixing The 91.9% of material gross mass percentage ratio, additive includes the following component accounting for compound gross mass percentage ratio, the calcium fluoride of 3%, 3.5% Zirconium dioxide, the titanium dioxide of 1%, the boric acid of 5 ‰ and the chromic oxide of 1 ‰;Then, with forcing press, compound is carried out Twice compacting, the ram pressures value of forcing press is 16MPa for the first time, and the ram pressures value of forcing press is 12MPa for the second time, will Compound is pressed into the brick shape goods of every piece of 2kg;
Brick shape goods are piled up neatly in temp. Control electric stove by step 3, carry out the sintering of temperature control for the first time, and sintering process is: by 1 Hour intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 3 hours, by ambient temperature from 300 DEG C rise to 1000 DEG C, and are incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 1 hour;Afterwards by the intensification of 2 hours, ambient temperature is risen to 1680 DEG C from 1380 DEG C, and is incubated 2 hours, whole Individual 11.5 hours temperature-rise period used times;After temperature control has sintered for the first time, natural cooling, obtain sintering feed;
Step 4, the sintering feed after first time temperature control being sintered carries out crushing, sieving, and then makes a distinction with the granularity of sintering feed, And according to following mass percent proportioning mix homogeneously, form grog:
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold It is compressing with the ram pressures of 160MPa that tool puts into cold isostatic press, and pressurize 60s obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time temperature control sintering, and sintering process was: by 1 hour Intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 3 hours, by ambient temperature from 300 DEG C Rise to 1000 DEG C, and be incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 1 hour;Afterwards by the intensification of 2 hours, ambient temperature is risen to 1680 DEG C from 1380 DEG C, and is incubated 2 hours, whole Individual 11.5 hours temperature-rise period used times;After temperature control has sintered for the second time, after natural cooling, i.e. obtain lime crucible.
Embodiment 2
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, carries out crushing, refining by the calcium oxide purity quick lime block more than 96%, obtains the granularity life less than 2mm Calx fines;
Step 2, mixs homogeneously above-mentioned quick lime fines with additive and obtains the compound of 2kg, and wherein quick lime fines accounts for mixing The 91.5% of material gross mass percentage ratio, additive includes the following component accounting for compound gross mass percentage ratio, 1% calcium fluoride, 3% Zirconium dioxide, the titanium dioxide of 4%, the boric acid of 2 ‰ and the chromic oxide of 3 ‰;Then, with forcing press, compound is carried out two Secondary compacting, the ram pressures value of forcing press is 16MPa for the first time, and the ram pressures value of forcing press is 19MPa for the second time, will be mixed Close material and be pressed into the brick shape goods of every piece of 2kg;
Brick shape goods are piled up neatly in temp. Control electric stove by step 3, carry out the sintering of temperature control for the first time, and sintering process is: by 1 Hour intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 3 hours, by ambient temperature from 300 DEG C rise to 1000 DEG C, and are incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 2.5 hours, whole 9 hours temperature-rise period used times;After temperature control has sintered for the first time, natural cooling obtains sintering feed;
Step 4, the sintering feed after first time temperature control being sintered carries out crushing, sieving, and then makes a distinction with the granularity of sintering feed, And according to following mass percent proportioning mix homogeneously, form grog:
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold It is compressing with the ram pressures of 170MPa that tool puts into cold isostatic press, and pressurize 90s obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time temperature control sintering, and sintering process was: by 1 hour Intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 3 hours, by ambient temperature from 300 DEG C Rise to 1000 DEG C, and be incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 2.5 hours, whole 9 hours temperature-rise period used times;After temperature control has sintered for the second time, after natural cooling, i.e. obtain oxidation Calcium crucible.
Embodiment 3
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, carries out crushing, refining by the calcium oxide purity quick lime block more than 98%, obtains the granularity life less than 2mm Calx fines;
Step 2, mixs homogeneously above-mentioned quick lime fines with additive and obtains the compound of 2.25kg, and wherein quick lime fines accounts for mixed Closing the 91.2% of material gross mass percentage ratio, additive includes the following component accounting for compound gross mass percentage ratio, the calcium fluoride of 4%, The zirconium dioxide of 4.5%, the boric acid of 3 ‰ and the chromic oxide of 5 ‰;Then, with forcing press, compound is carried out twice compacting, The ram pressures value of forcing press is 20MPa for the first time, and the ram pressures value of forcing press is 15MPa for the second time, is suppressed by compound Become the brick shape goods of every piece of 2.25kg;
Brick shape goods are piled up neatly in temp. Control electric stove by step 3, carry out the sintering of temperature control for the first time, and sintering process is: by 1.5 Hour intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 2 hours, by ambient temperature from 300 DEG C rise to 1000 DEG C, and are incubated 0.5 hour;Afterwards by the intensification of 1 hour, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 4 hours, whole 9.5 hours temperature-rise period used times;After temperature control has sintered for the first time, natural cooling obtains sintering feed;
Step 4, the sintering feed after first time temperature control being sintered carries out crushing, sieving, and then makes a distinction with the granularity of sintering feed, And according to following mass percent proportioning mix homogeneously, form grog:
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold It is compressing with the ram pressures of 200MPa that tool puts into cold isostatic press, and pressurize 60s obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time temperature control sintering, and sintering process was: by 2 hours Intensification, ambient temperature is risen to 300 DEG C, and is incubated 1 hour;Afterwards by the intensification of 1.5 hours, by ambient temperature from 300 DEG C Rise to 1000 DEG C, and be incubated 0.5 hour;Afterwards by the intensification of 1 hour, ambient temperature is risen to 1380 DEG C from 1000 DEG C, and It is incubated 0.5 hour;Afterwards by the intensification of 1 hour, ambient temperature is risen to 1680 DEG C from 1380 DEG C, and is incubated 4 hours, whole Individual 11.5 hours temperature-rise period used times;After temperature control has sintered for the second time, after natural cooling, i.e. obtain lime crucible.
Embodiment 4
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, carries out crushing, refining by the calcium oxide purity quick lime block more than 97%, obtains the granularity life less than 2mm Calx fines;
Step 2, mixs homogeneously above-mentioned quick lime fines with additive and obtains the compound of 2.25kg, and wherein quick lime fines accounts for mixed Closing the 90.5% of material gross mass percentage ratio, additive includes the following component accounting for compound gross mass percentage ratio, the calcium fluoride of 3%, The zirconium dioxide of 6% and the boric acid of 5 ‰;Then, with forcing press, compound carried out twice compacting, for the first time the pressure head pressure of forcing press Force value is 18MPa, and the ram pressures value of forcing press is 15MPa for the second time, and compound is pressed into the brick shape system of every piece of 2.25kg Product;
Brick shape goods are piled up neatly in temp. Control electric stove by step 3, carry out the sintering of temperature control for the first time, and sintering process is: by 1.5 Hour intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, by ambient temperature Rise to 1000 DEG C from 300 DEG C, and be incubated 0.5 hour;Afterwards by the intensification of 2 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 0.5 hour;Afterwards by the intensification of 2 hours, ambient temperature is risen to 1680 DEG C from 1380 DEG C, and is incubated 3 hours, Whole 11.5 hours temperature-rise period used times;After temperature control has sintered for the first time, natural cooling obtains sintering feed;
Step 4, the sintering feed after first time temperature control being sintered carries out crushing, sieving, and then makes a distinction with the granularity of sintering feed, And according to following mass percent proportioning mix homogeneously, form grog:
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold It is compressing with the ram pressures of 190MPa that tool puts into cold isostatic press, and pressurize 90s obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time temperature control sintering, and sintering process was: by 3 hours Intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 2 hours, by ambient temperature from 300 DEG C Rise to 1000 DEG C, and be incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 1 hour;Afterwards by the intensification of 1 hour, ambient temperature is risen to 1680 DEG C from 1380 DEG C, and is incubated 2 hours, whole Individual 11.5 hours temperature-rise period used times.After temperature control has sintered for the second time, after natural cooling, i.e. obtain lime crucible.
Embodiment 5
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, carries out crushing, refining by the calcium oxide purity quick lime block more than 98%, obtains the granularity life less than 2mm Calx fines;
Step 2, mixs homogeneously above-mentioned quick lime fines with additive and obtains the compound of 2.5kg, and wherein quick lime fines accounts for mixed Closing the 90.8% of material gross mass percentage ratio, additive includes the following component accounting for compound gross mass percentage ratio, the calcium fluoride of 3.5%, The zirconium dioxide of 2%, the titanium dioxide of 3%, the boric acid of 5 ‰ and the chromic oxide of 2 ‰;Then, with forcing press, compound is entered Twice compacting of row, the ram pressures value of forcing press is 12MPa for the first time, and the ram pressures value of forcing press is 18MPa for the second time, Compound is pressed into the brick shape goods of every piece of 2.5kg;
Brick shape goods are piled up neatly in temp. Control electric stove by step 3, carry out the sintering of temperature control for the first time, and sintering process is: by 1 Hour intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 2 hours, by ambient temperature from 300 DEG C rise to 1000 DEG C, and are incubated 1.5 hours;Afterwards by the intensification of 2 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 3.5 hours, whole 10.5 hours temperature-rise period used times;After temperature control has sintered for the first time, natural cooling is sintered Material;
Step 4, the sintering feed after first time temperature control being sintered carries out crushing, sieving, and then makes a distinction with the granularity of sintering feed, And according to following mass percent proportioning mix homogeneously, form grog:
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold It is compressing with the ram pressures of 200MPa that tool puts into cold isostatic press, and pressurize 120s obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time temperature control sintering, and sintering process is: little by 2.5 Time intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 2.5 hours, by ambient temperature from 300 DEG C rise to 1000 DEG C, and are incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 4 hours, whole 11.5 hours temperature-rise period used times;After temperature control has sintered for the second time, after natural cooling, i.e. obtain oxygen Change calcium crucible.
Embodiment 6
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, carries out crushing, refining by the calcium oxide purity quick lime block more than 98%, obtains the granularity life less than 2mm Calx fines;
Step 2, mixs homogeneously above-mentioned quick lime fines with additive and obtains the compound of 2.5kg, and wherein quick lime fines accounts for mixed Closing the 91.2% of material gross mass percentage ratio, additive includes the following component accounting for compound gross mass percentage ratio, the calcium fluoride of 6%, The zirconium dioxide of 1%, the titanium dioxide of 1%, the boric acid of 4 ‰ and the chromic oxide of 4 ‰;Then, with forcing press, compound is entered Twice compacting of row, the ram pressures value of forcing press is 12MPa for the first time, and the ram pressures value of forcing press is 20MPa for the second time, Compound is pressed into the brick shape goods of every piece of 2.5kg;
Brick shape goods are piled up neatly in temp. Control electric stove by step 3, carry out the sintering of temperature control for the first time, and sintering process is: by 2 Hour intensification, ambient temperature is risen to 300 DEG C, and is incubated 2 hours;Afterwards by the intensification of 3 hours, by ambient temperature from 300 DEG C Rise to 1000 DEG C, and be incubated 2 hours;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, and It is incubated 1 hour, whole 11.5 hours temperature-rise period used times;After temperature control has sintered for the first time, natural cooling obtains sintering feed;
Step 4, the sintering feed after first time temperature control being sintered carries out crushing, sieving, and then makes a distinction with the granularity of sintering feed, And according to following mass percent proportioning mix homogeneously, form grog:
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold It is compressing with the ram pressures of 175MPa that tool puts into cold isostatic press, and pressurize 180s obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time temperature control sintering, and sintering process was: by 1 hour Intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, by ambient temperature from 300 DEG C Rise to 1000 DEG C, and be incubated 1.5 hours;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 1 hour;Afterwards by the intensification of 1 hour, ambient temperature is risen to 1680 DEG C from 1380 DEG C, and is incubated 3 hours, whole Individual 11 hours temperature-rise period used times;After temperature control has sintered for the second time, after natural cooling, i.e. obtain lime crucible.
Embodiment 7
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, carries out crushing, refining by the calcium oxide purity quick lime block more than 96%, obtains the granularity life less than 2mm Calx fines;
Step 2, mixs homogeneously above-mentioned quick lime fines with additive and obtains the compound of 2.5kg, and wherein quick lime fines accounts for mixed Closing the 90.9% of material gross mass percentage ratio, additive includes the following component accounting for compound gross mass percentage ratio, the calcium fluoride of 1%, The zirconium dioxide of 2%, the titanium dioxide of 6% and the boric acid of 1 ‰;Then, with forcing press compound carried out twice compacting, first The ram pressures value of secondary forcing press is 18MPa, and the ram pressures value of forcing press is 16MPa for the second time, is pressed into often by compound The brick shape goods of block 2.5kg;
Brick shape goods are piled up neatly in temp. Control electric stove by step 3, carry out the sintering of temperature control for the first time, and sintering process is: by 2.5 Hour intensification, ambient temperature is risen to 300 DEG C, and is incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, by ambient temperature Rise to 1000 DEG C from 300 DEG C, and be incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to from 1000 DEG C 1380 DEG C, hand over insulation 2.5 hours, whole 9 hours temperature-rise period used times;After temperature control has sintered for the first time, natural cooling obtains To sintering feed;
Step 4, the sintering feed after first time temperature control being sintered carries out crushing, sieving, and then makes a distinction with the granularity of sintering feed, And according to following mass percent proportioning mix homogeneously, form grog:
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold It is compressing with the ram pressures of 180MPa that tool puts into cold isostatic press, and pressurize 150s obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time temperature control sintering, and sintering process was: by 1 hour Intensification, ambient temperature is risen to 300 DEG C, and is incubated 2 hours;Afterwards by the intensification of 1 hour, by ambient temperature from 300 DEG C Rise to 1000 DEG C, and be incubated 0.5 hour;Afterwards by the intensification of 1.5 hours, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 1 hour;Afterwards by the intensification of 2 hours, ambient temperature is risen to 1680 DEG C from 1380 DEG C, and is incubated 2 hours, whole Individual 11 hours temperature-rise period used times;After temperature control has sintered for the second time, after natural cooling, i.e. obtain lime crucible.
Embodiment 8
A kind of hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, comprise the following steps:
Step one, carries out crushing, refining by the calcium oxide purity quick lime block more than 98%, obtains the granularity life less than 2mm Calx fines;
Step 2, mixs homogeneously above-mentioned quick lime fines with additive and obtains the compound of 2kg, and wherein quick lime fines accounts for mixing The 92.1% of material gross mass percentage ratio, additive includes the following component accounting for compound gross mass percentage ratio, the calcium fluoride of 5%, 2% Titanium dioxide, the boric acid of 3 ‰ and the chromic oxide of 6 ‰;Then, with forcing press compound carried out twice compacting, first The ram pressures value of secondary forcing press is 16MPa, and the ram pressures value of forcing press is 18MPa for the second time, is pressed into often by compound The brick shape goods of block weight 2kg;
Brick shape goods are piled up neatly in temp. Control electric stove by step 3, carry out the sintering of temperature control for the first time, and sintering process is: by 1 Hour intensification, ambient temperature is risen to 300 DEG C, and is incubated 1.5 hours;Afterwards by the intensification of 1 hour, by ambient temperature from 300 DEG C rise to 1000 DEG C, and are incubated 0.5 hour;Afterwards by the intensification of 1 hour, ambient temperature is risen to 1380 DEG C from 1000 DEG C, And it is incubated 4 hours, whole 9 hours temperature-rise period used times;After temperature control has sintered for the first time, natural cooling obtains sintering feed;
Step 4, the sintering feed after first time temperature control being sintered carries out crushing, sieving, and then carries out district by the granularity with sintering feed Point, and according to following mass percent proportioning mix homogeneously, form grog:
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold It is compressing with the ram pressures of 180MPa that tool puts into cold isostatic press, and pressurize 250s obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time temperature control sintering, and sintering process was: by 1 hour Intensification, ambient temperature is risen to 300 DEG C, and is incubated 2 hours;Afterwards by the intensification of 1.5 hours, by ambient temperature from 300 DEG C Rise to 1000 DEG C, and be incubated 2.5 hours;Afterwards by the intensification of 1 hour, ambient temperature is risen to 1380 DEG C from 1000 DEG C, and It is incubated 2 hours;Afterwards by the intensification of 1 hour, ambient temperature is risen to 1680 DEG C from 1380 DEG C, and is incubated 2.5 hours, whole Individual 13.5 hours temperature-rise period used times;After temperature control has sintered for the second time, after natural cooling, i.e. obtain lime crucible.
The preparation method of the present invention carries out two-step sintering, and additive package during first sintering, and distribution of additives is the most equal Even, sinter finer and close, crucible intensity is good;Use the additive of Multiple components, i.e. reduce sintering temperature, improve again hydration-resisting Property and thermal shock resistance, use the present invention preparation method manufacture lime crucible, its hydration-resisting ability is higher, simple evacuation 1 month not aquation can be kept after packaging;Thermal shock resistance more preferably, is reused often, averagely can use 20 stoves.

Claims (10)

1. a hydration-resisting, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that comprise the following steps:
Step one, quick lime block purifies, and by broken for the calcium oxide purity quick lime block more than 96% and refinement, obtains quick lime Fines;
Step 2, is mixed to form compound by quick lime fines and additive, then compound is pressed into brick shape goods;
Brick shape goods are piled up in temp. Control electric stove neatly, are carried out first sintering by step 3, have sintered rear natural cooling and have obtained Sintering feed;
Step 4, carries out the sintering feed after first sintering crushing, sieving, and is then the sintering feed of below 4mm by granularity Mix homogeneously, forms grog;
Step 5, in step 4, the grog of mix homogeneously loads crucible die, jolt ramming on vibration platen, then by crucible mold Tool puts into cold isostatic press compacting, obtains lime crucible idiosome;
Step 6, puts in electric furnace by lime crucible idiosome, carries out second time and sinters, has sintered rear natural cooling, obtained oxygen Change calcium crucible.
Hydration-resisting the most according to claim 1, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute State the quick lime fines granularity in step one less than 2mm.
Hydration-resisting the most according to claim 1, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute Stating and use forcing press to suppress in step 2, the ram pressures value of forcing press is 10~20MPa, and twice mixed with forcing press compacting Closing material and obtain brick shape goods, the weight of brick shape goods is 2~2.5kg.
Hydration-resisting the most according to claim 1, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute State the additive in step 2 and include the following components by compound oeverall quality percentage mix:
Hydration-resisting the most according to claim 1, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute State first sintering to comprise the following steps:
By the intensification of 1~2.5 hour, ambient temperature is risen to 300 DEG C, and is incubated 0.5~2 hour;
Afterwards by the intensification of 1~3 hour, ambient temperature is risen to 1000 DEG C from 300 DEG C, and is incubated 0.5~2 hour;
Afterwards by the intensification of 1~2 hour, ambient temperature is risen to 1380 DEG C from 1000 DEG C, and is incubated 0.5~4 hour.
Hydration-resisting the most according to claim 5, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute State first sintering to may also include and state following steps: by the intensification of 2 hours, from 1380 DEG C, ambient temperature is risen to 1680 DEG C, And it is incubated 2~3 hours.
Hydration-resisting the most according to claim 1, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute The sintering feed stated in step 4 makes a distinction according to following mass percent proportioning mix homogeneously with the granularity of sintering feed:
Hydration-resisting the most according to claim 1, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute State isostatic cool pressing compressing head to suppress with the pressure of 160-200MPa, and pressurize 60-180s.
Hydration-resisting the most according to claim 1, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute State second time sintering to comprise the following steps:
By the intensification of 1~3 hour, ambient temperature is risen to 300 DEG C, and is incubated 0.5~2 hour;
Afterwards by the intensification of 1~3 hour, ambient temperature is risen to 1000 DEG C from 300 DEG C, and is incubated 0.5~2.5 hour;
Afterwards by the intensification of 1~1.5 hour, ambient temperature is risen to 1380 DEG C from 1000 DEG C, and is incubated 0.5~4 hour.
Hydration-resisting the most according to claim 9, the dry oxidation calcium crucible preparation method of anti-thermal shock, it is characterised in that: institute State to sinter may also include for the second time and state following steps: by the intensification of 1~2 hour, ambient temperature is risen to 1680 DEG C from 1380 DEG C, And it is incubated 2~4 hours.
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CN109485441A (en) * 2019-01-10 2019-03-19 明光瑞尔非金属材料有限公司 A kind of blast furnace ceramic cup refractory material and preparation method thereof
CN113443923A (en) * 2020-03-24 2021-09-28 中国科学院金属研究所 Preparation method of CaO crucible for vacuum induction melting of Ti alloy
CN115991594A (en) * 2022-12-18 2023-04-21 本钢板材股份有限公司 Lime tundish slag blocking weir

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Publication number Priority date Publication date Assignee Title
CN109095902A (en) * 2018-09-12 2018-12-28 江苏徐耐新材料科技股份有限公司 A kind of glass furnace paving brick and its production technology
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CN109485441A (en) * 2019-01-10 2019-03-19 明光瑞尔非金属材料有限公司 A kind of blast furnace ceramic cup refractory material and preparation method thereof
CN113443923A (en) * 2020-03-24 2021-09-28 中国科学院金属研究所 Preparation method of CaO crucible for vacuum induction melting of Ti alloy
CN115991594A (en) * 2022-12-18 2023-04-21 本钢板材股份有限公司 Lime tundish slag blocking weir
CN115991594B (en) * 2022-12-18 2024-01-09 本钢板材股份有限公司 Lime tundish slag blocking weir

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