CN106116571A - A kind of compact zircon brick and preparation method thereof - Google Patents

A kind of compact zircon brick and preparation method thereof Download PDF

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CN106116571A
CN106116571A CN201610509045.0A CN201610509045A CN106116571A CN 106116571 A CN106116571 A CN 106116571A CN 201610509045 A CN201610509045 A CN 201610509045A CN 106116571 A CN106116571 A CN 106116571A
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zircon
micropowder
brick
calcining
compact
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萧子良
蒋亚丝
刘华利
朱其贞
刘仲超
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GUANGZHOU SHIJI REFRACTORIES FACTORY
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Abstract

The invention discloses a kind of compact zircon brick and preparation method thereof, following components is included: the quartz micropowder of 31% 33%, zirconium oxide micropowder, 0 0.5% organic bond and the additive surplus of 65% 68% according to weight ratio, each component peeked amount sum is equal to 100%, mean diameter D50≤10 μm of described quartz micropowder, mean diameter D50≤10 μm of zirconium oxide micropowder.The compact zircon brick of the present invention has the advantage high-quality, stable, highly purified and impurity content is few.

Description

A kind of compact zircon brick and preparation method thereof
Technical field
The present invention relates to the synthesis field of refractory material, be specifically related to a kind of compact zircon brick and preparation method thereof.
Background technology
Common zircon brick typically uses zircon sand to produce, by zircon sand being worn into micropowder aftershaping, after re-sintering It is processed as finished product.And the zircon stone brick material that some purity requirements are higher, the most simply use selected zircon sand, and by pickling, Produce as raw material after the certain methods remove impurity such as calcining.But it is special that existing zircon stone brick material still can not meet some The requirement of glass.
Along with the development of glass material, special glass requires more and more higher, and some old zircon materials have been opened Beginning not catch up with development, its cupric or iron content all severe overweights, impurity does not the most adapt to the requirement of specific glass.
Summary of the invention
In place of it is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of compact zircon brick and preparation side thereof Method.
A kind of compact zircon brick of the present invention, according to weight ratio include following components: 31%-33% quartz micropowder, The zirconium oxide micropowder of 65%-68%, 0-0.5% organic bond and additive surplus, each component peeked amount sum is equal to 100%, mean diameter D50≤10 μm of described quartz micropowder, mean diameter D50≤10 μm of zirconium oxide micropowder.
As a further improvement on the present invention, described additive includes that titanium oxide, yittrium oxide, lanthana, cerium oxide, silicon are molten Glue or waterglass.
As a further improvement on the present invention, described additive include the titanium oxide of 0-1.0%, the yittrium oxide of 0-0.3%, Lanthana or cerium oxide, the Ludox of 0-1.5% or the waterglass of 0-1.5%, additive also includes the water reducer of 0-0.3%.
The preparation method of the compact zircon brick of the present invention, comprises the following steps:
S1: glass sand and the high-purity mangesium oxide zirconium of buying are calcined respectively, obtains calcining quartz sand and forges Burn zirconium oxide, SiO in described glass sand2Content >=99.5%, ZrO in high-purity mangesium oxide zirconium2Content >= 99.5%.
S2: calcining quartz sand and calcined zirconia are obtained quartz mud and zirconium oxide mud by ball mill pulverizing respectively.
S3: pass through respectively to dry by quartz mud and zirconium oxide mud, obtains the drying material of correspondence, then by drying material difference Beat powder;Sieve respectively after beating powder, obtain quartz micropowder and zirconium oxide micropowder.
S4: according to formula proportion quartz micropowder to be asked for, zirconium oxide micropowder, organic bond and additive, carry out mix grinding, Obtain mixing mud.
S5: dried by above-mentioned mixing mud, obtains drying material and beating powder, sieves, obtain high-purity synthesis zirconium after beating powder Diamond stone raw material.
S6: above-mentioned high-purity synthesis zircon raw material is carried out high-temperature calcination, obtains high-purity synthesis zircon calcining material.
S7: high-purity synthesis zircon calcining material is carried out ball mill pulverizing, drying, obtains drying material and beating powder processing, obtains Synthesize high-purity zircon micropowder.
S8: high-purity for above-mentioned synthesis zircon micropowder hydrostatic profile is obtained the raw embryo of compact zircon brick.
S9: raw for above-mentioned compact zircon brick embryo is carried out high temperature sintering, obtains semi-finished product brick.
S10: above-mentioned semi-finished product brick is carried out cold working, obtains compact zircon brick finished product.
As a further improvement on the present invention, in described step S1, calcining heat is 1360-1400 DEG C.
As a further improvement on the present invention, in described step S6, calcining heat is 1350 DEG C-1650 DEG C, the insulation of calcining Time is no less than 9h;In described step S9, the temperature of high temperature sintering is 1580 DEG C-1680 DEG C, and the temperature retention time of calcining is no less than 12h。
As a further improvement on the present invention, mean diameter D50≤10 μm of described quartz micropowder, putting down of zirconium oxide micropowder All particle diameter D50≤10 μm.In step S7, synthesize mean diameter D50≤8 μm of high-purity zircon micropowder, need to add during ball mill pulverizing Enter≤lanthana, yittrium oxide or the cerium oxide of 0.3%, add the bonding agent of 0.2%, add the water reducer of≤0.2%.
As a further improvement on the present invention, described step S3, moisture≤0.4% drying material of S5 and S7, step S3, S5 and S7 needed 30 mesh sieves after beating powder.
As a further improvement on the present invention, described step S7 needs before starting to carry out high-purity synthesis zircon calcining material Thing detects mutually, ZrSiO4Phase content >=90% be considered as qualified, step S7 can be carried out, otherwise carry out reheating process;Step The compact zircon brick finished product of S10 needs to carry out thing and detects mutually, ZrSiO4Phase content >=95%, it is qualified to be considered as;Described thing phase It is detected as using X-ray diffractometer to carry out detection by quantitative.
The present invention compared with prior art, has the advantage that
The present invention is by using highly purified SiO2、ZrO2Synthesize high-purity zirconium diamond stone, i.e. ZrO2+SiO2→ZrSiO4, The preparation method coordinating the present invention obtains the synthesis zircon brick high-quality, stable, highly purified and impurity content is few, from And the glass being special provides good kiln material, copper content Cu≤10ppm, iron content Fe in the zircon brick of the present invention ≤ 200ppm, the zircon brick prepared by factory formula and the method for the present invention, its impurity F e, Cu, Ni or Cr content is far away Less than existing zircon brick, with the compact zircon brick masonry kiln of the present invention, it is possible to it is special that the use present invention produces The gain performance of the equipment of glass improves further.
Detailed description of the invention
Below in conjunction with embodiment the present invention will be further explained explanation.
Embodiment 1
A kind of compact zircon brick, includes following components according to weight ratio:
Wherein, the mean diameter D50=6.81 μm of quartz micropowder, the mean diameter D50=6.50 μm of zirconium oxide micropowder, add Adding agent and include titanium oxide, yittrium oxide, lanthana, cerium oxide, Ludox or waterglass, additive also includes water reducer.
The preparation method of above-mentioned compact zircon brick, comprises the following steps:
S1: glass sand and the high-purity mangesium oxide zirconium of buying are calcined respectively, obtains calcining quartz sand and forges Burn zirconium oxide, SiO in described glass sand2Content >=99.5%, ZrO in high-purity mangesium oxide zirconium2Content >= 99.5%.
S2: calcining quartz sand and calcined zirconia are obtained quartz mud and zirconium oxide mud by ball mill pulverizing respectively.
S3: quartz mud and zirconium oxide mud are passed through microwave drying respectively, obtains the drying material of correspondence, then drying is expected Beat powder respectively;Sieve respectively after beating powder, obtain quartz micropowder and zirconium oxide micropowder.
S4: according to formula proportion quartz micropowder to be asked for, zirconium oxide micropowder, organic bond and additive, carry out mix grinding, Obtain mixing mud.
S5: dried by above-mentioned mixing mud, obtains drying material, by its dozen of powder, sieves after beating powder, obtain high-purity synthesis Zircon raw material.
S6: above-mentioned high-purity synthesis zircon raw material is carried out high-temperature calcination, obtains high-purity synthesis zircon calcining material.By height Isozygotying into zircon calcining material uses X-ray diffractometer to carry out detection by quantitative, ZrSiO4Phase content >=90% be considered as qualified, Step S7 can be carried out, otherwise carry out reheating process.
S7: high-purity synthesis zircon calcining material is carried out ball mill pulverizing, drying, obtains drying material and beating powder processing, obtains Synthesize high-purity zircon micropowder.Synthesize mean diameter D50≤8 μm of high-purity zircon micropowder, need during ball mill pulverizing add≤ Lanthana, yittrium oxide or the cerium oxide of 0.3%, adds the bonding agent of 0.2%, the water reducer sodium tripolyphosphate of≤0.2%.
S8: high-purity for above-mentioned synthesis zircon micropowder hydrostatic profile is obtained the raw embryo of compact zircon brick.
S9: raw for above-mentioned compact zircon brick embryo is carried out high temperature sintering, obtains semi-finished product brick.
S10: above-mentioned semi-finished product brick is carried out cold working, obtains compact zircon brick finished product, by above-mentioned compact zircon brick Finished product uses X-ray diffractometer to carry out detection by quantitative, ZrSiO4Phase content >=95%, is considered as certified products.
Wherein, in step S1, calcining heat is 1360-1400 DEG C.In step S6, calcining heat is 1350 DEG C-1650 DEG C, forges The temperature retention time burnt is no less than 9h;In step S9, the temperature of high temperature sintering is 1580 DEG C-1680 DEG C, and the temperature retention time of calcining is many In 12h.Step S3, moisture≤0.4% drying material of S5 and S7, step S3, S5 and S7 needed 30 mesh sieves after beating powder.
Embodiment 2
A kind of compact zircon brick, includes following components according to weight ratio:
Wherein, the mean diameter D50=5.50 μm of quartz micropowder, the mean diameter D50=4.23 μm of zirconium oxide micropowder, add Adding agent and include titanium oxide, yittrium oxide, lanthana, cerium oxide, Ludox or waterglass, additive also includes water reducer.
The preparation method of above-mentioned compact zircon brick is consistent with embodiment 1.
Wherein, in step S1, calcining heat is 1360-1400 DEG C.In step S6, calcining heat is 1350 DEG C-1650 DEG C, forges The temperature retention time burnt is no less than 9h;In step S9, the temperature of high temperature sintering is 1580 DEG C-1680 DEG C, and the temperature retention time of calcining is many In 12h.Step S3, moisture≤0.4% drying material of S5 and S7, step S3, S5 and S7 needed 30 mesh sieves after beating powder.
Embodiment 3
A kind of compact zircon brick, includes following components according to weight ratio:
Wherein, the mean diameter D50=5.20 μm of quartz micropowder, the mean diameter D50=4.10 μm of zirconium oxide micropowder, add Adding agent and include titanium oxide, yittrium oxide, lanthana, cerium oxide, Ludox or waterglass, additive also includes water reducer.
The preparation method of above-mentioned compact zircon brick is consistent with embodiment 1.
Wherein, in step S1, calcining heat is 1360-1400 DEG C.In step S6, calcining heat is 1350 DEG C-1650 DEG C, forges The temperature retention time burnt is no less than 9h;In step S9, the temperature of high temperature sintering is 1580 DEG C-1680 DEG C, and the temperature retention time of calcining is many In 12h.Step S3, moisture≤0.4% drying material of S5 and S7, step S3, S5 and S7 needed 30 mesh sieves after beating powder.
Embodiment 4
A kind of compact zircon brick, includes following components according to weight ratio:
Wherein, the mean diameter D50=7.2 μm of quartz micropowder, the mean diameter D50=6.8 μm of zirconium oxide micropowder, add Agent includes titanium oxide, yittrium oxide, lanthana, cerium oxide, Ludox or waterglass, and additive also includes water reducer.
The preparation method of above-mentioned compact zircon brick is consistent with embodiment 1.
Embodiment 5
A kind of compact zircon brick, includes following components according to weight ratio:
Wherein, the mean diameter D50=8 μm of quartz micropowder, the mean diameter D50=7.2 μm of zirconium oxide micropowder, additive Including titanium oxide, yittrium oxide, lanthana, cerium oxide, Ludox or waterglass, additive also includes water reducer.
The preparation method of above-mentioned compact zircon brick is consistent with embodiment 1.
Embodiment 6
A kind of compact zircon brick, includes following components according to weight ratio:
Wherein, the mean diameter D50=9 μm of quartz micropowder, the mean diameter D50=8.8 μm of zirconium oxide micropowder, additive Including titanium oxide, yittrium oxide, lanthana, cerium oxide, Ludox or waterglass, additive also includes water reducer.
The preparation method of above-mentioned compact zircon brick is consistent with embodiment 1.
Embodiment 7
The compact zircon brick obtaining embodiment 1-6 carries out defects inspecting, and it contains Cu≤10ppm, containing Fe≤200ppm, Compact zircon brick obtained by embodiment 1-6 is recorded data below: detect apparent porosity≤5%, bulk density For bulk density >=4.20g/cm3, cold crushing strength >=200Mpa.
In step S6 of embodiment 1-6, when temperature rises to 1650 DEG C from 1350 DEG C to high-purity zirconium diamond stone ZrSiO4's Phase content uses X-ray diffractometer to carry out detection by quantitative, obtains following table:
Temperature Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
1350℃ 25.19% 25.43% 8.74% 13.35% 10.72% 22.43%
1400℃ 32.85% 40.13% 27.72% 31.48% 26.60% 49.40%
1450℃ 40.43% 59.14% 47.89% 44.94% 47.16% 61.40%
1500℃ 49.76% 67.65% 62.37% 61.26% 59.05% 73.62%
1550℃ 53.46% 77.26% 74.41% 66.85% 71.14% 80.66%
1580℃ 80.00% 77.45% 76.85% 71.92% 71.24% 83.49%
1600℃ 82.55% 80.10% 86.07% 80.71% 84.41% 83.66%
1620℃ 86.93% 87.63% 90.71% 89.38% 90.63% 85.18%
1650℃ 85.48% 88.61% 91.05% 90.34% 92.36% 87.05%
High-purity zirconium diamond stone ZrSiO in upper table4The non-final sintering soak of phase content after data.
High-purity zirconium diamond stone ZrSiO is understood according to upper table4Phase content obvious when temperature is from 1350 DEG C to 1620 DEG C Increase, but after reaching certain temperature, just synthesis degree is basicly stable.The formula of embodiment 1 is to synthesis degree after uniform temperature Meeting decline by a small margin, but it does not interferes with final high-purity zirconium diamond stone ZrSiO4Phase content.Understood by upper table and close The optimum range becoming the temperature of Zirconium orthosilicate. calcining material is 1580 DEG C~1650 DEG C.
Foregoing is example and the explanation of the present invention, but does not means that the obtainable advantage of the present invention is so limited, all It is may be to wherein the one of the advantage realized in the simple transformation of structure and/or some embodiments in practice process of the present invention Individual or multiple all in the protection domain of the application.

Claims (9)

1. a compact zircon brick, it is characterised in that: according to weight ratio include following components: 31%-33% quartz micropowder, The zirconium oxide micropowder of 65%-68%, 0-0.5% organic bond and additive surplus, each component peeked amount sum is equal to 100%, mean diameter D50≤10 μm of described quartz micropowder, mean diameter D50≤10 μm of zirconium oxide micropowder.
Compact zircon brick the most according to claim 1, it is characterised in that: described additive include titanium oxide, yittrium oxide, Lanthana, cerium oxide, Ludox or waterglass.
Compact zircon brick the most according to claim 1, it is characterised in that: described additive includes the oxidation of 0-1.0% Titanium, the yittrium oxide of 0-0.3%, lanthana or cerium oxide, the Ludox of 0-1.5% or the waterglass of 0-1.5%, additive also wraps Include the water reducer of 0-0.3%.
4. the preparation method of a compact zircon brick, it is characterised in that: comprise the following steps:
S1: glass sand and the high-purity mangesium oxide zirconium of buying are calcined respectively, obtains calcining quartz sand and calcining oxygen Change zirconium, SiO in described glass sand2Content >=99.5%, ZrO in high-purity mangesium oxide zirconium2Content >=99.5%;
S2: calcining quartz sand and calcined zirconia are obtained quartz mud and zirconium oxide mud by ball mill pulverizing respectively;
S3: pass through respectively to dry by quartz mud and zirconium oxide mud, obtains the drying material of correspondence, then is beaten respectively by drying material Powder;Sieve respectively after beating powder, obtain quartz micropowder and zirconium oxide micropowder;
S4: according to formula proportion quartz micropowder to be asked for, zirconium oxide micropowder, organic bond and additive, carry out mix grinding, obtain Mixing mud;
S5: dried by above-mentioned mixing mud, obtains drying material and beating powder, sieves, obtain high-purity synthesis zircon after beating powder Raw material;
S6: above-mentioned high-purity synthesis zircon raw material is carried out high-temperature calcination, obtains high-purity synthesis zircon calcining material;
S7: high-purity synthesis zircon calcining material is carried out ball mill pulverizing, drying, obtains drying material and beating powder processing, is synthesized High-purity zircon micropowder;
S8: high-purity for above-mentioned synthesis zircon micropowder hydrostatic profile is obtained the raw embryo of compact zircon brick;
S9: raw for above-mentioned compact zircon brick embryo is carried out high temperature sintering, obtains semi-finished product brick;
S10: above-mentioned semi-finished product brick is carried out cold working, obtains compact zircon brick finished product.
The preparation method of compact zircon brick the most according to claim 4, it is characterised in that: calcining temperature in described step S1 Degree is for 1360-1400 DEG C.
The preparation method of compact zircon brick the most according to claim 4, it is characterised in that: calcining temperature in described step S6 Degree is 1350 DEG C-1650 DEG C, and the temperature retention time of calcining is no less than 9h;In described step S9 the temperature of high temperature sintering be 1580 DEG C- 1680 DEG C, the temperature retention time of calcining is no less than 12h.
The preparation method of compact zircon brick the most according to claim 4, it is characterised in that: in step S7, synthesize high-purity Mean diameter D50≤8 μm of zircon micropowder;Need to add lanthana, yittrium oxide or the cerium oxide of≤0.3% during ball mill pulverizing, Add the bonding agent of 0.2%, add the water reducer of≤0.2%.
The preparation method of compact zircon brick the most according to claim 4, it is characterised in that: described step S3, S5 and S7 Dry material moisture≤0.4%, step S3, S5 and S7 needed 30 mesh sieves after beating powder.
The preparation method of compact zircon brick the most according to claim 4, it is characterised in that: described step S7 needs before starting High-purity synthesis zircon calcining material is carried out thing to detect mutually, ZrSiO4Phase content >=90% be considered as qualified, can carry out Step S7, otherwise carries out reheating process;The compact zircon brick finished product of step S10 needs to carry out thing and detects mutually, ZrSiO4 thing phase Content >=95%, it is qualified to be considered as;Described thing is detected as using X-ray diffractometer to carry out detection by quantitative mutually.
CN201610509045.0A 2016-06-29 2016-06-29 A kind of compact zircon brick and preparation method thereof Pending CN106116571A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107325593A (en) * 2017-06-07 2017-11-07 常州海瑞纺织品有限公司 A kind of preparation method of waterproof and heat-insulating powder
CN108033796A (en) * 2017-12-08 2018-05-15 安徽雷萨重工机械有限公司 A kind of refractory material of high-strength mechanical properties
CN108727019A (en) * 2018-08-31 2018-11-02 广州市石基耐火材料厂 Zircon brick and preparation method thereof

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CN102992787A (en) * 2012-11-13 2013-03-27 登封市宏发煤矿机械厂 Special zirconium oxide fireproof brick for liner layer of smelting kiln
CN103011851A (en) * 2012-11-13 2013-04-03 登封市宏发煤矿机械厂 Mullite-silicon-corundum abrasive brick and manufacturing method thereof
CN105174979A (en) * 2015-08-21 2015-12-23 淄博裕民基诺新材料有限公司 Zircon/zirconia multiphase material based on zircon covered zirconium dioxide powder and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN102992787A (en) * 2012-11-13 2013-03-27 登封市宏发煤矿机械厂 Special zirconium oxide fireproof brick for liner layer of smelting kiln
CN103011851A (en) * 2012-11-13 2013-04-03 登封市宏发煤矿机械厂 Mullite-silicon-corundum abrasive brick and manufacturing method thereof
CN105174979A (en) * 2015-08-21 2015-12-23 淄博裕民基诺新材料有限公司 Zircon/zirconia multiphase material based on zircon covered zirconium dioxide powder and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107325593A (en) * 2017-06-07 2017-11-07 常州海瑞纺织品有限公司 A kind of preparation method of waterproof and heat-insulating powder
CN108033796A (en) * 2017-12-08 2018-05-15 安徽雷萨重工机械有限公司 A kind of refractory material of high-strength mechanical properties
CN108727019A (en) * 2018-08-31 2018-11-02 广州市石基耐火材料厂 Zircon brick and preparation method thereof
CN108727019B (en) * 2018-08-31 2020-06-12 广州市石基耐火材料厂 Zircon brick and preparation method thereof

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