CN107445628A - 一种抗水化镁钙砂的制备方法 - Google Patents
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- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 47
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- 239000001095 magnesium carbonate Substances 0.000 title claims abstract description 44
- 235000014380 magnesium carbonate Nutrition 0.000 title claims abstract description 44
- 229910000021 magnesium carbonate Inorganic materials 0.000 title claims abstract description 44
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
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- 239000010459 dolomite Substances 0.000 claims description 63
- 229910000514 dolomite Inorganic materials 0.000 claims description 63
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 235000019353 potassium silicate Nutrition 0.000 claims description 24
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 24
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- 235000007164 Oryza sativa Nutrition 0.000 claims description 18
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- 239000000376 reactant Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 12
- 239000000084 colloidal system Substances 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
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- 235000012239 silicon dioxide Nutrition 0.000 claims description 12
- 239000004575 stone Substances 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000010903 husk Substances 0.000 claims description 6
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- 239000002243 precursor Substances 0.000 claims description 6
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- 238000003801 milling Methods 0.000 claims 2
- 238000002242 deionisation method Methods 0.000 claims 1
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- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 19
- 239000000395 magnesium oxide Substances 0.000 abstract description 12
- 239000000292 calcium oxide Substances 0.000 abstract description 9
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract description 9
- 238000006703 hydration reaction Methods 0.000 abstract description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000010408 film Substances 0.000 abstract description 3
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- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
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- 239000000243 solution Substances 0.000 description 27
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- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 206010037844 rash Diseases 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
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- 235000019786 weight gain Nutrition 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
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- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
本发明公开了一种抗水化镁钙砂的制备方法，属于镁钙砂技术领域。本发明的抗水化镁钙砂首先利用水化碳酸化作用，使镁钙砂表面游离的氧化钙转变为稳定的碳酸钙，碳酸盐薄膜可有效阻止在高温情况下，水汽侵入镁钙砂，与其内部的氧化镁和氧化钙发生水化反应，从而达到抗水化的目的；在常温下，含有的SiO2超微粉遇水后，会在表面形成羟基，即Si‑OH键，经干燥后，脱水架桥形成了硅氧烷网络结构，由于其表面有大量未键合的O2‑，而O2‑它们很容易被吸附在MgO颗粒表面的Mg2＋上，形成镁氧硅链，从而减少了与Mg2＋结合的OH‑数量，与同时形成H‑O‑Mg‑O‑H及氢氧硅链相比，水分子减少了，每形成一个镁氧硅链即可减少一个水分子，进一步提高镁钙砂的抗水性效果。
Description
技术领域
本发明公开了一种抗水化镁钙砂的制备方法，属于镁钙砂制备技术领域。
背景技术
目前国内不锈钢及特殊钢的冶炼用的耐火材料普遍采用烧成镁钙砖，这类镁钙砖致密程度不高，气孔率一般在8～15%，体积密度在2.90～3.00g/cm3，使用过程中，在AOD渣线及风枪四周其抗侵蚀性能不佳，在不锈钢钢包的包底处其抗冲刷性能也不理想，这些都成为使用过程中的瓶颈，而造成提前下线。
镁钙砂一般是指以MgO和CaO为主要化学成分的高温烧结混合物，主要用于制备镁钙砖、镁白云石砖、镁钙碳砖等碱性耐火材料制品。然而，镁钙砂及镁钙质耐火材料制品易吸收外界环境中的水分发生水化反应，引发明显的体积膨胀而粉化损毁。可以说，改善镁钙砂的烧结及抗水化性能直接关系到镁钙质耐火材料的工业生产、储运和使用。
目前，制备镁钙砂主要选用添加物加入法，以白云石矿起始原料、或以菱镁矿和石灰石为起始原料，经破碎、轻烧后加入少量添加剂进行混合，成型，高温（1500～1650℃）烧成，破碎即得合成镁钙砂。
采用“添加物加入法”制备镁钙砂，主要通过添加剂与MgO或CaO在高温条件下发生反应，形成低熔点物相或固溶体促进烧结，以此提高镁钙砂的烧结性能和致密度，减少MgO和CaO与外界接触的通道，减缓镁钙砂的水化反应。但采用添加物加入法制备镁钙砂，不仅烧成温度较高和能耗大，且添加物的引入（如稀土氧化物）进一步增大了镁钙砂的生产成本。此外，采用添加物加入法并未有效解决镁钙砂的水化问题，一旦镁钙砂由表及里发生水化，则水化反应持续进行，进而损毁材料。
因此，发明一种新型的具有抗水性的镁钙砂对镁钙砂制备技术领域具有积极地意义。
发明内容
本发明主要解决的技术问题，针对目前镁钙砂吸收外界环境中的水分容易发生水化反应，引发明显的体积膨胀而粉化损毁的缺陷，提供了一种抗水化镁钙砂的制备方法。
为了解决上述技术问题，本发明所采用的技术方案是：
（1）称取600～800g稻壳，点燃，得到稻壳灰，将得到的稻壳灰装入带有搅拌器和进气口的三口烧瓶中，向三口烧瓶中加入400～500mL质量分数为60%氢氧化钠溶液，启动搅拌器，在搅拌的同时通入氮气30～45min，得到水玻璃溶液；（2）用200～300mL质量分数10%的盐酸调节水玻璃溶液pH值至6～7，得到中和后的水玻璃溶液，将中和后的水玻璃溶液在70～80℃下，置于200～250r/min转速的搅拌器下搅拌，得到超细二氧化硅胶体；称取2～3kg白云石在磨石机中研磨2～3h，研磨结束后过80目标准筛得到白云石粉末，将白云石粉末放入煅烧炉中，加热升温至800～900℃，保温煅烧3～5h，出料，得到轻烧白云石料；（3）将轻烧白云石料置于研钵中研磨1～2h后，过200目标准筛得白云石细粉，在180～200℃条件下将白云石细粉与去离子水按质量比3︰1混合搅拌，并持续通入二氧化碳气体反应30～45min，得到反应物，再将反应物置于烘箱中，在100～110℃下干燥1～2h，得到水化碳酸化的白云石颗粒料；
（4）将水化碳酸化的白云石颗粒料浸入超细二氧化硅胶体中，得到包覆结构白云石颗粒料；将包覆结构白云石颗粒料放在电阻炉中，依次在100～110℃，1300～1400℃下分别保温干燥2～3h后即可得到抗水化的镁钙砂。
本发明的有益效果是：
（1）本发明的抗水化镁钙砂首先利用了水化碳酸化作用，使得镁钙砂表面游离的氧化钙转变为稳定的碳酸钙，从而在镁钙砂表面覆盖一层碳酸盐薄膜；碳酸盐薄膜可有效阻止在高温情况下，水汽侵入镁钙砂，与其内部的氧化镁和氧化钙发生水化反应，从而达到抗水化的目的；
（2）本发明的抗水化镁钙砂在常温下，其中含有的SiO2超微粉遇水后，会在表面形成羟基，即Si-OH键，经干燥后，脱水架桥形成了硅氧烷网络结构，同时，由于其表面有大量未键合的O2-，而O2-它们很容易被吸附在MgO颗粒表面的Mg2＋上，形成镁氧硅链，从而减少了与Mg2 ＋结合的OH-数量，与同时形成H-O-Mg-O-H及氢氧硅链相比，水分子减少了，每形成一个镁氧硅链即可减少一个水分子，因此通过镁氧硅链的形成可以减少水分子侵入镁钙砂内部，进一步提高镁钙砂的抗水性效果。
具体实施方式
称取600～800g稻壳，点燃，得到稻壳灰，将得到的稻壳灰装入带有搅拌器和进气口的三口烧瓶中，向三口烧瓶中加入400～500mL质量分数为60%氢氧化钠溶液，启动搅拌器，在搅拌的同时通入氮气30～45min，得到水玻璃溶液；用200～300mL质量分数10%的盐酸调节水玻璃溶液pH值至6～7，得到中和后的水玻璃溶液，将中和后的水玻璃溶液在70～80℃下，置于200～250r/min转速的搅拌器下搅拌，得到超细二氧化硅胶体；称取2～3kg白云石在磨石机中研磨2～3h，研磨结束后过80目标准筛得到白云石粉末，将白云石粉末放入煅烧炉中，加热升温至800～900℃，保温煅烧3～5h，出料，得到轻烧白云石料；将轻烧白云石料置于研钵中研磨1～2h后，过200目标准筛得白云石细粉；在180～200℃条件下将白云石细粉与去离子水按质量比3︰1混合搅拌，并持续通入二氧化碳气体反应30～45min，得到反应物，再将反应物置于烘箱中，在100～110℃下干燥1～2h，得到水化碳酸化的白云石颗粒料；将水化碳酸化的白云石颗粒料浸入超细二氧化硅胶体中，得到包覆结构白云石颗粒料；将包覆结构白云石颗粒料放在电阻炉中，依次在100～110℃，1300～1400℃下分别保温干燥2～3h后即可得到抗水化的镁钙砂。
实例1
称取600g稻壳，点燃，得到稻壳灰，将得到的稻壳灰装入带有搅拌器和进气口的三口烧瓶中，向三口烧瓶中加入400mL质量分数为60%氢氧化钠溶液，启动搅拌器，在搅拌的同时通入氮气30min，得到水玻璃溶液；用200mL质量分数10%的盐酸调节水玻璃溶液pH值至6，得到中和后的水玻璃溶液，将中和后的水玻璃溶液在70℃下，置于200r/min转速的搅拌器下搅拌，得到超细二氧化硅胶体；称取2kg白云石在磨石机中研磨2h，研磨结束后过80目标准筛得到白云石粉末，将白云石粉末放入煅烧炉中，加热升温至800℃，保温煅烧3h，出料，得到轻烧白云石料；将轻烧白云石料置于研钵中研磨1h后，过200目标准筛得白云石细粉；在180℃条件下将白云石细粉与去离子水按质量比3︰1混合搅拌，并持续通入二氧化碳气体反应30min，得到反应物，再将反应物置于烘箱中，在100℃下干燥1h，得到水化碳酸化的白云石颗粒料；将水化碳酸化的白云石颗粒料浸入超细二氧化硅胶体中，得到包覆结构白云石颗粒料；将包覆结构白云石颗粒料放在电阻炉中，依次在100℃，1300℃下分别保温干燥2h后即可得到抗水化的镁钙砂。
实例2
称取700g稻壳，点燃，得到稻壳灰，将得到的稻壳灰装入带有搅拌器和进气口的三口烧瓶中，向三口烧瓶中加入450mL质量分数为60%氢氧化钠溶液，启动搅拌器，在搅拌的同时通入氮气40min，得到水玻璃溶液；用250mL质量分数10%的盐酸调节水玻璃溶液pH值至6，得到中和后的水玻璃溶液，将中和后的水玻璃溶液在75℃下，置于225r/min转速的搅拌器下搅拌，得到超细二氧化硅胶体；称取2kg白云石在磨石机中研磨2h，研磨结束后过80目标准筛得到白云石粉末，将白云石粉末放入煅烧炉中，加热升温至850℃，保温煅烧4h，出料，得到轻烧白云石料；将轻烧白云石料置于研钵中研磨1h后，过200目标准筛得白云石细粉；在190℃条件下将白云石细粉与去离子水按质量比3︰1混合搅拌，并持续通入二氧化碳气体反应40min，得到反应物，再将反应物置于烘箱中，在105℃下干燥1h，得到水化碳酸化的白云石颗粒料；将水化碳酸化的白云石颗粒料浸入超细二氧化硅胶体中，得到包覆结构白云石颗粒料；将包覆结构白云石颗粒料放在电阻炉中，依次在105℃，1350℃下分别保温干燥2h后即可得到抗水化的镁钙砂。
实例3
称取800g稻壳，点燃，得到稻壳灰，将得到的稻壳灰装入带有搅拌器和进气口的三口烧瓶中，向三口烧瓶中加入500mL质量分数为60%氢氧化钠溶液，启动搅拌器，在搅拌的同时通入氮气45min，得到水玻璃溶液；用300mL质量分数10%的盐酸调节水玻璃溶液pH值至7，得到中和后的水玻璃溶液，将中和后的水玻璃溶液在80℃下，置于250r/min转速的搅拌器下搅拌，得到超细二氧化硅胶体；称取3kg白云石在磨石机中研磨3h，研磨结束后过80目标准筛得到白云石粉末，将白云石粉末放入煅烧炉中，加热升温至900℃，保温煅烧5h，出料，得到轻烧白云石料；将轻烧白云石料置于研钵中研磨2h后，过200目标准筛得白云石细粉；在200℃条件下将白云石细粉与去离子水按质量比3︰1混合搅拌，并持续通入二氧化碳气体反应45min，得到反应物，再将反应物置于烘箱中，在110℃下干燥2h，得到水化碳酸化的白云石颗粒料；将水化碳酸化的白云石颗粒料浸入超细二氧化硅胶体中，得到包覆结构白云石颗粒料；将包覆结构白云石颗粒料放在电阻炉中，依次在110℃，1400℃下分别保温干燥3h后即可得到抗水化的镁钙砂。
对比例 以海城市某公司生产的镁钙砂作为对比例 对本发明制得的抗水化镁钙砂和对比例中的镁钙砂进行检测，检测结果如表1所示： 1、测试方法
水化增重率测试按高压釜蒸压法的标准进行检测。
粉化率测试用H2C2H4溶液浸渍处理的标准测试方法进行检测。
表1
根据表1中数据可知，本发明制得的抗水化镁钙砂的水化增重率低，粉化率低，有较好的抗水化能力，具有广阔的使用前景。
Claims (5)
1.一种抗水化镁钙砂的制备方法，其特征在于具体制备步骤为：
（1）称取600～800g稻壳，点燃，得到稻壳灰，将得到的稻壳灰装入带有搅拌器和进气口的三口烧瓶中，向三口烧瓶中加入400～500mL氢氧化钠溶液，启动搅拌器，在搅拌的同时通入氮气，得到水玻璃溶液；
（2）用200～300mL盐酸调节水玻璃溶液pH值至一定值，得到中和后的水玻璃溶液，将中和后的水玻璃溶液，置于搅拌器下搅拌，得到超细二氧化硅胶体，称取2～3kg白云石在磨石机中研磨，研磨结束后过标准筛得到白云石粉末，将白云石粉末放入煅烧炉中，加热升温，保温煅烧，出料，得到轻烧白云石料；
（3）将轻烧白云石料置于研钵中研磨后，过标准筛得白云石细粉，将白云石细粉与去离子水混合搅拌，并持续通入二氧化碳气体反应，得到反应物，再将反应物置于烘箱中，干燥，得到水化碳酸化的白云石颗粒料；
（4）将水化碳酸化的白云石颗粒料浸入超细二氧化硅胶体中，得到包覆结构白云石颗粒料；将包覆结构白云石颗粒料放在电阻炉中，保温干燥后即可得到抗水化镁钙砂。
2.根据权利要求1所述的一种抗水化镁钙砂的制备方法，其特征在于：步骤（1）所述的氢氧化钠溶液的质量分数为60%，搅拌的同时通入氮气的时间为30～45min。
3.根据权利要求1所述的一种抗水化镁钙砂的制备方法，其特征在于：步骤（2）所述的盐酸的质量分数10%，盐酸调节后的pH值为6～7，搅拌温度为70～80℃，搅拌器转速为200～250r/min，研磨时间为2～3h，标准筛规格为80目，煅烧炉保温温度为800～900℃，保温煅烧时间为3～5h。
4.根据权利要求1所述的一种抗水化镁钙砂的制备方法，其特征在于：步骤（3）所述的研磨时间为1～2h，标准筛规格为200目，混合搅拌温度为180～200℃，白云石细粉与去离子水混合时质量比为3︰1，30～45min，烘箱温度为100～110℃，干燥时间1～2h。
5.根据权利要求1所述的一种抗水化镁钙砂的制备方法，其特征在于：步骤（4）所述的保温干燥是依次在100～110℃，1300～1400℃下进行，保温时间2～3h。
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| CN105439577A (zh) * | 2015-11-25 | 2016-03-30 | 武汉科技大学 | 一种核壳包覆结构镁钙砂及其制备方法 |
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| CN108640697A (zh) * | 2018-07-31 | 2018-10-12 | 王祖少 | 一种建筑用喷补料的制备方法 |
| CN115677327A (zh) * | 2022-10-26 | 2023-02-03 | 中国地质大学（武汉） | 一种内部流道构件用的水溶性氧化钙基支撑型芯及其制备方法 |
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