CN102153144B - Method for preparing calcium ferroaluminates - Google Patents
Method for preparing calcium ferroaluminates Download PDFInfo
- Publication number
- CN102153144B CN102153144B CN 201010109398 CN201010109398A CN102153144B CN 102153144 B CN102153144 B CN 102153144B CN 201010109398 CN201010109398 CN 201010109398 CN 201010109398 A CN201010109398 A CN 201010109398A CN 102153144 B CN102153144 B CN 102153144B
- Authority
- CN
- China
- Prior art keywords
- gel
- temperature
- calcium
- nitrate hydrate
- sol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000011575 calcium Substances 0.000 title claims abstract description 22
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 15
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- ZZCONUBOESKGOK-UHFFFAOYSA-N aluminum;trinitrate;hydrate Chemical compound O.[Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O ZZCONUBOESKGOK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 12
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 12
- 238000003980 solgel method Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- NEOOEFDJRSCWOU-UHFFFAOYSA-N iron(2+);dinitrate;hydrate Chemical compound O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NEOOEFDJRSCWOU-UHFFFAOYSA-N 0.000 claims description 7
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 4
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims 1
- 238000007669 thermal treatment Methods 0.000 claims 1
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 abstract description 22
- JJIQGEZLLWXYKV-UHFFFAOYSA-N calcium;dinitrate;hydrate Chemical compound O.[Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O JJIQGEZLLWXYKV-UHFFFAOYSA-N 0.000 abstract description 10
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 abstract description 10
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 9
- ULGYAEQHFNJYML-UHFFFAOYSA-N [AlH3].[Ca] Chemical compound [AlH3].[Ca] ULGYAEQHFNJYML-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000499 gel Substances 0.000 description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 239000004568 cement Substances 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- WNQQFQRHFNVNSP-UHFFFAOYSA-N [Ca].[Fe] Chemical compound [Ca].[Fe] WNQQFQRHFNVNSP-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910001392 phosphorus oxide Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001778 solid-state sintering Methods 0.000 description 1
- -1 stirred for 3h Chemical compound 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- VSAISIQCTGDGPU-UHFFFAOYSA-N tetraphosphorus hexaoxide Chemical compound O1P(O2)OP3OP1OP2O3 VSAISIQCTGDGPU-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compounds Of Iron (AREA)
- Colloid Chemistry (AREA)
Abstract
本发明涉及一种铁铝酸钙的制备方法，采用溶胶-凝胶法将硝酸铝水合物、硝酸钙水合物、硝酸铁水合物、六次甲基四胺、乙酰丙酮、去离子水等按照比例混合均匀后，在50℃～70℃下搅拌得到溶胶，经陈化后形成凝胶，在750℃～800℃下热处理2h～4h，慢冷至室温即得铁铝酸钙。与现有技术相比，本发明的制备工艺简单，反应过程易于控制，产品均匀度高且纯度高，能在低于传统方法的温度下烧成。The present invention relates to a preparation method of calcium aluminum ferrite, which comprises aluminum nitrate hydrate, calcium nitrate hydrate, ferric nitrate hydrate, hexamethylenetetramine, acetylacetone, deionized water, etc. according to the sol-gel method. After mixing evenly, stir at 50°C to 70°C to obtain a sol, form a gel after aging, heat treatment at 750°C to 800°C for 2h to 4h, and slowly cool to room temperature to obtain calcium aluminoferrite. Compared with the prior art, the preparation process of the present invention is simple, the reaction process is easy to control, the product has high uniformity and purity, and can be fired at a temperature lower than that of the traditional method.
Description
技术领域 technical field
本发明涉及一种无机材料的制备方法，尤其是涉及一种铁铝酸钙的制备方法。The invention relates to a preparation method of an inorganic material, in particular to a preparation method of calcium aluminum ferrite.
背景技术 Background technique
铁铝酸钙作为水泥熟料的主要矿物之一，其合成方法一直倍受人们关注。采用传统高温烧结反应的方法合成，所需反应温度高，若采用矿化剂等来降低烧成温度或使某些晶型的单矿物晶体在室温下可以稳定存在，则会在单矿物中引入其他成分。为了克服传统固相烧结方法的合成温度高、反应不易控制等缺点，努力在合成产物的性能方面有所突破，各种化学方法开始应用于铁铝酸钙的制备，如采用简单分子长链有机物为聚合物载体用溶液-聚合物法在700℃下制备出铁铝酸钙，但该方法对于所采用的聚合物载体要求苛刻。溶胶-凝胶法是一种胶体化学的方法，它使用液体化学试剂或溶胶为原料，将金属醇盐或无机盐经水解直接形成溶胶或经解凝形成溶胶，然后使溶质聚合凝胶化，再将凝胶干燥、灼烧去除有机成分，最后达到所需无机材料。制备过程包括溶胶的制备、凝胶的形成和凝胶干燥及热处理。由于在溶胶-凝胶过程中，溶胶由溶液制得，所以胶粒内及胶粒间化学成分一致，产品纯度高，凝胶热处理过程中不易使粉末颗粒产生严重团聚，容易控制粉末颗粒的尺寸。现在用溶胶-凝胶法已经成功制备出β-C2S、磷铝酸盐水泥、白水泥和彩色水泥。As one of the main minerals of cement clinker, the synthesis method of calcium aluminate has attracted much attention. It is synthesized by traditional high-temperature sintering reaction method, and the required reaction temperature is high. If a mineralizer is used to reduce the sintering temperature or to make certain crystal forms of single mineral crystals stable at room temperature, it will be introduced into the single mineral. other ingredients. In order to overcome the shortcomings of the traditional solid-state sintering method, such as high synthesis temperature and uneasy control of the reaction, and strive to make breakthroughs in the performance of the synthesized products, various chemical methods have begun to be applied to the preparation of calcium aluminoferrite, such as the use of simple molecular long-chain organic compounds Calcium aluminoferrite was prepared at 700°C by solution-polymer method for polymer carrier, but this method has strict requirements on the polymer carrier used. The sol-gel method is a method of colloid chemistry, which uses liquid chemical reagents or sols as raw materials, hydrolyzes metal alkoxides or inorganic salts to directly form sols or decondenses to form sols, and then polymerizes and gels the solutes. Then the gel is dried and burned to remove the organic components, and finally the desired inorganic material is obtained. The preparation process includes sol preparation, gel formation, gel drying and heat treatment. In the sol-gel process, the sol is made from the solution, so the chemical composition inside and between the colloidal particles is consistent, the product is of high purity, and it is not easy to cause serious agglomeration of the powder particles during the gel heat treatment process, and it is easy to control the size of the powder particles . Now β-C 2 S, aluminophosphate cement, white cement and colored cement have been successfully prepared by sol-gel method.
传统采用高温烧结反应的方法合成铁铝酸钙。这种方法所需反应温度高，需1200℃以上的高温煅烧；反应过程不易控制，要使游离氧化钙含量降低到1％以下，需要经过反复多次研磨、粉末压制和烧结才能完成；由于通常采用矿化剂(如氧化铜、氟化钙、硫酸钙、氧化磷、氧化钛)等来降低烧成温度或使某些晶型的单矿物晶体在室温下可以稳定存在，会在水泥熟料单矿物中引入除设计产物以外的物相。Calcium aluminoferrite is traditionally synthesized by high temperature sintering reaction. This method requires a high reaction temperature, which requires high-temperature calcination above 1200°C; the reaction process is not easy to control, and to reduce the free calcium oxide content to below 1%, it needs to be repeatedly ground, powder pressed and sintered to complete; Use mineralizers (such as copper oxide, calcium fluoride, calcium sulfate, phosphorus oxide, titanium oxide) to reduce the firing temperature or make certain crystal forms of single mineral crystals stable at room temperature, which will be in cement clinker Phases other than the designed product are introduced into the single mineral.
发明内容 Contents of the invention
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种纯度高、产品粒度小、过程简单、烧结温度低的铁铝酸钙的制备方法。The object of the present invention is to provide a method for preparing calcium aluminoferrite with high purity, small particle size, simple process and low sintering temperature in order to overcome the above-mentioned defects in the prior art.
本发明的目的可以通过以下技术方案来实现：The purpose of the present invention can be achieved through the following technical solutions:
一种铁铝酸钙的制备方法，其特征在于，该方法采用溶胶-凝胶法，将分析纯化学试剂混合反应后得到凝胶，将凝胶进行高温热处理后再冷却至室温，即得到铁铝酸钙。A method for preparing calcium aluminate ferrite, characterized in that the method adopts a sol-gel method, and the analytical pure chemical reagents are mixed and reacted to obtain a gel, and the gel is subjected to high-temperature heat treatment and then cooled to room temperature to obtain iron calcium aluminate.
该方法具体包括以下步骤：将硝酸铝水合物(Al(NO3)3·9H2O)、硝酸钙水合物(Ca(NO3)2·4H2O)、硝酸铁水合物(Fe(NO3)3)·9H2O)、六次甲基四胺((CH2)6N4)、乙酰丙酮((CH3CO)2CH(AcAcH))及去离子水按重量比为1∶1.26∶1.08∶(0.2-0.6)∶(0.08-0.16)∶(5-10)混合，控制反应温度为50-70℃，搅拌10-12h至形成透明溶胶，将溶胶置于水浴中，控制水浴温度为50-70℃，陈化3-6天形成凝胶，得到的凝胶烘干后经热处理后缓慢冷却至室温，即得到铁铝酸钙。The method specifically includes the following steps: aluminum nitrate hydrate (Al(NO 3 ) 3 ·9H 2 O), calcium nitrate hydrate (Ca(NO 3 ) 2 ·4H 2 O), iron nitrate hydrate (Fe(NO 3 ) 3 )·9H 2 O), hexamethylenetetramine ((CH 2 ) 6 N 4 ), acetylacetone ((CH 3 CO) 2 CH(AcAcH)) and deionized water in a weight ratio of 1: 1.26: 1.08: (0.2-0.6): (0.08-0.16): (5-10) mix, control the reaction temperature at 50-70 ° C, stir for 10-12 hours until a transparent sol is formed, put the sol in a water bath, control the temperature of the water bath The temperature is 50-70°C, aging for 3-6 days to form a gel, and the obtained gel is dried, heat-treated, and then slowly cooled to room temperature to obtain calcium aluminoferrite.
所述的硝酸铝水合物、硝酸钙水合物、硝酸铁水合物、六次甲基四胺、乙酰丙酮均为分析纯化学试剂。The aluminum nitrate hydrate, calcium nitrate hydrate, ferric nitrate hydrate, hexamethylenetetramine and acetylacetone are analytically pure chemical reagents.
所述的热处理温度为750-800℃。The heat treatment temperature is 750-800°C.
所述的热处理时间为2-4h。The heat treatment time is 2-4h.
与现有技术相比，本发明采用溶胶-凝胶法，通过调整和控制溶液中的化学反应，以合适的形式获得所需的成分和结构，可在低于传统方法的温度下制备水泥熟料单矿物铁铝酸钙，产品均匀度高，化学均匀性好，由于在溶胶-凝胶过程中，溶胶由溶液制得，所以胶粒内及胶粒间化学成分一致，且纯度高，游离氧化钙含量均低于0.5％，产品粒度小，不需经过烧结反应，比传统烧结法更容易制备细粉末，凝胶经过热处理后用玛瑙研钵研磨所得粉末平均粒径2～4μm，颗粒表面粗糙并有很多裂纹，使得其水化活化点较多，制备工艺简单，反应过程易于控制，通过一次烧结即能完成制备。Compared with the prior art, the present invention adopts the sol-gel method, by adjusting and controlling the chemical reaction in the solution, to obtain the required composition and structure in a suitable form, and can prepare cement clinker at a temperature lower than that of the traditional method. Calcium aluminate ferrite, a single mineral material, has high product uniformity and good chemical uniformity. Since the sol is prepared from a solution in the sol-gel process, the chemical composition in and between the colloidal particles is consistent, and the purity is high, free Calcium oxide content is lower than 0.5%. The particle size of the product is small and does not require sintering reaction. It is easier to prepare fine powder than traditional sintering method. It is rough and has many cracks, so that it has more hydration activation points, the preparation process is simple, the reaction process is easy to control, and the preparation can be completed by one-time sintering.
具体实施方式 Detailed ways
下面结合具体实施例对本发明进行详细说明。The present invention will be described in detail below in conjunction with specific embodiments.
实施例1Example 1
一种铁铝酸钙的制备方法，该方法为溶胶-凝胶法，具体包括以下步骤：将硝酸铝水合物(Al(NO3)3·9H2O)、硝酸钙水合物(Ca(NO3)2·4H2O)、硝酸铁水合物(Fe(NO3)3)·9H2O)混合加入去离子水中，然后向混合溶液中加入乙酰丙酮((CH3CO)2CH(AcAcH))，搅拌30min，然后加入溶解于去离子水中的六次甲基四胺，搅拌3h，硝酸铝水合物(Al(NO3)3·9H2O)、硝酸钙水合物(Ca(NO3)2·4H2O)、硝酸铁水合物(Fe(NO3)3)·9H2O)、六次甲基四胺((CH2)6N4)、乙酰丙酮((CH3CO)2CH(AcAcH))及去离子水的重量比为1∶1.26∶1.08∶0.47∶0.12∶6，均为分析纯化学试剂。控制温度为60℃，充分搅拌12h至形成透明溶胶，将溶胶置于水浴中，控制水浴温度为60℃，陈化5天形成凝胶，得到的凝胶置于高温裂解炉中进行热处理，控制温度为800℃，灼烧3h，最后缓慢冷却至室温，即得到铁铝酸钙。A preparation method of calcium aluminum ferrite, the method is a sol-gel method, specifically comprising the following steps: aluminum nitrate hydrate (Al(NO 3 ) 3 9H 2 O), calcium nitrate hydrate (Ca(NO 3 ) 2 ·4H 2 O), iron nitrate hydrate (Fe(NO 3 ) 3 )·9H 2 O) were mixed and added to deionized water, and then acetylacetone ((CH 3 CO) 2 CH(AcAcH )), stirred for 30min, then added hexamethylenetetramine dissolved in deionized water, stirred for 3h, aluminum nitrate hydrate (Al(NO 3 ) 3 ·9H 2 O), calcium nitrate hydrate (Ca(NO 3 ) 2 ·4H 2 O), iron nitrate hydrate (Fe(NO 3 ) 3 )·9H 2 O), hexamethylenetetramine ((CH 2 ) 6 N 4 ), acetylacetone ((CH 3 CO) 2 CH(AcAcH)) and deionized water in a weight ratio of 1:1.26:1.08:0.47:0.12:6, both of which are analytically pure chemical reagents. Control the temperature at 60°C, stir fully for 12 hours until a transparent sol is formed, place the sol in a water bath, control the temperature of the water bath at 60°C, age for 5 days to form a gel, and place the obtained gel in a high-temperature cracking furnace for heat treatment. The temperature is 800°C, burning for 3 hours, and finally cooling down to room temperature slowly to obtain calcium aluminoferrite.
实施例2Example 2
一种铁铝酸钙的制备方法，该方法为溶胶-凝胶法，具体包括以下步骤：将硝酸铝水合物(Al(NO3)3·9H2O)、硝酸钙水合物(Ca(NO3)2·4H2O)、硝酸铁水合物(Fe(NO3)3)·9H2O)、六次甲基四胺((CH2)6N4)、乙酰丙酮((CH3CO)2CH(AcAcH))及去离子水按重量比为1∶1.26∶1.08∶0.2∶0.08∶5混合，硝酸铝水合物、硝酸钙水合物、硝酸铁水合物、六次甲基四胺、乙酰丙酮均为分析纯化学试剂，控制反应温度为70℃，搅拌12h至形成透明溶胶，将溶胶置于水浴中，控制水浴温度为70℃，陈化6天形成凝胶，得到的凝胶烘干后置于高温裂解炉中进行热处理，控制温度为750℃，灼烧4h，最后缓慢冷却至室温，即得到铁铝酸钙。A preparation method of calcium aluminum ferrite, the method is a sol-gel method, specifically comprising the following steps: aluminum nitrate hydrate (Al(NO 3 ) 3 9H 2 O), calcium nitrate hydrate (Ca(NO 3 ) 2 ·4H 2 O), ferric nitrate hydrate (Fe(NO 3 ) 3 )·9H 2 O), hexamethylenetetramine ((CH 2 ) 6 N 4 ), acetylacetone ((CH 3 CO ) 2 CH(AcAcH)) and deionized water in a weight ratio of 1:1.26:1.08:0.2:0.08:5, aluminum nitrate hydrate, calcium nitrate hydrate, iron nitrate hydrate, hexamethylenetetramine, Acetylacetone is an analytically pure chemical reagent, control the reaction temperature at 70°C, stir for 12 hours until a transparent sol is formed, place the sol in a water bath, control the temperature of the water bath at 70°C, age for 6 days to form a gel, and bake the obtained gel After drying, place it in a high-temperature cracking furnace for heat treatment, control the temperature at 750°C, burn for 4 hours, and finally cool slowly to room temperature to obtain calcium aluminoferrite.
实施例3Example 3
一种铁铝酸钙的制备方法，该方法为溶胶-凝胶法，具体包括以下步骤：将硝酸铝水合物(Al(NO3)3·9H2O)、硝酸钙水合物(Ca(NO3)2·4H2O)、硝酸铁水合物(Fe(NO3)3)·9H2O)、六次甲基四胺((CH2)6N4)、乙酰丙酮((CH3CO)2CH(AcAcH))及去离子水按重量比为1∶1.26∶1.08∶0.6∶0.16∶10混合，硝酸铝水合物、硝酸钙水合物、硝酸铁水合物、六次甲基四胺、乙酰丙酮均为分析纯化学试剂，控制反应温度为70℃，搅拌10h至形成透明溶胶，将溶胶置于水浴中，控制水浴温度为70℃，陈化3天形成凝胶，得到的凝胶烘干后置于高温裂解炉中进行热处理，控制温度为800℃，灼烧2h，最后缓慢冷却至室温，即得到铁铝酸钙。A preparation method of calcium aluminum ferrite, the method is a sol-gel method, specifically comprising the following steps: aluminum nitrate hydrate (Al(NO 3 ) 3 9H 2 O), calcium nitrate hydrate (Ca(NO 3 ) 2 ·4H 2 O), ferric nitrate hydrate (Fe(NO 3 ) 3 )·9H 2 O), hexamethylenetetramine ((CH 2 ) 6 N 4 ), acetylacetone ((CH 3 CO ) 2 CH(AcAcH)) and deionized water in a weight ratio of 1:1.26:1.08:0.6:0.16:10, aluminum nitrate hydrate, calcium nitrate hydrate, iron nitrate hydrate, hexamethylenetetramine, Acetylacetone is an analytically pure chemical reagent. Control the reaction temperature at 70°C, stir for 10 hours until a transparent sol is formed, place the sol in a water bath, control the temperature of the water bath at 70°C, and age for 3 days to form a gel. The obtained gel is baked After drying, place it in a high-temperature cracking furnace for heat treatment, control the temperature at 800°C, burn for 2 hours, and finally cool slowly to room temperature to obtain calcium aluminoferrite.
实施例4Example 4
一种铁铝酸钙的制备方法，该方法为溶胶-凝胶法，具体包括以下步骤：将硝酸铝水合物(Al(NO3)3·9H2O)、硝酸钙水合物(Ca(NO3)2·4H2O)及硝酸铁水合物(Fe(NO3)3)·9H2O)混合加入去离子水中，得到混合溶液，然后向混合溶液中加入乙酰丙酮((CH3CO)2CH(AcAcH))，搅拌30min，然后加入溶解于去离子水中的六次甲基四胺，搅拌3h，加入的硝酸铝水合物(Al(NO3)3·9H2O)、硝酸钙水合物(Ca(NO3)2·4H2O)、硝酸铁水合物(Fe(NO3)3)·9H2O)、六次甲基四胺((CH2)6N4)、乙酰丙酮((CH3CO)2CH(AcAcH))及去离子水的重量比为1∶1.26∶1.08∶0.5∶0.13∶8，均为分析纯化学试剂，控制温度为50℃，充分搅拌12h至形成透明溶胶，将溶胶置于水浴中，控制水浴温度为50℃，陈化5天形成凝胶，得到的凝胶置于高温裂解炉中进行热处理，控制温度为800℃，灼烧3h，最后缓慢冷却至室温，即得到铁铝酸钙。A preparation method of calcium aluminum ferrite, the method is a sol-gel method, specifically comprising the following steps: aluminum nitrate hydrate (Al(NO 3 ) 3 9H 2 O), calcium nitrate hydrate (Ca(NO 3 ) 2 · 4H 2 O) and ferric nitrate hydrate (Fe(NO 3 ) 3 ) · 9H 2 O) were mixed and added to deionized water to obtain a mixed solution, and then acetylacetone ((CH 3 CO) 2 CH(AcAcH)), stirred for 30min, then added hexamethylenetetramine dissolved in deionized water, stirred for 3h, added aluminum nitrate hydrate (Al(NO 3 ) 3 ·9H 2 O), calcium nitrate hydrated (Ca(NO 3 ) 2 4H 2 O), iron nitrate hydrate (Fe(NO 3 ) 3 ) 9H 2 O), hexamethylenetetramine ((CH 2 ) 6 N 4 ), acetylacetone ((CH 3 CO) 2 CH(AcAcH)) and deionized water in a weight ratio of 1:1.26:1.08:0.5:0.13:8, both of which are analytically pure chemical reagents, the temperature is controlled at 50°C, and the mixture is fully stirred for 12 hours to form Transparent sol, put the sol in a water bath, control the temperature of the water bath to 50°C, and age for 5 days to form a gel. The obtained gel is placed in a high-temperature cracking furnace for heat treatment, the temperature is controlled at 800°C, burned for 3 hours, and finally slowly Cool to room temperature to obtain calcium aluminum ferrite.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010109398 CN102153144B (en) | 2010-02-11 | 2010-02-11 | Method for preparing calcium ferroaluminates |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010109398 CN102153144B (en) | 2010-02-11 | 2010-02-11 | Method for preparing calcium ferroaluminates |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102153144A CN102153144A (en) | 2011-08-17 |
| CN102153144B true CN102153144B (en) | 2013-02-13 |
Family
ID=44434879
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010109398 Expired - Fee Related CN102153144B (en) | 2010-02-11 | 2010-02-11 | Method for preparing calcium ferroaluminates |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102153144B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102897843A (en) * | 2012-09-24 | 2013-01-30 | 同济大学 | Method for synthesis of tetracalcium aluminoferrite by sol-gel technology |
| CN105753341B (en) * | 2016-02-26 | 2017-08-29 | 西南石油大学 | A kind of preparation method of calcium aluminoferrite |
| CN106220005B (en) * | 2016-07-26 | 2017-11-10 | 武汉大学 | A kind of method that ultra-dispersed high pure state nano cement is prepared using sol-gel technique |
| CN106746801B (en) * | 2016-12-26 | 2019-01-11 | 西南石油大学 | A method of crystallite calcium aluminoferrite is prepared using red mud |
| CN109748326A (en) * | 2019-03-22 | 2019-05-14 | 西南石油大学 | A process for preparing tetracalcium ferric aluminate by sol-gel method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382657A (en) * | 2002-06-05 | 2002-12-04 | 武汉理工大学 | Process for supplying heat while preparing aluminat cement/active powdered coal ash by coal burning boiler and its products |
| CN1600872A (en) * | 2004-10-26 | 2005-03-30 | 上海彭浦冶金辅料有限公司 | Dephosphorising agent for converter and preparation method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8409344B2 (en) * | 2007-02-26 | 2013-04-02 | Metamateria Technologies Llc | Cement and methods of preparing cement |
-
2010
- 2010-02-11 CN CN 201010109398 patent/CN102153144B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382657A (en) * | 2002-06-05 | 2002-12-04 | 武汉理工大学 | Process for supplying heat while preparing aluminat cement/active powdered coal ash by coal burning boiler and its products |
| CN1600872A (en) * | 2004-10-26 | 2005-03-30 | 上海彭浦冶金辅料有限公司 | Dephosphorising agent for converter and preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102153144A (en) | 2011-08-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108946787B (en) | A kind of preparation method of rare earth-based fluorite type high-entropy oxide powder material | |
| CN102775985B (en) | There is a Sr2MgSi2O7:Eu2+ for long-persistence luminous function, the synthetic method of Dy3+ nano wire | |
| CN106747541A (en) | A kind of method of the mullite ceramic of On In-situ Synthesis of Mullite Whisker self toughening | |
| CN102153144B (en) | Method for preparing calcium ferroaluminates | |
| CN103182514B (en) | Method for preparing neodymium iron boron magnetic powder by self-propagating combustion | |
| CN104973615B (en) | Microwave burning preparation method of nano gadolinium oxide powder | |
| CN104030693B (en) | A kind of preparation method of triple cationic Ce:LuAG ceramic fluorescent powder | |
| CN105130502B (en) | A method of firing photochromic Jun porcelain under oxidative atmosphere conditions | |
| Liao et al. | Structure refinement and up-conversion of Ho3+/Er3+ Co-doped 12CaO· 7Al2O3 | |
| CN105777140B (en) | A kind of Yb2SiO5Raw powder's production technology | |
| CN105271427B (en) | Method for fast preparing polycrystalline tetra calcium aluminoferrite | |
| CN102897843A (en) | Method for synthesis of tetracalcium aluminoferrite by sol-gel technology | |
| CN105859165B (en) | A method of high-purity monocalcium aluminate is prepared using solid phase reaction | |
| CN105000911B (en) | Preparation method of purple ceramic pigment with cobalt-silicon olivine structure | |
| CN110817927A (en) | Method for preparing light porous nano cerium oxide by combustion method | |
| CN101508438A (en) | Method for producing mullite with kleit as raw material | |
| CN111747434A (en) | A method for preparing modified γ-Al2O3 powder by microwave-assisted combustion method | |
| CN102153295B (en) | Method for preparing Portland cement clinker | |
| CN102206077B (en) | Preparation method of zinc cobalt sodium silicate nano powder | |
| CN112480917B (en) | Europium-doped zinc orthotitanate red fluorescent powder with hexagonal prism shape and preparation method thereof | |
| CN104591292A (en) | A method for synthesizing iron-aluminum spinel | |
| CN101215167A (en) | Preparation method of far infrared powder material | |
| CN100537083C (en) | Preparation method of Ag composite (Ca0.95Bi0.05)3Co4O9 based oxide thermoelectric material | |
| CN103420341A (en) | Method for preparing oxide nanobelt through burning | |
| CN106745259A (en) | A kind of method that expoxy propane low-temperature sol-gel method prepares copper-chrome black |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130213 Termination date: 20160211 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |