CN101852726B - Method for detecting activity of metakaolin by using spectrophotometer - Google Patents
Method for detecting activity of metakaolin by using spectrophotometer Download PDFInfo
- Publication number
- CN101852726B CN101852726B CN201010109823XA CN201010109823A CN101852726B CN 101852726 B CN101852726 B CN 101852726B CN 201010109823X A CN201010109823X A CN 201010109823XA CN 201010109823 A CN201010109823 A CN 201010109823A CN 101852726 B CN101852726 B CN 101852726B
- Authority
- CN
- China
- Prior art keywords
- metakaolin
- solution
- spectrophotometer
- add
- hydrochloric acid
- 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
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 230000000694 effects Effects 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 44
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 42
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002835 absorbance Methods 0.000 claims abstract description 15
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 15
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 15
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000012086 standard solution Substances 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 10
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008247 solid mixture Substances 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims 7
- 229960004011 methenamine Drugs 0.000 claims 3
- 235000021110 pickles Nutrition 0.000 claims 3
- 238000007865 diluting Methods 0.000 claims 2
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims 2
- 238000010908 decantation Methods 0.000 claims 1
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 230000003252 repetitive effect Effects 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000012546 transfer Methods 0.000 abstract description 5
- 238000005554 pickling Methods 0.000 abstract description 4
- 239000005995 Aluminium silicate Substances 0.000 description 29
- 235000012211 aluminium silicate Nutrition 0.000 description 29
- 238000001354 calcination Methods 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 239000000463 material Substances 0.000 description 14
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 10
- 239000000523 sample Substances 0.000 description 8
- -1 aluminum ions Chemical class 0.000 description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 235000010755 mineral Nutrition 0.000 description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 6
- 238000002386 leaching Methods 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 235000019353 potassium silicate Nutrition 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000011575 calcium Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 229920000876 geopolymer Polymers 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000646 scanning calorimetry Methods 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 2
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 229910052622 kaolinite Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 239000004246 zinc acetate Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- NNBFNNNWANBMTI-UHFFFAOYSA-M brilliant green Chemical compound OS([O-])(=O)=O.C1=CC(N(CC)CC)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](CC)CC)C=C1 NNBFNNNWANBMTI-UHFFFAOYSA-M 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000003926 complexometric titration Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
Images
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
一种利用分光光度计检测偏高岭土活性的方法,涉及一种偏高岭土。提供一种方法操作简单方便、测定快速、结果可靠的利用分光光度计检测偏高岭土活性的方法。样品倒入容器中,加入盐酸,加热反应后,滤液加水定容;置铝片于容器中,用盐酸浸溶至表面氧化层溶解,倒去盐酸溶液,将铝片置于容器中,加入王水,加热溶解,移入容量瓶内,用水稀释,移取到容量瓶内,用水稀释,分别取1μg/mL铝标准溶液于容量瓶内,加入抗坏血酸溶液、铬天青-S乙醇溶液、六亚甲基四胺溶液,加水定容,再移入吸收皿中,于分光光度计波长545nm处测量吸光度,求铝工作标准曲线的斜率;测定酸浸液中铝含量,再计算偏高岭土中活性氧化铝含量。A method for detecting the activity of metakaolin by using a spectrophotometer relates to a metakaolin. A method for detecting metakaolin activity by using a spectrophotometer is provided, which is simple and convenient in operation, fast in determination and reliable in result. Pour the sample into a container, add hydrochloric acid, heat the reaction, add water to the filtrate to make up the volume; put the aluminum sheet in the container, soak and dissolve the surface oxide layer with hydrochloric acid, pour off the hydrochloric acid solution, put the aluminum sheet in the container, add Wang Water, heat to dissolve, transfer into the volumetric flask, dilute with water, pipette into the volumetric flask, dilute with water, take 1μg/mL aluminum standard solution in the volumetric flask, add ascorbic acid solution, chromazurin-S ethanol solution, six sub- Methyltetramine solution, add water to constant volume, then move it into an absorption dish, measure the absorbance at a spectrophotometer wavelength of 545nm, and find the slope of the aluminum working standard curve; measure the aluminum content in the pickling solution, and then calculate the active alumina in metakaolin content.
Description
技术领域technical field
本发明涉及一种偏高岭土,尤其是涉及一种利用分光光度计检测偏高岭土活性的方法。The invention relates to metakaolin, in particular to a method for detecting the activity of metakaolin by using a spectrophotometer.
背景技术Background technique
偏高岭土是高岭土经过适当温度煅烧后得到的具有一定化学活性的介稳态物质。偏高岭土中原子排列不规则,呈现热力学介稳状态,具有较高的火山灰活性。因而,偏高岭土是一种高活性的人工火山灰材料。偏高岭土以其特有的矿物特性,既可作为一种新型的矿物掺合料加以利用,又可用于新型胶凝材料的研究及应用。Metakaolin is a metastable substance with certain chemical activity obtained after calcining kaolin at an appropriate temperature. The atomic arrangement in metakaolin is irregular, showing a thermodynamic metastable state, and has high pozzolanic activity. Therefore, metakaolin is a highly active artificial pozzolanic material. Due to its unique mineral properties, metakaolin can be used not only as a new type of mineral admixture, but also in the research and application of new cementitious materials.
偏高岭土能与水泥水化产物Ca(OH)2反应生成水化铝酸钙、C-S-H凝胶等胶凝物质,具有较高的水化活性,可以用作混凝土矿物掺合料,它具有改善硬化混凝土的工作性和耐久性,减少水泥石的自收缩等方面的作用。偏高岭土也可以用来制备地聚合胶凝材料。地聚合胶凝材料是偏高岭土在碱性激活剂及促硬剂等外掺料的共同作用下形成的,不但生产能耗低,污染少,而且能大量利用工业废渣,是一种有发展前景的绿色建筑材料,符合低碳经济和可持续发展的要求。Metakaolin can react with cement hydration product Ca(OH) 2 to form gelling substances such as calcium aluminate hydrate and CSH gel. It has high hydration activity and can be used as a concrete mineral admixture. It has the ability to improve hardening Improve the workability and durability of concrete, and reduce the self-shrinkage of cement stone. Metakaolin can also be used to prepare geopolymeric cementitious materials. The geopolymeric cementitious material is formed by metakaolin under the combined action of alkaline activators and hardening accelerators and other external materials. It not only has low production energy consumption and less pollution, but also can utilize a large amount of industrial waste residues. It is a promising development prospect. Green building materials meet the requirements of low-carbon economy and sustainable development.
只有高活性的偏高岭土才能够被广泛应用。因此,活性是偏高岭土的首要检测指标。经验指出,不同来源的高岭土,得到高活性偏高岭土的煅烧温度会有所不同,因此,需要对偏高岭土的活性进行检验。Only highly active metakaolin can be widely used. Therefore, activity is the primary detection index of metakaolin. Experience has pointed out that the calcination temperature of metakaolin with high activity will be different for different sources of kaolin. Therefore, the activity of metakaolin needs to be tested.
目前,评价偏高岭土活性的方法有:X射线衍射分析、热重分析、扫描量热分析、碱吸收法、钙吸收法、压缩测强法、强度对比法和活性氧化铝含量法等。At present, the methods for evaluating the activity of metakaolin include: X-ray diffraction analysis, thermogravimetric analysis, scanning calorimetry analysis, alkali absorption method, calcium absorption method, compression strength measurement method, strength comparison method and activated alumina content method, etc.
相关文献(Torres Sánchez R M,Basaldella E I,Marco J F.The effect of thermal andmechanical treatment on kaolinite:Characterization by XPS and IEP measurements[J].Journal ofColloid and Interface Science,1999,215:339-344.;曹德光,陈益兰,欧绍权.烧粘土的碱胶凝性研究[J].中国非金属矿工业导刊,2000,21-22(2):28.;Kakali G,Perraki T,Tsivilis S,et al Thermal treatment of kaolin:the effect of mineralogy on the pozzolanic activity.[J].AppliedClay Science,2001,20:73-81.)按不同煅烧制度煅烧高岭土,并对煅烧出来的偏高岭土进行X射线衍射分析、热重分析、扫描量热分析等,从而间接判断出煅烧得到的偏高岭土的活性。但X射线衍射分析、热重分析、扫描量热分析等仪器分析法是直接对偏高岭土进行分析,着重描述高岭土在一定煅烧制度下其晶型结构的变化规律,不能直接说明所得偏高岭土的活性大小。Related literature (Torres Sánchez R M, Basaldella E I, Marco J F. The effect of thermal and mechanical treatment on kaolinite: Characterization by XPS and IEP measurements[J]. Journal of Colloid and Interface Science, 1999, 215: 339-344.; Cao Deguang, Chen Yilan, Ou Shaoquan. Alkali gelation of burnt clay[J]. China Non-Metallic Mineral Industry Guide, 2000, 21-22(2): 28.; Kakali G, Perraki T, Tsivilis S, et al Thermal Treatment of kaolin: the effect of mineralology on the pozzolanic activity. [J]. Applied Clay Science, 2001, 20: 73-81.) Kaolin was calcined according to different calcination systems, and the calcined metakaolin was analyzed by X-ray diffraction, thermal Gravity analysis, scanning calorimetry analysis, etc., so as to indirectly judge the activity of the calcined metakaolin. However, X-ray diffraction analysis, thermogravimetric analysis, scanning calorimetry and other instrumental analysis methods directly analyze metakaolin, emphatically describe the change rule of the crystal structure of kaolin under a certain calcination system, and cannot directly explain the activity of metakaolin obtained. size.
法国教授Davidovits认为(Davidovits J.Geopolymer Chemistry and Properties[J].Proceedings ofthe First European Conference on Soft Mineralogy,1988,(1):429-441.)土壤聚合物的形成过程是由溶解、单体重构和聚缩3个阶段组成,经重构的单体发生类似于有机高分子聚合物形成时的聚缩反应,而碱金属离子在最终产物中起到平衡电价的作用。偏高岭土由于煅烧温度和保温时间不同,其羟基脱去的数量和结构有所不同,因而偏高岭土在碱溶液中的溶解速度不同,导致对碱的吸收情况也不相同。因此,碱吸收法(郭文瑛,吴国林,文梓芸,等.偏高岭土活性评价方法的研究[J].武汉理工大学学报,2006,(03):76-79.)可以区分偏高岭土是否具有活性。但实验研究表明,活性较好的偏高岭土其活性高低的规律与土壤聚合物3d强度的规律不一致。French professor Davidovits believes (Davidovits J.Geopolymer Chemistry and Properties[J].Proceedings of the First European Conference on Soft Mineralogy, 1988, (1): 429-441.) The formation process of soil polymer is by dissolution, monomer reconstruction Composed of three stages of polycondensation, the restructured monomer undergoes a polycondensation reaction similar to the formation of organic polymers, and the alkali metal ions play a role in balancing the electricity price in the final product. Due to the different calcination temperature and holding time of metakaolin, the number and structure of its hydroxyl groups are different, so the dissolution rate of metakaolin in alkali solution is different, resulting in different absorption of alkali. Therefore, the alkali absorption method (Guo Wenying, Wu Guolin, Wen Ziyun, etc. Research on the activity evaluation method of metakaolin [J]. Journal of Wuhan University of Technology, 2006, (03): 76-79.) can distinguish whether metakaolin has activity . However, experimental studies have shown that the law of activity of metakaolin with better activity is not consistent with the law of 3D strength of soil polymer.
钙吸收法主要是依据材料中的活性二氧化硅和三氧化铝同石灰作用生成含水硅酸钙和含水铝酸钙。因而在一定时间内,材料吸收石灰溶液中石灰量的多少可以表示它活性的大小。但对于用硅酸钠溶液激发偏高岭土的试验系统,由于缺少了钙,该方法不适合评价此类系统中偏高岭土的活性。The calcium absorption method is mainly based on the action of active silica and alumina in the material with lime to generate hydrous calcium silicate and hydrous calcium aluminate. Therefore, within a certain period of time, the amount of lime in the lime solution absorbed by the material can indicate its activity. However, for the test system of metakaolin excited by sodium silicate solution, due to the lack of calcium, this method is not suitable for evaluating the activity of metakaolin in such systems.
偏高岭土是一种无定形的不稳定状态的硅铝酸盐,是一种拥有自由能的物质,根据ΓУXOBCКИЙ的接触硬化理论(ΓJIУXOBCКИЙBД,PУHOBAPΦ,MACУHOBCE.接触硬化胶凝材料及复合材料[M].蒲心诚译.重庆:重庆大学出版社,2004.),偏高岭土应该具有缩聚的倾向,因而可以采用压缩的方法使其产生强度,郭文瑛等的研究结果亦表明该方法不能定量地描述活性的大小。Metakaolin is an amorphous aluminosilicate in an unstable state. It is a substance with free energy. According to the contact hardening theory of ΓУXOBCКИЙ (ΓJIУXOBCКИЙBД, PУHOBAPΦ, MACУHOBCE. Contact hardening cementitious materials and composite materials [M] Translated by Pu Xincheng. Chongqing: Chongqing University Press, 2004.), metakaolin should have a tendency to polycondensate, so compression methods can be used to make it produce strength. The research results of Guo Wenying and others also show that this method cannot quantitatively describe the size of the activity .
强度对比法是指直接用硅酸钠激发偏高岭土制备地聚合胶凝材料,养护到一定龄期测定其抗压强度或抗折强度等参数来评价偏高岭土的活性。该方法是评价偏高岭土活性最有效、最直观的方法,但一般需要3d或7d才能出结果,耗时太长,不适用于生产。The strength comparison method refers to the direct use of sodium silicate to stimulate metakaolin to prepare geopolymeric cementitious materials, and to measure the parameters such as compressive strength or flexural strength after curing to a certain age to evaluate the activity of metakaolin. This method is the most effective and intuitive method to evaluate the activity of metakaolin, but it usually takes 3 days or 7 days to get the result, which is too long and not suitable for production.
煅烧高岭土中的氧化铝可分为二类:一类在酸中具有良好的活性,如γ-Al2O3,一般称之为活性铝;另一类在酸中的活性很差,如α-Al2O3,称之为惰性铝。实际上活性氧化铝是高岭土中所有能和酸起反应的各种形态铝的集合,折算成γ-Al2O3出现。在高岭土的酸浸反应中,惰性铝对反应基本上没有贡献。The alumina in calcined kaolin can be divided into two types: one type has good activity in acid, such as γ-Al 2 O 3 , which is generally called active aluminum; the other type has poor activity in acid, such as α -Al 2 O 3 , called inert aluminum. In fact, activated alumina is a collection of all forms of aluminum in kaolin that can react with acids, and it is converted into γ-Al 2 O 3 to appear. In the acid leaching reaction of kaolin, inert aluminum basically does not contribute to the reaction.
徐超等(徐超,张兴法,韩效钊,许民才.高岭土中活性氧化铝测定[J].非金属矿,1998,21(5):13-14)在一定实验条件下对偏高岭土先作酸浸处理,后用EDTA容量法,分析确定其中的活性氧化铝含量的多少,来定量地比较偏高岭土活性的高低。测定方法可以概括为:偏高岭土在加热条件下用盐酸浸出活性氧化铝。加过量EDTA,与铝等离子络合,在PH=6时,用乙酸锌溶液滴定过量的EDTA,然后加氟化钠,使被EDTA络合的铝离子变为氟铝络离子,并释出等量的EDTA,再用乙酸锌溶液滴定释出的EDTA,计算活性氧化铝含量。对于铁染高岭土,其酸浸液中含有较多铁离子。由于铝离子和铁离子都能与EDTA络合,若采用徐超、张兴法等的EDTA络合滴定法测定酸浸液,则测出的活性氧化铝含量是偏高的。Xu Chao et al. (Xu Chao, Zhang Xingfa, Han Xiaozhao, Xu Mincai. Determination of active alumina in kaolin [J]. Nonmetallic Minerals, 1998, 21(5): 13-14) made acid leaching of metakaolin under certain experimental conditions After treatment, use the EDTA volumetric method to analyze and determine the content of activated alumina in it, so as to quantitatively compare the activity of metakaolin. The determination method can be summarized as follows: metakaolin is leached with hydrochloric acid to activate alumina under heating conditions. Add excess EDTA to complex with aluminum plasma. When PH = 6, titrate the excess EDTA with zinc acetate solution, then add sodium fluoride, so that the aluminum ions complexed by EDTA become fluoride-aluminum complex ions, and release etc. amount of EDTA, and then titrate the released EDTA with zinc acetate solution to calculate the content of activated alumina. For iron-stained kaolin, the pickling solution contains more iron ions. Since both aluminum ions and iron ions can be complexed with EDTA, if the EDTA complexometric titration method of Xu Chao and Zhang Xing is used to measure the acid leaching solution, the content of activated alumina measured is relatively high.
徐小彬等(徐小彬,殷素红,杨建军,文梓芸.偏高岭土活性快速检验方法的研究[J].硅酸盐通报,2008,27(4):690-694.)采用相似方法,用氧化铝在酸中的溶出率来表示偏高岭土的活性大小。实验结果表明偏高岭土中氧化铝溶出率与用其制备的地聚合物的抗压强度值有很好的对应关系,氧化铝溶出率高的偏高岭土激发得到的地聚合物的抗压强度值也高。该方法检测一个样品只需3h,是一种能够应用到工业生产中的快速检验偏高岭土活性的方法。但由于常温条件下,铝离子与EDTA络合速度缓慢,必须先加入过量EDTA,加热促使反应加速进行。“以表面皿盖住瓶口后加热煮沸3min,冷却至室温”。再滴加指示剂。由于需要加热煮沸,冷却后才能滴加指示剂,给检测带来不便。且该方法以“指示剂由黄色经翠绿色突变为草绿色为终点”,颜色变化并不明显,滴定终点难以判断,存在较多的人为认为误差。因此,需要发明一种能够快速准确测定偏高岭土活性的方法。Xu Xiaobin et al. (Xu Xiaobin, Yin Suhong, Yang Jianjun, Wen Ziyun. Research on the rapid test method of metakaolin activity [J]. Silicate Bulletin, 2008, 27(4): 690-694.) adopted a similar method, using alumina in The dissolution rate in the acid indicates the activity of metakaolin. The experimental results show that the dissolution rate of alumina in metakaolin has a good correspondence with the compressive strength value of the geopolymer prepared with it, and the compressive strength value of the geopolymer excited by metakaolin with a high alumina dissolution rate is also the same. high. The method only needs 3 hours to detect a sample, and it is a method for quickly testing the activity of metakaolin that can be applied in industrial production. However, under normal temperature conditions, the complexation speed of aluminum ions and EDTA is slow, so an excess of EDTA must be added first, and heating will accelerate the reaction. "Cover the bottle with a watch glass, heat to boil for 3 minutes, and cool to room temperature." Then add the indicator dropwise. Since it needs to be heated and boiled, the indicator can only be added dropwise after cooling, which brings inconvenience to the detection. And this method takes "the indicator changes from yellow to emerald green to grass green as the end point", the color change is not obvious, the titration end point is difficult to judge, and there are many human errors. Therefore, it is necessary to invent a method that can quickly and accurately measure the activity of metakaolin.
发明内容Contents of the invention
本发明的目的在于提供一种方法操作简单方便、测定快速、结果可靠的利用分光光度计检测偏高岭土活性的方法。The purpose of the present invention is to provide a method for detecting the activity of metakaolin with a spectrophotometer, which is simple and convenient in operation, fast in determination and reliable in result.
本发明的技术方案是对偏高岭土进行酸浸处理,然后采用分光光度法测定酸浸液中的铝含量,再换算成活性氧化铝的含量,以此标定偏高岭土活性。The technical scheme of the present invention is to carry out acid leaching treatment on metakaolin, then adopt spectrophotometry to measure the aluminum content in the acid leaching solution, and then convert it into the content of activated alumina, so as to calibrate the activity of metakaolin.
本发明包括以下步骤:The present invention comprises the following steps:
1)偏高岭土的酸浸处理:1) Acid leaching treatment of metakaolin:
将偏高岭土样品倒入容器中,再加入盐酸,在恒温水浴中加热,搅拌反应后,将容器中的液固混合物冷却、过滤、洗涤,将滤液移入容量瓶内,加蒸馏水定容;Pour the metakaolin sample into the container, then add hydrochloric acid, heat in a constant temperature water bath, stir and react, then cool, filter and wash the liquid-solid mixture in the container, transfer the filtrate into a volumetric flask, and add distilled water to constant volume;
2)铝标准溶液的配制:2) Preparation of aluminum standard solution:
置光谱铝片于容器中,用盐酸浸溶至表面氧化层溶解,用倾泻法倒去盐酸溶液,洗涤后,干燥,将铝片置于容器中,加入王水,加热溶解后,冷却,移入容量瓶内,用蒸馏水稀释,用移液枪移取到容量瓶内,用蒸馏水稀释,摇匀;Put the spectroscopic aluminum flakes in a container, dip and dissolve them with hydrochloric acid until the surface oxide layer is dissolved, pour off the hydrochloric acid solution by pouring, wash and dry, put the aluminum flakes in the container, add aqua regia, heat to dissolve, cool, and move into In the volumetric flask, dilute with distilled water, transfer to the volumetric flask with a pipette gun, dilute with distilled water, and shake well;
3)铝工作标准曲线的绘制:3) Drawing of aluminum working standard curve:
分别取1μg/mL铝标准溶液1mL,2mL,3mL,4mL,5mL,7mL,9mL,12mL,15mL,18mL,24mL,于容量瓶内,加入抗坏血酸溶液,然后加入铬天青-S乙醇溶液,再加入六亚甲基四胺溶液,最后加蒸馏水定容,再移入吸收皿中,于分光光度计波长545nm处测量其吸光度,以铝的质量为横坐标,吸光度为纵坐标,绘制铝工作标准曲线,可得一直线。求出其斜率,即为铝工作标准曲线的斜率;Take 1mL, 2mL, 3mL, 4mL, 5mL, 7mL, 9mL, 12mL, 15mL, 18mL, 24mL of 1μg/mL aluminum standard solution respectively in the volumetric flask, add ascorbic acid solution, then add chromazurin-S ethanol solution, and then Add hexamethylenetetramine solution, finally add distilled water to constant volume, then move it into an absorption dish, measure its absorbance at a spectrophotometer wavelength of 545nm, take the mass of aluminum as the abscissa, and the absorbance as the ordinate, draw the aluminum working standard curve , a straight line can be obtained. Find its slope, which is the slope of the aluminum working standard curve;
4)酸浸液中铝含量的测定:4) Determination of aluminum content in pickling solution:
用移液枪移取偏高岭土酸浸液1mL,稀释到100mL,取稀释后的偏高岭土酸浸液1mL于50mL容量瓶内,加入抗坏血酸,然后加入铬天青-S乙醇,再加入六亚甲基四氨,最后加蒸馏水定容,再移入吸收皿中,于分光光度计波长545nm处测量其吸光度,每次分析均随同试样进行空白试验,空白试验与试样测定采用完全相同的试剂和分析步骤,并进行平行操作,测得的吸光度,记为空白吸光度,根据吸光度,利用铝工作标准曲线的斜率计算出50mL样液中铝含量m1:Pipette 1mL of metakaolin acid immersion solution with a pipette gun, dilute to 100mL, take 1mL of the diluted metakaolin acid immersion solution in a 50mL volumetric flask, add ascorbic acid, then add chromazurin-S ethanol, and then add hexamethylene Finally, add distilled water to constant volume, then move it into an absorption dish, measure its absorbance at the wavelength of 545nm of the spectrophotometer, and carry out a blank test with the sample for each analysis. The blank test and sample determination use exactly the same reagents and Analysis steps, and carry out parallel operation, the measured absorbance is recorded as blank absorbance, according to the absorbance, the aluminum content m1 in the 50mL sample solution is calculated by using the slope of the aluminum working standard curve:
5)偏高岭土中活性氧化铝含量的计算5) Calculation of active alumina content in metakaolin
活性氧化铝的质量分数按下式计算:The mass fraction of activated alumina is calculated according to the following formula:
其中m2为偏高岭土的质量, Where m2 is the mass of metakaolin,
在步骤1)中,所述盐酸的加入量可以是在每1g偏高岭土样品中,加入20mL的盐酸,所述盐酸的质量百分比浓度可为15%;所述加热的温度可为80℃,所述搅拌反应的时间可为2h。In step 1), the addition of the hydrochloric acid can be in every 1g metakaolin sample, add the hydrochloric acid of 20mL, the mass percent concentration of described hydrochloric acid can be 15%; The temperature of described heating can be 80 ℃, so The time of the stirring reaction can be 2h.
在步骤2)中,所述盐酸可采用1∶9盐酸,所述洗涤最好是先用水洗涤3次后,再用无水乙醇洗涤3次;所述铝片的质量最好为1.0000g,加入王水的量最好为10mL。In step 2), the hydrochloric acid can be 1:9 hydrochloric acid, and the washing is preferably first washed with water for 3 times, and then washed with absolute ethanol for 3 times; the quality of the aluminum sheet is preferably 1.0000g, The best amount of adding aqua regia is 10mL.
在步骤3)中,所述抗坏血酸溶液可为2.5mL,10g/L现配的抗坏血酸溶液,所述铬天青-S乙醇溶液可为5mL,0.3g/L铬天青-S乙醇溶液,所述六亚甲基四胺溶液可为2.5mL,300g/L的六亚甲基四胺溶液。In step 3), described ascorbic acid solution can be 2.5mL, the ascorbic acid solution that 10g/L prepares now, and described chromazurin-S ethanol solution can be 5mL, 0.3g/L chromazurin-S ethanol solution, so The hexamethylenetetramine solution can be 2.5mL, 300g/L hexamethylenetetramine solution.
在步骤4)中,所述抗坏血酸可为2.5mL,10g/L现配的抗坏血酸,所述铬天青-S乙醇可为5mL,0.3g/L铬天青-S乙醇,所述六亚甲基四氨可为2.5mL,300g/L的六亚甲基四氨。In step 4), described ascorbic acid can be 2.5mL, the ascorbic acid that 10g/L mixes now, and described chromazurin-S ethanol can be 5mL, 0.3g/L chromazurin-S ethanol, and described hexamethylene Hexamethylenetetramine can be 2.5mL, 300g/L hexamethylenetetramine.
本发明采用铬天青-S分光光度法测定偏高岭土酸浸液中铝离子的含量,然后换算成活性氧化铝的含量。活性氧化铝含量越多,说明偏高岭土的活性越高。该方法将铝与铬天青-S络合,在pH=5.5~6.1的六亚甲基四胺介质中生成紫红色络合物。同时加入抗坏血酸来掩蔽铁的干扰,因而该方法特别适用于铁染高岭土中活性氧化铝含量的测定。而且该方法具有灵敏度和精密度高、需要的样品量少、操作简单、分析速度快、设备成本低等优点。The invention adopts the chrome azure-S spectrophotometric method to measure the content of aluminum ions in the metakaolin acid dipping solution, and then converts it into the content of activated alumina. The more activated alumina content, the higher the activity of metakaolin. In the method, aluminum is complexed with chromazurin-S, and a purple-red complex is formed in a hexamethylenetetramine medium with a pH of 5.5-6.1. At the same time, ascorbic acid is added to mask the interference of iron, so this method is especially suitable for the determination of active alumina content in iron-stained kaolin. Moreover, the method has the advantages of high sensitivity and precision, less required sample volume, simple operation, fast analysis speed, and low equipment cost.
附图说明Description of drawings
图1为本发明实施例的铝工作标准曲线。在图1中,横坐标铝含量/μg,纵坐标为吸光度。Fig. 1 is the aluminum working standard curve of the embodiment of the present invention. In Fig. 1, the abscissa is the aluminum content/μg, and the ordinate is the absorbance.
具体实施方式Detailed ways
以下实施例将结合附图对本发明作进一步的说明。The following embodiments will further illustrate the present invention in conjunction with the accompanying drawings.
加入不同体积1μg/mL铝标准溶液制得的溶液的吸光度如表1所示。The absorbance of solutions prepared by adding different volumes of 1 μg/mL aluminum standard solution is shown in Table 1.
表1Table 1
铝工作标准曲线如图1所示,由图1可知,该工作标准曲线的R值达到0.99966,线性拟合度很好。其斜率为0.05137。The working standard curve of aluminum is shown in Figure 1. It can be seen from Figure 1 that the R value of the working standard curve reaches 0.99966, and the linear fitting degree is very good. Its slope is 0.05137.
实施例1Example 1
1)采用漳州铁染高岭土作为原料。其中Al2O3含量为38.24%,Fe2O3含量为0.94%。主要矿物组成为高岭石和少量的石英,矿物结构为片状以及大量的管状。1) Zhangzhou iron dyed kaolin is used as raw material. Among them, the content of Al 2 O 3 is 38.24%, and the content of Fe 2 O 3 is 0.94%. The main mineral composition is kaolinite and a small amount of quartz, and the mineral structure is flake and a large number of tubes.
2)将漳州铁染高岭土置于高温节能电炉内煅烧。高岭土经磨细,过100目筛。升温速率为7.5℃/min,煅烧温度分别为500℃,600℃,700℃,800℃,900℃,1000℃,煅烧时间为2h。煅烧结束后,高岭土随炉冷却至室温,取出得到偏高岭土样品。2) Calcining Zhangzhou iron-dyed kaolin in a high-temperature energy-saving electric furnace. Kaolin is finely ground and passed through a 100-mesh sieve. The heating rate was 7.5°C/min, the calcination temperatures were 500°C, 600°C, 700°C, 800°C, 900°C, 1000°C, and the calcination time was 2h. After the calcination, the kaolin was cooled to room temperature with the furnace, and the metakaolin sample was taken out.
3)称取1g左右的偏高岭土样品,倒入250mL三口烧瓶中。然后倒入20mL 15%的盐酸,在恒温水浴中加热到80℃,搅拌反应2h。将三口烧瓶中的液固混合物冷却、过滤、洗涤。将滤液移入250mL容量瓶内,加蒸馏水定容,摇匀。3) Weigh about 1g of metakaolin sample and pour it into a 250mL three-necked flask. Then pour 20mL of 15% hydrochloric acid, heat to 80°C in a constant temperature water bath, and stir for 2h. The liquid-solid mixture in the three-necked flask was cooled, filtered and washed. Transfer the filtrate into a 250mL volumetric flask, add distilled water to volume, and shake well.
4)用移液枪移取偏高岭土酸浸液中1mL,稀释到100mL。取稀释后的酸浸液1mL于50mL容量瓶内。加入2.5mL,10g/L现配的抗坏血酸,摇匀。然后加入5mL,0.3g/L铬天青-S乙醇,摇匀。再加入2.5mL,300g/L的六亚甲基四氨,摇匀。最后加蒸馏水定容,摇匀。充分混合后,将上述溶液移入1cm吸收皿中,于分光光度计波长545nm处测量其吸光度。同时进行空白试验。4) Use a pipette gun to pipette 1 mL of the metakaolin acid immersion solution and dilute to 100 mL. Take 1mL of the diluted pickling solution in a 50mL volumetric flask. Add 2.5mL, 10g/L fresh ascorbic acid, shake well. Then add 5mL, 0.3g/L chromazurin-S ethanol and shake well. Then add 2.5mL, 300g/L hexamethylenetetramine and shake well. Finally add distilled water to make up to volume and shake well. After thorough mixing, transfer the above solution into a 1cm absorption dish, and measure its absorbance at a spectrophotometer wavelength of 545nm. Simultaneously conduct a blank test.
5)测定结果如下:煅烧温度分别为500℃,600℃,700℃,800℃,900℃,1000℃得到的偏高岭土中,活性氧化铝含量分别为0.37%,2.95%,17.84%,15.23%,15.35%,0.19%。5) The measurement results are as follows: in the metakaolin obtained by calcination temperatures of 500°C, 600°C, 700°C, 800°C, 900°C, and 1000°C, the contents of activated alumina were 0.37%, 2.95%, 17.84%, and 15.23%, respectively , 15.35%, 0.19%.
6)将上述煅烧得到的偏高岭土加入水玻璃制成地聚合胶凝材料。水玻璃的掺入量折算成Na2O为偏高岭土质量的15%;水玻璃的模数为1.35;按质量比,偏高岭土∶水玻璃为0.94。加入水玻璃后,搅拌制成标准稠度净浆,倒入20mm×20mm×20mm的钢制试模中,振动成型。将试块在自然条件下(温度为(20±5)℃,湿度≥70%)养护24h后脱模,继续养护,3d后测其抗压强度。抗压强度的测量按照国家标准GB/T17671-1999进行。6) Adding the metakaolin obtained by the above calcining into water glass to make a geopolymeric cementitious material. The dosing amount of water glass converted into Na 2 O is 15% of the mass of metakaolin; the modulus of water glass is 1.35; according to the mass ratio, metakaolin: water glass is 0.94. After adding water glass, stir to make a standard consistency slurry, pour it into a 20mm×20mm×20mm steel test mold, and vibrate to form it. The test block is demolded after curing for 24 hours under natural conditions (temperature is (20±5) °C, humidity ≥70%), and the curing is continued, and its compressive strength is measured after 3 days. The measurement of compressive strength is carried out according to the national standard GB/T17671-1999.
7)测得试块的抗压强度分别为:1.18MPa,8.95MPa,55.26MPa,50.47MPa,51.89MPa,0.62MPa。与测定的活性氧化铝含量有很好的对应关系。7) The measured compressive strengths of the test blocks are: 1.18MPa, 8.95MPa, 55.26MPa, 50.47MPa, 51.89MPa, 0.62MPa. It has a good correspondence with the determined active alumina content.
实施例2Example 2
原料及分析测试过程同实施例1。高岭土过100目筛。煅烧高岭土时,升温速率为7.5℃/min,煅烧温度为700℃,煅烧时间分别为2h,4h,6h,8h,10h。测得的活性氧化铝含量分别为:17.84%,18.72%,19.02%,19.56%,19.86%。制成的地聚合胶凝材料的抗压强度分别为55.26MPa,57.59MPa,58.02MPa,58.96MPa,59.46MPa。与测定的活性氧化铝含量有很好的对应关系。Raw material and analysis test process are with embodiment 1. Kaolin is passed through a 100-mesh sieve. When calcining kaolin, the heating rate is 7.5°C/min, the calcining temperature is 700°C, and the calcining time is 2h, 4h, 6h, 8h, and 10h respectively. The measured activated alumina contents are respectively: 17.84%, 18.72%, 19.02%, 19.56%, 19.86%. The compressive strengths of the prepared geopolymeric cementitious materials are 55.26MPa, 57.59MPa, 58.02MPa, 58.96MPa, 59.46MPa respectively. It has a good correspondence with the determined active alumina content.
实施例3Example 3
原料及分析测试过程同实施例1。高岭土过100目筛。煅烧高岭土时,升温速率分别为2.5℃/min,5℃/min,7.5℃/min,10℃/min。煅烧温度为700℃,煅烧时间分别为2h。测得的活性氧化铝含量分别为:16.32%,17.13%,17.84%,18.26%。制成的地聚合胶凝材料的抗压强度分别为54.78MPa,54.92MPa,55.26MPa,55.56MPa。与测定的活性氧化铝含量有很好的对应关系。Raw material and analysis test process are with embodiment 1. Kaolin is passed through a 100-mesh sieve. When calcining kaolin, the heating rates were 2.5°C/min, 5°C/min, 7.5°C/min, and 10°C/min. The calcination temperature is 700° C., and the calcination time is 2 hours respectively. The measured activated alumina contents are respectively: 16.32%, 17.13%, 17.84%, and 18.26%. The compressive strengths of the prepared geopolymeric cementitious materials are 54.78MPa, 54.92MPa, 55.26MPa and 55.56MPa respectively. It has a good correspondence with the determined active alumina content.
实施例4Example 4
原料及分析测试过程同实施例1。高岭土分别过60目筛,100目筛,120目筛,140目筛。煅烧高岭土时,升温速率分别为7.5℃/min。煅烧温度为700℃,煅烧时间分别为2h。测得的活性氧化铝含量分别为:17.45%,17.84%,18.12%,18.34%。制成的地聚合胶凝材料的抗压强度分别为55.02MPa,55.26MPa,55.38MPa,55.65MPa。与测定的活性氧化铝含量有很好的对应关系。Raw material and analysis test process are with embodiment 1. The kaolin was passed through a 60-mesh sieve, a 100-mesh sieve, a 120-mesh sieve, and a 140-mesh sieve. When calcining kaolin, the heating rate was 7.5°C/min. The calcination temperature is 700° C., and the calcination time is 2 hours respectively. The measured activated alumina contents are respectively: 17.45%, 17.84%, 18.12%, 18.34%. The compressive strengths of the prepared geopolymeric cementitious materials are 55.02MPa, 55.26MPa, 55.38MPa and 55.65MPa respectively. It has a good correspondence with the determined active alumina content.
实施例5Example 5
分析测试过程同实施例1。原料分别采用漳州铁染高岭土,龙岩铁染高岭土,武平湘店铁染高岭土,龙岩成品高岭土。其中龙岩铁染高岭土Al2O3含量为35.41%,Fe2O3含量为0.92%;武平湘店铁染高岭土Al2O3含量为34.93%,Fe2O3含量为1.08%;龙岩成品高岭土Al2O3含量为36.58%,Fe2O3含量为0.17%。高岭土过100目筛。煅烧高岭土时,升温速率分别为7.5℃/min。煅烧温度为600℃,煅烧时间分别为2h。测得的活性氧化铝含量分别为:17.84%,16.15%,16.03%,16.96%。制成的地聚合胶凝材料的抗压强度分别为55.26MPa,52.14MPa,50.98MPa,53.18MPa。与测定的活性氧化铝含量有很好的对应关系。The analysis and test process is the same as in Example 1. The raw materials are Zhangzhou iron-dyed kaolin, Longyan iron-dyed kaolin, Wuping Xiangdian iron-dyed kaolin and Longyan finished kaolin. Among them, Longyan iron-dyed kaolin contains 35.41% Al 2 O 3 and Fe 2 O 3 0.92%; Wuping Xiangdian iron-dyed kaolin contains 34.93% Al 2 O 3 and Fe 2 O 3 1.08%; Longyan finished kaolin The Al 2 O 3 content is 36.58%, and the Fe 2 O 3 content is 0.17%. Kaolin is passed through a 100-mesh sieve. When calcining kaolin, the heating rate was 7.5°C/min. The calcination temperature is 600° C., and the calcination time is 2 hours respectively. The measured activated alumina contents are respectively: 17.84%, 16.15%, 16.03%, and 16.96%. The compressive strengths of the prepared geopolymeric cementitious materials are 55.26MPa, 52.14MPa, 50.98MPa, 53.18MPa respectively. It has a good correspondence with the determined active alumina content.
Claims (9)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201010109823XA CN101852726B (en) | 2010-02-09 | 2010-02-09 | Method for detecting activity of metakaolin by using spectrophotometer |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201010109823XA CN101852726B (en) | 2010-02-09 | 2010-02-09 | Method for detecting activity of metakaolin by using spectrophotometer |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101852726A CN101852726A (en) | 2010-10-06 |
CN101852726B true CN101852726B (en) | 2011-09-07 |
Family
ID=42804316
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201010109823XA Expired - Fee Related CN101852726B (en) | 2010-02-09 | 2010-02-09 | Method for detecting activity of metakaolin by using spectrophotometer |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN101852726B (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107621483A (en) * | 2017-08-16 | 2018-01-23 | 西安建筑科技大学 | A method for testing the pH value of micro-concrete pore solution |
CN109827917B (en) * | 2019-03-28 | 2024-07-09 | 中国三峡建设管理有限公司 | Device and method for continuously measuring ammonia release amount in concrete |
-
2010
- 2010-02-09 CN CN201010109823XA patent/CN101852726B/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
CN101852726A (en) | 2010-10-06 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Sanalkumar et al. | Investigating the potential reactivity of fly ash for geopolymerization | |
Sun et al. | Effects of synthetic CSH/PCE nanocomposites on early cement hydration | |
Hu et al. | Estimation of reaction kinetics of geopolymers at early ages | |
Yang et al. | Durability of alkali-activated materials with different C–S–H and NASH gels in acid and alkaline environment | |
Chi et al. | Investigation of the hydration properties of cement with EDTA by alternative current impedance spectroscopy | |
Zhang et al. | Efflorescence: a critical challenge for geopolymer applications? | |
Zhang et al. | Long-term performance of silane coupling agent/metakaolin based geopolymer | |
CN102331422B (en) | Process for continuously and rapidly determining components in desulfurization gypsum | |
CN103964483B (en) | A kind of normal pressure solution method prepares the method for high strength gypsum | |
CN102621090B (en) | Method for measuring iron content in kaolin through using spectrophotometer | |
Mendoza et al. | An alternative thermal method for identification of pozzolanic activity in Ca (OH) 2/pozzolan pastes | |
CN111205008A (en) | Li ion doped nanometer C-A-S-H seed crystal and application thereof | |
CN108455622A (en) | CASH mineral suitable for improving volume stability of alkali-activated slag system and preparation method thereof | |
Zhao et al. | State-of-the-art review of geopolymer concrete carbonation: From impact analysis to model establishment | |
Pan et al. | Corrosion mechanism of recycled mortar prepared from CO2-treated hardened cement paste powder | |
CN101852726B (en) | Method for detecting activity of metakaolin by using spectrophotometer | |
CN105836774B (en) | A kind of method that quick low energy consumption prepares tricalcium aluminate | |
CN103983752B (en) | Method for rapidly testing content of attapulgite clay in same ore source and different batches | |
Zhang et al. | Variation in mineral composition by hydration and carbonation in calcium hydroxide matrix containing zeolite | |
Guo et al. | Preparation and performance of geopolymers | |
Braganca et al. | The use of 1% nano-Fe3O4 and 1% nano-TiO2 as partial replacement of cement to enhance the chemical performance of reinforced concrete structures | |
CN105403479A (en) | Determination method of bound water and free water of hardened cement paste matrix | |
Sui et al. | Investigation on the compressive strength, chloride migration of MK-FA-LS blended cementitious materials with electrochemical techniques | |
CN118405867A (en) | A method for inhibiting volume expansion of steel slag aggregate and its application | |
Zou et al. | Investigation of geopolymerization and setting process of metakaolin-based geopolymer based on low-field nuclear magnetic resonance relaxometry |
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 | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110907 Termination date: 20140209 |