CN101852726B - Method for detecting activity of metakaolin by using spectrophotometer - Google Patents
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Abstract
The invention discloses a method for detecting activity of metakaolin by using a spectrophotometer, and relates to metakaolin. The invention provides the method for detecting the activity of the metakaolin by using the spectrophotometer, with the advantages of simple and convenient operation, quick measurement and reliable result. The method comprises the following steps of: pouring a sample into a container, adding hydrochloric acid into the container, performing heating reaction on the mixture, and adding water into the filtrate to fix the volume; placing an aluminum sheet into the container, infiltrating the aluminum sheet by using the hydrochloric acid till a surface oxidation layer is dissolved, pouring out the hydrochloric acid solution, placing the aluminum sheet into the container, adding aqua regia into the container, heating and dissolving the aluminum sheet, transferring the solution into a volumetric flask, diluting the solution by using water, transferring the solution into the volumetric flask, diluting the solution by using water, injecting 1mu g/mL aluminum standard solution into the volumetric flasks respectively, adding ascorbic acid solution, chromazurine-S ethanol solution and hexamethylenetetramine solution into the volumetric flask, adding water into the volumetric flask to fix the volume, then transferring the mixture to an absorption vessel, measuring the absorbance at the 545nm wavelength of the spectrophotometer, and solving the slope of an aluminum working standard curve; and measuring the aluminum content of the acid extract, and then calculating the active aluminum oxide content of the metakaolin.
Description
Technical field
The present invention relates to a kind of metakaolin, especially relate to a kind of method of utilizing spectrophotometer to detect activity of metakaolin.
Background technology
Metakaolin is the certain chemically active metasable state material that has that obtains after porcelain earth is calcined through proper temperature.Atom irregular arrangement in the metakaolin presents the thermodynamics steady state that is situated between, and has higher pozzolanic activity.Thereby metakaolin is a kind of highly active artificial pozzolanic material.Metakaolin both can be used as a kind of novel mineral admixture and had been used with its distinctive mineralogical character, can be used for the research and the application of novel gelled material again.
Metakaolin can with hydrated cementitious product C a (OH)
2Gum materials such as water generation reaction calcium aluminate, C-S-H gel have higher hydration activity, can be used as concrete mineral admixture, and it has workability and the permanance of improving maturing, reduce the effect of the aspects such as self-constriction of cement stone.Metakaolin the polymeric gel gel material with also can being used for preparation.Ground polymeric gel gel material is that metakaolin forms under the acting in conjunction of extra materials such as alkaline activating agent and accelerator for hardening, not only energy consumption is low, pollutes and lacks, and can utilize industrial residue in a large number, be a kind of promising green construction material, meet the requirement of low-carbon economy and sustainable development.
Have only highly active metakaolin to be widely used.Therefore, activity is the primary detection index of metakaolin.Experience is pointed out, the porcelain earth of separate sources, and the calcining heat that obtains high-activity metakaolin can be different, therefore, need test to the activity of metakaolin.
At present, the method for evaluation activity of metakaolin has: strong method, intensity contrast method and activated alumina content method etc. are surveyed in X-ray diffraction analysis, thermogravimetric analysis, scanning thermometric analysis, alkali absorb method, calcium absorption method, compression.
Pertinent literature (Torres S á nchez 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.; Cao Deguang, Chen Yilan, Ou Shaoquan. the alkali gelling research [J] of burnedc lay. Chinese 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 mineralogy on the pozzolanic activity.[J] .AppliedClay Science, 2001,20:73-81.) press different calcinating system calcined kaolins, and carry out X-ray diffraction analysis, thermogravimetric analysis, scanning thermometric analysis etc. to calcining the metakaolin that comes out, thus judge the activity of calcining the metakaolin that obtains indirectly.But instrumental methods such as X-ray diffraction analysis, thermogravimetric analysis, scanning thermometric analysis are directly metakaolin to be analyzed, describe the Changing Pattern of porcelain earth its crystalline structure under certain calcinating system emphatically, the active size of gained metakaolin can not directly be described.
France professor Davidovits think (Davidovits J.Geopolymer Chemistry and Properties[J] .Proceedings ofthe First European Conference on Soft Mineralogy, 1988, (1): 429-441.) forming process of soil polyalcohol was made up of dissolving, monomer reconstruct and 3 stages of bunching, bunching reaction when the monomer of reconstruct is similar to organic high molecular polymer formation, and alkali metal ion plays the effect of balance electricity price in final product.Metakaolin is because calcining heat is different with temperature retention time, and quantity and structure that its hydroxyl is sloughed are different, thereby the dissolution velocity difference of metakaolin in aqueous slkali, cause the absorbing state of alkali also inequality.Therefore, alkali absorb method (Guo Wenying, Wu Guolin, Wen Ziyun, etc. the research of activity of metakaolin evaluation method [J]. Wuhan University of Technology's journal, 2006, (03): 76-79.) can distinguish metakaolin and whether have activity.But experimental study shows that the rule of active its active height of metakaolin preferably and the rule of soil polyalcohol 3d intensity are inconsistent.
The calcium absorption method mainly is to generate moisture calcium silicate and moisture calcium aluminate according to active silica in the material and alchlor with the lime effect.Thereby within a certain period of time, the size that how much can represent its activity of amount of lime in the absorbed lime solution.But for the pilot system that excites metakaolin with sodium silicate solution, owing to lacked calcium, this method is not suitable for estimating the activity of metakaolin in this type systematic.
Metakaolin is a kind of silico-aluminate of unbodied non-steady state, it is a kind of material that has free energy, contact hardening theory (Γ JIyXOBC К И Й B Д according to Γ yXOBC К И Й, PyHOBAP Φ, MACyHOBCE. contact hardening Binder Materials and compound substance [M]. Pu Xincheng translates. Chongqing: publishing house of University Of Chongqing, 2004.), metakaolin should have the tendency of polycondensation, thereby the method that can adopt compression makes it produce intensity, and the result of study of Guo Wenying etc. also shows that this method can not describe active size quantitatively.
The intensity contrast method is meant directly and excites metakaolin preparation ground polymeric gel gel material with sodium silicate that the activity that parameters such as its compressive strength or rupture strength are estimated metakaolin is measured in maintenance to certain length of time.This method is to estimate the most effective, the method the most intuitively of activity of metakaolin, but generally needs 3d or 7d just can go out the result, and is consuming time oversize, is not suitable for production.
Aluminium oxide in the calcined kaolin can be divided into two classes: a class has good activity in acid, as γ-Al
2O
3, generally be referred to as activated aluminum; Another kind of active very poor in acid is as α-Al
2O
3, be referred to as inertia aluminium.In fact activated alumina be in the porcelain earth all can and the set of the various shape aluminiums that react of acid, be converted to γ-Al
2O
3Occur.In kaolinic acid-leaching reaction, inertia aluminium is to reaction not contribution basically.
Superfine (the Xu Chao of Xu, Zhang Xingfa, Han Xiaozhao, Xu Mincai. activated alumina is measured [J] in the porcelain earth. nonmetalliferous ore, 1998,21 (5): 13-14) under certain experiment condition, metakaolin is done acidleach earlier and handle, back EDTA volumetric method, analyze to determine what of activated alumina content wherein, come quantitatively the relatively height of activity of metakaolin.Assay method may be summarized to be: metakaolin leaches activated alumina with hydrochloric acid under heating condition.Add excessive EDTA, with the complexing of aluminium plasma, when PH=6, with the EDTA of acetic acid zinc solution overtitration, add sodium fluoride then, make by the aluminium ion of EDTA complexing to become fluorine aluminium complex ion, and disengage the EDTA of equivalent, the EDTA that disengages with the acetic acid zinc solution titration again, calculated activity alumina content.Dye porcelain earth for iron, contain more ferric ion in its pickle liquor.Since aluminium ion and ferric ion can both with the EDTA complexing, if adopt the EDTA complexometric titration pickle liquor of Xu Chao, Zhang Xingfa etc., the activated alumina content of then measuring is higher.
(Xu Xiaobin, Yin Suhong, Yang Jianjun such as Xu Xiaobin, Wen Zi rues. the research of activity of metakaolin method for quickly detecting [J]. and the silicate circular, 2008,27 (4): 690-694.) adopt similarity method, represent the active size of metakaolin with the dissolution rate of aluminium oxide in acid.Experimental result shows that digesting efficiency of alumina in the metakaolin and compression strength value with the geopolymer of its preparation have good corresponding relation, and the metakaolin that digesting efficiency of alumina is high excites the compression strength value of the geopolymer that obtains also high.This method detects a sample and only needs 3h, is a kind of method that can be applied to the quick test activity of metakaolin in the commercial production.But because under the normal temperature condition, aluminium ion and EDTA complexing speed are slow, must add excessive EDTA earlier, heating impels the reaction acceleration." cover heated and boiled 3min behind the bottleneck with surface plate, be cooled to room temperature ".Drip indicator again.Owing to need heated and boiled, could drip indicator after the cooling, make troubles to detection.And this method is with " indicator is terminal point by yellow through the emerald green grass green that sports ", and change color is also not obvious, and titration end-point is difficult to judge, exists more people for thinking error.Therefore, need a kind of method that can the rapid and accurate determination activity of metakaolin of invention.
Summary of the invention
The object of the present invention is to provide a kind of method simple to operation, measure fast, the spectrophotometer that utilizes of reliable results detects the method for activity of metakaolin.
Technical scheme of the present invention is metakaolin to be carried out acidleach handle, and adopts the aluminium content in the spectrophotometry pickle liquor then, is converted into the content of activated alumina again, demarcates activity of metakaolin with this.
The present invention includes following steps:
1) acidleach of metakaolin is handled:
The metakaolin sample is poured in the container, added hydrochloric acid again, in water bath with thermostatic control, heat, behind the stirring reaction,, filtrate is moved in the volumetric flask adding distil water constant volume the cooling of the liquid-solid mixture in the container, filtration, washing;
2) preparation of aluminum standard solution:
Put the spectrum aluminium flake in container, molten with the salt acidleach to the surface oxide layer dissolving, with the decantation acid solution that desalts, after the washing, drying places container with aluminium flake, add chloroazotic acid, after the heating for dissolving, cooling moves in the volumetric flask, use distilled water diluting, pipette in the volumetric flask with liquid-transfering gun, use distilled water diluting, shake up;
3) drafting of aluminium working stamndard curve:
Get 1 μ g/mL aluminum standard solution 1mL respectively, 2mL, 3mL, 4mL, 5mL, 7mL, 9mL, 12mL, 15mL, 18mL, 24mL is in volumetric flask, add ascorbic acid solution, add chromazurine-S ethanolic solution then, add hexamethylene tetramine solution again, last adding distil water constant volume, moving in the absorption vessel again, measure its absorbance in spectrophotometer wavelength 545nm place, is horizontal ordinate with the quality of aluminium, absorbance is an ordinate, draws aluminium working stamndard curve, can get a straight line.Obtain its slope, be aluminium working stamndard slope of a curve;
4) aluminium Determination on content in the pickle liquor:
Pipette metakaolin pickle liquor 1mL with liquid-transfering gun, be diluted to 100mL, get metakaolin pickle liquor 1mL after the dilution in the 50mL volumetric flask, add ascorbic acid, add chromazurine-S ethanol then, add hexamethylene tetraammonia again, last adding distil water constant volume moves in the absorption vessel again, measure its absorbance in spectrophotometer wavelength 545nm place, the each analysis all carried out blank test in company with sample, and blank test and sample are measured and adopted identical reagent and analytical procedure, and carry out operation repetitive, the absorbance that records, be designated as blank absorbency,, utilize aluminium working stamndard slope of a curve to calculate aluminium content m1 in the 50mL sample liquid according to absorbance:
5) calculating of activated alumina content in the metakaolin
The massfraction of activated alumina is calculated as follows:
M wherein
2Be the quality of metakaolin,
In step 1), the addition of described hydrochloric acid can be in every 1g metakaolin sample, adds the hydrochloric acid of 20mL, and the mass percent concentration of described hydrochloric acid can be 15%; The temperature of described heating can be 80 ℃, and the time of described stirring reaction can be 2h.
In step 2) in, described hydrochloric acid can adopt 1: 9 hydrochloric acid, after described washing preferably washes 3 times earlier with water, uses absolute ethanol washing again 3 times; The best in quality of described aluminium flake is 1.0000g, and the amount that adds chloroazotic acid is preferably 10mL.
In step 3), described ascorbic acid solution can be 2.5mL, the ascorbic acid solution that 10g/L now joins, described chromazurine-S ethanolic solution can be 5mL, 0.3g/L chromazurine-S ethanolic solution, described hexamethylene tetramine solution can be 2.5mL, the hexamethylene tetramine solution of 300g/L.
In step 4), described ascorbic acid can be 2.5mL, the ascorbic acid that 10g/L now joins, and described chromazurine-S ethanol can be 5mL, 0.3g/L chromazurine-S ethanol, described hexamethylene tetraammonia can be 2.5mL, the hexamethylene tetraammonia of 300g/L.
The present invention adopts aluminum ions content in chromazurine-S spectrophotometry metakaolin pickle liquor, is converted into the content of activated alumina then.Activated alumina content is many more, illustrates that the activity of metakaolin is high more.This method generates the aubergine complex compound with aluminium and chromazurine-S complexing in the hexamethylene tetramine medium of pH=5.5～6.1.Add ascorbic acid simultaneously and shelter the interference of iron, thereby this method is specially adapted to iron and dyes activated alumina Determination on content in the porcelain earth.And advantage such as this method has sensitivity and precision height, the sample size that needs is few, simple to operate, analysis speed is fast, equipment cost is low.
Description of drawings
Fig. 1 is the aluminium working stamndard curve of the embodiment of the invention.In Fig. 1, horizontal ordinate aluminium content/μ g, ordinate are absorbance.
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
The solution absorbency that adding different volumes 1 μ g/mL aluminum standard solution makes is as shown in table 1.
Table 1
Aluminium working stamndard curve as shown in Figure 1, as shown in Figure 1, the R value of this working stamndard curve reaches 0.99966, the linear fit degree is fine.Its slope is 0.05137.
Embodiment 1
1) adopt ZhangZhou iron to dye porcelain earth as raw material.Al wherein
2O
3Content is 38.24%, Fe
2O
3Content is 0.94%.Essential mineral consists of smalite and a spot of quartz, and mineral structure is sheet and a large amount of tubuloses.
2) ZhangZhou iron being dyed porcelain earth places in the high temperature Energy-saving electric stove and calcines.Porcelain earth is crossed 100 mesh sieves through levigate.Heating rate is 7.5 ℃/min, and calcining heat is respectively 500 ℃, and 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃, calcination time is 2h.After calcining finished, porcelain earth cooled to room temperature with the furnace, took out to obtain the metakaolin sample.
3) take by weighing metakaolin sample about 1g, pour in the 250mL there-necked flask.Pour the hydrochloric acid of 20mL 15% then into, in water bath with thermostatic control, be heated to 80 ℃, stirring reaction 2h.With the cooling of the liquid-solid mixture in the there-necked flask, filtration, washing.Filtrate is moved in the 250mL volumetric flask, and the adding distil water constant volume shakes up.
4) pipette 1mL in the metakaolin pickle liquor with liquid-transfering gun, be diluted to 100mL.Get pickle liquor 1mL after the dilution in the 50mL volumetric flask.Add 2.5mL, the ascorbic acid that 10g/L now joins shakes up.Add 5mL then, 0.3g/L chromazurine-S ethanol shakes up.Add 2.5mL again, the hexamethylene tetraammonia of 300g/L shakes up.Last adding distil water constant volume shakes up.After fully mixing, above-mentioned solution is moved in the 1cm absorption vessel, measure its absorbance in spectrophotometer wavelength 545nm place.Carry out blank test simultaneously.
5) measurement result is as follows: calcining heat is respectively 500 ℃, and 600 ℃, 700 ℃, 800 ℃, 900 ℃, in the metakaolin that 1000 ℃ obtain, activated alumina content is respectively 0.37%, 2.95%, and 17.84%, 15.23%, 15.35%, 0.19%.
6) metakaolin that above-mentioned calcining is obtained adds water glass and makes ground polymeric gel gel material.The incorporation of water glass is converted to Na
2O is 15% of a metakaolin quality; The modulus of water glass is 1.35; Press mass ratio, metakaolin: water glass is 0.94.After adding water glass, stirring is made normal consistency and is starched only, pours in the steel die trial of 20mm * 20mm * 20mm vibration moulding into.With the test block demoulding behind (temperature is (20 ± 5) ℃, humidity 〉=70%) maintenance 24h under field conditions (factors), continue maintenance, survey its compressive strength behind the 3d.The measurement of compressive strength is carried out according to standard GB/T17671-1999.
7) compressive strength that records test block is respectively: 1.18MPa, 8.95MPa, 55.26MPa, 50.47MPa, 51.89MPa, 0.62MPa.With the activated alumina content of measuring good corresponding relation is arranged.
Embodiment 2
Raw material and analytical test process are with embodiment 1.Porcelain earth is crossed 100 mesh sieves.During calcined kaolin, heating rate is 7.5 ℃/min, and calcining heat is 700 ℃, and calcination time is respectively 2h, 4h, 6h, 8h, 10h.The activated alumina content that records is respectively: 17.84%, 18.72%, 19.02%, 19.56%, 19.86%.The compressive strength of the ground polymeric gel gel material of making is respectively 55.26MPa, 57.59MPa, 58.02MPa, 58.96MPa, 59.46MPa.With the activated alumina content of measuring good corresponding relation is arranged.
Embodiment 3
Raw material and analytical test process are with embodiment 1.Porcelain earth is crossed 100 mesh sieves.During calcined kaolin, heating rate is respectively 2.5 ℃/min, and 5 ℃/min, 7.5 ℃/min, 10 ℃/min.Calcining heat is 700 ℃, and calcination time is respectively 2h.The activated alumina content that records is respectively: 16.32%, 17.13%, 17.84%, 18.26%.The compressive strength of the ground polymeric gel gel material of making is respectively 54.78MPa, 54.92MPa, 55.26MPa, 55.56MPa.With the activated alumina content of measuring good corresponding relation is arranged.
Embodiment 4
Raw material and analytical test process are with embodiment 1.Porcelain earth is crossed 60 mesh sieves, 100 mesh sieves, 120 mesh sieves, 140 mesh sieves respectively.During calcined kaolin, heating rate is respectively 7.5 ℃/min.Calcining heat is 700 ℃, and calcination time is respectively 2h.The activated alumina content that records is respectively: 17.45%, 17.84%, 18.12%, 18.34%.The compressive strength of the ground polymeric gel gel material of making is respectively 55.02MPa, 55.26MPa, 55.38MPa, 55.65MPa.With the activated alumina content of measuring good corresponding relation is arranged.
The analytical test process is with embodiment 1.Raw material adopts ZhangZhou iron to dye porcelain earth respectively, and Longyan iron dyes porcelain earth, and Wuping Xiang Dian iron dyes porcelain earth, Longyan finished product porcelain earth.Wherein Longyan iron dyes porcelain earth Al
2O
3Content is 35.41%, Fe
2O
3Content is 0.92%; Wuping Xiang Dian iron dyes porcelain earth Al
2O
3Content is 34.93%, Fe
2O
3Content is 1.08%; Longyan finished product porcelain earth Al
2O
3Content is 36.58%, Fe
2O
3Content is 0.17%.Porcelain earth is crossed 100 mesh sieves.During calcined kaolin, heating rate is respectively 7.5 ℃/min.Calcining heat is 600 ℃, and calcination time is respectively 2h.The activated alumina content that records is respectively: 17.84%, 16.15%, 16.03%, 16.96%.The compressive strength of the ground polymeric gel gel material of making is respectively 55.26MPa, 52.14MPa, 50.98MPa, 53.18MPa.With the activated alumina content of measuring good corresponding relation is arranged.
Claims (9)
1. method of utilizing spectrophotometer to detect activity of metakaolin is characterized in that may further comprise the steps:
1) acidleach of metakaolin is handled:
The metakaolin sample is poured in the container, added hydrochloric acid again, in water bath with thermostatic control, heat, behind the stirring reaction,, filtrate is moved in the volumetric flask adding distil water constant volume the cooling of the liquid-solid mixture in the container, filtration, washing;
2) preparation of aluminum standard solution:
Put specpure aluminium flake in container, molten with the salt acidleach to the surface oxide layer dissolving, with the decantation acid solution that desalts, after the washing, drying places container with aluminium flake, add chloroazotic acid, after the heating for dissolving, cooling moves in the volumetric flask, use distilled water diluting, pipette in the volumetric flask with liquid-transfering gun, use distilled water diluting, shake up;
3) drafting of aluminium working stamndard curve:
Get 1 μ g/mL aluminum standard solution 1mL respectively, 2mL, 3mL, 4mL, 5mL, 7mL, 9mL, 12mL, 15mL, 18mL, 24mL is in volumetric flask, add ascorbic acid solution, the ethanolic solution that adds chromazurine-S then adds hexamethylene tetramine solution again, last adding distil water constant volume, move in the absorption vessel again, measuring its absorbance in spectrophotometer wavelength 545nm place, is horizontal ordinate with the quality of aluminium, and absorbance is an ordinate, draw aluminium working stamndard curve, can get a straight line, go out its slope, be aluminium working stamndard slope of a curve;
4) aluminium Determination on content in the pickle liquor:
Pipette metakaolin pickle liquor 1mL with liquid-transfering gun, be diluted to 100mL, get metakaolin pickle liquor 1mL after the dilution in the 50mL volumetric flask, add ascorbic acid, the ethanolic solution that adds chromazurine-S then, add hexamethylene tetraammonia again, last adding distil water constant volume moves in the absorption vessel again, measure its absorbance in spectrophotometer wavelength 545nm place, the each analysis all carried out blank test in company with sample, and blank test and sample are measured and adopted identical reagent and analytical procedure, and carry out operation repetitive, the absorbance that records, be designated as blank absorbency,, utilize aluminium working stamndard slope of a curve to calculate aluminium content m in the 50mL sample liquid according to absorbance
1:
5) calculating of activated alumina content in the metakaolin
The massfraction of activated alumina is calculated as follows:
M wherein
2Be the quality of metakaolin,
2. a kind of method of utilizing spectrophotometer to detect activity of metakaolin as claimed in claim 1 is characterized in that in step 1) the addition of described hydrochloric acid is in every 1g metakaolin sample, adds the hydrochloric acid of 20mL.
3. a kind of method of utilizing spectrophotometer to detect activity of metakaolin as claimed in claim 1 is characterized in that in step 1) the mass percent concentration of described hydrochloric acid is 15%.
4. a kind of method of utilizing spectrophotometer to detect activity of metakaolin as claimed in claim 1 is characterized in that in step 1) the temperature of described heating is 80 ℃, and the time of described stirring reaction is 2h.
5. a kind of method of utilizing spectrophotometer to detect activity of metakaolin as claimed in claim 1 is characterized in that in step 2) in, described hydrochloric acid adopts 1: 9 hydrochloric acid.
6. a kind of method of utilizing spectrophotometer to detect activity of metakaolin as claimed in claim 1 is characterized in that in step 2) in, described washing is after washing 3 times earlier with water, uses absolute ethanol washing again 3 times.
7. a kind of method of utilizing spectrophotometer to detect activity of metakaolin as claimed in claim 1 is characterized in that in step 2) in, the quality of described aluminium flake is 1.0000g, the amount that adds chloroazotic acid is 10mL.
8. a kind of method of utilizing spectrophotometer to detect activity of metakaolin as claimed in claim 1, it is characterized in that in step 3), described ascorbic acid solution is 2.5mL, the ascorbic acid solution that 10g/L now joins, described chromazurine-S ethanolic solution is 5mL, 0.3g/L chromazurine-S ethanolic solution, described hexamethylene tetramine solution is 2.5mL, the hexamethylene tetramine solution of 300g/L.
9. a kind of method of utilizing spectrophotometer to detect activity of metakaolin as claimed in claim 1, it is characterized in that in step 4), described ascorbic acid is 2.5mL, the ascorbic acid that 10g/L now joins, described chromazurine-S ethanol is 5mL, 0.3g/L chromazurine-S ethanol, described hexamethylene tetraammonia are 2.5mL, the hexamethylene tetraammonia of 300g/L.
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