CN104897511B - A kind of method for measuring desulfurization quick lime active ingredient - Google Patents
A kind of method for measuring desulfurization quick lime active ingredient Download PDFInfo
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- CN104897511B CN104897511B CN201510204519.6A CN201510204519A CN104897511B CN 104897511 B CN104897511 B CN 104897511B CN 201510204519 A CN201510204519 A CN 201510204519A CN 104897511 B CN104897511 B CN 104897511B
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- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium monoxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 title claims abstract description 333
- 239000000292 calcium oxide Substances 0.000 title claims abstract description 175
- 235000012255 calcium oxide Nutrition 0.000 title claims abstract description 113
- 230000003009 desulfurizing Effects 0.000 title claims abstract description 98
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 97
- 239000004480 active ingredient Substances 0.000 title claims abstract description 75
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 30
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 26
- 238000000921 elemental analysis Methods 0.000 claims abstract description 7
- 230000004580 weight loss Effects 0.000 claims description 37
- 239000000203 mixture Substances 0.000 claims description 24
- 238000000354 decomposition reaction Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 4
- 235000015450 Tilia cordata Nutrition 0.000 claims description 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 4
- 239000004571 lime Substances 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 17
- 241000894007 species Species 0.000 abstract description 4
- 238000001228 spectrum Methods 0.000 abstract description 3
- 238000004876 x-ray fluorescence Methods 0.000 abstract description 3
- 239000011575 calcium Substances 0.000 description 40
- 229910052791 calcium Inorganic materials 0.000 description 26
- 239000000047 product Substances 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 10
- 150000001674 calcium compounds Chemical class 0.000 description 9
- 239000004615 ingredient Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000000875 corresponding Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 239000003546 flue gas Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000920 calcium hydroxide Substances 0.000 description 5
- 238000004448 titration Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 239000004575 stone Substances 0.000 description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L Calcium hydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 101700023688 LIME1 Proteins 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N acetic acid ethyl ester Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229940077747 antacids containing calcium compounds Drugs 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229940043430 calcium compounds Drugs 0.000 description 3
- 235000011116 calcium hydroxide Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N 2-Butanol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- DSLZVSRJTYRBFB-LLEIAEIESA-L D-glucarate(2-) Chemical compound [O-]C(=O)[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O DSLZVSRJTYRBFB-LLEIAEIESA-L 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N D-sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- KJFMBFZCATUALV-UHFFFAOYSA-N Phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 1
- 229960005382 Phenolphthalein Drugs 0.000 description 1
- CZMRCDWAGMRECN-GDQSFJPYSA-N Sucrose Natural products O([C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O1)[C@@]1(CO)[C@H](O)[C@@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-GDQSFJPYSA-N 0.000 description 1
- 238000010928 TGA analysis Methods 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 238000003556 assay method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 238000005039 chemical industry Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
Abstract
The present invention provides a kind of method for measuring desulfurization quick lime active ingredient, the method is：Analysis determines the species and its content of decomposable active ingredient in desulfurization quick lime sample, then carries out elemental analysis to undecomposed sample, determines the content of contained active ingredient in undecomposed sample, so that it is determined that in desulfurization quick lime sample active ingredient content.The present invention measures the content of active ingredient in desulfurization quick lime using the infrared combination of thermogravimetric and with reference to X-ray fluorescence spectra, and this method drastically reduces the error that manual operation is brought, and can effectively distinguish desulfurization quick lime sample CaO, Ca (OH)2And CaCO3Content, as a result accurately and reliably.
Description
Technical field
The invention belongs to flue gas desulfurization fields, are related to a kind of method for measuring desulfurization quick lime active ingredient.
Background technology
Quick lime is mainly used for the industries such as coal-burning power plant, coal-burning boiler, Industrial Stoves as a kind of important desulfurizing agent
Flue gas desulfurization technique, the content of active ingredient directly determine the effect of flue gas desulfurization.The main component of quick lime is calcium oxide
(CaO), due to the physicochemical characteristics of CaO uniquenesses, the easily H in deliquescence, with air occur for air2O and CO2It reacts
Generate Ca (OH)2、CaCO3Substances are waited, quick lime activity is caused to reduce.Requirement of the different sulfur removal technologies to active ingredient is different,
As there was only CaO and Ca (OH) in dry flue gas desulphurization technique2It can be as the active ingredient of desulfurization quick lime.But in wet flue gas
CaCO in sulfur removal technology3It can also be used as the active ingredient of desulfurization quick lime.Therefore, to the definite right and wrong of desulfurization quick lime ingredient
It is often necessary.
At present, have much on the test method to quick lime ingredient, wherein national standard HG/T 4205-2011 regulations
CaO content is come definite by chemical titration, and principle is the CaO lime saccharate larger with sucrose generation solubility, with phenol
Phthalein is indicator solution, is titrated to Hydrochloric Standard Titration colourless for terminal.But this method has the following disadvantages：(1) titrating
Rapid during with addition quick lime, quick lime on the contrary may occur deliquescence and bring error to measurement result；(2) in operating process
Human factor influence is more, and error is larger；(3) test result cannot effectively distinguish CaO, Ca (OH)2、CaCO3Deng content.
CN101201325A discloses a kind of assay method of dissociation calcium oxide content in calces, and this method utilizes acetyl
For the mixed liquor of ethyl acetate and 2- butanol under conditions of boiling reflux condensation, selectivity extracts the calcium oxide to dissociate in quick lime
It takes out, by filtering CaCO in quick lime3It can be consumed Deng other insoluble in solid and quick lime of hydrochloric acid standard solution
Property residue separation, then carries out titrimetry to the calcium oxide in filtrate with hydrochloric acid, calcium oxide free in quick lime is calculated
Content.This method can only determine dissociation calcium oxide content in calces, have no idea to survey for the content of other calcium compounds
It is fixed.
CN 103776990A disclose a kind of test method of quick lime effective content, and this method is needed by surface
The effective content that aptitude test goes out quick lime is measured to the calcium ion in liquid again after the operations such as reason, cutting, dissolving.The survey
Method for testing shortcoming is that time-consuming, energy consumption is big, human error is big and measurement result can only illustrate the content of calcium in sample, without
CaO, Ca (OH) can effectively be distinguished2、CaCO3Deng content.
CN 104090066A disclose a kind of device and method for measuring CaO content in quick lime, and continuous mode is such as
Under：Check device after sample and container are weighed, then a certain amount of raw material life stone is put into reaction container, then add in suitable water
Digestion forms milk of lime and lime-ash, then is separated milk of lime and lime-ash with water, finally passes through formula with titration with hydrochloric acid milk of lime again
(1) content of CaO is calculated：This method shortcoming exists
In process complexity, in operating process human error is brought to cause measurement result inaccurate.
Therefore, existing quick lime test method is tight there are process complexity, mostly using chemical analysis, artifical influence factor
Weight, test result error are big, distinguish the problems such as difficult to active ingredient, and there is an urgent need for exploitation one kind can effectively measure desulfurization quick lime
The method of middle active ingredient species and content.
The content of the invention
In view of the deficiencies of the prior art, it is an object of the invention to provide a kind of sides for measuring desulfurization quick lime active ingredient
Method, this method can effectively distinguish CaO, Ca (OH) in desulfurization quick lime sample2And CaCO3Content.
To reach the invention purpose, the present invention uses following technical scheme：
The present invention provides a kind of method for measuring desulfurization quick lime active ingredient, and the method is：
Analysis determines the species and its content of decomposable active ingredient in desulfurization quick lime sample, then to undecomposed
Sample carries out elemental analysis, the content of contained active ingredient in undecomposed sample is determined, so that it is determined that in desulfurization quick lime sample
The content of active ingredient.
CaO、Ca(OH)2And CaCO3Can be as the active ingredient of desulfurization quick lime, it can be accurate using the method for the present invention
The content of each ingredient really is measured, wherein decomposable active ingredient refers to Ca (OH) in desulfurization quick lime sample2And/or
CaCO3, and contained active ingredient is CaO in undecomposed sample.
In the method for measure desulfurization quick lime active ingredient of the present invention, the analysis determines desulfurization quick lime sample
In decomposable active ingredient species and its content realized using ftir Analysis combined instrument；It is described to undecomposed
Sample is carried out elemental analysis and is realized using Xray fluorescence spectrometer.
Thermogravimetric analysis can be used for thermal stability, decomposable process, adsorption and desorption, oxidation and the reduction of research material, moisture
With determination of volatile matter, make quantitative analysis and Reaction kinetics research of material composition etc..The infrared composition for being mainly used for material and
Structural analysis, the two combination can analyze the product in thermal decomposition process.Thermogravimetric analyzer and infrared spectrometer are combined
It is one of current most common emergent gas analysis means.By thermogravimetric heat sample, sample can because volatile matter presence or
Combustion decomposition goes out gas, these gases are transferred in infrared collecting pit, are identified.The analysis of infrared spectrum can detect work(
Energy group, can preferably analyze thermogravimetric result, may thereby determine that the content of ingredient in sample.
Industrial oxidation calcium described in HG/T 4205-2011 chemical industry standards, including I class (CaO >=92%), II class
(CaO >=82%), III class (CaO >=90%) and IV class (CaO >=85%), wherein the industrial calcium oxide of regulation flue gas desulfurization
CaO content must be IV class industrial oxidation calcium, the content of the calcium oxide is to use chemical titration in this regulation more than 85%
It measures, cannot effectively distinguish CaO, Ca in sample (OH)2、CaCO3Wait the content of calcium compounds.
The method of the present invention for measuring desulfurization quick lime active ingredient can be measured effectively each in desulfurization quick lime
Active ingredient and its content, the described method comprises the following steps：
(1) desulfurization quick lime sample is put into thermogravimetric analyzer and carries out thermal weight loss measure, and infrared spectrum associated with passing through
Instrument analyzes decomposition product, determines the active ingredient and its content decomposed in sample；
(2) elemental analysis is carried out to undecomposed sample using Xray fluorescence spectrometer, determine it is contained therein it is effective into
Divide the percentage composition for accounting for undecomposed sample, the percentage composition of active ingredient in undecomposed sample is converted into and accounts for former desulfurization life stone
The percentage composition of grey sample then subtracts the undecomposable product that active ingredient decomposition generates in decomposable asymmetric choice net sample and accounts for former desulfurization life
The percentage composition of lime sample, and then obtain the content of undecomposed active ingredient in former desulfurization quick lime sample.
It is of the present invention measure desulfurization quick lime active ingredient method in, be additionally included in carry out thermal weight loss measure before it is right
Processing is dried in desulfurization quick lime sample, and the purpose of the drying process is mainly the moisture for removing and being carried in sample, described
Methods known in the art progress may be employed in drying process, as long as this method will not cause the decomposition of active ingredient,
Such as dry, be dried in vacuo or be freeze-dried in an oven etc..
In the method for measure desulfurization quick lime active ingredient of the present invention, step (1) is described to be put into thermogravimetric analyzer
In desulfurization quick lime sample quality for 50-500mg, such as 50mg, 80mg, 100mg, 120mg, 150mg, 180mg,
200mg、230mg、250mg、280mg、300mg、320mg、340mg、360mg、380mg、400mg、430mg、450mg、480mg
Or 500mg.
In the method for measure desulfurization quick lime active ingredient of the present invention, step (1) the thermal weight loss continuous mode
Middle heating rate be 5-15 DEG C/min, such as 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min, 10 DEG C/min,
11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min or 15 DEG C/min, from room temperature to 900-1100 DEG C, such as from room
Temperature be warming up to 900 DEG C, 920 DEG C, 940 DEG C, 950 DEG C, 960 DEG C, 980 DEG C, 1000 DEG C, 1020 DEG C, 1040 DEG C, 1060 DEG C, 1080
DEG C or 1100 DEG C.
In the method for measure desulfurization quick lime active ingredient of the present invention, decompose described in step (1) effective
Ingredient is Ca (OH)2And/or CaCO3。
In the method for measure desulfurization quick lime active ingredient of the present invention, in the decomposable asymmetric choice net sample described in step (2)
It is CaO that active ingredient, which decomposes the undecomposable product generated,.
In the method for measure desulfurization quick lime active ingredient of the present invention, in step (2) the undecomposed sample
Active ingredient for CaO, it includes active ingredients in the CaO and decomposable asymmetric choice net sample contained in former desulfurization quick lime sample to decompose
The CaO of generation.
It is of the present invention measure desulfurization quick lime active ingredient method, using ftir Analysis combination come determination sample
In the ingredient and content of sample that can decompose, carry out thermal weight loss by the way that sample is put into thermogravimetric analyzer, by it is infrared can
The ingredient of the product generated is decomposed to detect as H2O and CO2, and it can be seen that the first and second two from thermogravimetric curve
Zero-g period, according to the temperature of the two zero-g periods and infrared detection to product component may determine that first stage weightlessness
It is due to Ca (OH)2Decompose and caused by, second stage weightlessness is due to CaCO3Decompose and caused by, that is, the sample decomposed
In active ingredient be Ca (OH)2And CaCO3, can be according to two zero-g period product H2O and CO2Corresponding percent weight lossWithCa (OH) in desulfurization quick lime sample is drawn according to the following formula (1) and (2)2And CaCO3Percentage compositionWithAnd can also Ca (OH) be drawn according to formula (3) and (4)2And CaCO3It decomposes the CaO generated and accounts for original
The percentage composition y of desulfurization quick limeCaOAnd zCaO.Since CaO is more stable, in the temperature range (900-1100 of thermogravimetic analysis (TGA)
DEG C) in will not decompose, constituent content analysis is carried out by X-ray fluorescence spectra, it can be deduced that main in undecomposed sample
Ingredient CaO is wanted (comprising Ca (OH) in the CaO and decomposable asymmetric choice net sample contained in former desulfurization quick lime sample2And CaCO3Decompose production
Raw CaO) account for the percentage composition x of undecomposed sampleCaO, since undecomposed sample accounts for the percentage of former desulfurization quick lime sample
For xU Therefore x is usedCaOIt is multiplied by xUJust obtain main component CaO in undecomposed sample and account for original
The percentage composition of desulfurization quick lime sample, then subtract yCaOAnd zCaO, i.e., former desulfurization quick lime sample can be obtained by according to formula (5)
The percentage composition X of the CaO contained in productCaO, calculation formula is as follows：
Wherein M represents the molecular weight of each substance.
As optimal technical scheme, the method for the measure desulfurization quick lime active ingredient of the invention, specifically include with
Lower step：
(1) the desulfurization quick lime sample 50-500mg after drying process is put into thermogravimetric analyzer and carries out thermal weight loss measure,
Heating rate is 5-15 DEG C/min in thermal weight loss continuous mode, from room temperature to 900-1100 DEG C, and it is infrared associated with passing through
Spectrometer analyzes decomposition product, determines the ingredient decomposed in sample and its content；
(2) elemental analysis is carried out to undecomposed sample using Xray fluorescence spectrometer, determine it is contained therein it is effective into
Divide the percentage composition for accounting for undecomposed sample, the percentage composition of active ingredient in undecomposed sample is converted into and accounts for former desulfurization life stone
The percentage composition of grey sample then subtracts the undecomposable product that active ingredient decomposition generates in decomposable asymmetric choice net sample and accounts for former desulfurization life
The percentage composition of lime sample, and then obtain the content of undecomposed active ingredient in former desulfurization quick lime sample.
Compared with the prior art, the invention has the advantages that：
The present invention is combined using ftir Analysis and measures active ingredient in desulfurization quick lime with reference to X-ray fluorescence spectra
Content, this method drastically reduces the error that manual operation is brought, can effectively distinguish CaO in desulfurization quick lime sample,
Ca(OH)2And CaCO3Content, as a result accurately and reliably.
Description of the drawings
Fig. 1 is the method flow diagram for measuring desulfurization quick lime active ingredient；
Fig. 2 is that the infrared graph that desulfurization quick lime decomposes active ingredient in sample is measured in the embodiment of the present invention 1；
Fig. 3 is that the thermogravimetric curve figure that desulfurization quick lime decomposes active ingredient in sample is measured in the embodiment of the present invention 1.
Specific embodiment
The technical solution further illustrated the present invention below by specific embodiment.Those skilled in the art should be bright
, the embodiment be only to aid in understand the present invention, be not construed as to the present invention concrete restriction.
Embodiment 1
In the present embodiment, the method for measuring desulfurization quick lime active ingredient by the following method specifically includes following
Step (method flow is as shown in Figure 1)：
(1) the desulfurization quick lime sample 100mg after drying process is put into thermogravimetric analyzer and carries out thermal weight loss measure, heat is lost
Resurvey it is fixed during heating rate be 10 DEG C/min, from room temperature to 1100 DEG C, and infrared spectrometer associated with passing through to point
Solution product is analyzed.As shown in Fig. 2, desulfurization quick lime, which is decomposed in the infrared curve of sample, has only detected H2O and CO2, it is corresponding
Thermal weight loss temperature in thermogravimetric curve as shown in Figure 3 is 267-607 DEG C and 667-875 DEG C of section, analyzes and understands, the
The product that one zero-g period decomposes is H2O, percent weight loss are 4.567% (xH2O), according to decomposition temperature and detect product
It understands, first stage weightlessness is Ca (OH)2Caused by decomposition；The product that second zero-g period decomposes is CO2, percent weight loss
For 4.485% (xCO2), according to decomposition temperature and according to detecting product, second stage weightlessness is CaCO3Caused by decomposition, change
It is as follows to learn reaction equation：
Ca in sample (OH) can be calculated according to the following formula (1) and (2)2And CaCO3Content, i.e.,For
18.78%,For 10.19%, Ca (OH) can be drawn according to formula (3) and (4)2The CaO of generation accounts for former desulfurization life stone
The percentage composition y of grey sampleCaOFor 14.21%, CaCO3The CaO of generation accounts for the percentage composition z of former desulfurization quick lime sampleCaOFor
5.71%；
(2) by undecomposed sample, (sample i.e. after thermal weight loss calcining, accounts for the 90.948% of former desulfurization quick lime sample
(xU)) elemental analysis is carried out to undecomposed sample using Xray fluorescence spectrometer after tabletting, test result shows undecomposed de-
Sulphur quick lime sample contains the elements such as Ca, Mg, Si, O, their mass percent is respectively 67.32%, 1.34%, 0.91%,
29.46%.Ca and O calcium compound (in terms of CaO) contents after oxide conversion account for 94.19% (x of undecomposed sampleCaO)。
The percentage composition X of CaO in former desulfurization quick lime sample is obtained according to formula (5)CaOFor 65.74%；
The calculation formula is as follows：
XCaO=xCaO×xU-yCaO-zCaO (5)
Wherein M represents the molecular weight of each substance.
Therefore, in summary draw, the active ingredient and content surveyed in desulfurization quick lime sample are：CaO is
65.74%, Ca (OH)2For 18.78%, CaCO3For 10.19%.
Embodiment 2
As different from Example 1, desulfurization quick lime amount of samples is put into thermogravimetric analyzer progress to the present embodiment for 50mg
Thermal weight loss measures, and heating rate is 5 DEG C/min in thermal weight loss continuous mode, from room temperature to 900 DEG C, through with 1 phase of embodiment
Same method measures the active ingredient and content of desulfurization quick lime sample, and similary desulfurization quick lime is decomposed in the infrared curve of sample
H is only detected2O and CO2, the first and second zero-g periods corresponding temperature range in thermogravimetric curve is respectively 302-634
DEG C and 673-882 DEG C, first zero-g period percent weight loss is 4.893%, and the second zero-g period percent weight loss is
4.673%；Xray fluorescence spectrometer is measured in undecomposed sample containing the elements such as Ca, Mg, Si, O, their mass percent
Respectively 70.41%, 1.86%, 1.02%, 30.63%, Ca and O calcium compound after oxide conversion contain (in terms of CaO)
Amount accounts for the 95.4% of undecomposed sample.In summary measurement result analysis draws the content of active ingredient in desulfurization quick lime sample
For：CaO is 65.10%, Ca (OH)2For 20.11%, CaCO3For 10.62%.
Embodiment 3
As different from Example 1, desulfurization quick lime amount of samples is put into thermogravimetric analyzer progress to the present embodiment for 50mg
Thermal weight loss measures, and heating rate is 10 DEG C/min in thermal weight loss continuous mode, from room temperature to 980 DEG C, through with 1 phase of embodiment
Same method draws the content of active ingredient in desulfurization quick lime sample after measuring, similary desulfurization quick lime decomposes the infrared of sample
H has been only detected in curve2O and CO2, the first and second zero-g periods corresponding temperature range in thermogravimetric curve is respectively
268-613 DEG C and 672-882 DEG C, first zero-g period percent weight loss is 4.582%, second zero-g period weightlessness percentage
Than for 4.621%；Xray fluorescence spectrometer is measured in undecomposed sample containing the elements such as Ca, Mg, Si, O, their quality hundred
Divide than being respectively 65.2%, 2.35%, 0.62%, 30.5%.Ca and O calcium compounds after oxide conversion (in terms of CaO)
Content accounts for the 93.6% of undecomposed sample.In summary measurement result analysis draws containing for active ingredient in desulfurization quick lime sample
It measures and is：CaO is 64.85%, Ca (OH)2For 18.84%, CaCO3For 10.50%.
Embodiment 4
As different from Example 1, desulfurization quick lime amount of samples is put into thermogravimetric analyzer progress to the present embodiment for 200mg
Thermal weight loss measures, and heating rate is 15 DEG C/min in thermal weight loss continuous mode, from room temperature to 1100 DEG C, through with embodiment 1
Identical method measures the active ingredient and content of desulfurization quick lime sample, and similary desulfurization quick lime decomposes the infrared curve of sample
In only detected H2O and CO2, the first and second zero-g periods corresponding temperature range in thermogravimetric curve is respectively 246-
598 DEG C and 654-863 DEG C, first zero-g period percent weight loss is 4.325%, and second zero-g period percent weight loss is
4.652%；Xray fluorescence spectrometer is measured in undecomposed sample containing the elements such as Ca, Mg, Si, O, their mass percent
Respectively 63.5%, 1.5%, 1.2%, 28.7%.Ca and O calcium compound (in terms of CaO) contents after oxide conversion account for
The 92.3% of undecomposed sample.In summary measurement result analysis show that the content of active ingredient in desulfurization quick lime sample is：
CaO is 64.64%, Ca (OH)2For 17.78%, CaCO3For 10.57%.
Embodiment 5
As different from Example 1, desulfurization quick lime amount of samples is put into thermogravimetric analyzer progress to the present embodiment for 500mg
Thermal weight loss measures, and heating rate is 5 DEG C/min in thermal weight loss continuous mode, from room temperature to 1100 DEG C, through with 1 phase of embodiment
Same method measures the active ingredient and content of desulfurization quick lime sample, and similary desulfurization quick lime is decomposed in the infrared curve of sample
H is only detected2O and CO2, the first and second zero-g periods corresponding temperature range in thermogravimetric curve is respectively 246-587
DEG C and 654-864 DEG C, first zero-g period percent weight loss is 4.376%, and second zero-g period percent weight loss is
4.281%；Xray fluorescence spectrometer is measured in undecomposed sample containing the elements such as Ca, Mg, Si, O, their mass percent
Respectively 69.3%, 1.6%, 1.2%, 30.1%.Ca and O calcium compound (in terms of CaO) contents after oxide conversion account for
The 96.3% of undecomposed sample.In summary measurement result analysis show that the content of active ingredient in desulfurization quick lime sample is：
CaO is 68.91%, Ca (OH)2For 17.99%, CaCO3For 9.73%.
Embodiment 6
As different from Example 1, desulfurization quick lime amount of samples is put into thermogravimetric analyzer progress to the present embodiment for 150mg
Thermal weight loss measures, and heating rate is 8 DEG C/min in thermal weight loss continuous mode, from room temperature to 1100 DEG C, through with 1 phase of embodiment
Same method measures the active ingredient and content of desulfurization quick lime sample, and similary desulfurization quick lime is decomposed in the infrared curve of sample
H is only detected2O and CO2, the first and second zero-g periods corresponding temperature range in thermogravimetric curve is respectively 254-618
DEG C and 671-882 DEG C, first zero-g period percent weight loss is 4.532%, and second zero-g period percent weight loss is
4.982%；Xray fluorescence spectrometer is measured in undecomposed sample containing the elements such as Ca, Mg, Si, O, their mass percent
Respectively 68.2%, 2.8%, 1.5%, 30.1%.Ca and O calcium compound (in terms of CaO) contents after oxide conversion account for
The 95.1% of undecomposed sample.In summary measurement result analysis show that the content of active ingredient in desulfurization quick lime sample is：
CaO is 65.62%, Ca (OH)2For 18.63%, CaCO3For 11.32%.
Embodiment 7
As different from Example 1, desulfurization quick lime amount of samples is put into thermogravimetric analyzer progress to the present embodiment for 300mg
Thermal weight loss measures, and heating rate is 12 DEG C/min in thermal weight loss continuous mode, from room temperature to 1000 DEG C, through with embodiment 1
Identical method measures the active ingredient and content of desulfurization quick lime sample, and similary desulfurization quick lime decomposes the infrared curve of sample
In only detected H2O and CO2, the first and second zero-g periods corresponding temperature range in thermogravimetric curve is respectively 272-
635 DEG C and 675-891 DEG C, first zero-g period percent weight loss is 4.124%, and second zero-g period percent weight loss is
4.981%；Xray fluorescence spectrometer is measured in undecomposed sample containing the elements such as Ca, Mg, Si, O, their mass percent
Respectively 65.1%, 0.8%, 1.5%, 28.1%.Ca and O calcium compound (in terms of CaO) contents after oxide conversion account for
The 92.4% of undecomposed sample.In summary measurement result analysis show that the content of active ingredient in desulfurization quick lime sample is：
CaO is 64.82%, Ca (OH)2For 16.95%, CaCO3For 11.32%.
Applicant states that the present invention illustrates the measure desulfurization quick lime active ingredient of the present invention by above-described embodiment
Method, but the invention is not limited in above-mentioned processing step, that is, do not mean that the present invention has to rely on above-mentioned processing step ability
Implement.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention, to raw material selected by the present invention etc.
Effect replacement and the addition of auxiliary element, the selection of concrete mode etc., all fall within protection scope of the present invention and the open scope.
Claims (7)
- A kind of 1. method for measuring desulfurization quick lime active ingredient, which is characterized in that the described method comprises the following steps：(1) desulfurization quick lime sample is put into thermogravimetric analyzer and carries out thermal weight loss measure, and infrared spectrometer pair associated with passing through Decomposition product is analyzed, and determines the active ingredient and its content decomposed in sample；(2) elemental analysis is carried out to undecomposed sample using Xray fluorescence spectrometer, determines that active ingredient contained therein accounts for The percentage composition of active ingredient in undecomposed sample is converted into and accounts for former desulfurization quick lime sample by the percentage composition of undecomposed sample The percentage composition of product then subtracts the undecomposable product that active ingredient decomposition generates in decomposable asymmetric choice net sample and accounts for former desulfurization quick lime The percentage composition of sample, and then obtain the content of undecomposed active ingredient in former desulfurization quick lime sample.
- 2. according to the method described in claim 1, it is characterized in that, the method is additionally included in before progress thermal weight loss measures to de- Processing is dried in sulphur quick lime sample.
- 3. according to the method described in claim 1, it is characterized in that, step (1) the desulfurization life being put into thermogravimetric analyzer The quality of lime sample is 50-500mg.
- 4. according to the method described in claim 1, it is characterized in that, heating rate in step (1) the thermal weight loss continuous mode For 5-15 DEG C/min, from room temperature to 900-1100 DEG C.
- 5. according to the method described in claim 1, it is characterized in that, step (1) active ingredient decomposed is Ca (OH)2And/or CaCO3。
- 6. according to the method described in claim 1, it is characterized in that, active ingredient point in decomposable asymmetric choice net sample described in step (2) The undecomposable product that solution generates is CaO.
- 7. according to the method described in claim 1, it is characterized in that, active ingredient in step (2) the undecomposed sample For CaO, the CaO generated is decomposed it includes active ingredient in the CaO and decomposable asymmetric choice net sample contained in former desulfurization quick lime sample.
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| CN201510204519.6A CN104897511B (en) | 2015-04-27 | A kind of method for measuring desulfurization quick lime active ingredient |
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| CN201510204519.6A CN104897511B (en) | 2015-04-27 | A kind of method for measuring desulfurization quick lime active ingredient |
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