CN104897511A - Desulfurized quicklime effective ingredient determination method - Google Patents

Desulfurized quicklime effective ingredient determination method Download PDF

Info

Publication number
CN104897511A
CN104897511A CN201510204519.6A CN201510204519A CN104897511A CN 104897511 A CN104897511 A CN 104897511A CN 201510204519 A CN201510204519 A CN 201510204519A CN 104897511 A CN104897511 A CN 104897511A
Authority
CN
China
Prior art keywords
sample
desulfurization
unslaked lime
effective constituent
content
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.)
Granted
Application number
CN201510204519.6A
Other languages
Chinese (zh)
Other versions
CN104897511B (en
Inventor
朱廷钰
郭旸旸
高翔
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Process Engineering of CAS
Original Assignee
Institute of Process Engineering of CAS
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Institute of Process Engineering of CAS filed Critical Institute of Process Engineering of CAS
Priority to CN201510204519.6A priority Critical patent/CN104897511B/en
Priority claimed from CN201510204519.6A external-priority patent/CN104897511B/en
Publication of CN104897511A publication Critical patent/CN104897511A/en
Application granted granted Critical
Publication of CN104897511B publication Critical patent/CN104897511B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention provides a desulfurized quicklime effective ingredient determination method, and the method is as follows: analysis and determination of kind and content of decomposable effective ingredients in a desulfurized quicklime sample, and element analysis of the undecomposed sample to determine the content of effective ingredients in the undecomposed sample so as to determine the content of effective ingredients in the desulfurized quicklime sample. By use of thermo-gravimetric and infrared spectroscopy coupled technology combining X-ray fluorescence spectrum, the content of the effective ingredients in the desulfurized quicklime can be determined, the method greatly reduces the artificial operation error, and can effectively distinguish the content of CaO, Ca (OH) 2 and CaCO3 in the desulfurized quicklime sample, and the results are accurate and reliable.

Description

A kind of method measuring desulfurization unslaked lime effective constituent
Technical field
The invention belongs to flue gas desulfurization field, relate to a kind of method measuring desulfurization unslaked lime effective constituent.
Background technology
Unslaked lime is as a kind of important desulfurizing agent, and be mainly used in the flue gas desulfurization technique of the industries such as coal-burning power plant, coal-burning boiler, Industrial Stoves, the content of its effective constituent directly determines the effect of flue gas desulfurization.The principal ingredient of unslaked lime is calcium oxide (CaO), and due to the physicochemical characteristics of CaO uniqueness, it is easily at air generation deliquescence, with the H in air 2o and CO 2react and generate Ca (OH) 2, CaCO 3deng material, unslaked lime activity is caused to reduce.Different sulfur removal technologies is different to the requirement of effective constituent, as only having CaO and Ca (OH) in dry process stack gas desulfur technology 2can as the effective constituent of desulfurization unslaked lime.But CaCO in wet fuel gas desulfurizing technology 3also can as the effective constituent of desulfurization unslaked lime.Therefore, the determination of desulfurization unslaked lime composition is very important.
At present, have a lot about to the method for testing of unslaked lime composition, wherein national standard HG/T 4205-2011 regulation CaO content is determined by chemical titration, its principle is that CaO and sucrose generate the larger lime saccharate of solubleness, take phenolphthalein as indicator solution, being titrated to colourless with Hydrochloric Standard Titration is terminal.But the method has the following disadvantages: (1) wants rapidly in titration with when adding unslaked lime, otherwise may to there is deliquescence in unslaked lime bring error to measurement result; (2) in operating process, human factor impact is more, and error is larger; (3) test result effectively can not distinguish CaO, Ca (OH) 2, CaCO 3deng content.
CN101201325A discloses a kind of assay method of dissociation calcium oxide content in calces, the method utilizes the mixed liquor of ethyl acetoacetate and 2-butanols under the condition of boiling reflux condensation, the calcium oxide dissociated in unslaked lime extracts by selectivity, is passing through to filter CaCO in unslaked lime 3insoluble sludge in the solid of hydrochloric acid standard solution and unslaked lime can be consumed be separated Deng other, then with hydrochloric acid, titrimetry be carried out to the calcium oxide in filtrate, calculate calcium oxide content free in unslaked lime.The method can only determine dissociation calcium oxide content in calces, and the content for other calcium compounds has no idea to measure.
CN 103776990A discloses a kind of method of testing of unslaked lime effective content, and the method needs to carry out measuring the effective content that aptitude test goes out unslaked lime to the calcium ion in liquid again after the operations such as surface treatment, cutting, dissolving.This method of testing shortcoming is that length consuming time, energy consumption are large, personal error is large and measurement result can only the content of calcium in interpret sample, and effectively can not distinguish CaO, Ca (OH) 2, CaCO 3deng content.
CN 104090066A discloses a kind of device and method measuring CaO content in unslaked lime, it is as follows that it measures process: testing fixture after sample and container being weighed, again raw for a certain amount of raw material stone is put into reaction container, then add appropriate water digestion and form milk of lime and lime-ash, with water, milk of lime and lime-ash are separated again, finally use HCI milk of lime again, calculated the content of CaO by formula (1): the method shortcoming is that process is complicated, bring personal error to cause measurement result inaccurate in operating process.
Therefore, there is process complexity, adopt chemical analysis more in existing unslaked lime method of testing, artifical influence factor is serious, test result error is large, distinguish the problems such as difficulty to effective constituent, needs a kind of method that effectively can measure effective constituent kind and content in desulfurization unslaked lime of exploitation badly.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of method measuring desulfurization unslaked lime effective constituent, the method effectively can distinguish CaO, Ca (OH) in desulfurization unslaked lime sample 2and CaCO 3content.
For reaching this goal of the invention, the present invention by the following technical solutions:
The invention provides a kind of method measuring desulfurization unslaked lime effective constituent, described method is:
Analyze kind and the content thereof of determining decomposable effective constituent in desulfurization unslaked lime sample, then ultimate analysis is carried out to undecomposed sample, determine the content of contained effective constituent in undecomposed sample, thus determine the content of effective constituent in desulfurization unslaked lime sample.
CaO, Ca (OH) 2and CaCO 3all can be used as the effective constituent of desulfurization unslaked lime, apply the content that method of the present invention can measure each composition exactly, wherein in desulfurization unslaked lime sample, decomposable effective constituent refers to Ca (OH) 2and/or CaCO 3, and in undecomposed sample, contained effective constituent is CaO.
In the method for mensuration desulfurization unslaked lime effective constituent of the present invention, described analysis determines that the kind of decomposable effective constituent in desulfurization unslaked lime sample and content thereof utilize ftir Analysis combined instrument to realize; Describedly ultimate analysis is carried out to undecomposed sample utilize Xray fluorescence spectrometer to realize.
Thermogravimetric analysis can be used for the thermal stability of research material, decomposable process, adsorption and desorption, oxidation and induction, moisture and determination of volatile matter, does the quantitative test and reaction kinetics research etc. of material composition.The infrared the Nomenclature Composition and Structure of Complexes analysis being mainly used in material, the two coupling can be analyzed the product in thermal decomposition process.By one of emergent gas analysis means that thermogravimetric analyzer and infrared spectrometer coupling are the most frequently used at present.By thermogravimetric heated sample, sample can go out gas because of the existence of volatile matter or combustion decomposition, and these gases are transferred in infrared collecting pit, are identified.The analysis of infrared spectrum can measuring ability group, can analyze better, thus can determine the content of composition in sample to thermogravimetric result.
Industrial oxidation calcium described in HG/T 4205-2011 chemical industry standard, comprise I class (CaO>=92%), II class (CaO>=82%), III class (CaO>=90%) and IV class (CaO>=85%), wherein specify that flue gas desulfurization must more than 85% with the CaO content of industrial calcium oxide, be IV class industrial oxidation calcium, the content chemical titration of this calcium oxide in this regulation, it effectively can not distinguish CaO, Ca in sample (OH) 2, CaCO 3deng the content of calcium compound.
The method of mensuration desulfurization unslaked lime effective constituent of the present invention, effectively can measure each effective constituent and content thereof in desulfurization unslaked lime, said method comprising the steps of:
(1) desulfurization unslaked lime sample is put into thermogravimetric analyzer and carry out thermal weight loss mensuration, and by the infrared spectrometer of coupling, decomposition product is analyzed, determine effective constituent and content thereof that decomposition occurs in sample;
(2) Xray fluorescence spectrometer is utilized to carry out ultimate analysis to undecomposed sample, determine that wherein contained effective constituent accounts for the percentage composition of undecomposed sample, the percentage composition of effective constituent in undecomposed sample is converted into the percentage composition accounting for former desulfurization unslaked lime sample, then deduct effective constituent in decomposable asymmetric choice net sample and decompose the percentage composition that the undecomposable product produced accounts for former desulfurization unslaked lime sample, and then obtain the content of undecomposed effective constituent in former desulfurization unslaked lime sample.
In the method for mensuration desulfurization unslaked lime effective constituent of the present invention, also be included in and carry out carrying out drying process to desulfurization unslaked lime sample before thermal weight loss measures, described drying process object mainly remove in sample with moisture, described drying process can adopt methods known in the art to carry out, as long as this method can not cause the decomposition of effective constituent, such as oven dry, vacuum drying or freeze drying etc. in an oven.
In the method for mensuration desulfurization unslaked lime effective constituent of the present invention, the quality putting into the desulfurization unslaked lime sample of thermogravimetric analyzer described in step (1) is 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 mensuration desulfurization unslaked lime effective constituent of the present invention, in step (1) described thermal weight loss mensuration process, heating rate is 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 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 mensuration desulfurization unslaked lime effective constituent of the present invention, the described effective constituent occurring to decompose of step (1) is Ca (OH) 2and/or CaCO 3.
In the method for mensuration desulfurization unslaked lime effective constituent of the present invention, in the decomposable asymmetric choice net sample described in step (2), effective constituent decomposes the undecomposable product produced is CaO.
In the method for mensuration desulfurization unslaked lime effective constituent of the present invention, effective constituent in the described undecomposed sample of step (2) is CaO, and it comprises effective constituent in the CaO and decomposable asymmetric choice net sample contained in former desulfurization unslaked lime sample and decomposes the CaO produced.
In the method for mensuration desulfurization unslaked lime effective constituent of the present invention, ftir Analysis coupling is utilized to come composition and the content of the sample that can decompose in working sample, carry out thermal weight loss by sample is put into thermogravimetric analyzer, can detect that the composition decomposing the product produced is H by infrared 2o and CO 2, and the first and second two zero-g periods can be seen from thermogravimetric curve, according to the temperature of these two zero-g periods and infrared detection to product component can judge that first stage weightlessness is due to Ca (OH) 2decompose and cause, subordinate phase weightlessness is due to CaCO 3decompose and cause, the effective constituent namely occurred in the sample decomposed is Ca (OH) 2and CaCO 3, can according to two zero-g period product H 2o and CO 2corresponding percent weight loss with ca (OH) in desulfurization unslaked lime sample is drawn according to following formula (1) and (2) 2and CaCO 3percentage composition with and Ca (OH) can be drawn according to formula (3) and (4) 2and CaCO 3decompose the percentage composition y that the CaO produced accounts for former desulfurization unslaked lime caOand z caO.Because CaO is more stable, can not decompose in the temperature range (900-1100 DEG C) of thermogravimetic analysis (TGA), carry out constituent content analysis by X-ray fluorescence spectra, can show that principal ingredient CaO in undecomposed sample (comprises Ca (OH) in the CaO and decomposable asymmetric choice net sample contained in former desulfurization unslaked lime sample 2and CaCO 3decompose the CaO produced) account for the percentage composition x of undecomposed sample caO, the number percent accounting for former desulfurization unslaked lime sample due to undecomposed sample is x u therefore x is used caObe multiplied by x ujust obtain the percentage composition that principal ingredient CaO in undecomposed sample accounts for former desulfurization unslaked lime sample, then deduct y caOand z caO, the percentage composition X of the CaO contained in former desulfurization unslaked lime sample namely just can be obtained according to formula (5) caO, computing formula is as follows:
X Ca ( OH ) 2 = ( M Ca ( OH ) 2 / M H 2 O ) × x H 2 O - - - ( 1 )
X CaCo 3 = ( M CaCo 3 / M CO 2 ) × x CO 2 - - - ( 2 )
y CaO = ( M CaO / M H 2 O ) × x H 2 O - - - ( 3 )
z CaO = ( M CaO / M H 2 O ) × x Co 2 - - - ( 4 )
X CaO = x CaO × x U - y CaO - z CaO - - - ( 5 )
Wherein M represents the molecular weight of each material.
As optimal technical scheme, the method for described mensuration desulfurization unslaked lime effective constituent of the present invention, specifically comprises the following steps:
(1) the desulfurization unslaked lime sample 50-500mg after drying process is put into thermogravimetric analyzer and carry out thermal weight loss mensuration, in thermal weight loss mensuration process, heating rate is 5-15 DEG C/min, from room temperature to 900-1100 DEG C, and by the infrared spectrometer of coupling, decomposition product is analyzed, determine composition and content thereof that decomposition occurs in sample;
(2) Xray fluorescence spectrometer is utilized to carry out ultimate analysis to undecomposed sample, determine that wherein contained effective constituent accounts for the percentage composition of undecomposed sample, the percentage composition of effective constituent in undecomposed sample is converted into the percentage composition accounting for former desulfurization unslaked lime sample, then deduct effective constituent in decomposable asymmetric choice net sample and decompose the percentage composition that the undecomposable product produced accounts for former desulfurization unslaked lime sample, and then obtain the content of undecomposed effective constituent in former desulfurization unslaked lime sample.
Relative to prior art, the present invention has following beneficial effect:
The present invention utilizes ftir Analysis coupling and in conjunction with X-ray fluorescence spectra to measure the content of effective constituent in desulfurization unslaked lime, the method drastically reduce the area the error that manual operation brings, and effectively can distinguish CaO, Ca (OH) in desulfurization unslaked lime sample 2and CaCO 3content, result is accurately and reliably.
Accompanying drawing explanation
Fig. 1 is the method flow diagram measuring desulfurization unslaked lime effective constituent;
Fig. 2 is the infrared curve map measuring effective constituent in desulfurization unslaked lime decomposition sample in the embodiment of the present invention 1;
Fig. 3 is the thermogravimetric curve figure measuring effective constituent in desulfurization unslaked lime decomposition sample in the embodiment of the present invention 1.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
embodiment 1
In the present embodiment, measure the method for desulfurization unslaked lime effective constituent by the following method, specifically comprise the following steps (method flow is as shown in Figure 1):
(1) the desulfurization unslaked lime sample 100mg after drying process is put into thermogravimetric analyzer and carry out thermal weight loss mensuration, in thermal weight loss mensuration process, heating rate is 10 DEG C/min, from room temperature to 1100 DEG C, and by the infrared spectrometer of coupling, decomposition product is analyzed.As shown in Figure 2, desulfurization unslaked lime decompose sample infrared curve in only detect H 2o and CO 2, the thermal weight loss temperature corresponded in thermogravimetric curve is as shown in Figure 3 the interval of 267-607 DEG C and 667-875 DEG C, analyzes known, and the product of first zero-g period decomposition is H 2o, percent weight loss is 4.567% (x h2O), according to decomposition temperature and product detected, first stage weightlessness is Ca (OH) 2decomposition causes; The product of second zero-g period decomposition is CO 2, percent weight loss is 4.485% (x cO2), according to decomposition temperature and product detected, subordinate phase weightlessness is CaCO 3decomposition causes, and chemical equation is as follows:
Ca in sample (OH) can be calculated according to following formula (1) and (2) 2and CaCO 3content, namely be 18.78%, be 10.19%, Ca (OH) can be drawn according to formula (3) and (4) 2the CaO generated accounts for the percentage composition y of former desulfurization unslaked lime sample caObe 14.21%, CaCO 3the CaO generated accounts for the percentage composition z of former desulfurization unslaked lime sample caObe 5.71%;
(2) by undecomposed sample, (sample namely after thermal weight loss calcining, accounts for 90.948% (x of former desulfurization unslaked lime sample u)) utilize Xray fluorescence spectrometer to carry out ultimate analysis to undecomposed sample after compressing tablet, test result shows that undecomposed desulfurization unslaked lime sample contains the elements such as Ca, Mg, Si, O, and their mass percent is respectively 67.32%, 1.34%, 0.91%, 29.46%.Ca and O accounts for 94.19% (x of undecomposed sample by this calcium compound (in CaO) content after oxide conversion caO).The percentage composition X of CaO in former desulfurization unslaked lime sample is obtained according to formula (5) caObe 65.74%;
Described computing formula is as follows:
X Ca ( OH ) 2 = ( M Ca ( OH ) 2 / M H 2 O ) × x H 2 O - - - ( 1 )
X CaCo 3 = ( M CaCo 3 / M CO 2 ) × x CO 2 - - - ( 2 )
y CaO = ( M CaO / M H 2 O ) × x H 2 O - - - ( 3 )
z CaO = ( M CaO / M H 2 O ) × x CO 2 - - - ( 4 )
X CaO=x CaO×x U-y CaO-z CaO(5)
Wherein M represents the molecular weight of each material.
Therefore, comprehensive above to draw, survey effective constituent in desulfurization unslaked lime sample and content is: CaO is 65.74%, Ca (OH) 2be 18.78%, CaCO 3be 10.19%.
embodiment 2
The present embodiment as different from Example 1, desulfurization unslaked lime amount of samples is that 50mg puts into thermogravimetric analyzer and carries out thermal weight loss mensuration, in thermal weight loss mensuration process, heating rate is 5 DEG C/min, from room temperature to 900 DEG C, measure effective constituent and the content of desulfurization unslaked lime sample through the method identical with embodiment 1, in the infrared curve of same desulfurization unslaked lime decomposition sample, only detect H 2o and CO 2, temperature range corresponding to the first and second zero-g periods in thermogravimetric curve is respectively 302-634 DEG C and 673-882 DEG C, and first zero-g period percent weight loss is the 4.893%, second zero-g period percent weight loss is 4.673%; Xray fluorescence spectrometer measures in undecomposed sample containing elements such as Ca, Mg, Si, O, their mass percent be respectively 70.41%, 1.86%, 1.02%, 30.63%, Ca and O account for 95.4% of undecomposed sample by this calcium compound (in CaO) content after oxide conversion.Comprehensive above measurement result analysis show that the content of effective constituent in desulfurization unslaked lime sample is: CaO is 65.10%, Ca (OH) 2be 20.11%, CaCO 3be 10.62%.
embodiment 3
The present embodiment as different from Example 1, desulfurization unslaked lime amount of samples is that 50mg puts into thermogravimetric analyzer and carries out thermal weight loss mensuration, in thermal weight loss mensuration process, heating rate is 10 DEG C/min, from room temperature to 980 DEG C, after the method identical with embodiment 1 measures, draw the content of effective constituent in desulfurization unslaked lime sample, in the infrared curve of same desulfurization unslaked lime decomposition sample, only detect H 2o and CO 2, temperature range corresponding to the first and second zero-g periods in thermogravimetric curve is respectively 268-613 DEG C and 672-882 DEG C, and first zero-g period percent weight loss is 4.582%, second zero-g period percent weight loss is 4.621%; Xray fluorescence spectrometer measures containing elements such as Ca, Mg, Si, O in undecomposed sample, and their mass percent is respectively 65.2%, 2.35%, 0.62%, 30.5%.Ca and O accounts for 93.6% of undecomposed sample by this calcium compound (in CaO) content after oxide conversion.Comprehensive above measurement result analysis show that the content of effective constituent in desulfurization unslaked lime sample is: CaO is 64.85%, Ca (OH) 2be 18.84%, CaCO 3be 10.50%.
embodiment 4
The present embodiment as different from Example 1, desulfurization unslaked lime amount of samples is that 200mg puts into thermogravimetric analyzer and carries out thermal weight loss mensuration, in thermal weight loss mensuration process, heating rate is 15 DEG C/min, from room temperature to 1100 DEG C, measure effective constituent and the content of desulfurization unslaked lime sample through the method identical with embodiment 1, in the infrared curve of same desulfurization unslaked lime decomposition sample, only detect H 2o and CO 2, temperature range corresponding to the first and second zero-g periods in thermogravimetric curve is respectively 246-598 DEG C and 654-863 DEG C, and first zero-g period percent weight loss is 4.325%, second zero-g period percent weight loss is 4.652%; Xray fluorescence spectrometer measures containing elements such as Ca, Mg, Si, O in undecomposed sample, and their mass percent is respectively 63.5%, 1.5%, 1.2%, 28.7%.Ca and O accounts for 92.3% of undecomposed sample by this calcium compound (in CaO) content after oxide conversion.Comprehensive above measurement result analysis show that the content of effective constituent in desulfurization unslaked lime sample is: CaO is 64.64%, Ca (OH) 2be 17.78%, CaCO 3be 10.57%.
embodiment 5
The present embodiment as different from Example 1, desulfurization unslaked lime amount of samples is that 500mg puts into thermogravimetric analyzer and carries out thermal weight loss mensuration, in thermal weight loss mensuration process, heating rate is 5 DEG C/min, from room temperature to 1100 DEG C, measure effective constituent and the content of desulfurization unslaked lime sample through the method identical with embodiment 1, in the infrared curve of same desulfurization unslaked lime decomposition sample, only detect H 2o and CO 2, temperature range corresponding to the first and second zero-g periods in thermogravimetric curve is respectively 246-587 DEG C and 654-864 DEG C, and first zero-g period percent weight loss is 4.376%, second zero-g period percent weight loss is 4.281%; Xray fluorescence spectrometer measures containing elements such as Ca, Mg, Si, O in undecomposed sample, and their mass percent is respectively 69.3%, 1.6%, 1.2%, 30.1%.Ca and O accounts for 96.3% of undecomposed sample by this calcium compound (in CaO) content after oxide conversion.Comprehensive above measurement result analysis show that the content of effective constituent in desulfurization unslaked lime sample is: CaO is 68.91%, Ca (OH) 2be 17.99%, CaCO 3be 9.73%.
embodiment 6
The present embodiment as different from Example 1, desulfurization unslaked lime amount of samples is that 150mg puts into thermogravimetric analyzer and carries out thermal weight loss mensuration, in thermal weight loss mensuration process, heating rate is 8 DEG C/min, from room temperature to 1100 DEG C, measure effective constituent and the content of desulfurization unslaked lime sample through the method identical with embodiment 1, in the infrared curve of same desulfurization unslaked lime decomposition sample, only detect H 2o and CO 2, temperature range corresponding to the first and second zero-g periods in thermogravimetric curve is respectively 254-618 DEG C and 671-882 DEG C, and first zero-g period percent weight loss is 4.532%, second zero-g period percent weight loss is 4.982%; Xray fluorescence spectrometer measures containing elements such as Ca, Mg, Si, O in undecomposed sample, and their mass percent is respectively 68.2%, 2.8%, 1.5%, 30.1%.Ca and O accounts for 95.1% of undecomposed sample by this calcium compound (in CaO) content after oxide conversion.Comprehensive above measurement result analysis show that the content of effective constituent in desulfurization unslaked lime sample is: CaO is 65.62%, Ca (OH) 2be 18.63%, CaCO 3be 11.32%.
embodiment 7
The present embodiment as different from Example 1, desulfurization unslaked lime amount of samples is that 300mg puts into thermogravimetric analyzer and carries out thermal weight loss mensuration, in thermal weight loss mensuration process, heating rate is 12 DEG C/min, from room temperature to 1000 DEG C, measure effective constituent and the content of desulfurization unslaked lime sample through the method identical with embodiment 1, in the infrared curve of same desulfurization unslaked lime decomposition sample, only detect H 2o and CO 2, temperature range corresponding to the first and second zero-g periods in thermogravimetric curve is respectively 272-635 DEG C and 675-891 DEG C, and first zero-g period percent weight loss is 4.124%, second zero-g period percent weight loss is 4.981%; Xray fluorescence spectrometer measures containing elements such as Ca, Mg, Si, O in undecomposed sample, and their mass percent is respectively 65.1%, 0.8%, 1.5%, 28.1%.Ca and O accounts for 92.4% of undecomposed sample by this calcium compound (in CaO) content after oxide conversion.Comprehensive above measurement result analysis show that the content of effective constituent in desulfurization unslaked lime sample is: CaO is 64.82%, Ca (OH) 2be 16.95%, CaCO 3be 11.32%.
Applicant states, the present invention illustrates the method for mensuration desulfurization unslaked lime effective constituent of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned processing step, does not namely mean that the present invention must rely on above-mentioned processing step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.

Claims (10)

1. measure a method for desulfurization unslaked lime effective constituent, it is characterized in that, described method is:
Analyze kind and the content thereof of determining decomposable effective constituent in desulfurization unslaked lime sample, then ultimate analysis is carried out to undecomposed sample, determine the content of contained effective constituent in undecomposed sample, thus determine the content of effective constituent in desulfurization unslaked lime sample.
2. method according to claim 1, is characterized in that, described analysis determines that the kind of decomposable effective constituent in desulfurization unslaked lime sample and content thereof utilize ftir Analysis combined instrument to realize.
3. method according to claim 1 and 2, is characterized in that, describedly carries out ultimate analysis to undecomposed sample and utilizes Xray fluorescence spectrometer to realize.
4. the method according to any one of claim 1-3, is characterized in that, said method comprising the steps of:
(1) desulfurization unslaked lime sample is put into thermogravimetric analyzer and carry out thermal weight loss mensuration, and by the infrared spectrometer of coupling, decomposition product is analyzed, determine effective constituent and content thereof that decomposition occurs in sample;
(2) Xray fluorescence spectrometer is utilized to carry out ultimate analysis to undecomposed sample, determine that wherein contained effective constituent accounts for the percentage composition of undecomposed sample, the percentage composition of effective constituent in undecomposed sample is converted into the percentage composition accounting for former desulfurization unslaked lime sample, then deduct effective constituent in decomposable asymmetric choice net sample and decompose the percentage composition that the undecomposable product produced accounts for former desulfurization unslaked lime sample, and then obtain the content of undecomposed effective constituent in former desulfurization unslaked lime sample.
5. method according to claim 4, is characterized in that, described method is also included in carries out carrying out drying process to desulfurization unslaked lime sample before thermal weight loss measures.
6. the method according to claim 4 or 5, is characterized in that, the quality putting into the desulfurization unslaked lime sample of thermogravimetric analyzer described in step (1) is 50-500mg.
7. the method according to any one of claim 4-6, is characterized in that, in step (1) described thermal weight loss mensuration process, heating rate is 5-15 DEG C/min, from room temperature to 900-1100 DEG C.
8. the method according to any one of claim 4-7, is characterized in that, the described effective constituent occurring to decompose of step (1) is Ca (OH) 2and/or CaCO 3.
9. the method according to any one of claim 4-8, is characterized in that, in the decomposable asymmetric choice net sample described in step (2), effective constituent decomposes the undecomposable product produced is CaO.
10. the method according to any one of claim 4-9, it is characterized in that, effective constituent in the described undecomposed sample of step (2) is CaO, and it comprises effective constituent in the CaO and decomposable asymmetric choice net sample contained in former desulfurization unslaked lime sample and decomposes the CaO produced.
CN201510204519.6A 2015-04-27 A kind of method for measuring desulfurization quick lime active ingredient Active CN104897511B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510204519.6A CN104897511B (en) 2015-04-27 A kind of method for measuring desulfurization quick lime active ingredient

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510204519.6A CN104897511B (en) 2015-04-27 A kind of method for measuring desulfurization quick lime active ingredient

Publications (2)

Publication Number Publication Date
CN104897511A true CN104897511A (en) 2015-09-09
CN104897511B CN104897511B (en) 2018-06-01

Family

ID=

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106018157A (en) * 2016-05-06 2016-10-12 美巢集团股份公司 Detection method for ingredients of ash calcium powder
CN106153492A (en) * 2016-07-22 2016-11-23 河北省电力建设调整试验所 A kind of solid particulate matter pyrolysis characteristics and product generate method of testing
CN113406126A (en) * 2021-06-17 2021-09-17 青铜峡铝业股份有限公司宁东铝业分公司 Method for measuring content of calcium hydroxide in flue gas desulfurizer

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4914297A (en) * 1987-12-23 1990-04-03 Nicolet Instrument Corporation Infrared spectrometer interface for thermogravimetric analysis
CN101718664A (en) * 2009-11-10 2010-06-02 天津出入境检验检疫局化矿金属材料检测中心 Method for measuring and calculating all iron content in imported iron ore

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4914297A (en) * 1987-12-23 1990-04-03 Nicolet Instrument Corporation Infrared spectrometer interface for thermogravimetric analysis
CN101718664A (en) * 2009-11-10 2010-06-02 天津出入境检验检疫局化矿金属材料检测中心 Method for measuring and calculating all iron content in imported iron ore

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张珂 等: ""一种石灰系复合脱硫剂组分的定量分析方法探讨"", 《冶金分析》 *
李安萍: ""X-射线荧光光谱法测定石灰石中CaO、MgO含量"", 《山西焦煤科技》 *
韩浩 等: ""X-射线荧光光谱法测定生石灰的化学成分"", 《冶金分析》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106018157A (en) * 2016-05-06 2016-10-12 美巢集团股份公司 Detection method for ingredients of ash calcium powder
CN106153492A (en) * 2016-07-22 2016-11-23 河北省电力建设调整试验所 A kind of solid particulate matter pyrolysis characteristics and product generate method of testing
CN113406126A (en) * 2021-06-17 2021-09-17 青铜峡铝业股份有限公司宁东铝业分公司 Method for measuring content of calcium hydroxide in flue gas desulfurizer

Similar Documents

Publication Publication Date Title
Zhao et al. Follow-up research for integrative process of pre-oxidation and post-absorption cleaning flue gas: Absorption of NO2, NO and SO2
Baciocchi et al. Innovative process for biogas upgrading with CO2 storage: results from pilot plant operation
US5879948A (en) Determination of total mercury in exhaust gases
CN105352945A (en) ICP analysis method of calcium sulfate and calcium sulfite in desulfurized gypsum
CN101852736A (en) Method for measuring calcium sulfate in desulfuration gypsum
CN101334365B (en) Determination method for chloride ion content of temper rolling liquor for steel plate rolling
CN102331422A (en) Process for continuously and rapidly determining components in desulfurization gypsum
Zhou et al. The effect of hydrogen peroxide solution on SO2 removal in the semidry flue gas desulfurization process
CN105424836A (en) Method for detecting content of ammonia in fly ash
Erich et al. Titrimetric determination of calcium carbonate equivalence of wood ash
CN103712933A (en) Method and system for determining content of calcium element in tungsten product
Rattanaya et al. Upgrading biogas to biomethane: Alkaline recovery of absorbed solution by thermal decomposition
Du et al. Particulate amines in the background atmosphere of the Yangtze River Delta, China: Concentration, size distribution, and sources
CN102353637A (en) Method of determining silver content in rock minerals
CN106124353A (en) A kind of carbon and hydrogen method in solid biomass fuel
Wang et al. Studies on mercury adsorption species and desorption activation energy on activated carbon under oxy combustion
Kuokkanen et al. Sequential leaching of heavy metals and sulfur in bottom ash and fly ash from the co-combustion of wood and peat at a municipal district heating plant
CN113060913B (en) Optimization method for carrying out harmless treatment on strongly alkaline red mud by utilizing easily-obtained industrial waste
Natali et al. Thermal separation coupled with elemental and isotopic analysis: A method for soil carbon characterisation
CN109115590A (en) A kind of method that micro-wave digestion-inductively coupled plasma emission spectrography measures calcium, magnesium, iron, copper in Industrial Boiler water
Rubio et al. Determination of chromium in environmental and biological samples by atomic absorption spectroscopy: a review
CN104897511A (en) Desulfurized quicklime effective ingredient determination method
CN104897511B (en) A kind of method for measuring desulfurization quick lime active ingredient
Mondal Absorption equilibria of dilute sulphur dioxide in Mg (OH) 2 slurry
CN114062186A (en) Method for determining content of calcium sulfate in sintering desulfurization and denitrification ash

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant