CN109799160A - A kind of desulphurization catalyst efficiency detection method - Google Patents
A kind of desulphurization catalyst efficiency detection method Download PDFInfo
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Abstract
The invention discloses a kind of desulphurization catalyst efficiency detection methods, include the following steps, step 1, after getting medicament required for detection sample and instrument ready, prepare two kinds of doctor solutions, i.e. blank doctor solution and catalyst desulfurizing liquid respectively；Step 2, the detection test of doctor solution standard coal gas desulfurization, standard coal gas containing nominal value is each led into the absorption bottle of a blank doctor solution and two catalyst desulfurizing liquid, wherein after a catalyst desulfurizing liquid absorption bottle sampling, it is passed through air average rate again up to catalyst desulfurizing regenerated liquid, the absorption bottle of another catalyst desulfurizing liquid is not passed through air, with stand-by；Step 3, it detects respectively, the parameter of computational representation desulfurization and decyanation catalyst removal effect；Step 4, the removal effect of catalyst is evaluated according to evaluating catalyst system table.The present invention reflects the quality of desulphurization catalyst with comparing objective reality, is convenient to production firm and effectively manages product quality and preferably check and accept use using unit, lays the foundation to produce stable natural labor.
Description
Technical field
The present invention relates to the field of detection and analysis more particularly to a kind of desulphurization catalyst efficiency detection methods.
Background technique
Gas cleaning system plays vital effect in terms of the recycling and purification of byproduct in coke-oven plant's coal gas,
H2S, HCN is the higher substance of content in raw coke oven gas, H2S content commonly reaches 6-8g/m3, H in coal gas2S and HCN is that have
Harmful impurity, they are to recovery of chemical products equipment and coal gas Storing and conveying equipment seriously corroded, and environmental pollution is serious, with containing
H2S and HCN higher coal gas steel-making, can reduce the quality of steel, be used as town gas pollution environment and toxic personnel easily caused to hurt
Evil, especially H2The SO that S and HCN burning generates2It is more toxic with nitrogen oxide, seriously pollutes environment, therefore, in coal gas
H2S, HCN must be removed, and remove the H in coal gas2S has iron hydroxide dry desulfurization, the desulfurization of AS method, the desulfurization of HPF method, modified ADA method
The different sulfur removal technology with desulfurizing tanning extract etc..HPF method sulfur removal technology category liquid phase catalytic oxidation desulfurization, it is using ammonia as alkali
Source, the wet type coke-oven-gas desulfurization and decyanation new process that HPF is desulphurization catalyst.H in coal gas2The acidic components such as S are in desulfurizing tower
In liquid phase entered by gas phase reacted with ammonia, be converted into the acid ammonium salts such as ammonium hydro sulfide, sent out in regenerator with the oxygen in air
Raw oxidation is converted into elementary sulfur, is condensed into sulphur cream with steam in sulfur melting kettle.HPF method desulfurization selection uses HPF (quinone ferro-cobalt
Class) composite catalyst, the desulfuration efficiency in coke-stove gas can be made to reach 98% or so.Desulphurization catalyst is double-core phthalein cyanogen cobalt
Sulfonates catalyst, abbreviation PDS, such catalyst desulfurization effect with higher, and in industry obtained widely
It uses.But due to the catalyst reaction complicated mechanism, index and the detection method for characterizing medicament desulfurization effect are ideal not to the utmost, no
The quality properties of the correct effectively evaluating desulphurization catalyst of energy.Activity determination index generally is used using unit assay index at present
As the characteristic index parameter of its desulfurization effect uniqueness, measuring principle is fixed there-necked flask on the oscillator, by vulcanized sodium
And catalyst PDS is put into wherein, and connection has the glass tube of accurate calibration, hydrogen sulfide gas is generated under catalyst PDS effect,
To drive the liquid in glass tube to rise, the activity of catalyst PDS is calculated according to the volume that liquid level rises, catalysis is characterized with this
The mass effect of agent PDS.Although the detection method can characterize the quality of catalyst PDS to a certain extent, with regard to checkout procedure
There are many drawbacks with index characterization.It is mainly manifested in, first is that, quality table of the measuring quality index to characterization catalyst PDS
Sign property is not strong, cannot accurately measure the quality of product truly and effectively, basic reason is experimental design existing defects, main table
Test process generation hydrogen sulfide gas is unbalanced now, and influence factor is more, and catalyst is sometimes difficult to the weight of its influence factor
To reach decisive role, the reasonability of the design of index is worth discussion.Second is that test process influences accuracy and objectivity
There are many factor, do not form normative operating process, and major influence factors are that hydrogen sulfide gas band glass liquid in pipe moves
It is accurate that dynamic displacement is difficult to measure, and the core parameter that index is measured is exactly shift value, therefore the error that detection process generates
With regard to bigger, the repeatability of same batch products differs greatly.Third is that detection device does not have a special instrument, in detection process not
With laboratory, difference is larger in installing instruments, and especially connection there-necked flask and graduated glass pipe and there-necked flask and oscillator connect
It connects and test result is had an important influence.Fourth is that the index of characterization PDS mass is single extensive, PDS is evaluated with being unable to objective science
Quality, it is more difficult to sentence the effect in production application of weighing.
Based on the reaction principle of catalyst PDS, in line with the thought of accurate objective Efficient Characterization catalyst PDS mass, design
Characterize the index parameter and test principle, process and characterization parameter of catalyst PDS mass.The mentality of designing can be accurate objective
The removal effect of Efficient Characterization catalyst PDS, abandons present Testing index and thinking completely, establish it is new convenient for detection, be convenient for
Judgement, the good detection parameters of detection data repeatability and detection scheme, reflect to objective reality catalyst PDS mass, convenient
Product quality is effectively managed in production firm and preferably checks and accepts use using unit, is laid the foundation to produce stable natural labor.
Summary of the invention
The purpose of the present invention is to solve the shortcomings of the prior art and a kind of desulphurization catalyst efficiency detection method is provided, visitor
The quality for being truly reflected desulphurization catalyst is seen, production firm is convenient to and effectively manages product quality and use unit preferably
It checks and accepts and uses, lay the foundation to produce stable natural labor.
In order to achieve the above objectives, the present invention is achieved through the following technical solutions.
A kind of desulphurization catalyst efficiency detection method, includes the following steps,
Step 1, after getting medicament required for detection sample and instrument ready, two kinds of doctor solutions, i.e. blank desulfurization are prepared respectively
Liquid and catalyst desulfurizing liquid；
Step 2, the standard coal gas containing nominal value, is each led into a sky by doctor solution standard coal gas desulfurization detection test
In the absorption bottle of white doctor solution and two catalyst desulfurizing liquid, wherein after a catalyst desulfurizing liquid absorption bottle sampling, then
It is passed through air average rate up to catalyst desulfurizing regenerated liquid, it is stand-by that the absorption bottle of another catalyst desulfurizing liquid is not passed through air；
Step 3, respectively detection, computational representation desulfurization and decyanation catalyst removal effect parameter, i.e., suspension sulphur, sulphur purity,
HS-Conversion ratio, hydrogen sulfide extrusion rate four indices；
Step 4, the removal effect of catalyst is evaluated according to evaluating catalyst system table.
Further, the detection of the suspension sulphur is with content of suspension sulfur in gravimetric method detection regenerative sulfur binding liquid, i.e., with quantitative
Filter paper filtration catalytic agent desulfurization regeneration liquid dries the weight difference of weighing filter paper after constant weight, is for suspension sulphur weight.
Further, sulphur purity Emhorn block-regulations or the measurement of coulomb method.
Further, the HS-Conversion ratio using iodimetric titration detect, i.e., respectively detect catalyst desulfurizing liquid, catalyst
HS in desulfurization regeneration liquid, blank solution-Ion, by HS in doctor solution-Ion subtracts HS in blank solution-Ion is denoted as CTHS-, then
HS in raw liquid-Ion subtracts HS in blank solution-Ion is denoted as CZHS-, with HS in regenerated liquid-Ion subtracts HS in blank solution-Ion
Divided by HS in doctor solution-Ion subtracts HS in blank solution-Ion, i.e. CZHS-/CTHS-, it is denoted as EHS-% characterizes the desulfurization of catalyst
Efficiency.
Further, the calculating of the hydrogen sulfide extrusion rate passes through content of suspension sulfur in catalyst desulfurizing regenerated liquid
Molecular weights calculate hydrogen sulfide content, in the body for being passed through doctor solution by the standard coal gas containing actual concentrations hydrogen sulfide content
Product calculates the hydrogen sulfide total amount of doctor solution absorption, and the two, which is divided by, is considered as hydrogen sulfide extrusion rate, in Quality Percentage.
The present invention provides the new technical parameter of desulphurization catalyst performance rating and detection technique methods, compare objective reality
Ground reflects the quality of desulphurization catalyst, solves many drawbacks of existing catalyst quality evaluation, it is effective to be convenient to production firm
It manages product quality and preferably checks and accepts use using unit, lay the foundation to produce stable natural labor.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but is not limited to the content on specification.
A kind of desulphurization catalyst efficiency detection method, includes the following steps,
Step 1, after getting medicament required for detection sample and instrument ready, two kinds of doctor solutions, that is, blank doctor solution is prepared respectively
With catalyst desulfurizing liquid.
Step 2, the standard coal gas containing nominal value, is each led into blank and taken off by doctor solution standard coal gas desulfurization detection test
In the absorption bottle of sulphur liquid and catalyst desulfurizing liquid, wherein after the sampling of catalyst desulfurizing liquid absorption bottle, then average rate lead to
Entering air makes its regeneration, and it is stand-by that the absorption bottle of another catalyst desulfurizing liquid is not passed through air.
Step 3, it detects respectively, the parameter of computational representation desulfurization and decyanation catalyst PDS removal effect, i.e. sulphur purity
(CS%), HS-Conversion ratio (EHS-%), hydrogen sulfide extrusion rate (RH2S%) three Xiang Zhibiao.
Step 4, the removal effect of catalyst is evaluated according to PDS evaluating catalyst system table.
Wherein, suspension sulphur (S) detection is with content of suspension sulfur in gravimetric method detection regenerative sulfur binding liquid, again with quantitative filter paper filtering
Doctor solution after life dries the weight difference of weighing filter paper after constant weight, is for suspension sulphur weight.
Emhorn block-regulations or coulomb method measure sulphur purity (CS%), by the Emhorn block-regulations of the filter paper after filtering drying or coulomb method
Measure suspension sulphur purity.
HS is detected using iodimetric titration-Ion.Detect doctor solution, regenerated liquid, the HS in blank solution-Ion, will be in doctor solution
HS-Ion subtracts HS in blank solution-Ion is denoted as CTHS-, HS in regenerated liquid-Ion subtracts HS in blank solution-Ion is denoted as
CZHS-, with HS in regenerated liquid-Ion subtracts HS in blank solution-Ion is divided by HS in doctor solution-Ion subtracts HS in blank solution-From
Son, i.e. CZHS-/CTHS-, it is denoted as EHS-%, can the clear strong desulfuration efficiency for illustrating catalyst.
Hydrogen sulfide extrusion rate (RH2SContent of suspension sulfur in regenerative sulfur binding liquid is calculated sulphur by Molecular weights by calculating %)
Change hydrogen content, calculates doctor solution in the volume for being passed through doctor solution by the standard coal gas containing actual concentrations hydrogen sulfide content
The hydrogen sulfide total amount of absorption, the two, which is divided by, is considered as hydrogen sulfide extrusion rate, in Quality Percentage.
According to the method for the present invention, domestic main PDS catalyst manufacturer quotient's particular product performance parameters, i.e. sulphur purity are detected
(CS%), HS-Conversion ratio (EHS-%), hydrogen sulfide extrusion rate (RH2S%) three Xiang Zhibiao, three Xiang Zhibiao of Comprehensive Assessment are determined and are produced
The grade appraisement system of product.Appraisement system is with hydrogen sulfide extrusion rate (RH2S%) and HS-Conversion ratio (EHS-It %) is core index,
With sulphur purity (CSIt is %) important reference indicator, establishes PDS evaluating catalyst system table, be shown in Table 1.
1 PDS catalyst quality appraisement system table of table
| Index name | Indicate symbol | Index parameter |
| Sulphur purity | CS% | >=92% |
| HS-Conversion ratio | EHS-% | >=95% |
| Hydrogen sulfide extrusion rate | RH2S% | >=96% |
The method of the present invention is based on Wet-type oxidation sweetening reaction principle, using simulated production scene desulfurization effect as means, design
The a set of desulphurization catalyst PDS quality characterization and detection method that multi-parameter evaluation detection method is mutually proved.According to live desulfurization
Liquid component prepares the doctor solution of two groups of additions PDS catalyst to be measured using one group of pure ammonia spirit as blank reagent, respectively respectively
It is passed through in the standard coal gas that hydrogen sulfide content is definite value, removes the hydrogen sulfide in standard coal gas, then again to doctor solution blow air
It is raw, wherein one group of doctor solution is not passed through air regenesis, Emhorn block-regulations is detected respectively and measures sulphur purity, HS-Conversion ratio measurement, sulphur
Change 3 quality characterization parameters of hydrogen extrusion rate.
The method of the present invention design is based on Wet-type oxidation sweetening reaction principle, i.e. the acidic components such as hydrogen sulfide in coal gas are by gas
Mutually enter liquid phase to react with ammonia, is converted into the acid ammonium salts such as ammonium hydro sulfide, then under the oxidation of oxygen be converted into elementary sulfur in air.
Desulphurization reaction:
Regenerative response
NH4HS+1/2O2→S↓+NH4OH
(NH4)2Sx+1/2O2+H2O→Sx+2NH4OH
Side reaction
2NH4HS+2O2→(NH4)2S2O3+H2O
2(NH4)2S2O3+O2→(NH4)2SO4+2S↓
The method of the present invention design characterization desulphurization catalyst PDS mass parameter test process is described below:
Illustrated below with specific embodiment:
1, main agents and instrument: ammonium hydroxide, use for laboratory water, Eschka reagent, iodine standard solution 0.1mol/L, thio sulphur
Sour sodium standard solution 0.1mol/L, barium sulfate, standard coal gas bottle, Muffle furnace, baking oven etc.
2, test operation process
2.1, doctor solution: blank doctor solution --- 10g/L ammonia spirit (no catalyst) catalyst desulfurizing liquid --- is prepared
Solvent is made with 10g/L ammonia spirit, PDS catalyst preparation is added into the doctor solution of 100ppm
2.2, lead to standard coal gas desulfurization: taking 150ml to be added to respectively the blank doctor solution being configured to, catalyst desulfurizing liquid
In three absorption bottles, absorption bottle contains blank doctor solution, and another two absorption bottles distinguish holding catalyst doctor solution, containing
The standard coal gas of nominal value is each led into the absorption bottle of blank doctor solution and catalyst desulfurizing liquid, controls logical standard coal gas
100L controls standard gas flow 3L/min.Wherein with 5-7L/min's after a catalyst desulfurizing liquid absorption bottle sampling
Speed average rate, which is passed through air 30min, makes its regeneration, while hydrogen sulfide reaction generates elementary sulfur, the suction of another catalyst desulfurizing liquid
It is stand-by that receipts bottle is not passed through air.
3, desulphurization catalyst PDS mass parameter and its detection are characterized
3.1, suspension sulphur detects: with content of suspension sulfur in gravimetric method detection regenerative sulfur binding liquid, with quantitative filter paper filter regeneration
Doctor solution afterwards dries the weight difference of weighing filter paper after constant weight, is for suspension sulphur weight.Blank test is done simultaneously.This is that detection is urged
The most direct technical parameter of agent PDS mass.Suspension sulphur is more, hydrogen sulfide significant effect in characterization catalyst PDS removing coal gas；Instead
It, then show that hydrogen sulfide effect is bad in catalyst PDS removing coal gas；
3.2, Emhorn block-regulations or coulomb method measure sulphur purity (CS%): by the filter paper after filtering drying Emhorn block-regulations or library
Human relations method measures suspension sulphur purity, hydrogen sulfide effect in further characterization catalyst PDS removing coal gas.With Emhorn card when generation objection
Method is referee method.
3.3、HS-Conversion ratio (EHS-It %) measures: HPF method desulfurization category liquid phase catalytic oxidation technique.Its main desulfurization is anti-
Ying ShiThe NH of generation4HS hydrolysis, therefore will largely there is HS in doctor solution-Ion.
The reaction of its main regeneration is NH4HS+1/2O2→S↓+NH4OH, NH4HS is largely oxidized to sulphur simple substance (sulphur), de- after regeneration
HS in sulphur liquid-Ion will largely reduce.Detect doctor solution, regenerated liquid, the HS in blank solution-Ion, by HS in doctor solution-From
Son subtracts HS in blank solution-Ion is denoted as CTHS-, HS in regenerated liquid-Ion subtracts HS in blank solution-Ion is denoted as CZHS-, with again
HS in raw liquid-Ion subtracts HS in blank solution-Ion is divided by HS in doctor solution-Ion subtracts HS in blank solution-Ion, i.e. CZHS-/
CTHS-, it is denoted as EHS-%, can the clear strong desulfuration efficiency for illustrating catalyst.Detect HS-Ion uses iodometric determination.
3.4., hydrogen sulfide extrusion rate (RH2SContent of suspension sulfur in regenerative sulfur binding liquid is calculated by Molecular weights %) and is vulcanized
Hydrogen content calculates doctor solution in the volume for being passed through doctor solution by the standard coal gas containing actual concentrations hydrogen sulfide content and inhales
The hydrogen sulfide total amount of receipts, the two, which is divided by, is considered as hydrogen sulfide extrusion rate, in Quality Percentage.
3.5, according to the above method, domestic main PDS catalyst manufacturer quotient's particular product performance parameters, i.e. sulphur purity are detected
(CS%), HS-Conversion ratio (EHS-%), hydrogen sulfide extrusion rate (RH2S%) four indices, three Xiang Zhibiao of Comprehensive Assessment are determined and are produced
The grade appraisement system of product.Appraisement system is with hydrogen sulfide extrusion rate (RH2S%) and HS-Conversion ratio (EHS-It %) is core index,
With sulphur purity (CSIt is %) important reference indicator, establishes PDS evaluating catalyst system table.Several PDS catalyst plants in the specific country
Commodity inspection measured data is shown in Table 2
The domestic several PDS catalyst plant commodity inspection measured data of table 2
The quality for reflecting to objective reality of the present invention desulphurization catalyst, be convenient to production firm effectively manage product quality with
And use is preferably checked and accepted using unit, it lays the foundation to produce stable natural labor.
Obviously, above embodiment of the invention be only to clearly illustrate example of the present invention, and not be
Restriction to embodiments of the present invention.For those of ordinary skill in the art, on the basis of the above description also
It can make other variations or changes in different ways.Here all embodiments can not be exhaustive.It is all to belong to this
The obvious changes or variations that the technical solution of invention is extended out are still in the scope of protection of the present invention.
Claims (5)
1. a kind of desulphurization catalyst efficiency detection method, it is characterised in that: include the following steps,
Step 1, two kinds of doctor solutions are prepared after getting medicament and instrument required for detection sample ready, respectively, i.e., blank doctor solution and
Catalyst desulfurizing liquid；
Step 2, the standard coal gas containing nominal value, is each led into a blank and taken off by doctor solution standard coal gas desulfurization detection test
In the absorption bottle of sulphur liquid and two catalyst desulfurizing liquid, wherein after a catalyst desulfurizing liquid absorption bottle sampling, then average rate
Ground is passed through air up to catalyst desulfurizing regenerated liquid, and it is stand-by that the absorption bottle of another catalyst desulfurizing liquid is not passed through air；
Step 3, it detects respectively, the parameter of computational representation desulfurization and decyanation catalyst removal effect, i.e. sulphur purity, HS-Conversion ratio,
Three Xiang Zhibiao of hydrogen sulfide extrusion rate calculates the intermediate parameters of detection content of suspension sulfur；
Step 4, the removal effect of catalyst is evaluated according to evaluating catalyst system table.
2. a kind of desulphurization catalyst efficiency detection method according to claim 1, it is characterised in that: the inspection of the suspension sulphur
It surveys with content of suspension sulfur in gravimetric method detection regenerative sulfur binding liquid, that is, uses quantitative filter paper filtration catalytic agent desulfurization regeneration liquid, drying is permanent
The weight difference that filter paper is weighed after weight, is for suspension sulphur weight.
3. a kind of desulphurization catalyst efficiency detection method according to claim 1, it is characterised in that: the sulphur purity Chinese mugwort
Family name's block-regulations or the measurement of coulomb method.
4. a kind of desulphurization catalyst efficiency detection method according to claim 1, it is characterised in that: the HS-Conversion ratio
It is detected using iodimetric titration, i.e., detects catalyst desulfurizing liquid, catalyst desulfurizing regenerated liquid, the HS in blank solution respectively-Ion will take off
HS in sulphur liquid-Ion subtracts HS in blank solution-Ion is denoted as CTHS-, HS in regenerated liquid-Ion subtracts HS in blank solution-Ion, note
Make CZHS-, with HS in regenerated liquid-Ion subtracts HS in blank solution-Ion is divided by HS in doctor solution-Ion subtracts HS in blank solution-From
Son, i.e. CZHS-/CTHS-, it is denoted as EHS-% characterizes the desulfuration efficiency of catalyst.
5. a kind of desulphurization catalyst efficiency detection method according to claim 1, it is characterised in that: the hydrogen sulfide abjection
Content of suspension sulfur in catalyst desulfurizing regenerated liquid is calculated hydrogen sulfide content by Molecular weights by the calculating of rate, then by containing
Have the standard coal gas of actual concentrations hydrogen sulfide content be passed through doctor solution volume calculate doctor solution absorption hydrogen sulfide total amount, two
Person, which is divided by, is considered as hydrogen sulfide extrusion rate, in Quality Percentage.
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Cited By (1)
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| CN115792081A (en) * | 2022-11-22 | 2023-03-14 | 广西电网有限责任公司电力科学研究院 | Detection method for judging catalytic effect of catalyst for removing sulfur dioxide from flue gas |
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