CN106124558B - A kind of measurement method of decomposition heat - Google Patents
A kind of measurement method of decomposition heat Download PDFInfo
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- CN106124558B CN106124558B CN201610438631.0A CN201610438631A CN106124558B CN 106124558 B CN106124558 B CN 106124558B CN 201610438631 A CN201610438631 A CN 201610438631A CN 106124558 B CN106124558 B CN 106124558B
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- crucible
- coal dust
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
Abstract
The present invention discloses a kind of measurement method of decomposition heat, belongs to technical field of blast furnace ironmaking, solves the problems, such as that the coal dust fugitive constituent of blast furnace blowing decomposes heat dissipation.Based on coal dust in Blast Furnace Raceway decomposition behavior, proposes and be fired step using alumina crucible the oxidation aluminium material in the alumina crucible is completely converted into α-Al2O3, obtain α-Al2O3Crucible measures sky α-Al using DSC differential scanning calorimeter2O3The heat flow curve of crucible and α-Al with a certain amount of coal dust2O3The heat flow curve of crucible, finally according to the sky α-Al2O3Heat flow curve, the band coal dust α-Al of crucible2O3α-Al under the heat flow curve and constant-pressure conditions of crucible2O3The decomposition heat of coal dust is calculated in enthalpy change and temperature dependence.This method convenience of calculation, science are accurate, have directive significance to practical calorific value of the coal injection in blast furnace is grasped.
Description
Technical field
The present invention principally falls into technical field of blast furnace ironmaking, and in particular to a kind of measurement method of decomposition heat.
Background technique
China's coal powder injection on blast furnace since the sixties in last century is relatively early in the world coal injection technology to be applied to industrial life
Country in production.Pulverized coal injection is mainly to be blown storage non caking coal abundant to reduce to coking coal dependence increasingly in short supply, excellent
Reach reduction ironmaking cost on the basis of the change utilization of resources, raise labour productivity, improve metallurgical environmental protection condition, improves steel enterprise
The purpose of the industry market competitiveness.Blast-furnace tuyere carbon-bearing polyoxy is few, and temperature is high, and volatile organic matter in coal dust can only be oxidized to
CO、H2, can not be as forming CO in atmosphere2、H2O, therefore its higher decomposition heat of volatile matter is higher in coal dust, this is to influence blast furnace
The key factor of coal powder injection offer heat.It is aobvious for obtaining accurate decomposition heat with increasing substantially for Coal Injection Amount into BF
It obtains more urgent.However, produced on-site mostly uses the empirical value of decomposition heat according to coal classification, and it is subjective, lack science
Property；Some scholars by assuming that, establish various models to calculate the decomposition heat of volatile organic matter in coal, there is certain science
Property, but the data volume needed is larger, calculates complexity, brings difficulty for the utilization of iron and steel enterprise.
Summary of the invention
In view of the above-mentioned problems, the present invention provides a kind of method of the measurement decomposition heat of science, the method is based on coal
Powder is in Blast Furnace Raceway decomposition behavior, according to the sky α-Al2O3Heat flow curve, the band coal dust α-Al of crucible2O3The heat of crucible
α-Al under flow curve and constant-pressure conditions2O3The decomposition heat of coal dust is calculated in enthalpy change and temperature dependence.The method can
Reflect the accurate decomposition heat of coal dust, experimental method is easy to operate, solves the problems, such as that background technique exists.
The present invention is achieved by the following technical solutions:
A kind of measurement method of decomposition heat, the method use alumina crucible, are fired step for the oxidation
Oxidation aluminium material in aluminium crucible is completely converted into α-Al2O3, obtain α-Al2O3Crucible, after being cooled to room temperature, using DSC differential
It scans calorimeter measurement and obtains sky α-Al2O3The heat flow curve of crucible；To the α-Al2O3Crucible is cooled to room temperature, and coal is added
Powder measures using DSC differential scanning calorimeter and obtains band coal dust α-Al2O3The heat flow curve of crucible, finally according to the sky α-
Al2O3Heat flow curve, the band coal dust α-Al of crucible2O3α-Al under the heat flow curve and constant-pressure conditions of crucible2O3Enthalpy change and
The decomposition heat of coal dust is calculated in temperature dependence.
Further, according to the sky α-Al2O3Heat flow curve, the band coal dust α-Al of crucible2O3The heat flow of crucible is bent
α-Al under line and constant-pressure conditions2O3Enthalpy change and temperature dependence calculate the decomposition heat of coal dust specifically:
(1) sky α-Al is calculated2O3The hot Q of unit mass reactive absorption of crucible1: it is equal to according to enthalpy change amount △ H under constant-pressure conditions
α-Al under the hot Q of reactive absorption and constant-pressure conditions2O3Enthalpy change and temperature dependence temperature is calculated under constant-pressure conditions is T space-time
α-Al2O3The hot Q of unit mass reactive absorption of crucible1；
(2) sky α-Al is calculated2O3The hot q of the reactive absorption of crucible1, calculation formula are as follows:
q1=m1*Q1
Wherein, Q1Empty α-the Al being calculated for step (1)2O3The unit mass reactive absorption heat of crucible, m1For empty α-
Al2O3The quality of crucible, the sky α-Al2O3The quality determination condition of crucible is to measure after roasting is cooled to room temperature；
(3) calculating of decomposition heat: by absorb known to common sense hot q=Q*m and heat flow curve integral area S at than
Example, then (Q2*m2)/(S2-S1)=(Q1*m1)/S1Release decomposition heat Q2=(Q1*m1*(S2-S1))/(S1*m2)(J/g)
Wherein, S1For to the sky α-Al2O3The heat flow curve of crucible is integrated and calculates the absorption peak face of acquisition
Product, integral temperature section are 105 DEG C to 1200 DEG C；
S2For to the band coal dust α-Al2O3The heat flow curve of crucible is integrated and is calculated the absorption peak area of acquisition,
Integral temperature section is 105 DEG C to 1200 DEG C；
m1For empty α-Al2O3The quality of crucible；
m2For the α-Al is added2O3The quality of coal dust in crucible；
In practical application, coal dust enters the drying that stokehold passes through 105 DEG C, and coal dust fires under 1200 DEG C of environment temperature after entering furnace
It burns, in order to simulate above-mentioned operating condition, so integral temperature section is set to 105 DEG C to 1200 DEG C.
Further, the calcination steps actual conditions are as follows: the alumina crucible is placed in Muffle furnace, in being higher than
1h is roasted under the conditions of 1300 DEG C, this step purpose is to guarantee that the aluminium oxide in crucible material is completely converted into calorimetric standard substance α-
Al2O3Form.
Further, it is measured using DSC differential scanning calorimeter and obtains sky α-Al2O3Heat flow curve, the band coal dust of crucible
α-Al2O3During the heat flow curve of crucible, specific DSC differential scanning calorimeter parameter is controlled are as follows: heating rate 5-30
DEG C/min, and 1200 DEG C of outlet temperature, N under normal pressure2As protection gas, ventilation flow rate 20-100ml/min.
Further, because how much influences that quality is added under a constant volume are conducted heat, it should control and crucible coal dust matter is added
Amount, is added the α-Al2O3The quality of coal dust in crucible is 5-20mg, on the other hand, under actual condition, enters the coal dust of stokehold
It is ground by coal pulverizer, granularity is generally in 0.074mm or so, in order to which the standard selection coal powder size of experiment is less than 0.074mm.
Further, the coal dust needs to be pre-processed before crucible is added, and pretreatment condition is in 105 DEG C of drying boxes
1h is placed, is sealed up for safekeeping after taking-up stand-by.
Further, α-Al under the constant-pressure conditions2O3Enthalpy change △ H and temperature T relationship formula are as follows:
H=-282.175+0.855153*T+2.46033 × 10 △-4*T2-4.11844×10-8*T3Wherein, T represents exhausted
To temperature.
Further, the coal dust is replaced with into biological straw, tire.
Advantageous effects of the invention: the present invention solves scientific and various by empirical value shortage in background technique
Model data amount is big to calculate complicated problem, fast and accurately obtains coal dust using the method that DSC differential scanning calorimeter is tested
Decomposition heat can purchase injection coal for enterprise and provide reference data, have important finger to the optimum choice of live coal suitable for blowing
Lead meaning.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments to the present invention
It is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, it is not used to
Limit the present invention.
On the contrary, the present invention covers any substitution done on the essence and scope of the present invention being defined by the claims, repairs
Change, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to of the invention thin
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
The present invention can also be understood completely in description.
Embodiment 1
A kind of measurement method of decomposition heat, more specific processing step are as follows:
(1) empty crucible used is put into 1300 DEG C of Muffle furnace roasting 1h, guarantees Al in crucible2O3With α-Al2O3In the presence of,
Taking-up is cooled to room temperature spare；Coal dust by granularity less than 0.074mm, which is placed in after 105 DEG C of drying box 1h to take out, to be sealed up for safekeeping, Yi Mianyu
Moisture in air contact.
(2) quality (m of empty crucible after roasting is weighed1), it then places it on DSC differential scanning calorimeter pallet；
If the heating rate of DSC differential scanning calorimeter is 20 DEG C/min, outlet temperature is 1200 DEG C, N2As protection
Gas, flow 60ml/min.
The empty crucible absorption peak heat flow curve area (S that DSC differential scanning calorimeter is obtained using Origin software1)
It is integrated, integral temperature section is 105 DEG C to 1200 DEG C.
According to α-Al2O3The relational expression of crucible enthalpy change and temperature, the absorption for obtaining sky crucible are hot (q1)；
q1=Q1*m1=△ H*m1=(- 282.175+0.855153*T+2.46033 × 10-4*T2-4.11844×10-8*
T3)*m1(J/g)
(3) m is weighed2Coal dust be placed in above-mentioned empty crucible, then place it in DSC differential scanning calorimeter pallet
On, the temperature increasing schedule of DSC differential scanning calorimeter is identical as above-mentioned steps.
The decomposition heat that DSC differential scanning calorimeter is obtained using Origin software and empty crucible absorption peak heat flow
Area under the curve (S2) integrated, integral temperature section is 105 DEG C to 1200 DEG C.
The coal dust of certain mass, which decomposes, absorbs peak area for △ S=S2-S1。
(4) decomposition heat is according to following calculation method:
It is proportional to heat flow curve integral area S that hot q=Q*m is absorbed known to common sense, then (Q2*m2)/(S2-S1)=
(Q1*m1)/S1Release unit mass decomposition heat Q2=(Q1*m1*(S2-S1))/(S1*m2)(J/g)
Table 1 is the Industrial Analysis of certain coal dust:
| Ash content | Volatile matter | Fixed carbon | |
| Coal | 6.16 | 33.87 | 59.97 |
Table 2 is the coal dust relevant parameter calculated according to decomposition heat measurement method
By the calculating of the above decomposition heat, obtaining the decomposition heat in example is 1535.3J/g, and scene is for waving
Hair point is more than that 30% jet coal decomposition heat is typically set at 1400J/g, and it is more quasi- that experimental result of the invention compares empirical value
Really, this has important directive function for the selection of injection coal.
Claims (7)
1. a kind of measurement method of decomposition heat, which is characterized in that the method uses alumina crucible, and being fired step will
Oxidation aluminium material in the alumina crucible is completely converted into α-Al2O3, obtain α-Al2O3Crucible after being cooled to room temperature, is answered
It is measured with DSC differential scanning calorimeter and obtains sky α-Al2O3The heat flow curve of crucible；To the α-Al2O3Crucible is cooled to room
Coal dust is added in temperature, measures using DSC differential scanning calorimeter and obtains band coal dust α-Al2O3The heat flow curve of crucible, last root
According to the sky α-Al2O3Heat flow curve, the band coal dust α-Al of crucible2O3α-under the heat flow curve and constant-pressure conditions of crucible
Al2O3The decomposition heat of coal dust is calculated in enthalpy change and temperature dependence,
Wherein, according to the sky α-Al2O3Heat flow curve, the band coal dust α-Al of crucible2O3The heat flow curve and perseverance of crucible
α-Al under the conditions of pressure2O3Enthalpy change and temperature dependence calculate the decomposition heat of coal dust specifically:
(1) sky α-Al is calculated2O3The hot Q of unit mass reactive absorption of crucible1: reaction is equal to according to enthalpy change amount △ H under constant-pressure conditions
Absorb α-Al under hot Q and constant-pressure conditions2O3Enthalpy change and temperature dependence temperature is calculated under constant-pressure conditions is T space-time α-
Al2O3The hot Q of unit mass reactive absorption of crucible1；
(2) sky α-Al is calculated2O3The hot q of the reactive absorption of crucible1, calculation formula are as follows:
q1=m1*Q1
Wherein, Q1Empty α-the Al being calculated for step (1)2O3The unit mass reactive absorption heat of crucible, m1For empty α-Al2O3Earthenware
The quality of crucible, the sky α-Al2O3The quality determination condition of crucible is to measure after roasting is cooled to room temperature；
(3) calculating of decomposition heat: decomposition heat calculation formula are as follows:
Q2=(Q1*m1*(S2-S1))/(S1*m2)
Wherein, S1For to the sky α-Al2O3The heat flow curve of crucible is integrated and is calculated the absorption peak area of acquisition, product
Dividing temperature range is 105 DEG C to 1200 DEG C；
S2For to the band coal dust α-Al2O3The heat flow curve of crucible is integrated and is calculated the absorption peak area of acquisition, integral
Temperature range is 105 DEG C to 1200 DEG C；
m1For empty α-Al2O3The quality of crucible；
m2For the α-Al is added2O3The quality of coal dust in crucible.
2. a kind of measurement method of decomposition heat according to claim 1, which is characterized in that apply DSC differential scanning amount
Hot instrument measurement obtains sky α-Al2O3Heat flow curve, the band coal dust α-Al of crucible2O3During the heat flow curve of crucible,
DSC differential scanning calorimeter parameter are as follows: 5-30 DEG C of heating rate/min, 1200 DEG C of outlet temperature, N under normal pressure2As protection gas,
Ventilation flow rate is 20-100ml/min.
3. a kind of measurement method of decomposition heat according to claim 1, which is characterized in that α-under the constant-pressure conditions
Al2O3Enthalpy change △ H and temperature T relationship formula are as follows: H=-282.175+0.855153*T+2.46033 × 10 △-4*T2-4.11844
×10-8*T3
Wherein, T represents absolute temperature.
4. a kind of measurement method of decomposition heat according to claim 1, which is characterized in that the specific item of calcination steps
Part are as follows: the alumina crucible is placed in Muffle furnace, roasts 1h under the conditions of being higher than 1300 DEG C.
5. a kind of measurement method of decomposition heat according to claim 1, which is characterized in that the α-Al is added2O3Crucible
In coal dust quality be 5-20mg, and coal powder size be less than 0.074mm.
6. a kind of measurement method of decomposition heat according to claim 4, which is characterized in that crucible is being added in the coal dust
Before need to be pre-processed, pretreatment condition is that 1h is placed in 105 DEG C of drying boxes, is sealed up for safekeeping after taking-up stand-by.
7. a kind of measurement method of decomposition heat according to claim 1, it is characterised in that: coal dust replacement is made a living
Object stalk, tire.
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Inventor after: Zhang Jianliang Inventor after: Lan Dawei Inventor after: Song Tengfei Inventor after: Xu Runsheng Inventor after: Wang Haiyang Inventor after: Liu Siyuan Inventor before: Zhang Jianliang Inventor before: Song Tengfei Inventor before: Xu Runsheng Inventor before: Wang Haiyang Inventor before: Liu Siyuan |
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