CN106383062B - A method of assessment raw mineral materials - Google Patents
A method of assessment raw mineral materials Download PDFInfo
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- CN106383062B CN106383062B CN201610740805.9A CN201610740805A CN106383062B CN 106383062 B CN106383062 B CN 106383062B CN 201610740805 A CN201610740805 A CN 201610740805A CN 106383062 B CN106383062 B CN 106383062B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The present invention provides a kind of methods for assessing raw mineral materials, take the mixture of fluxing agent, raw mineral materials and fluxing agent in crucible respectively, are placed in thermal analyzer furnace body；Control thermal analyzer furnace body is warming up to predetermined temperature, then cools to room temperature with the furnace；To generate the heat content of the mixture of fluxing agent, raw mineral materials and fluxing agent, the relation curve of weight percent and temperature respectively；It is poor that two relation curves are made, to obtain the fusion temperature and weight percent of raw mineral materials.This method can not only accurately evaluate the fusing complexity of raw mineral materials, also have the advantages such as quick, easy to operate, nontoxic.
Description
Technical field
The present invention relates to a kind of methods for assessing raw mineral materials, more particularly to assessment raw mineral materials high temperature melting complexity
Method.
Background technique
Raw mineral materials is the main production raw material of silicate industry, and the superiority and inferiority of taste decides the energy consumption of silicate industry
And product quality.
Currently, raw mineral materials fusing complexity is mainly made of the mineral phase structure for testing material composition, identification mineral, is former
The methods of heavy mineral in material is evaluated.Wherein, material composition test result is mainly indicated in the form of the various oxides, no
It can definitely show the fusing complexity of raw mineral materials；Although mine phase composition shows the knot of raw mineral materials from microstructure
Structure composition determines the type of raw material, but some objects, mutually there is different crystallographic systems and crystal structure, fusion temperature is also poor
It is different, therefore the fusing complexity for accurately judging raw mineral materials is not achieved.
Heavy mineral in raw material is commonly defined as density in raw mineral materials and is greater than quartz sand (ρ=2.65g/cm3) mine
Object.Therefore, it measures heavy mineral content in raw mineral materials and is not necessarily completely infusibility substance, how much mine is judged with heavy mineral content
The fusing complexity of raw material is unilateral.In addition, the detection agents useful for same of heavy mineral is containing toxic, during long period of operation exists
Malicious risk, and the test period is long.
Summary of the invention
Present invention seek to address that problem as described above.It is an object of the invention to be silicate industry, especially glass
Industry provides a kind of method for assessing raw mineral materials fusibility.The fusing that this method can not only accurately evaluate raw mineral materials is difficult
Easy degree also has the advantages such as quick, easy to operate, nontoxic.
The present invention provides a kind of method for assessing raw mineral materials, comprising the following steps:
1S: it takes fluxing agent in crucible, is placed in thermal analyzer furnace body；
2S: control thermal analyzer furnace body is warming up to predetermined temperature, then cools to room temperature with the furnace, generates the heat of fluxing agent
The relation curve of enthalpy, weight percent and temperature；
3S: taking raw mineral materials and fluxing agent, is uniformly mixed with scheduled mass ratio, forms the mixed of raw mineral materials and fluxing agent
Close object；
4S: it takes the mixture of step 3S chats raw material and fluxing agent in crucible, is placed in thermal analyzer furnace body；
5S: control thermal analyzer furnace body is warming up to the predetermined temperature, then cools to room temperature with the furnace, generates raw mineral materials
With the relation curve of the heat content of the mixture of fluxing agent, weight percent and temperature；
6S: with the heat content of step 5S and the resulting fluxing agent of step 2S, the relation curve and mine of weight percent and temperature
It is poor that the relation curve of the heat content of the mixture of raw material and fluxing agent, weight percent and temperature is made, to obtain raw mineral materials
Fusion temperature and weight percent.
Wherein, scheduled mass ratio described in the step 3S is 0.5:1~3.5:1.
Wherein, scheduled mass ratio described in the step 3S is 1.5:1~3:1.
Wherein, the heating rate of the step 2S and step 5S is 5-20 DEG C/min, and the predetermined temperature is 1400-1550
℃。
Wherein, the predetermined temperature is 1450-1500 DEG C.
Wherein, which is characterized in that the fluxing agent is one of boric acid, anhydrous lithium tetraborate, lithium metaborate or a variety of.
Wherein, which is characterized in that the raw mineral materials is one of siliceous raw material, aluminum-containing raw material or a variety of.
Wherein, the siliceous raw material includes one of sandstone, quartz, clay or a variety of.
Wherein, the aluminum-containing raw material includes one of kaolin, pyrophillite, feldspar or a variety of.
The present invention also provides a kind of methods for assessing raw mineral materials in assessment raw mineral materials high temperature melting complexity
Application.
It is heated to obtain raw mineral materials by heating to raw mineral materials for the method for assessment raw mineral materials of the invention
The relation curve of the hot enthalpy change of journey, weight percent and temperature, the accordingly fusion temperature of available raw mineral materials.
Fluxing agent is placed in crucible first, then is placed in and carries out being warming up to predetermined temperature in thermal analyzer furnace body, it is cold with furnace
But to room temperature, the relation curve of the heat content of available fluxing agent, weight percent and temperature；Wherein, crucible is corundum crucible,
The furnace body material of thermal analyzer is silicon carbide, and maximum operation (service) temperature can reach 1550 DEG C, it is possible to provide uniform temperature field, built-in essence
The close gentle sensor in day, can automatic and accurate record heating process object heat content variation and mass change.
Then raw mineral materials is uniformly mixed with fluxing agent with scheduled mass ratio again and is placed on crucible, then be placed in heat point
Be warming up to predetermined temperature in analyzer furnace body, cool to room temperature with the furnace, obtain the heat content of the mixture of raw mineral materials and fluxing agent with
The relation curve of weight percent and temperature.Wherein, raw mineral materials needs to meet actual production granularity requirements, specifically, partial size
Granule content greater than 0.075mm is less than 0.1%.
Subtract each other function using software curve, by the mixture of raw mineral materials and fluxing agent and cosolvent heat content, weight percent
It is poorer than making with temperature curve, obtain the heat content of raw mineral materials, the relation curve of weight percent and temperature.Heat content curve
One chemical reaction of one peak value representative species, such as fusing, phase transformation can read melting sources temperature and weight accordingly
Percentage, at the same observation of steps 5S it is cooling after in crucible sample molten state, if unmelted object is remained, to assess mineral
The fusing complexity of raw material.
The mass ratio of raw mineral materials and fluxing agent has a great impact for the accuracy for assessing raw mineral materials.Ratio mistake
Low, raw mineral materials fusion temperature itself is high, in laboratory conditions, is extremely difficult to very high temperature, and waste of resource；Ratio mistake
Height, raw mineral materials relative usage is just few, influences the confidence level of result.The present inventor passes through test of many times, obtains mineral
The mass ratio of raw material and fluxing agent is 0.5:1~3.5:1, it is further preferred that being 1.5:1~3:1.
Curve, according to the feature and instrument performance of mineral, step 2S and step 5S are analyzed to obtain preferable MI heater
Heating rate be 5-20 DEG C/min, predetermined temperature be 1400-1550 DEG C, it is further preferred that be 1450-1500 DEG C.
The cosolvent used in the present invention is one of boric acid, anhydrous lithium tetraborate, lithium metaborate or a variety of, above-mentionedization
Close object heating process stable reaction, characteristic temperature and the characteristic temperature of institute assaying are without being overlapped.
The raw mineral materials of the invention to be assessed is one of siliceous raw material, aluminum-containing raw material or a variety of.Wherein, siliceous original
Material includes one of sandstone, quartz, clay or a variety of；Aluminum-containing raw material includes one of kaolin, pyrophillite, feldspar or more
Kind.It can be above any one in raw material, be also possible to the mixture of different material.Wherein, pyrophillite includes that low aluminium contains
Measure pyrophillite and high aluminium content pyrophillite.
The relation curve of weight change percentage in the present invention and temperature, mainly to the relationship in conjunction with heat content and temperature
Curve determines the characteristic temperature point of raw material heating process, obtains accurate fusion temperature.
Compared with prior art, the present invention can accurately obtain the fusion temperature of raw mineral materials, raw for silicate industry
The formulation offer of production. art system reasonably instructs foundation, and this method is easily operated, quick and precisely, time saving and energy saving, nontoxic no dirt
Dye.
Detailed description of the invention
It is incorporated into specification and the attached drawing for constituting part of specification shows the embodiment of the present invention, and with
Principle for explaining the present invention together is described, in the drawings, similar appended drawing reference is used to indicate similar element, under
Attached drawing in the description of face is some embodiments of the present invention, rather than whole embodiments, and those of ordinary skill in the art are come
It says, without creative efforts, other drawings may be obtained according to these drawings without any creative labor.
Fig. 1 shows the step of method of assessment raw mineral materials according to the present invention figure；
Fig. 2 is the relation curve of the raw material heating process heat content variation of the embodiment of the present invention 1, weight percent and temperature；
Fig. 3 is the relation curve of the raw material heating process heat content variation of the embodiment of the present invention 2, weight percent and temperature；
Fig. 4 is the relation curve of the raw material heating process heat content variation of the embodiment of the present invention 3, weight percent and temperature；
Fig. 5 is the relation curve of the raw material heating process heat content variation of the embodiment of the present invention 4, weight percent and temperature；
Fig. 6 is the relation curve of the raw material heating process heat content variation of the embodiment of the present invention 5, weight percent and temperature；
Fig. 7 is the relation curve of the raw material heating process heat content variation of the embodiment of the present invention 6, weight percent and temperature.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.It needs
Illustrate, in the absence of conflict, the features in the embodiments and the embodiments of the present application can mutual any combination.
The method of assessment raw mineral materials of the invention, comprising the following steps:
1S: it takes fluxing agent in crucible, is placed in thermal analyzer furnace body；
2S: control thermal analyzer furnace body is warming up to predetermined temperature, then cools to room temperature with the furnace, generates the heat of fluxing agent
The relation curve of enthalpy, weight percent and temperature；
3S: taking raw mineral materials and fluxing agent, is uniformly mixed with scheduled mass ratio, forms the mixed of raw mineral materials and fluxing agent
Close object；
4S: it takes the mixture of step 3S chats raw material and fluxing agent in crucible, is placed in thermal analyzer furnace body；
5S: control thermal analyzer furnace body is warming up to the predetermined temperature, then cools to room temperature with the furnace, generates raw mineral materials
With the relation curve of the heat content of the mixture of fluxing agent, weight percent and temperature；
6S: with the heat content of step 5S and the resulting fluxing agent of step 2S, the relation curve and mine of weight percent and temperature
It is poor that the relation curve of the heat content of the mixture of raw material and fluxing agent, weight percent and temperature is made, to obtain raw mineral materials
Fusion temperature and weight percent.Wherein, the heating rate of step 2S and step 5S are 5-20 DEG C/min, and predetermined temperature is
1400-1550 DEG C, it is further preferred that predetermined temperature is 1450-1500 DEG C.
Wherein, the mass ratio of raw mineral materials and fluxing agent is 0.5:1~3.5:1, it is further preferred that mass ratio is 1.5:
1~3:1.Raw mineral materials is one of siliceous raw material, aluminum-containing raw material or a variety of, and siliceous raw material includes sandstone, quartz, in clay
It is one or more；Aluminum-containing raw material includes one of kaolin, pyrophillite, feldspar or a variety of.Fluxing agent is boric acid, anhydrous four
One of lithium borate, lithium metaborate are a variety of
The specific embodiment of assessment raw mineral materials method is listed below:
Embodiment 1
5-10mg boric acid is put into crucible, crucible is put into thermal analyzer furnace body.Thermal analyzer by room temperature with 5 DEG C/
The heating rate of min rises to 1500 DEG C, then cools to room temperature with the furnace.Obtain boric acid heat content, weight percent and temperature relation
Curve.
By silica flour: boric acid=2:1 mass ratio is uniformly mixed, and 10-15mg sample is taken to be placed in crucible (such as corundum earthenware
Crucible) in, crucible is put into thermal analyzer furnace body.Thermal analyzer rises to 1500 DEG C by room temperature with the heating rate of 5 DEG C/min, with
Furnace is cooled to room temperature.The heat content of silica flour and boric acid, the relation curve of weight percent and temperature are obtained, software curve phase is utilized
Subtract function, it is poor with boric acid heat content, weight percent and temperature curve work, obtain heat content, the weight percent of silica flour
Than the relation curve with temperature, as shown in Fig. 2, one of a peak value representative species of heat content curve chemically reacts, such as fusing,
Phase transformation etc., accordingly, can read melting sources temperature is 1470.8 DEG C.Crucible after cooling is taken out from heat analysis furnace body,
It can obviously find the unfused substance of noresidue in crucible.
Embodiment 2
5-10mg boric acid is put into crucible, crucible is put into thermal analyzer furnace body.Thermal analyzer by room temperature with 10 DEG C/
The heating rate of min rises to 1500 DEG C, then cools to room temperature with the furnace.Obtain boric acid heat content, weight percent and temperature relation
Curve.
By low-aluminum-content pyrophillite: boric acid=2:1 mass ratio is uniformly mixed, and is taken 10-15mg sample to be placed in crucible, is put
Enter in thermal analyzer furnace body.Thermal analyzer is rising to 1500 DEG C by room temperature with the heating rate of 10 DEG C/min, cools to room with the furnace
Temperature.The heat content of low-aluminum-content pyrophillite and boric acid, the relation curve of weight percent and temperature are obtained, is subtracted each other using software curve
Function, it is poor that it is made with boric acid heat content, weight percent and temperature curve, obtains the heat content, again of low-aluminum-content pyrophillite
The relation curve of percentage and temperature is measured, as shown in figure 3, can read melting sources temperature is 1472.8 DEG C.It will be after cooling
Crucible takes out from heat analysis furnace body, can obviously find the unfused substance of noresidue in crucible.
Embodiment 3
5-10mg boric acid is put into crucible, crucible is put into thermal analyzer furnace body.Thermal analyzer by room temperature with 15 DEG C/
The heating rate of min rises to 1500 DEG C, then cools to room temperature with the furnace.Obtain boric acid heat content, weight percent and temperature relation
Curve.
By high aluminium content pyrophillite: boric acid=2:1 mass ratio is uniformly mixed, and 10-15mg sample is taken to be placed in corundum crucible
In, it is put into thermal analyzer furnace body.Thermal analyzer is rising to 1500 DEG C by room temperature with the heating rate of 15 DEG C/min, furnace cooling
To room temperature.The heat content of high aluminium content pyrophillite and boric acid, the relation curve of weight percent and temperature are obtained, software curve is utilized
Subtract each other function, it is poor with boric acid heat content, weight percent and temperature curve work, obtain the heat of high aluminium content pyrophillite
The relation curve of enthalpy, weight percent and temperature, as shown in figure 4, can read melting sources temperature is 1477.5 DEG C.It will cool down
Crucible afterwards takes out from heat analysis furnace body, can obviously find still there is a small amount of unfused substance in crucible.
Embodiment 4
5-10mg boric acid is put into crucible, crucible is put into thermal analyzer furnace body.Thermal analyzer by room temperature with 20 DEG C/
The heating rate of min rises to 1500 DEG C, then cools to room temperature with the furnace.Obtain boric acid heat content, weight percent and temperature relation
Curve.
By kaolin: boric acid=2:1 mass ratio is uniformly mixed, and is taken 10-15mg sample to be placed in corundum crucible, is put into heat
In analyzer furnace body.Thermal analyzer is rising to 1500 DEG C by room temperature with the heating rate of 20 DEG C/min, cools to room temperature with the furnace.?
To the heat content of kaolin and boric acid, the relation curve of weight percent and temperature, subtract each other function using software curve, by itself and boron
It is poor that acid heat enthalpy, weight percent and temperature curve are made, and the relationship for obtaining kaolinic heat content, weight percent and temperature is bent
Line, as shown in figure 5, without fusing characteristic temperature point.Illustrate that kaolin is not easy to melt, by crucible after cooling from heat analysis furnace body
Middle taking-up can obviously find to go back the unfused raw material of residual fraction in crucible.
Embodiment 5
5-10mg boric acid is put into crucible, crucible is put into thermal analyzer furnace body.Thermal analyzer by room temperature with 10 DEG C/
The heating rate of min rises to 1550 DEG C, then cools to room temperature with the furnace.Obtain boric acid heat content, weight percent and temperature relation
Curve.
By kaolin: boric acid=1:1 mass ratio is uniformly mixed, and is taken 10-15mg sample to be placed in corundum crucible, is put into heat
In analyzer furnace body.Thermal analyzer is rising to 1550 DEG C by room temperature with the heating rate of 10 DEG C/min, cools to room temperature with the furnace.?
To the heat content of kaolin and boric acid, the relation curve of weight percent and temperature, subtract each other function using software curve, by itself and boron
It is poor that acid heat enthalpy, weight percent and temperature curve are made, and the relationship for obtaining kaolinic heat content, weight percent and temperature is bent
Line, as shown in fig. 6, can read melting sources temperature is 1460.8 DEG C.Illustrate kaolin in the raw mineral materials fluxing agent quality
It can melt than under.Crucible after cooling is taken out from heat analysis furnace body, can obviously find that noresidue is unfused in crucible
Raw material.
Embodiment 6
The mixture of 5-10mg anhydrous lithium tetraborate and lithium metaborate is put into crucible, crucible is put into thermal analyzer furnace
In body.Thermal analyzer rises to 1500 DEG C by room temperature with the heating rate of 10 DEG C/min, then cools to room temperature with the furnace.It obtains anhydrous
Mixture heat content, weight percent and the temperature curve of lithium tetraborate and lithium metaborate.
By silica flour: mixture=2.5:1 mass ratio of anhydrous lithium tetraborate and lithium metaborate is uniformly mixed, and takes 10-
15mg sample is placed in corundum crucible, is put into thermal analyzer furnace body.Thermal analyzer is fast with the heating of 10 DEG C/min by room temperature
Rate rises to 1500 DEG C, cools to room temperature with the furnace.Obtain heat content, the weight percent of silica flour Yu anhydrous lithium tetraborate and lithium metaborate
Than the relation curve with temperature, subtract each other function using software curve, by it with anhydrous lithium tetraborate and lithium metaborate mixture
It is poor that heat content, weight percent and temperature curve are made, and obtains the heat content of silica flour, the relationship song of weight percent and temperature
Line, as shown in fig. 7, can read melting sources temperature is 1470.2 DEG C.Crucible after cooling is taken out from heat analysis furnace body,
It can obviously find the unfused substance of noresidue in crucible.
In figure 2 above-Fig. 7, X-axis represents temperature, and Y1 axis represents heat content, and Y2 axis represents weight percent；Curve A is heat content
With the relation curve of temperature, curve B is weight percentage the relation curve with temperature.
The method of assessment raw mineral materials of the invention obtains the mass ratio of raw mineral materials and fluxing agent by a large amount of experiment
For 0.5:1~3.5:1, it is further preferred that being 1.5:1~3:1.Different raw mineral materials and cosolvent is given below in difference
Mass ratio under, test the melting sources temperature data situation measured, as shown in Table 1 and Table 2.
Table 1
Table 2
As can be seen from the above table, the mass ratio outside the quality of raw mineral materials of the present invention and cosolvent is than range, in quality
In the case where more too low than ratio or excessively high, no fusing characteristic temperature point cannot accurately read the temperature of raw mineral materials.
To sum up, the method for assessment raw mineral materials fusibility of the invention, the fusing that can accurately evaluate raw mineral materials are difficult
Easy degree also has the advantages such as quick, easy to operate, nontoxic.
Finally, it should be noted that herein, the terms "include", "comprise" or its any other variant are intended to non-
It is exclusive to include, so that the process, method, article or equipment comprising a series of elements not only includes those elements,
It but also including other elements that are not explicitly listed, or further include solid by this process, method, article or equipment
Some elements.In the absence of more restrictions, the element limited by sentence " including one ... ", it is not excluded that including institute
State in the process, method, article or equipment of element that there is also other identical elements.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations.Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (8)
1. a kind of method for assessing raw mineral materials, which comprises the following steps:
1S: it takes fluxing agent in crucible, is placed in thermal analyzer furnace body；
2S: control thermal analyzer furnace body is warming up to predetermined temperature, then cools to room temperature with the furnace, generates the heat content, again of fluxing agent
Measure the relation curve of percentage and temperature；
3S: taking raw mineral materials and fluxing agent, is uniformly mixed with scheduled mass ratio, forms the mixing of raw mineral materials and fluxing agent
Object；
4S: it takes the mixture of step 3S chats raw material and fluxing agent in crucible, is placed in thermal analyzer furnace body；
5S: control thermal analyzer furnace body is warming up to the predetermined temperature, then cools to room temperature with the furnace, generates raw mineral materials and helps
The relation curve of the heat content of the mixture of flux, weight percent and temperature；
6S: former with the heat content of step 5S and the resulting fluxing agent of step 2S, the relation curve of weight percent and temperature and mineral
It is poor to expect to make with the relation curve of the heat content of the mixture of fluxing agent, weight percent and temperature, to obtain the fusing of raw mineral materials
Temperature and weight percent；
Scheduled mass ratio described in the step 3S is 1.5:1~3:1；
The predetermined temperature of the step 2S and step 5S is 1400-1550 DEG C.
2. the method for assessment raw mineral materials as described in claim 1, which is characterized in that the heating of the step 2S and step 5S
Rate is 5-20 DEG C/min.
3. the method for assessment raw mineral materials as claimed in claim 2, which is characterized in that the predetermined temperature is 1450-1500
℃。
4. the method for assessment raw mineral materials as described in claim 1, which is characterized in that the fluxing agent is boric acid, anhydrous four
One of lithium borate, lithium metaborate are a variety of.
5. as described in claim 1 assessment raw mineral materials method, which is characterized in that the raw mineral materials be siliceous raw material,
One of aluminum-containing raw material is a variety of.
6. the method for assessment raw mineral materials as claimed in claim 5, which is characterized in that the siliceous raw material includes sandstone, stone
One of English, clay are a variety of.
7. as claimed in claim 5 assessment raw mineral materials method, which is characterized in that the aluminum-containing raw material include kaolin,
One of pyrophillite, feldspar are a variety of.
8. a kind of if the method for assessment raw mineral materials of any of claims 1-7 is in assessment raw mineral materials high temperature melting
Application in complexity.
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